WorldWideScience

Sample records for bridges synthesis characterization

  1. Conjugated polymers with pyrrole as the conjugated bridge: synthesis, characterization, and two-photon absorption properties.

    Science.gov (United States)

    Li, Qianqian; Zhong, Cheng; Huang, Jing; Huang, Zhenli; Pei, Zhiguo; Liu, Jun; Qin, Jingui; Li, Zhen

    2011-07-14

    The synthesis, one- and two-photon absorption (2PA) and emission properties of two novel pyrrole-based conjugated polymers (P1 and P2) are reported. They emitted strong yellow-green and orange fluorescence with fluorescent quantum yields (Φ) of 46 and 33%, respectively. Their maximal 2PA cross sections (δ) measured by the two-photon-induced fluorescence method using femtosecond laser pulses in THF were 2392 and 1938 GM per repeating unit, respectively, indicating that the 2PA chromophores consisting of the triphenylamine with nonplanar structure as the donor and electron-rich pyrrole as the conjugated bridge could be the effective repeating units to enhance the δ values.

  2. Bimetallic Heteronuclear Complexes Bridged with Ferrichexathiocyanate-Synthesis, Characterization and Antibacterial Properties

    Directory of Open Access Journals (Sweden)

    Mohammad Nasir Uddin

    2014-04-01

    Full Text Available A number of heterobinuclear thiocyanato-bridged complexes of cations, [M(NH2X6]2+ and [M(en3]2+ (where en= Ethylenediamine, X = H, Ph; M= Ni, Cu, Cd, Zn, with ferrichexathiocyanate have been prepared. The complexes have been characterized by FT-IR, 13C NMR and UV-vis spectroscopy, metal analysis, magnetic and conductance studies.  The composition complexes has been proposed on the basis of experimental and literature evidences. The antibacterial activity of the prepared complexes has also been investigated against the gram positive-Bacillus cereus and gram negative- Salmonella typhi and Escherichia coli pathogens.

  3. Synthesis and characterization of cubic mesoporous bridged polysilsesquioxane for removing organic pollutants from water.

    Science.gov (United States)

    Lin, Derong; Zhao, Qing; Hu, Lijiang; Xing, Baoshan

    2014-05-01

    Hexane, octane, phenyl, and biphenyl-bridged bis(triethoxysilyl) precursors were used in synthesizing cubic mesoporous bridged polysilsesquioxane (BPS) copolymers. Structural characterization was carried out by FTIR, small angle XRD, Brunauer-Emmett-Teller-N2 sorption, (1)H NMR, and TEM. We successfully synthesized both "rigid" and "soft" 3D cubic mesoporous BPS with high surface area and pore volume, as attested by the comprehensive characterization data. Adsorption of pyrene, phenanthrene, nitrobenzene, and 2,4-dichlorophenol on BPS was greatly affected by adsorbate properties, i.e., Kow, solvation properties and molecular size. Hydrophobic interaction dominantly controlled organic pollutants' sorption on BPS. Other interactions, e.g., π-π and H-bond interactions, also have effects on sorption as indicated by Kow normalized sorption isotherms. Rigid aromatic BPS (phenyl and biphenyl) showed a higher sorption capacity than soft aliphatic BPS (hexane and octane). A conceptual model was proposed to further explain the phenomena. This study suggests a promising application of cubic mesoporous BPS in wastewater treatment.

  4. Synthesis, characterization and photophysical studies of -triazolomethyl-bridged porphyrin-benzo--pyrone dyads

    Indian Academy of Sciences (India)

    Dileep Kumar Singh; Mahendra Nath

    2016-04-01

    A new series of zinc(II) -triazolomethyl-bridged porphyrin-benzo--pyrone dyads have been synthesized in appreciable yields through a copper(I)-catalyzed “click” reaction of zinc(II) 2-azidomethyl-5,10,15,20-tetraphenylporphyrin with various benzo--pyronoalkynes. These novel zinc(II) porphyrin-benzo--pyrone dyads successfully underwent demetallation in the presence of concentrated hydrochloric acid in chloroform at 25°C to form the corresponding free-base porphyrin analogues in good yields. The newly synthesized products were characterized on the basis of spectral data and evaluated for their electronic absorption and fluorescence properties. Some of these molecules have shown a significant intramolecular energy transfer between the benzo--pyrone and porphyrin subunits.

  5. Synthesis,characterization,structures and magnetic property of chiral oxalate-bridged dicopper(Ⅱ) complexes

    Institute of Scientific and Technical Information of China (English)

    2010-01-01

    The oxalato-bridged dicopper(II) complexes [Cu2(μ-ox)(LRR)2(H2O)2(ClO4)2] (1),[Cu2(μ-ox)(LRR)2(CH3COCH3)2(ClO4)2](1a),[Cu2(μ-ox)(LSS)2(H2O)2(ClO4)2] (2) and [Cu2(μ-ox)(LRR)(LSS)2(CH3COCH3)2(ClO4)2] (3) [LRR = (8R,10R)-(-)-[4,5]-pineno2,2′-bipyridine,LSS = (8S,10S)-(+)-[4,5]-pineno-2,2′-bipyridine;ox2= oxalate] were first prepared.A possible mechanism for the formation of the chial dicopper(II) complexes was proposed.Based on elemental analysis,conductance measurement,UV-Vis spectra,CD spectra and X-ray single-crystal diffraction,the oxalato-bridged structures of 1 and 2 were deduced to adopt two Cu(II) ions and the bridged oxalate lying in the nearly same plane.The crystal structures of 1a and 3 reveal that the coordination geometry around each Cu(II) ion is an elongated and distorted octahedron and two axial solvent molecules and two perchlorate ions are anti to each other respectively in both binuclear molecules.The solution CD spectra of 1 and 2 in the visible d-d range show very weak Cotton effects with peaks at 588 and 779 nm,which are approximately of mirror image,suggesting the optical activities may be derived from the vicinal effects of the chiragenic centers at the pinene group of LRR and LSS,respectively.Complex 1 has been characterized by variable-temperature magnetic susceptibility and the data was least-square fitted to the Blenaey-Bowers equation.The exchange integral J was found to be -338.41(4) cm-1,indicating a strong antiferromagnetic interaction between two copper(II) ions.

  6. Synthesis, structure characterization, and anticancer activity of a novel oxygen-bridged tricyclic Biginelli adduct

    Science.gov (United States)

    Ibrahim, Mohamed M.; El-Sheshtawy, Hamdy S.; El-Kemary, Maged; Al-Juaid, Salih; Youssef, Mohamed; El-Azab, Islam H.

    2017-06-01

    Herein, we report the one-pot cyclization of Biginelli Adduct, ethyl 4-(2-hydroxyphenyl)-6-methyl-2-thioxo-1,2,3,4-tetrahydropyrimidine-5-carboxylate (I) to the oxygen-bridged adduct, ethyl 2-methyl-4-thioxo-3,4,5,6-tetrahydro-2H-2,6-methanobenzo[g] [1,3,5]oxadiazocine-11-carboxylate (II) in a high yield and purity under mild reaction condition using zinc(II) perchlorate hexahydrate as a highly efficient catalyst. The cyclic product (II) was characterized both in the solid state and in solution using FT-IR, 1H NMR, and UV-visible spectroscopy. Theoretical calculations using density functional theory with B3LYP/6-311++G(d,p) level were used to further investigate the structure properties. DFT calculations (gas phase) revealed the stability of cyclic compound II (3.45 kcal/mol) than compound I. In addition, the anticancer activity of II was investigated using MCF-7 human breast cell line. The results revealed a moderate activity with 223.55 μg/ml IC50 value.

  7. Synthesis,Characterization,and Properties of Supported Tungstozincate Bridged by Co(II) Complex Fragment

    Institute of Scientific and Technical Information of China (English)

    LIU Kun; LI Jia; LIU Hong-bo; CHEN Ya-guang

    2008-01-01

    [CoII(phen)3]2[{(ZnW12O40)CoII(phen)2(H2O)}2CoII(trien)2(NaH20)2]·3H2O was synthesized via hydrothermal technique and characterized with elemental analyses,IR spectroscopy,TGA-DTA,and variable temperature magnetic susceptibility.The compound crystallized in the monoclinic system with the space group P21/n,a=1.8210 nm,b=2.3592 nm,c=2.2932 nm,β=110.31°,V=9.239 nm3,Z=2,R1=0.0827.The compound consists of two coordination cations,three lattice water molecules,and a macroanion[{(ZnW12O40)Co(phen)2(H2O)}2Co(C6H18N4)2'(NaH2O)2]4-in which each supported Keggin anion[(ZnW12O40CoII(phen)2(H2O)]4-acts as a ligand to coordinate to central bridging Co2+ ion via a terminal oxygen atom.Hydrogen bonds are responsible for the construction of 3D architecture of the compound.The compound is paramagnetic with a weak antiferromagnetie interaction(θ=-46.796 K).

  8. Synthesis, Characterization and Biological activity of Some Novel Sulphur Bridged Pyrazoles

    Directory of Open Access Journals (Sweden)

    Singaravel Mohan,

    2010-10-01

    Full Text Available Mercaptoheterocyclic compounds on treatment with ethyl bromoacetate in the presence of base afforded thioacetate derivative of mercaptoheterocyclic compounds. These on subsequent treatment with hydrazine hydrate yielded acylated hydrazine derivative of ercaptoheterocyclic compounds. Reaction of these acylated hydrazinederivatives of mercaptoheterocyclic compounds with ketene dithioacetal derivative afforded sulphur bridged pyrazole derivatives.

  9. Bifunctional bridging linker-assisted synthesis and characterization of TiO2/Au nanocomposites

    Science.gov (United States)

    Žunič, Vojka; Kurtjak, Mario; Suvorov, Danilo

    2016-11-01

    Using a simple organic bifunctional bridging linker, titanium dioxide (TiO2) nanoparticles were coupled with the Au nanoparticles to form TiO2/Au nanocomposites with a variety of Au loadings. This organic bifunctional linker, meso-2,3-dimercaptosuccinic acid, contains two types of functional groups: (i) the carboxyl group, which enables binding to the TiO2, and (ii) the thiol group, which enables binding to the Au. In addition, the organic bifunctional linker acts as a stabilizing agent to prevent the agglomeration and growth of the Au particles, resulting in the formation of highly dispersed Au nanoparticles. To form the TiO2/Au nanocomposites in a simple way, we deliberately applied a synthetic method that simultaneously ensures: (i) the capping of the Au nanoparticles and (ii) the binding of different amounts of Au to the TiO2. The TiO2/Au nanocomposites formed with this method show enhanced UV and Vis photocatalytic activities when compared to the pure TiO2 nanopowders.

  10. Tetracarboxylatodirhenium complexes linked by axial cyano bridges to metalpentacarbonyl ligands - synthesis and characterization

    Energy Technology Data Exchange (ETDEWEB)

    Kuehn, F.E.; Wachter, W. [Technische Univ. Muenchen (Germany). Anorganisch-Chemisches Inst.; Goncalves, I.S. [Nova de Lisboa Univ. (Portugal). Inst. de Tecnologia Quimica e Biologica]|[Aveiro Univ. (Portugal). Dept. de Quimica; Lopes, A.D.; Lopes, J.P.; Romao, C.C. [Nova de Lisboa Univ. (Portugal). Inst. de Tecnologia Quimica e Biologica; Mink, J. [Hungarian Academy of Sciences (Hungary). Inst. of Isotope and Surface Chemistry]|[Veszprem Univ. (Hungary). Dept. of Analytical Chemistry; Hajba, L. [Veszprem Univ. (Hungary). Dept. of Analytical Chemistry; Parola, A.J.; Pina, F.; Sotomayor, J. [Nova de Lisboa Univ. (Portugal). Faculdade de Ciencias e Tecnologia

    1999-02-15

    Reaction of Re{sub 2}{l_brace}{mu}-O{sub 2}CC(CH{sub 3}){sub 3}{r_brace}{sub 4}Cl{sub 2} with [(CO){sub 5}M-CN]Na (M=Cr, Mo, W) leads to tetranuclear complexes of formula Re{sub 2}{l_brace}{mu}-O{sub 2}CC(CH{sub 3}){sub 3}{r_brace}{sub 4}[-NC-M(CO){sub 5}]{sub 2} (M=Cr, Mo, W). These complexes were characterized by {sup 1}H-, {sup 13}C-, and {sup 95}Mo-NMR, IR and Raman spectroscopy, elemental analysis and examined by cyclic voltammetry. The applied methods show the donor capabilities of the [(CO){sub 5}M-CN]{sup -} ligands which shift electron density towards the Re centers weakening the Re-Re quadruple bond. The Re-Re bond lengths and the {nu}(Re-Re) force constants are estimated based on the FT-IR and Raman examinations. Photchemical examinations and TG/MS experiments have also been conducted. The latter method shows that the product complexes decompose around 100 C, but first loosing their carbonyl substituents; as do the Cr, Mo, W precursor compounds. The dirhenium tetrapivalate unit decomposes only at higher temperatures in a distinct second step. (orig.)

  11. Synthesis, crystal structure and magnetic characterization of a cyanide-bridged Mo-Ni nanosized molecular wheel

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Daopeng; Zhang, Hongyan; Wang, Ping [Shandong Univ. of Technology, College of Chemical Engineering, Zibo (China); Kong, Lingqian [Liaocheng Univ. (China). Dongchang College

    2015-11-01

    By using K{sub 4}[Mo(CN){sub 8}] and [Ni(L)(H{sub 2}O){sub 2}][ClO{sub 4}]{sub 2} as reagents (L = 2,12-dimethyl-3,7,11,17-tetraazabicyclo [11.3.1]heptadeca-1(17),13,15-triene), a new cyanide-bridged Mo-Ni complex containing the building blocks [Ni(H{sub 2}O)(L)]{sup 2+} and [Ni(L)]{sup 2+} bridged by [Mo(CN){sub 8}]{sup 4-} units has been obtained. The complex with the formula {[Ni(H_2O)(L)][Ni(L)][Mo(CN)_8]}{sub 6} . 36H{sub 2}O . 2CH{sub 3}OH (1) was characterized by elemental analysis, IR spectroscopy and single-crystal X-ray diffraction. The structure determination reveals an octadecanuclear cluster in the form of a 36-membered macrocycle, in which the largest intramolecular W..W and Ni..Ni distances are 16.5 and 14.4 Aa, respectively, indicating that complex 1 is a nanosized molecular wheel. Investigation of its magnetic properties has shown weak antiferromagnetic coupling between the adjacent Ni(II) ions bridged by the diamagnetic [Mo(CN){sub 8}]{sup 4-} ions.

  12. Synthesis, Characterization and Crystal Structure Determination of a Thiocyanato Bridged One-dimensional Polymeric Complex of Cadmium(Ⅱ)

    Institute of Scientific and Technical Information of China (English)

    BAI Yan; PAN Xiao-Jing; DANG Dong-Bin; SHANG Wei-Li; WANG Jing-Ping

    2008-01-01

    A new one-dimensional polymeric complex [Cd(SCN)2(H2O)]L (L = N,N'-bis(furan-2-ylmethylene)hydrazine) has been synthesized and characterized by IR, UV spectra, TG-DTA technique and single-crystal X-ray diffraction analysis. It crystallizes in triclinic, pace group P1 with a = 5.9268(8), b = 10.8678(15), c = 13.3671(19) A, α = 109.295(2), β = 95.092(2), γ =97.8580(10)°, V - 796.70(19) A3, Z = 2, C12H10CdN4O3S2, Mr = 434.76, μ = 1.648 mm-1, Dc = 1.812 g/cm3, F(000) = 428, R = 0.0308 and wR = 0.0769. The crystal structure reveals that the structure of [Cd(SCN)E(H2O)]n features di-μ-1,3-thiocyante bridges and 1D chains. The octahedrally coordinated Cd atom is surrounded by one oxygen atom from water molecule, three S atoms and two N atoms from five di-μ-1,3 thiocyanato bridges. The Cd atoms are connected by two di-μ-1,3 thiocyanato bridges with the Cd(1)…Cd(1A) separation of 4.239(1) (A) and Cd(1)…Cd(1B) of 5.852(1)(A). In addition, the one-dimensional straight chain structure is further connected by multiform intermolicular N-H…O hydrogen bonds and π…π interactions to form a three-dimensional supramolecular structure.

  13. Synthesis and spectral characterization of trinuclear, oxo-centered, carboxylate-bridged, mixed-valence iron complexes with Schiff bases.

    Science.gov (United States)

    Singh, Atresh Kumar; Singh, Alok Kumar

    2012-10-01

    Some novel trinuclear, oxo-centered, carboxylate-bridged, mixed-valence iron complexes of the general formula [Fe(3)O(OOCR)(3)(SB)(3)L(3)] (where R=C(13)H(27), C(15)H(31) or C(17)H(35,) HSB=Schiff bases and L=Ethanol) have been synthesized by the stepwise substitutions of acetate ions from μ(3)-oxo-hexa(acetato)tri(aqua)iron(II)diiron(III), first with straight chain carboxylic acids and then with Schiff bases. The complexes were characterized by elemental analyses, molecular weight determinations and spectral (electronic, infrared, FAB mass, Mössbauer and powder XRD) studies. Molar conductance measurements indicated the complexes to be non-electrolytes in nitrobenzene. Bridging nature of carboxylate and Schiff base anions in the complexes was established by their infrared spectra. Mössbauer spectroscopic studies indicated two quadrupole-split doublets due to Fe(II) and Fe(III) ions at 80, 200 and 295K, confirming the complexes are mixed-valence species. This was also supported by the observed electronic spectra of the complexes. Magnetic susceptibility measurements displayed octahedral geometry around iron in mixed-valence state and a net antiferromagnetic exchange coupling via μ-oxo atom. Trinuclear nature of the complexes was confirmed by their molecular weight determination and FAB mass spectra. A plausible structure for these complexes has been established on the basis of spectral and magnetic moment data.

  14. Synthesis and characterization of oxo-bridged, trinuclear, six-coordinate mixed-carboxylato complexes of chromium (III)

    Science.gov (United States)

    Baranwal, B. P.; Fatma, Talat

    2005-08-01

    Mixed-carboxylato β-diketonato complexes of chromium (III) (R=C13H27, C15H31 or C17H35 and L=CH3OH) [Cr3O(OOCR)3(dike)3L3]+ have been synthesized by enforced substitution reactions of [Cr3O(OOCCH3)7(H2O)] first with straight chain fatty acids (myristic, palmitic or stearic acid) and then with β-diketones (Hβ-dike) like acetylacetone(Hacac) or benzoylacetone(Hbzac) in toluene under reflux. These are new type of oxo-bridged chromium(III) complexes in which one ligand is a fatty acid while the other one is a β-diketone. The complexes were characterized by elemental analyses, spectral (infrared, electronic, FAB mass and powder XRD) studies, molar conductance and magnetic susceptibility measurements. Bridging coordination modes for both carboxylate and β-diketonate anions were indicated by presence of νasym(Cr3O) vibrations in the infrared spectra. Trinuclear nature of the complexes and their structural features have been discussed on the basis of physicochemical studies.

  15. Synthesis and structural characterization of a calcium coordination polymer based on a 3-bridging tetradentate binding mode of glycine

    Indian Academy of Sciences (India)

    Subramanian Natarajan; Bikshandarkoil R Srinivasan; J Kalyana Sundar; K Ravikumar; R V Krishnakumar; J Suresh

    2012-07-01

    A new coordination polymer namely [[Ca6(H-gly)12(H2O)18]Cl12·6H2O] (1) (H-gly = glycine) 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 eight oxygen atoms three of which are from terminal water molecules and five oxygen atoms from four symmetry related zwitterionic glycine ligands. The H-gly ligands exhibit two different binding modes viz. a monodentate carboxylate ligation and a 3-tetradentate bridging carboxylate binding mode, which results in the formation of a one-dimensional coordination polymer. In the infinite chain the Ca(II) atoms are organized in a zigzag fashion. A comparative study reveals a rich and diverse structural chemistry of calcium halide-glycine compounds.

  16. Dinuclear 1,4,7-triazacyclononane (tacn) complexes of cobalt(III) with amido and tacn bridges. Synthesis, characterization and reversible acid-accelerated bridge cleavage

    DEFF Research Database (Denmark)

    Andersen, Peter; Glerup, Jørgen; Gumm, Andreas

    2004-01-01

    Amido-bridged dinuclear cobalt(III) complexes with 1,4,7-triazacyclononane (tacn) were synthesized from [Co(tacn)(O3SCF3)3] by treatment with potassium amide in liquid ammonia at 100 degrees C. Two isomeric triply bridged complexes, [(tacn)Co(mu-NH2)3Co(tacn)]3+ and [(tacn)Co(mu-NH2)2[mu-tacn(-H)......Amido-bridged dinuclear cobalt(III) complexes with 1,4,7-triazacyclononane (tacn) were synthesized from [Co(tacn)(O3SCF3)3] by treatment with potassium amide in liquid ammonia at 100 degrees C. Two isomeric triply bridged complexes, [(tacn)Co(mu-NH2)3Co(tacn)]3+ and [(tacn)Co(mu-NH2)2[mu......)]4+. An isolated perchlorate of this complex appeared to be the salt of the trans-ammineaqua isomer as determined by X-ray diffraction. Equilibration from both sides fits the first-order rate constant dependence k(obs)=6.2(3) x 10(-5)[H+] + 2.1(2) x 10(-5)(s(-1)) at 40 degrees C. Prolonged treatment of the two...

  17. Synthesis of cyano-bridged bimetallic complexes of 5-indenyl ruthenium(II): Characterization and spectroscopic studies

    Indian Academy of Sciences (India)

    K Mohan Rao; E K Rymmai

    2001-02-01

    Reactions of the cyanide complexes of the type [(Ind)Ru(PPh3)2CN] (1), [(Ind)Ru(dppe)CN] (2), [(Cp)Ru(PPh3)2CN] (3), with the corresponding chloro complexes [(Ind)Ru(PPh3)2Cl] (4), [(Ind)Ru(dppe)Cl] (5), [(Cp)Ru(PPh3)2Cl] (6), in the presence of NH4PF6 salt give homometallic cyano-bridged compounds of the type [(Ind)(PPh3)2Ru-CN-Ru(PPh3)2(Cp)]PF6 (7), [(Ind)(PPh3)2Ru-CN-Ru(PPh3)2(Ind)] PF6 where Ind = indenyl, 5-C9H7, (8), [(Cp)(PPh3)2Ru-CN-Ru(dppe)(Ind)]PF6, dppe = (Ph2PCH2CH2PPh2) (9), [(Ind(dppe)Ru-CN-Ru(PPh3)2(Ind)PF6 (10) and [(Ind)(dppe)Ru-CN-Ru(PPh3)2(Cp)]PF6 (11) respectively. Reaction of complex 3 with [(p-cymene)RuCl2]2 dimer gave a mixed dimeric complex [(Cp)Ru(PPh3)2-CN-RuCl2(-cymene)] (12). All these complexes have been characterized by IR, 1H, 13C and 31 P NMR spectroscopy and C, H, N analyses.

  18. Synthesis, Characterization and Application of A Novel Carbon Bridged Half-metallocene Chromium Catalyst for Methyl Methacrylate Polymerization

    Institute of Scientific and Technical Information of China (English)

    CHENG Zhengzai; GONG Kai; WANG Yang; ZHOU Xue; ZHANG Weixing; LI Yin; SUN Junquan; LI Wenbing

    2014-01-01

    A new carbon bridged cyclopentadienyl chromium complex of the type [(C5H4)C(CH3)2 CH2(C5H4N)]CrCl2 was prepared by treatment of CrCl3•(THF)3 in THF solution with the lithium salt of ligand containing cyclopentadienyl and pyridyl groups. The chromium complex was characterized by 1H NMR and elemental analysis(EA), and the crystal structure was determined by X-ray diffraction analysis. Activated by Al(i-Bu)3, the chromium complex displayed a very high activity for methyl methacrylate (MMA) polymerization. After 24 hours,more than 95.5%MMA was converted to polymethyl methacrylate (PMMA) with a viscosity average molecular weight (Wη) of 416000 g•mol-1 at 60℃for MMA/Al(i-Bu)3/chromium catalyst molar ratio of up to 2000:20:1. Effects of temperature, molar ratios of MMA/catalyst and catalyst/cocatalyst on the polymerization have been studied. The high conversion of MMA and high molecular weight of PMMA with narrow molecular weight distribution is caused by the unique stable active site formed by the new chromium complex and aluminum cocatalyst.

  19. Synthesis of arylenealkyne conjugated macrocycles containing a long alkylene bridge

    Institute of Scientific and Technical Information of China (English)

    Xiaohong CHENG; Sigurd HOEGER

    2008-01-01

    The synthesis of the first two arylenealkyne conjugated macrocycles containing a long alkylene bridge via Glaser coupling of template-directed tetra-acetylenes was reported. Tetraacetylene intermediates with complex structures were constructed rapidly via quadruple Hagihara coupling of monoprotected bisace-tylenes to appropriate tetraiodides and subsequent desilylation. The characterization of such compounds was carried out by NMR, GPC and UV-Vis spectra. Unfortunately, the two compounds were not liquid crystals and had no biaxial nematic mesophase character as expected,

  20. Hydrothermal Synthesis, Crystal Structure, and Characterization of a Novel Terbium(Ⅲ) Coordination Polymer Bridged by 5-Sulfoisophthalate Trivalent Anions

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    Hydrothermal reaction of terbium( Ⅲ ) chloride with 5-sulfoisophthalic acid monosodium salt and 1, 10-phenanthroline(phen) at 415 K resulted in the formation of a novel coordination polymer, [Tb(sip) (phen) (H2O)]n( sip = 5-sulfoisophthalate trivalent anion) with a three-dimensional network structure. Each centrosymmetrically related pair of terbium ions are linked by two sip anions, forming a binuclear unit, and each binuclear unit links to four adjacent tetranuclear units, extending a two-dimensional hybrid layer at crystallographic bc plane. On the other hand,every three-terbium ion is connected by three sip anions, generating a trinuclear ring, and the trinuclear ring connects six neighboring trinuclear rings to produce another two-dimensional layer at crystallographic ab plane. Moreover, each sip anion acts as a pentadentate bridge, interconnecting two different types of layers to yield a novel three-dimensional framework.

  1. Synthesis, Characterization, and Photochemical Properties of a New Square Mn(I-Ru(II Complex Using Pyrazine as Bridge Ligand

    Directory of Open Access Journals (Sweden)

    Inara de Aguiar

    2013-01-01

    Full Text Available The photochemical properties of the complexes cis,fac- (I, cis-[Ru(phen2(pz2]2+ (II, and fac-Mn(CO3(pz2Br (III where phen is phenanthroline and pz is pyrazine in acetonitrile solution are reported. The three complexes were characterized using 1H NMR, UV-vis and FTIR spectroscopy and electrochemical (cyclic voltammetry and spectroelectrochemical techniques. The complexes show intense absorption in the visible region assigned to the population of MLCT excited states. The absorption spectrum of I is the sum of the spectra of the mononuclear species II and III, and the two oxidation potentials at +1.10 and +1.56 V versus Ag/AGCl observed in I are ascribed to the different coordination environments of metal centers. The photolysis in the acetonitrile solution resulted in the pz dissociation to give the monoacetonitrile complexes for I, II, and III, respectively.

  2. Synthesis and structural characterization of a novel peroxo bridged dinuclear cobalt(III) complex of succinimide showing three varieties of hydrogen bonding interactions

    Indian Academy of Sciences (India)

    Murat Taş; Orhan Büyükgüngör

    2009-05-01

    The reaction of aqueous cobaltous nitrate hexahydrate with the anion of succinimide (sucH) in the presence of excess ethylenediamine (en) in air results in the formation of a dinuclear complex -peroxo-bis[bis(ethylenediamine)succinimidato-cobalt(III)] dinitrate dihydrate, 1, in good yield. Compound 1 was characterized by elemental analysis, IR, visible spectra and magnetic susceptibility studies. The explosive nature of [Co(en)2(suc)(-O2)Co(en)2(suc)](NO3)2.2H2O, 1, precluded its thermal characterization. Compound 1 crystallises in the monoclinic space group 21/ and a half of the molecule, constitutes its asymmetric unit. In the centrosymmetric dinuclear complex 1, two Co(III) centres are linked by a planar peroxide bridge. Each cobalt atom is surrounded by four nitrogen atoms of ethylenediamine ligands, a nitrogen atom of succinimidato anion and an oxygen atom of peroxo bridge resulting in a slightly distorted {CoN5O} octahedron. Due to steric hindrance between the two Co(III) centres, the peroxide bridge is planar with a Co-O-O-Co torsion angle of 180°. The dinuclear complex cation, the nitrate anion and the lattice water are involved in three varieties of H-bonding interactions namely N-H$\\cdots$O, O-H$\\cdots$O and C-H$\\cdots$O.

  3. Graphene Synthesis and Characterization

    Science.gov (United States)

    2015-04-08

    AFRL-OSR-VA-TR-2015-0086 Graphene Synthesis and Characterization 130060 Andrea Cortes UNIVERSIDAD TECNICA FEDERICO SANTA MARIA Final Report 04/08...AND SUBTITLE Grant: Graphene synthesis and characterizatión 5a. CONTRACT NUMBER 5b. GRANT NUMBER FA9550-13-1-0060 5c. PROGRAM ELEMENT NUMBER 6...13. SUPPLEMENTARY NOTES 14. ABSTRACT Here is reported graphene synthesis by two methods, Chemical Vapor Deposition (CVD) using Acetylene as a

  4. Synthesis, characterization and magnetic property of a succinate bridged 1D coordination polymer of cobalt(II) containing benzidine as end-capping ligand

    Science.gov (United States)

    Roy, Subhasis; Choubey, Somnath; Khan, Sumitava; Bhar, Kishalay; Ribas, Joan; Ghosh, Barindra Kumar

    2014-03-01

    A new bis(monodentate) succinate bridged 1D coordination polymer [Co(bnzd)2(μ-suc)(OH2)2]nṡ(H2O)n (1) (bnzd = benzidine; suc = succinate dianion) has been isolated using a one-pot reaction of the building components, and characterized structurally and magneto-structurally. Single crystal X-ray diffraction measurement reveals that each cobalt(II) center adopts an octahedral geometry with a CoN2O4 chromophore coordinated by two N atoms of two bnzd ligands, two O atoms of two water molecules and two O atoms of two suc units. In crystalline state, individual units of 1 self-assemble through cooperative N-H⋯O, O-H⋯O and C-H⋯O hydrogen bonds and C-H⋯π interactions affording a 3D network structure. Variable-temperature magnetic susceptibility measurement of 1 in the 2-300 K temperature range shows weak antiferromagnetic coupling among the adjacent cobalt(II) centers presumably due to long bridging arm of the dicarboxylate.

  5. Synthesis, characterization, and reactivity studies of a water-soluble bis(alkoxo)(carboxylato)-bridged diMn(III) complex modeling the active site in catalase.

    Science.gov (United States)

    Palopoli, Claudia; Duhayon, Carine; Tuchagues, Jean-Pierre; Signorella, Sandra

    2014-12-07

    A new diMn(III) complex, Na[Mn2(5-SO3-salpentO)(μ-OAc)(μ-OMe)(H2O)]·4H2O, where 5-SO3-salpentOH = 1,5-bis(5-sulphonatosalicylidenamino)pentan-3-ol, has been prepared and characterized. ESI-mass spectrometry, paramagnetic (1)H NMR, EPR and UV-visible spectroscopic studies on freshly prepared solutions of the complex in methanol and 9 : 1 methanol-water mixtures showed that the compound retains the triply bridged bis(μ-alkoxo)(μ-acetato)Mn2(3+) core in solution. In the 9 : 1 methanol-water mixture, slow substitution of acetate by water molecules took place, and after one month, the doubly bridged diMn(III) complex, [Mn2(5-SO3-salpentO)(μ-OMe)(H2O)3]·5H2O, formed and could be characterized by X-ray diffraction analysis. In methanolic or aqueous basic media, acetate shifts from a bridging to a terminal coordination mode, affording the highly stable [Mn2(5-SO3-salpentO)(μ-OMe)(OAc)](-) anion. The efficiency of the complex in disproportionating H2O2 depends on the solvent and correlates with the stability of the complex (towards metal dissociation) in each medium: basic buffer > aqueous base > water. The buffer preserves the integrity of the catalyst and the rate of O2 evolution remains essentially constant after successive additions of excess of H2O2. Turnovers as high as 3000 mol H2O2 per mol of catalyst, without significant decomposition and with an efficiency of k(cat)/K(M) = 1028 M(-1) s(-1), were measured for the complex in aqueous buffers of pH 11. Kinetic and spectroscopic results suggest a catalytic cycle that runs between Mn(III)2 and Mn(IV)2 oxidation states, which is consistent with the low redox potential observed for the Mn(III)2/Mn(III)Mn(IV) couple of the catalyst in basic medium.

  6. Design, synthesis, characterization and study of novel conjugated polymers

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Wu [Iowa State Univ., Ames, IA (United States)

    1997-06-24

    After introducing the subject of conjugated polymers, the thesis has three sections each containing a literature survey, results and discussion, conclusions, and experimental methods on the following: synthesis, characterization of electroluminescent polymers containing conjugated aryl, olefinic, thiophene and acetylenic units and their studies for use in light-emitting diodes; synthesis, characterization and study of conjugated polymers containing silole unit in the main chain; and synthesis, characterization and study of silicon-bridged and butadiene-linked polythiophenes.

  7. Synthesis of bridged diketopiperazines by using the persistent radical effect and a formal synthesis of bicyclomycin.

    Science.gov (United States)

    Amatov, Tynchtyk; Pohl, Radek; Císařová, Ivana; Jahn, Ullrich

    2015-10-01

    A conceptually new and unified approach to diverse bridged diketopiperazines (DKPs) with widely variable ring sizes was developed by taking advantage of the persistent radical effect. This method enables synthesis of the core structures of bridged DKP alkaloids and was applied to a formal synthesis of the antibiotic bicyclomycin.

  8. Copper(II) complex as a precursor for formation of cyano-bridged pentanuclear FeIII-CuII bimetallic assembly: Synthesis, characterization, crystal structure and antibacterial activity

    Indian Academy of Sciences (India)

    SURACHAI KONGCHOO; KITTIPONG CHAINOK; ANOB KANTACHA; SUMPUN WONGNAWA

    2017-04-01

    [CuL(ClO ₄) ₂] (1) (L = 3,10-diisobutyl-1,3,5,8,10,12-hexaazacyclotetradecane) was synthesized by condensation reaction of ethylenediamine, formaldehyde and iso-butylamine in absolute ethanol. Characterization of 1 utilized various spectroscopic techniques, viz. elemental analysis, electrospray ionization-mass spectrometry (ESI-MS), Fourier-transform infrared spectroscopy (FT-IR), ultraviolet-visible spectroscopy (UV-Vis), diffuse reflectance spectroscopy (DRS) and thermogravimetric analysis (TGA). Based on these techniques, the structure of 1 was proposed as Cu(II) ion occupying octahedral geometry with four secondary amine nitrogens of the hexaazamacrocyclic ligand and two perchlorato anions. 1 was used as a precursor in the preparation of cyano-bridged bimetallic compound, [CuL] ₃ [Fe(CN) ₆] ₂•5H ₂O (2), by reaction with K ₃ [Fe(CN) ₆] in aqueous solution. Single-crystal X-ray analysis indicated that 2 crystallized in the monoclinic system with space group P21/n. The structure of 2 consisted of cyano-bridged FeIII-CuII pentanuclear molecules having two [Fe(CN) ₆] ³⁻ anions connected to three cis-[CuL] ²⁺ cations via two cis-cyanide ligands from each ferrate unit. In each of pentanuclear unit, the central [CuL] ²⁺ cation exhibited a distorted octahedral geometry while the other two units exhibited a distorted square pyramidal geometry. The room temperature magnetic moments of both complexes were measured to be 1.92 B.M. for 1 and 5.61 B.M. for 2. The in vitro antibacterial activity of 1 against Staphylococcus aureus ATCC 25923, Escherichia coli ATCC 25922, and Pseudomonas aeruginosa ATCC 27853 strains were studied and compared with standard drugs, which showed moderate antibacterial activity compared with Penicillin and Gentamicin.

  9. Structural characterization of thioether-bridged bacteriocins.

    Science.gov (United States)

    Lohans, Christopher T; Vederas, John C

    2014-01-01

    Bacteriocins are a group of ribosomally synthesized antimicrobial peptides produced by bacteria, some of which are extensively post-translationally modified. Some bacteriocins, namely the lantibiotics and sactibiotics, contain one or more thioether bridges. However, these modifications complicate the structural elucidation of these bacteriocins using conventional techniques. This review will discuss the techniques and strategies that have been applied to determine the primary structures of lantibiotics and sactibiotics. A major challenge is to identify the topology of thioether bridges in these peptides (i.e., which amino-acid residues are involved in which bridges). Edman degradation, NMR spectroscopy and tandem MS have all been commonly applied to characterize these bacteriocins, but can be incompatible with the post-translational modifications present. Chemical modifications to the modified residues, such as desulfurization and reduction, make the treated bacteriocins more compatible to analysis by these standard peptide analytical techniques. Despite their differences in structure, similar strategies have proved useful to study the structures of both lantibiotics and sactibiotics.

  10. Synthesis and spectroscopic characterization of tin(II) and tin(IV) complexes containing 2,3,5,6-tetrakis({alpha}-pyridyl)pyrazine as a bridging ligand

    Energy Technology Data Exchange (ETDEWEB)

    Bitzer, Rodrigo S.; Filgueiras, Carlos A.L. [Universidade Federal, Rio de Janeiro, RJ (Brazil). Inst. de Quimica]. E-mail: calf@iq.ufrj.br; Teles, Wagner M. [Universidade Federal de Juiz de Fora, MG (Brazil). Dept. de Quimica; Abras, Anuar [Universidade Federal de Minas Gerais, Belo Horizonte, MG (Brazil). Dept. de Fisica; Ardisson, Jose Domingos [Centro de Desenvolvimento da Tecnologia Nuclear CDTN/CNEN, Belo Horizonte, MG (Brazil)

    2005-09-15

    In this work we investigated the reactivity of the nitrogen heterocyclic ligand 2,3,5,6-tetrakis({alpha}-pyridyl)pyrazine, TPP, towards six tin-containing reagents, namely SnCl{sub 2}, SnX{sub 4} (X = Cl or Br), SnRCl{sub 3} (R = Ph or Me), and SnPh{sub 2}Cl{sub 2}. The products were characterized by microanalysis (C, H, N, and Sn), IR spectroscopy (4000-200 cm{sup -1}), {sup 1}H, {sup 13}C{l_brace}{sup 1}H{r_brace}, {sup 13}C-CP/MAS, {sup 119}Sn, and {sup 119}Sn-MAS NMR spectroscopy, as well as by {sup 119}Sn Moessbauer spectroscopy. All reactions yielded bimetallic adducts, in which TPP behaved as a bis-bidentate bridging ligand, binding to each metallic center through two pyridine nitrogen atoms. This coordination mode is so far quite rare and, for the first time, is reported for main group metal-TPP complexes. (author)

  11. Synthesis and Structural Characterization of a New Cadmium(Ⅱ) Complex Bridged by Endo-norbornene-cis-5,6-dicarboxylic Acid

    Institute of Scientific and Technical Information of China (English)

    CAI Xiao-Qing; HU Mao-Lin; CHEN Fan

    2007-01-01

    A polynuclear complex [Cd(endc)(H2O)]n·nH2O (endc = endo-norbomene-cis5,6-dicarboxylate anion) has been synthesized by the hydrothermal reaction of cadmium nitrate tetrahydrate with endo-norbomene-cis-5,6-dicarboxylic acid in 1:1 molar ratio,and structurally characterized by single-crystal X-ray diffraction.It crystallizes in monoclinic,space group P21/c with a = 1.16471(7),b = 0.95334(7),c = 0.91109(9) nm,Z = 4,V= 1.01035(14)nm3,Dc.= 2.160 g/cm3,μ= 2.172 mm-1,F(000) = 648,R =0.0302 and wR = 0.0752.According to structural analysis,each Cd(Ⅱ) ion is coordinated to six O atoms from three endc anions and one water molecule,giving a distorted octahedral geometry.Two- dimensional layer arrangement of the title complex is constructed from the bridging nature of endc.It is worth notice that adjacent two-dimensional layers are joined together to form a three-dimensional supramolecular framework via intermolecular hydrogen bonding interactions.

  12. Concise synthesis of new bridged-nicotine analogues

    DEFF Research Database (Denmark)

    Crestey, François; Hooyberghs, Geert; Kristensen, Jesper Langgaard

    2012-01-01

    This study describes a very efficient strategy for the synthesis of two new bridged-nicotine analogues. Starting from either 4- or 3-chloropyridine the desired tricyclic ring systems are accessed in just three steps in 23% and 40% overall yield, respectively....

  13. Synthesis, structural characterization and antimicrobial activities of diorganotin(IV) complexes with azo-imino carboxylic acid ligand: Crystal structure and topological study of a doubly phenoxide-bridged dimeric dimethyltin(IV) complex appended with free carboxylic acid groups

    Science.gov (United States)

    Roy, Manojit; Roy, Subhadip; Devi, N. Manglembi; Singh, Ch. Brajakishor; Singh, Keisham Surjit

    2016-09-01

    Diorganotin(IV) complexes appended with free carboxylic acids were synthesized by reacting diorganotin(IV) dichlorides [R2SnCl2; R = Me (1), Bu (2) and Ph (3)] with an azo-imino carboxylic acid ligand i.e. 2-{4-hydroxy-3-[(2-hydroxyphenylimino)methyl]phenylazo}benzoic acid in presence of triethylamine. The complexes were characterized by elemental analysis, IR and multinuclear NMR (1H, 13C and 119Sn) spectroscopy. The structure of 1 in solid state has been determined by X-ray crystallography. Crystal structure of 1 reveals that the compound crystallizes in monoclinic space group P21/c and is a dimeric dimethyltin(IV) complex appended with free carboxylic acid groups. In the structure of 1, the Sn(IV) atoms are hexacoordinated and have a distorted octahedral coordination geometry in which two phenoxy oxygen atoms and the azomethine nitrogen atom of the ligand coordinate to each tin atom. One of the phenoxy oxygen atom bridges the two tin centers resulting in a planar Sn2O2 core. Topological analysis is used for the description of molecular packing in 1. Tin NMR spectroscopy study indicates that the complexes have five coordinate geometry around tin atom in solution state. Since the complexes have free carboxylic acids, these compounds could be further used as potential metallo-ligands for the synthesis of other complexes. The synthesized diorganotin(IV) complexes were also screened for their antimicrobial activities and compound 2 showed effective antimicrobial activities.

  14. Synthesis and Nonlinear Optical Property of a Series of New Chromophores Containing Furan Ring as the Only Conjugation Bridge

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    This paper reports the synthesis and the nonlinear optical property of a series of new chromophores which contain furan ring as the only conjugation bridge for the first time. They are characterized by UV-VIS, FT-IR, 1H NMR, MS and elemental analysis. Their dipole moment and the first-order molecular hyperpolarizability (β) are calculated and compared with those of the analogues containing either benzene or thiophene as the conjugation bridge.

  15. Bridging complexes of rare earth and cobalt cluster as catalyst precursors for Fischer-Tropsch synthesis

    Institute of Scientific and Technical Information of China (English)

    ZENG Shanghong; DU Dongping; BAI Fenghua; SU Haiquan

    2011-01-01

    Three new bridging complexes of rare earth and cobalt cluster were synthesized and characterized via ICP, IR and TG techniques.The structure of the complexes was speculated as: two rare earth atoms were bridged with four CF3COO-, and rare earth atoms were coordinated with cobalt carbonyl clusters to form a steady structure. Application of the complexes as the catalyst precursors was explored for Fischer-Tropsch synthesis. The study showed that the bridging complexes of rare earth and cobalt cluster had large molecular size and were difficult to enter pore path of γ-Al2O3, so they were dispersed on the surface of γ-A12O3 support. In addition, the performance of Co(Ce)/γ-Al2O3 was the best among the catalysts with complex as precursor and maintained 77.7% CO conversion at 220 ℃ for 80 operation hours.

  16. Dynamic Characterization of an All-FRP Bridge

    Science.gov (United States)

    Casalegno, C.; Russo, S.

    2017-03-01

    The light weight and high deformability of bridges made with pultruded FRP (fiber-reinforced polymer) materials make them very promising, but, at the same time, vulnerable to dynamic loadings. As a consequence, the vibration serviceability limit state can govern their design. There is currently a lack of data about the dynamic characteristics of FRP bridges and of design guidelines for securing their vibration serviceability. The paper presents the results of dynamic testing and characterization of an all-FRP spatial footbridge. The main modal parameters of the bridge are evaluated by an experimental modal analysis and by comparison of experimental data with FE analysis results. The identified flexural and torsional modes of the bridge are characterized by relatively high values of frequencies and damping. Results of the dynamic characterization give useful information about the dynamic characteristics of this kind of structures and can contribute to the elaboration of future guidelines for providing them with the vibration serviceability.

  17. Synthesis and Characterization of a Ditriflate-Bridged, Diiron(II) Complex with Syn-N-Donor Ligands: [Fe(2)(μ-OTf)(2)(PIC(2)DET)(2)](BARF)(2).

    Science.gov (United States)

    Kodanko, Jeremy J; Lippard, Stephen J

    2008-03-03

    The synthesis and characterization of the diiron(II) complex [Fe(2)(μ-OTf)(2)-(PIC(2)DET)(2)](BARF)(2) (2), where PIC(2)DET is a 2,3-diethynyltriptycene-linked dipicolinic methyl ester ligand, are described. The dication in 2, contains, [Fe(2)(μ-OTf)(2)(PIC(2)DET)(2)](2+) two symmetry-equivalent iron atoms with octahedral coordination geometries. Each metal ion has a N(2)O(4) atom donor set that includes four atoms from two picolinic ester N,O chelate rings, as well as two oxygen atoms from the bridging trifluoromethanesulfonate groups. The Fe(2)(μ-OTf)(2) core of 2 is stabilized by two PIC(2)DET ligands that bind the two metal ions in a head-to-head fashion, leading to an Fe···Fe distance of 5.173(1)Å. Molar conductivity data for 2 are consistent with Fe(2)(μ-OTf)(2)(PIC(2)DET)(2)](2+) retaining its identity in acetone solutions, where it behaves as a 2:1 electrolyte. (1)H NMR spectroscopic, solution (d(6)-acetone) and solid-state magnetic susceptibility data all indicate that the iron atoms of 2 are high-spin (S = 2). A fit of the magnetic data (2 - 300K) to a spin-only isotropic exchange Hamiltonian H = -2JS(1)·S(2) are consistent with weak antiferromagnetic coupling between the two iron atoms with J ~ -0.99(2) cm(-1) and g = 2.10(1).

  18. Synthesis, Characterization and DFT-Based Investigation of a Novel Trinuclear Singly-Chloro-Bridged Copper(II)-1-Vinylimidazole Complex.

    Science.gov (United States)

    Yolcu, Zuhal; Demir, Serkan; Andaç, Ömer; Büyükgüngör, Orhan

    2016-01-01

    A novel trinuclear copper(II) complex [Cu3(μ-Cl)2Cl4(1-Vim)6] with monodentate 1-vinylimidazole (1-Vim) and chloro ligands has been prepared and experimentally characterized by elemental analysis, thermogravimetry (TGA, DTG, DTA), X-ray single crystal diffractometry, TOF-MS and FT-IR spectroscopies. The electronic and structural properties of the complex were further investigated by DFT/TD-DFT methods. Density functional hybrid method (B3LYP) was applied throughout the calculations. The calculated UV-Vis results based on TD-DFT approach were simulated and compared with experimental spectrum. Based on the data obtained, DFT calculations have been found in reasonable accordance with experimental data.

  19. Synthesis, spectral characterization, DNA binding ability and antibacterial screening of copper(II) complexes of symmetrical NOON tetradentate Schiff bases bearing different bridges

    Science.gov (United States)

    Bahaffi, Saleh O.; Abdel Aziz, Ayman A.; El-Naggar, Maher M.

    2012-08-01

    A novel series of four copper(II) complexes were synthesized by thermal reaction of copper acetate salt with symmetrical tetradentate Schiff bases, N,N'bis(o-vanillin)4,5-dimethyl-l,2-phenylenediamine (H2L1), N,N'bis(salicylaldehyde)4,5-dimethyl-1,2-phenylenediamine (H2L2), N,N'bis(o-vanillin)4,5-dichloro-1,2-phenylenediamine (H2L3) and N,N'bis(salicylaldehyde)4,5-dichloro-1,2-phenylenediamine (H2L4), respectively. All the new synthesized complexes were characterized by using of microanalysis, FT-IR, UV-Vis, magnetic measurements, ESR, and conductance measurements, respectively. The data revealed that all the Schiff bases (H2L1-4) coordinate in their deprotonated forms and behave as tetradentate NOON coordinated ligands. Moreover, their copper(II) complexes have square planar geometry with general formula [CuL1-4]. The binding of the complexes with calf thymus DNA (CT-DNA) was investigated by UV-Vis spectrophotometry, fluorescence quenching and viscosity measurements. The results indicated that the complexes bind to CT-DNA through an intercalative mode. From the biological activity view, the copper(II) complexes and their parent ligands were screened for their in vitro antibacterial activity against the bacterial species Staphylococcus aureus, Staphylococcus epidermidis, Escherichia coli and Pseudomonas aeruginosai by well diffusion method. The complexes showed an increased activity in comparison to some standard drugs.

  20. Synthesis, characterization, thermal behavior, and DNA-cleaving studies of cyano-bridged nickel(II)-copper(II) complexes of 4-(pyridin-2-ylazenyl)resorcinol.

    Science.gov (United States)

    Karipcin, Fatma; Ozmen, Ismail; Cülü, Burcin; Celikoğlu, Umut

    2011-10-01

    We present here the syntheses of a mononuclear Cu(II) complex and two polynuclear Cu(II)-Ni(II) complexes of the azenyl ligand, 4-(pyridin-2-ylazenyl)resorcinol (HL; 1). The reaction of HL (1) and copper(II) perchlorate with KCN gave a mononuclear complex [CuL(CN)] (4). Using 4, one pentanuclear complex, [{CuL(NC)}(4) Ni](ClO(4))(2) (5) and one trinuclear complex, [{CuL(CN)}(2) NiL]ClO(4) (6), were prepared and characterized by elemental analyses, magnetic susceptibility, molar conductance, IR, and thermal analysis. Stoichiometric and spectral results of the mononuclear Cu(II) complex indicated that the metal/ligand/CN ratio was 1 : 1 : 1, and the ligand behaved as a tridentate ligand forming neutral metal chelates through the pyridinyl and azenyl N-, and resorcinol O-atom. The interaction between the compounds (the ligand 1, its Ni(II) and Cu(II) complexes without CN, i.e., 2 and 3, and its complexes with CN, 4-6) and DNA has also been investigated by agarose gel electrophoresis. The pentanuclear Cu(4) Ni complex (5) with H(2) O(2) as a co-oxidant exhibited the strongest DNA-cleaving activity.

  1. Carbonyl-bridged energetic materials: biomimetic synthesis, organic catalytic synthesis, and energetic performances.

    Science.gov (United States)

    Feng, Yong-An; Qiu, Hao; Yang, Sa-Sha; Du, Jiang; Zhang, Tong-Lai

    2016-11-01

    In order to obtain high-performance energetic materials, in this work, carbonyl groups (C[double bond, length as m-dash]O) have been newly introduced as sole bridging groups in the field of energetic materials. To this end, two tailored green methods for the synthesis of carbonyl-bridged energetic compounds have been developed for the first time. One is a biomimetic synthesis, in which the conversion route of heme to biliverdin has been used to obtain metal-containing energetic compounds. The other one is an organocatalysis, in which guanidinium serves as an energetic catalyst to afford other energetic compounds. Experimental studies and theoretical calculations have shown that carbonyl-bridged energetic compounds exhibit excellent energetic properties, which is promising for the carbonyl group as a new important and effective linker in energetic materials.

  2. [1.1]Ferrocenophanes and bis(ferrocenyl) species with aluminum and gallium as bridging elements: synthesis, characterization, and electrochemical studies.

    Science.gov (United States)

    Bagh, Bidraha; Breit, Nora C; Harms, Klaus; Schatte, Gabriele; Burgess, Ian J; Braunschweig, Holger; Müller, Jens

    2012-10-15

    Salt-metathesis reactions between dilithioferrocene (Li(2)fc·2/3tmeda) and intramolecularly coordinated aluminum and gallium species RECl(2) [R = 5-Me(3)Si-2-(Me(2)NCH(2))C(6)H(3); E = Al (2a), Ga (2b); and R = (2-C(5)H(4)N)Me(2)SiCH(2); E = Al (3a), Ga (3b)] gave respective [1.1]ferrocenophanes ([1.1]FCPs). Those obtained from 2a and 2b, respectively, were isolated as analytically pure compounds and fully characterized including single-crystal X-ray structure determinations [4a (Al): 43%; 4b (Ga): 47%]. Bis(ferrocenyl) compounds of the type REFc(2) [R = 5-Me(3)Si-2-(Me(2)NCH(2))C(6)H(3); E = Al (5a), Ga (5b); and R = (2-C(5)H(4)N)Me(2)SiCH(2); E = Al (6a), Ga (6b)] and R(2)SiFc(2) [R = Me (7(Me)); Et (7(Et))] were prepared, starting from respective element dichlorides and lithioferrocene (LiFc). Molecular structures of 6a, 7(Me), and 7(Et) were solved by single-crystal X-ray analyses. One of the two Fc moieties of 6a was bent toward the open coordination site of the aluminum atom. The measured dip angles α* of the two independent molecules in the asymmetric unit were 11.9(5) and 13.3(5)°, respectively. The redox behavior of [1.1]FCPs 4 and bis(ferrocenyl) species 5, 6, 7, and (Mamx)EFc(2) [Mamx = 2,4-tBu(2)-6-(Me(2)NCH(2))C(6)H(2); E = Al (8a), Ga (8b)] were investigated with cyclic voltammetry. While all gallium and silicon compounds gave meaningful and interpretable data, all aluminum compounds were problematic with the exception of 8a. Aluminum species, compared to respective gallium species, are more sensitive and, presumably, fluoride ions or residual water from the electrolyte and solvent are causing degradation. The splitting between the formal potentials for bis(ferrocenyl) species was significantly smaller (5b, 6b, and 8b: ΔE°' = 0.138-0.159 V) than that of the [1.1]FCP 4b (ΔE°' = 0.309 V). These results were explained by assuming an electrostatic interaction between the two iron centers; differences between bis(ferrocenyl) species and [1.1]FCPs

  3. A dinuclear end-on azide-bridged copper(II) compound with weak antiferromagnetic interaction - Synthesis, characterization, magnetism and X-ray structure of bis[(μ-azido-κN1)-(azido-κN1)(1,3-bis(benzimidazol-2-yl)-2-methylpropane)copper(II)

    Science.gov (United States)

    van Albada, Gerard A.; Mutikainen, Ilpo; Roubeau, Olivier; Reedijk, Jan

    2013-03-01

    The centrosymmetric dinuclear compound of formula [Cu(μ-N3-κN1)(N3-κN1)(bbmp)]2 is reported. Synthesis, characterization, physical properties are determined in detail, together with its 3D structure. The dinuclear end-on azide-bridged copper(II) compound displays a weak antiferromagnetic interaction, despite the fact that the magnetic orbitals overlap. The Cu-Cu contact distance is 3.1867(8) Å, while the Cu-Nazide-Cu angle is 103.41(14)°. The IR spectra of the azido ligands are as expected for such coordinated azides.

  4. SYNTHESIS, CHARACTERIZATION AND ANTIBACTERIAL ...

    African Journals Online (AJOL)

    B. S. Chandravanshi

    conductance measurements, elemental analysis, infrared, UV/Vis, nuclear ... antipyretic properties [1, 2] and also used in the design and development of ... All chemicals used for the preparation of the complexes were of analytical ...... complexes also disturb the respiration process of the cell and thus block the synthesis of.

  5. SYNTHESIS, CHARACTERIZATION AND ANTIMICROBIAL ...

    African Journals Online (AJOL)

    Preferred Customer

    Institute of Chemical Sciences, University of Peshawar, N.W.F.P., Pakistan ... The inverse process, i.e. coordinating a metal ion from an important biomolecule for instance, a zinc finger protein has been used to design novel .... earlier [34], whereas, the complexes were characterized on the basis of elemental analysis,.

  6. Synthesis and Characterization of Multithiouracils

    Institute of Scientific and Technical Information of China (English)

    WANG Wei; LIU Hui-Min; ZHANG Wei; ZHANG Wen-Qin

    2003-01-01

    @@ Alkylation of bases group of nucleic acid, thymine and uracil, has attracted great attention. In order to investigate the intermolecular interactions, [1,2] and the photoreactions[3,4] between bases group of nucleic acid, many studies were focused on the synthesis of bisbases in the formation of B-(CH2)n-B (B′) in which trimethylene was commonly used as linker. Thiouracil is an important derivative of nucleic acid bases, and it can interfere with the synthesis of thyroxine, especially in the treatment of hyperthyroidism and angina. However, to our knowledge, the synthesis of bisthiouracils, even trithiouracils, using flexible or rigid linkers has not been reported. Herein, we have synthesized eight thiouracil derivatives by nucleophilic reaction between thiouracil and varied bromides. All the compounds have been characterized by IR, 1H NMR and element analysis.

  7. Imidazolidine ring as a reduced heterocyclic spacer in a new all-N-donor -bis(bidentate) Schiff base ligand: Synthesis, characterization and electron transfer properties of imidazolidine-bridged dicopper complexes

    Indian Academy of Sciences (India)

    Manindranath Bera; Prasant Kumar Nanda; Uday Mukhopadhyay; Debashis Ray

    2004-03-01

    Low-temperature stoichiometric Schiff base reaction in air in 3 : 1 mole ratio between benzaldehyde and triethylenetetramine (trien) in methanol yields a novel tetraaza m-bis(bidentate) acyclic ligand L. It was characterized by elemental analysis, IR, EI mass and NMR (1H and 13C) spectra. The formation of a five-membered imidazolidine ring from the ethylenediamine backbone as a spacer-cumbridging unit gives rise to a new type of imidazolidine-bridged ligand. A geometric optimisation was made of the synthesized ligand and its complexes by the method of molecular mechanics (MM2) method in order to establish the stable conformations. This hitherto unknown tetraaza acyclic ligand affords new cationic dicopper(I/I) and dicopper(II/II) complexes in good yield. Dicopper(II/II) complex displays weak - transition bands in the visible region, while dicopper(I/I) complex displays strong MLCT band in the same region. Both the dinuclear complexes are of non-intimate nature and show interesting solution electrochemical behaviour. EPR spectral study of -bis(imidazolidino) bridged dicopper(II/II) complex also supports the non-communicative nature of the two copper centres within the same molecule.

  8. HYDROTHERMAL SYNTHESIS AND CHARACTERIZATION OF A ...

    African Journals Online (AJOL)

    Preferred Customer

    tool for the construction of materials containing unique structures and special ... Recently, we reported hydrothermal synthesis of binuclear Co(II) complex [19] and a new .... to two neighboring ones, through four µ2-oxo bridges, to form infinite ...

  9. Synthesis, characterization, and reactivity of pentamethylcyclopentadienyl complexes of divalent cobalt and nickel

    Energy Technology Data Exchange (ETDEWEB)

    Smith, Michael Edward [Univ. of California, Berkeley, CA (United States)

    1993-10-01

    The thesis is divided into the following 4 chapters: synthesis, characterization, and reactivity of trinuclear pentamethylcyclopentadienyl cobalt and nickel clusters with triply-bridging methylidyne groups; chemical and physical properties of pentamethylcyclopentadienyl acetylacetonate complexes of Co(II) and Ni(II); synthesis, characterization, and reactivity of pentamethylcyclopentadienyl halide complexes of Co and Ni; and crystallographic studies of distortions in metallocenes with C5-symmetrical cyclopentadienyl rings.

  10. Synthesis, characterization, and reactivity of pentamethylcyclopentadienyl complexes of divalent cobalt and nickel

    Energy Technology Data Exchange (ETDEWEB)

    Smith, M.E.

    1993-10-01

    The thesis is divided into the following 4 chapters: synthesis, characterization, and reactivity of trinuclear pentamethylcyclopentadienyl cobalt and nickel clusters with triply-bridging methylidyne groups; chemical and physical properties of pentamethylcyclopentadienyl acetylacetonate complexes of Co(II) and Ni(II); synthesis, characterization, and reactivity of pentamethylcyclopentadienyl halide complexes of Co and Ni; and crystallographic studies of distortions in metallocenes with C{sub 5}-symmetrical cyclopentadienyl rings.

  11. Synthesis and characterization of Taurine

    Directory of Open Access Journals (Sweden)

    B Bayarmaa

    2014-10-01

    Full Text Available Have been obtained 2-aminoethanesulfonic acid (taurine from ethanolamine, sulfuric acid and sodium sulfite during the synthesis in laboratory condition. The process involves two steps of reactions, the first was esterification of ethanolamine with sulfuric acid to produce the intermediate product of 2-aminoethyl ester which than was extended to the second step by sulfonation with sodium sulfite to produce 2-aminoethanesulfonic acid. Resulting product was analyzed using 1H-NMR, IR, FAB-MS analysis and examined purity characterizations of the synthesized products. DOI: http://dx.doi.org/10.5564/mjc.v14i0.200 Mongolian Journal of Chemistry 14 (40, 2013, p57-60

  12. Site Characterization during Bridge Foundation Construction Using Electrical Resistivity Tomography

    Directory of Open Access Journals (Sweden)

    Aleksandra V. Varnavina

    2016-07-01

    Full Text Available A shallow underground water-filled cavity was encountered in limestone bedrock during the construction of a new column footing for the Gasconade River Bridge over Interstate 44. Five electrical resistivity tomography (ERT profiles and borehole control were acquired in immediate proximity to the existing and the new column footings in order to assess the integrity of the rock beneath the foundation columns and characterize the encountered cavity. Two parallel southwest- northeast trending fracture zones were identified on the acquired ERT profiles and competent rock was differentiated from more extensively fractured rock. The volumetric extent of the void was mapped based on the interpretation of the ERT, borehole and injected grout data. A conceptual model for the development of the water-filled cavity was proposed.

  13. Fabrication and Characterization of MWCNT-Based Bridge Devices

    KAUST Repository

    Chappanda, Karumbaiah N.

    2017-08-21

    Carbon nanotubes (CNTs) are one of the most actively researched structural materials due to their interesting electrical, mechanical, and chemical properties. Unlike single walled carbon nanotubes (SWCNTs), little work has been focused on multi-walled carbon nanotubes (MWCNTs) and their potential for practical devices. Here, we have fabricated bridge-shape devices integrating MWCNTs (> 50 nm in outer diameter) using three processes: optical lithography, electron beam-induced platinum deposition, and surface micromachining. Each device consists of a doubly-clamped nanotube suspended over gold electrodes on a highly conductive Si substrate. The suspended nanotubes are characterized individually using Raman spectroscopy and semiconductor parameters analysis and, overall, show, high crystallinity and low electrical resistance. The spring constants of doubly-clamped nanotubes were characterized using atomic force microscopy force-displacement measurements, with values as high as 70 N/m observed. Highly stiff MWCNTs are promising for a variety of applications, such as resonators and electrical interconnects. Through simulations, we estimate the resonance frequencies and pull-in voltages of these suspended nano-structures. The dependence of key parameters, such as the nanotube\\'s length, Young\\'s modulus, axial stress, and wall thickness is also discussed.

  14. Study on complexity of Sutong Bridge's objectives system and its meta-synthesis management

    Institute of Scientific and Technical Information of China (English)

    Fa Yueping; Li Zhen

    2009-01-01

    Objectives define the boundaries of complex engineering system. It is a hard work to identify the specific objectives of a complex engineering system. The objectives system development needs a complicated process, from nix to prototype, and to final definition. The total process will cover the following course: from chaos to well-ordered; from qualitativeness to combination of quantitativeness and qualitativenss, then from qualitativeness to quantitativeness (a recurrent process), expert experience and theoretical science, rationality and sensibility, synthesis analysis and meta-synthesis, routinization and non-routinization. Such process is explicit in phase development yet overlapped; mutually confined yet mutuaLly independent; permeated conflicts yet pregnant in harmony. This article explores the complexity of Sutong Bridge's objectives development and the process of meta-synthesis in the Sutong Bridge engineering.

  15. Synthesis, characterization, antimicrobial activity and molecular ...

    African Journals Online (AJOL)

    Synthesis, characterization, antimicrobial activity and molecular .... The solid product was filtered, washed with ether (3 × 20 ... dimethyl sulfoxide (DMSO) to obtain 5120 mg/mL ...... catalysts for direct diastereo-and regioselective Mannich.

  16. Synthesis and characterization of mibolerone

    Institute of Scientific and Technical Information of China (English)

    YANG Qing; FAN Bo-lin; TANG Rui-ren

    2007-01-01

    A simple and effective route for the synthesis of mibolerone was described starting from the estr-5(10)-en-3,17-dione in four steps with the overall yield of 47.0%. Thus, two methods for key intermediate methylnorandrost were investigated: one(method A) starting from estr-4-en-3,17-dione underwent 3-keto group protected with ethyl orthoformate to give 3-ethoxy-3,5-dien-estr-17-one, the other(method B) from estr-5(10)-en-3,17-dione and protected 3-keto group to give 3,3-dimethoxy-estr-5(10)-7-one in a mild acidic condition. Then, two intermediates were subsequently reacted with methyllithium followed by a mild hydrolytic procedure and gave methylnorandrost with total yield 25.0% and 86.0%, respectively. In the preparation of 6-dehydrogenation product of methylnorandrost, two procedures(method C and method D) were investigated: one was the protected 17α-methyl-17β-hydroxy △3,-5-enol ethers estrendiene brominated and the resulting 6-bromo-19-methylnortestosterone was then immediately dehydrohaloenated to give 6-dehydro-19-methylnortestosterone, the total yield only reaches 36.0%; the other was directly dehydrogenated with chloranil and the yield reaches 75.6% under the optimum conditions: in refluxing tetrahydrofuran,the molar ratio of methylnorandrost to chloranil is 0.66 and reaction time of 5 h. The titled compound and intermediates were characterized by 1H and 13C NMR, IRMS and elemental analysis.

  17. The synthesis of functionalized bridged polycycles via C–H bond insertion

    Science.gov (United States)

    Shih, Jiun-Le; Chen, Po-An

    2016-01-01

    Summary This review presents examples from the chemical literature of syntheses of bridged-polycyclic products via C–H bond insertion by carbenes and nitrenes. Applications to natural product synthesis, a description of the essential elements in substrate-controlled reactions, and mechanistic details of transformations are presented. Overall, these transformations allow the construction of important ring systems rapidly and efficiently, though additional catalyst development is needed. PMID:27340489

  18. The synthesis of functionalized bridged polycycles via C-H bond insertion.

    Science.gov (United States)

    Shih, Jiun-Le; Chen, Po-An; May, Jeremy A

    2016-01-01

    This review presents examples from the chemical literature of syntheses of bridged-polycyclic products via C-H bond insertion by carbenes and nitrenes. Applications to natural product synthesis, a description of the essential elements in substrate-controlled reactions, and mechanistic details of transformations are presented. Overall, these transformations allow the construction of important ring systems rapidly and efficiently, though additional catalyst development is needed.

  19. The synthesis of functionalized bridged polycycles via C–H bond insertion

    Directory of Open Access Journals (Sweden)

    Jiun-Le Shih

    2016-05-01

    Full Text Available This review presents examples from the chemical literature of syntheses of bridged-polycyclic products via C–H bond insertion by carbenes and nitrenes. Applications to natural product synthesis, a description of the essential elements in substrate-controlled reactions, and mechanistic details of transformations are presented. Overall, these transformations allow the construction of important ring systems rapidly and efficiently, though additional catalyst development is needed.

  20. Coinage Metal Hydrides: Synthesis, Characterization, and Reactivity.

    Science.gov (United States)

    Jordan, Abraham J; Lalic, Gojko; Sadighi, Joseph P

    2016-08-10

    Hydride complexes of copper, silver, and gold encompass a broad array of structures, and their distinctive reactivity has enabled dramatic recent advances in synthesis and catalysis. This Review summarizes the synthesis, characterization, and key stoichiometric reactions of isolable or observable coinage metal hydrides. It discusses catalytic processes in which coinage metal hydrides are known or probable intermediates, and presents mechanistic studies of selected catalytic reactions. The purpose of this Review is to convey how developments in coinage metal hydride chemistry have led to new organic transformations, and how developments in catalysis have in turn inspired the synthesis of reactive new complexes.

  1. An Efficient Synthesis of Cyclopeptides Bridged with Aliphafic-aryl Ether Bond

    Institute of Scientific and Technical Information of China (English)

    Zhe LIU; Gui Jei TIAN; De Xin WANG

    2005-01-01

    Based on the pseudo-dilution effect (PDE) on solid support, three cyclopeptides with an aliphatic-aryl ether bond as the bridge were synthesized via SN2 reaction between bromoacetylated at N-terminal and the phenol -OH group in C-terminal Tyr residue. All the products were obtained in good overall yields and characterized by related analytic data.

  2. SYNTHESIS OF LIQUID CRYSTALLINE POLYACRYLATES WITH THIOESTER AS BRIDGE-BOND

    Institute of Scientific and Technical Information of China (English)

    ZHANG Weibang; ZHANG Guodong; XU Jiarui; ZENG Hanmin

    1996-01-01

    A new series of acrylates with the same mesogens containing thioester as bridge-bond were synthesized, and the acrylates were characterized by H1 NMR, IR and MS. The polymers were obtained by radical polymerization using AIBN as initiator. The monomers and polymers exhibit thermotropic-enantiotropic liquid crystalline behavior.

  3. Synthesis and characterization of polypyrrole grafted chitin

    Science.gov (United States)

    Ramaprasad, A. T.; Latha, D.; Rao, Vijayalakshmi

    2017-05-01

    Synthesis and characterization of chitin grafted with polypyrrole (PPy) is reported in this paper. Chitin is soaked in pyrrole solution of various concentrations for different time intervals and polymerized using ammonium peroxy disulphate (APS) as an initiator. Grafting percentage of polypyrrole onto chitin is calculated from weight of chitin before and after grafting. Grafting of polymer is further verified by dissolution studies. The grafted polymer samples are characterized by FTIR, UV-Vis absorption spectrum, XRD, DSC, TGA, AFM, SEM and conductivity studies.

  4. Synthesis and Structural Characterization of a Cyano-bridged 1-D Lanthanum(Ⅲ)-iron(Ⅲ)Complex [La(DMSO)5(H2O)](μ-CN)2[Fe(CN)4]·H2O

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    A new lanthanumⅢ-ironⅢ complex [La(DMSO)5(H2O)](μ-CN)2[Fe(CN)4]·H2O 1 (DMSO=dimethylsulfoxide) has been prepared by a facile approach, ball-milling method, and characterized by X-ray diffraction. The crystal belongs to monoclinic, space group P21/n with a=9.7125(3), b=21.5336(7), c=14.3804(5) (A), β=93.242(3)°, C16H34FeLaN6O7S5, Mr=777.55, V=3002.8(2)(A)3, Z=4, Dc=1.720 g/cm3, S=1.053, μ(MoKα)=2.278 mm-1, F(000)=1564, R=0.0490 and wR=0.1270. The crystal structure analysis of 1 reveals a slightly distorted squareantiprism eightfold-coordinated La(Ⅲ) ion and a 1-D zigzag chain structure extending through the Fe-CN-La-NC-Fe linkages. The [La(DMSO)5(H2O)](μ-CN)2[Fe(CN)4] species are held together via hydrogen bonds to form a three-dimensional framework.

  5. Photocatalytic semiconductors synthesis, characterization, and environmental applications

    CERN Document Server

    Hernández-Ramírez, Aracely

    2014-01-01

    This critical volume examines the different methods used for the synthesis of a great number of photocatalysts, including TiO2, ZnO and other modified semiconductors, as well as characterization techniques used for determining the optical, structural and morphological properties of the semiconducting materials. Additionally, the authors discuss photoelectrochemical methods for determining the light activity of the photocatalytic semiconductors by means of measurement of properties such as band gap energy, flat band potential and kinetics of hole and electron transfer. Photocatalytic Semiconductors: Synthesis, Characterization and Environmental Applications provide an overview of the semiconductor materials from first- to third-generation photocatalysts and their applications in wastewater treatment and water disinfection. The book further presents economic and toxicological aspects in the production and application of photocatalytic materials.

  6. Bridged heterocyclium dicationic closo-icosahedral perfluoroborane, borane, and carborane salts via aqueous, open-air benchtop synthesis.

    Science.gov (United States)

    Shackelford, Scott A; Belletire, John L; Boatz, Jerry A; Schneider, Stefan; Wheaton, Amanda K; Wight, Brett A; Ammon, Herman L; Peryshkov, Dmitry V; Strauss, Steven H

    2010-06-18

    Thirteen bridged triazolium and imidazolium dicationic salts, which uniquely pair closo-icosahedral perfluoroborane [B(12)F(12)](2-), borane [B(12)H(12)](2-), or carborane [CB(11)H(12)](-) anionic species with unsaturated bridged heterocyclium dications, were synthesized using an aqueous benchtop method. This considerably extends the scope of a reported aqueous synthesis of binary [heterocyclium](2)[B(12)H(12)] and [heterocyclium][CB(11)H(12)] salts. Also, the one-step preparation of five new precursor bridged heterocyclium dicationic dihalide salts using conventional procedures and in one case a microwave-assisted method is described.

  7. Synthesis and Magnetic Studies of Copper ( Ⅱ )-Manganese (Ⅱ)Heterobinuclear Complexes with an Oxamido Bridge

    Institute of Scientific and Technical Information of China (English)

    LI, Yan-Tuan; YAN, Cui-Wei; LIAO, Dai-Zheng

    2001-01-01

    Four new copper ( Ⅱ )-manganese ( Ⅱ ) beterobinuclear complexes bridged by N, N' -bis[ 2- (dimethylamino) ethyl) ] oxamido dianion (dmoxae) and end-capped with 1,10-phenanthroline (phen), 5-methyl-1, l0-phenanthroline (Mephen), diaminoethane (en) or 1,3-di-aminopropane (pn), respectively, namely, [Cu(dmoxae)MnL2](CO4)2 (L= phen, Mephen, en, pn), have been synthesized and characterized by elemental analyses, IR, electronic spectral studies, and molar conductivity measurements. The electronic reflectance spectrum indicates the presence of spin exchange-coupling interaction between bridged copper (Ⅱ) and manganese (Ⅱ) ions.The cryomagnetic measurements (4.2-300 K) of [ Cu(dmoxae)Mn(phen)2](ClO4)2 ( 1 ) and [Cu(dmoxae)Mn(Mephen)2](ClO4)2(2) complexes demonstrated an antiferromagnetic interaction between the adjacent manganese(Ⅱ) and copper (Ⅱ) ions through the oxamido-bridge within each molecule. On the basis of spin Hamiltonian, H^ = - 2JS^1·S^2,the magnetic analysis was carried out for the two complexes and the spin-coupling constant (J) was evaluated as - 35.9cm-1 for 1 and - 32.6 cm-1 for 2. The influence of methyl substitutions in the amine groups of the bridging ligand on magnetic interactions between the metal ions of this kind of complexes is also discussed.

  8. Nitrogen and oxygen bridged calixaromatics: synthesis, structure, functionalization, and molecular recognition.

    Science.gov (United States)

    Wang, Mei-Xiang

    2012-02-21

    heteracalixaromatics had been reported, owing to the formidable synthetic challenges involved. Apart from thiacalixarene, the synthesis of nitrogen- and oxygen-bridged calixarenes appeared very difficult. But since our first publications in 2004, we have been delighted to see the rapid and tremendous development of the supramolecular chemistry of this new generation of macrocycles. In this Account, I summarize the synthesis of N- and O-bridged calixaromatics and their regiospecific functionalization on the rims and bridging positions, focusing on the fragment coupling approach and contributions from our laboratory. I describe the construction of molecular cages based on heteracalixaromatics and discuss the effect of both bridging heteroatoms and substituents on macrocyclic conformations and cavity sizes. Molecular recognition of neutral organic molecules and charged guest species is also demonstrated. The easy accessibility, rich molecular diversity, unique conformation, and cavity tunability of heteracalixaromatics make them invaluable macrocycles for research in supramolecular chemistry. New heteracalixaromatics, with well-defined conformations and cavity properties, will provide powerful tools for probing noncovalent interactions, leading to the development of new molecular sensing and imaging systems. Multicomponent molecular self-assembly of heteracalixaromatics as functional modules with metals, metal clusters, or charge-neutral species should result in multidimensional solid and soft materials with diverse applications. The profitable incorporation of heteracalixaromatics into molecular devices can also be anticipated in the future. Moreover, the construction of enantiopure, inherently chiral heteracalixaromatics should provide important applications in chiral recognition and asymmetric catalysis.

  9. Synthesis and Crystal Structure of a Binuclear Gadolinium(Ⅲ) Complex Bridged by Cucurbit[6]uril

    Institute of Scientific and Technical Information of China (English)

    Gui Ling ZHANG; Zhi Yong WU; Yan Tuan LI; Da Qi WANG; Jian Min DOU

    2006-01-01

    A new cucurbit[6]uril bridged binuclear complex {[Gd(H2O)6]2[Q6(H2O)]}Cl6·4H2O,where Q6 represents cucurbit[6]uril, has been synthesized and characterized by X-ray diffraction.The crystal structure shows that the complex has an extended cucurbit[6]uril-bridged structure consisting of two gadolinium(Ⅲ) ions, in which each gadolinium(Ⅲ) ion is coordinated with two neighboring carbonylic oxygen atoms of Q6 and six oxygen atoms of water molecules that leans toward one side of the portal. One disordered guest water molecule resides in the Q6 molecule cavity and occupies two different positions. Hydrogen bonds assemble the complex to three-dimensional supramolecular structure.

  10. Synthesis and crystal structures of three isophthalato-bridged macrocyclic nickel(II) complexes

    Indian Academy of Sciences (India)

    Guang-Chuan Ou; Zhi-Zhang Li; Lin Yuan; Xian-You Yuan

    2015-01-01

    Three dinuclear isophthalato-bridged nickel(II) complexes formulated as [Ni(rac-L)]2(-IPA)(ClO4)2 (1), [Ni(-L)]2(-IPA)(ClO4)2 (2) and [Ni(SS-L)]2(-IPA)(ClO4)2 (3) (L = 5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyc-lotetradecane, IPA = isophthalic acid) have been isolated and characterized. Single crystal X-ray diffraction analyses revealed that the Ni(II) atoms have six-coordinated distorted octahedral environments, and the isophthalato ligand bridges two Ni(II) centres in a bis bidentate fashion to form dimers in all three complexes. The monomers of {[Ni(-L)]2(-IPA)}2+ are connected through intermolecular hydrogen bonds to generate one-dimensional left-handed helical chains in complex 3. The homochiral natures of complexes 2 and 3 have been confirmed by CD spectroscopy.

  11. Electrolytic Synthesis and Characterizations of Silver Nanopowder

    CERN Document Server

    Theivasanthi, T

    2011-01-01

    This work reports a simple, novel, cost effective and eco-friendly electrolytic synthesis of silver nanoparticles using AgNO3 as metal precursor. The synthesis rate is much faster than other methods and this approach is suitable for large scale production. They are characterized by XRD, SEM and FT-IR techniques to analyze size, morphology and functional groups. XRD studies reveal a high degree of crystallinity and monophasic Ag nanoparticles. Their particle size is found to be 24 nm and specific surface area (SSA) is 24 m2/g. Analysis of Ag nanoparticles SSA reports that increasing their SSA improves their antibacterial actions. Microbiology assay founds that Ag nanoparticles are effective against E.coli and B.megaterium bacteria. SSA of bacteria analysis reveals that it plays a major role while reacting with antimicrobial agents.

  12. Solid-state emissive B,S-bridged p-terphenyls: synthesis, properties, and utility as bifunctional fluorescent sensor for Hg2+ and F- ions.

    Science.gov (United States)

    Chen, Dong-Mei; Wang, Sheng; Li, Hong-Xiang; Zhu, Xiao-Zhang; Zhao, Cui-Hua

    2014-12-01

    The efficient synthesis has been disclosed to achieve a new class of ladder-type molecules, B,S-bridged p-terphenyls (BS-TPs). Their properties were fully characterized by UV-vis and fluorescence spectroscopy in both solution and solid state, time-resolved fluorescence spectroscopy, DFT theoretical calculations, and cyclic voltammetry. A detailed comparison between anti-BS-TP and its analogue B,N-bridged p-terphenyl (BN-TP) was made to elucidate the effect of displacement of bridging N with S atom on the properties. The introduction of S rather than N atom as bridging atom leads to increased fluorescence efficiency in both solution and solid state as well as enhanced reduction stability. And thus this new class of ladder-type molecules are highly emissive in both solution and solid state and display reversible reduction wave in cyclic voltammograms, denoting their promising potentials as electron-transporting solid-state emitters. In addition, this new class of molecules are capable of detecting F(-) and Hg(2+) with different fluorescence responses, owing to the high Lewis acidity of the B center to coordinate with F(-) anions and the great mercury-philicity of the S center to complex with Hg(2+) cations.

  13. Graphene optoelectronics synthesis, characterization, properties, and applications

    CERN Document Server

    bin M Yusoff, Abdul Rashid

    2014-01-01

    This first book on emerging applications for this innovative material gives an up-to-date account of the many opportunities graphene offers high-end optoelectronics.The text focuses on potential as well as already realized applications, discussing metallic and passive components, such as transparent conductors and smart windows, as well as high-frequency devices, spintronics, photonics, and terahertz devices. Also included are sections on the fundamental properties, synthesis, and characterization of graphene. With its unique coverage, this book will be welcomed by materials scientists, solid-

  14. Synthesis and Characterization of Novel Quaternary Thioaluminogermanates

    KAUST Repository

    Al-Bloushi, Mohammed

    2013-05-01

    Metal chalcogenides form an important class of inorganic materials, which include several technologically important applications. The design of metal chlcogenides is of technological interest and has encouraged recent research into moderate temperature solid-state synthetic methods for the single crystal growth of new materials. The aim of this project is the investigation and development of synthetic methodology for the synthesis of novel metal chlcogenides. The new inorganic compounds of the type “M(AlS2)(GeS2)” (M = Na and K) are new metal-chalcogenides, synthesized by the classical solid state approach. The characterization of these compounds was carried out by Scanning Electron Microscopy (SEM), Energy Dispersive X-ray Spectroscopy (EDS), Single crystal and powder X-ray diffraction, solid state Nuclear Magnetic Resonance (NMR), Ultraviolet-visible (UV-VIS), Infrared (IR) and Raman spectroscopy. These theses study the synthesis of metal chalcogenides through the use of standard chemical techniques. The systematic studies demonstrate the effect of the reactants ratio and reaction temperature on the synthesis and growth of the single crystals. Metal chalcogenides have several potential applications in gas separation, ion exchange, environmental remediation, and energy storage. Especially, the ion exchange materials have found\\tpossible applications in waste-water treatment, water softening, metal separation, and production of high purity water.

  15. SYNTHESIS OF NOVEL THIOPHENEDIMETHYLENE BRIDGED HOMOBINUCLEAR METALLOCENES AND THEIR CATALYTIC PROPERTIES FOR ETHYLENE POLYMERIZATION

    Institute of Scientific and Technical Information of China (English)

    Xi-jie Liu; Jun-quan Sun; Hai-ying Zhang; Xiao-hui Xiao; Feng Lin

    2006-01-01

    By treating disodium(thiophenedimethylene)dicyclopentadienide C4H2S(CH2C5H4Na)2 with two equivalent of CpTiCl3 or CpZrCl3 DME at 0℃ in THF, two new thiophenedimethylene bridged binuclear metallocenes [Cl2MC5H5][C5H4CH2C4H2SCH2C5H4][C5H5MCl2] (M = Ti 3, M = Zr 4) were synthesized in high yield and their structures were characterized by 1H-NMR. These complexes were used as catalysts for ethylene polymerization in the presence of methylaluminoxane (MAO). The effects of polymerization temperature, time, concentration of catalyst, molar ratio of MAO/Cat on polymerization were studied in detail. The catalytic activities of thiophenedimethylene bridged binuclear are higher than that of pheneyldimethylene bridged binuclear metallocene catalysts and much higher than that of corresponding mononuclear metallocenes (Cp2TiCl2 and Cp2ZrCl2). The molecular weight distribution curves of polyethylenes produced by binuclear metallocene catalysts (3, 4) and by mononuclear metallocene catalyst have only single peak, but the former (MWD = 3.5-4.7) is obviously broader than the latter (MWD = 2.0-2.2).

  16. Synthesis and mesomorphism of diacetylene-bridged triphenylene discotic liquid crystal dimers

    Institute of Scientific and Technical Information of China (English)

    2009-01-01

    Connecting two discotic mesogens via a spacer not only stabilizes the columnar mesophase but also leads to the formation of glass columnar phase, and therefore improves the physical properties of discotic liquid crystals as organic semiconductor. Here, we report the synthesis of eight diacetylene-bridged triphenylene discotic liquid crystal dimers, [C18H6(OCnH2n+1)4(OMe)O2C-C8H16-C≡≡ C-]2, 3(n), (n = 4-8), [C18H6(OC6H13)5O2C-C8H16-C≡≡ C-]2, 6 and [C18H6(OC6H13)5O-(CH2)m-C≡≡ C-]2, 8(m), (m = 1, 3) by Eglinton coupling reaction. The thermotropic liquid crystal properties were studied by differential scanning calorimetry and polarized optical microscopy. The results are showed as follows: the length of peripheral alkyl chains of triphenylene influenced properties of liquid crystal dimers; dimers 3(n) (n = 5-8) and 6 had glass columnar phase, and no crystallization was observed above -50℃ for all the triphenylene dimers; compared with 3(6), 6 showed higher molecular symmetry, more stable columnar mesophase and wider mesophase range. The connecting group, length and rigidity of spacer had important influence on the mesomorphism of diacetylene-bridged triphenylene discotic liquid crystal dimers.

  17. Synthesis and mesomorphism of diacetylene-bridged triphenylene discotic liquid crystal dimers

    Institute of Scientific and Technical Information of China (English)

    JI Hong; ZHAO KeQing; YU WenHao; WANG BiQin; HU Pin

    2009-01-01

    Connecting two discotic mesogens via a spacer not only stabilizes the columnar mesophase but also leads to the formation of glass columnar phase,and therefore improves the physical properties of discotic liquid crystals as organic semiconductor.Here,we report the synthesis of eight diacetylene-bridged triphenylene discotic liquid crystal dimers,[C18H6(OCnH2n+1)4(OMe)O2C-CsH16-C≡C-]2,3(n),(n=4-8),[C18H6(OC6H13)5O2C-C8H16-C≡C-]2,6 and [C18H6(OC6H13)5O-(CH2)m-C≡C-]2,8(m),(m=1,3) by Eglinton coupling reaction.The thermotropic liquid crystal properties were studied by differential scanning calorimetry and polarized optical microscopy.The results are showed as follows:the length of peripheral alkyl chains of triphenylene influenced properties of liquid crystal dimers;dimers 3(n) (n=5-8) and 6 had glass columnar phase,and no crystallization was observed above -50℃ for all the triphenylene dimers;compared with 3(6),6 showed higher molecular symmetry,more stable columnar mesophase and wider mesophase range.The connecting group,length and rigidity of spacer had important influence on the mesomorphism of diacetylene-bridged triphenylene discotic liquid crystal dimers.

  18. Synthesis of highly phosphonic acid functionalized benzene-bridged periodic mesoporous organosilicas for use as efficient dye adsorbents

    Energy Technology Data Exchange (ETDEWEB)

    Deka, Juti Rani; Liu, Chia-Ling; Wang, Tzu-Hua; Chang, Wei-Chieh; Kao, Hsien-Ming, E-mail: hmkao@cc.ncu.edu.tw

    2014-08-15

    Highlights: • Synthesis of highly phosphonic acid functionalized benzene-bridged PMOs. • Phosphonic acid loaded PMOs as adsorbent for cationic and anionic dyes. • Due to electrostatic interaction the adsorbent has high dye adsorption capacity. • π–π stacking interaction between benzene and dye enhances adsorption capacity. • Intraparticle diffusion played a dominant role in the adsorption process. - Abstract: Periodic mesoporous organosilicas (PMOs) with benzene bridging groups in the silica wall were functionalized with a tunable content of phosphonic acid groups. These bifunctional materials were synthesized by co-condensation of two different organosilane precursors, that is, 1,4-bis(triethoxysilyl)benzene (BTEB) and sodium 3-(trihydroxysilyl)propyl methyl phosphate (SPMP), under acidic conditions using nonionic surfactant Brij-S10 as template. The materials exhibited well-ordered mesostructures and were characterized by X-ray diffraction, nitrogen sorption, TEM, TGA, FTIR, and solid-state NMR measurements. The materials thus obtained were employed as adsorbents to remove different types of dyes, for example, cationic dyes methylene blue and phenosafranine, anionic orange II, and amphoteric rhodamine B, from aqueous solutions. The materials exhibited a remarkably high adsorption capacity than activated carbon due to their ordered mesostructures, a large number of phosphonic acid groups, and high surface areas. The adsorption was mainly governed by electrostatic interaction, but also involved π–π stacking interaction as well as hydrogen bonding. The adsorption kinetics can be better fitted by the pseudo-second order model. The adsorption process was controlled by the mechanisms of external mass transfer and intraparticle diffusion. The materials retained more than 97% dye removal efficiency after use for five consecutive cycles.

  19. Synthesis, crystal structure and redox properties of dihydropyrazole-bridged ferrocene-based derivatives

    Science.gov (United States)

    Li, Heng-Dong; Ma, Zai-He; Yang, Kun; Xie, Li-Li; Yuan, Yao-Feng

    2012-09-01

    Dihydropyrazole-bridged ferrocene-based derivatives were prepared by corresponding chalcones with hydrazine hydrate, then acylation with 3-(ethoxycarbonyl)propionyl chloride directly in high yields and purity. All of these compounds were characterized by MS, IR, 1H NMR, 13C NMR and elemental analysis. The relationship between the structure and redox properties was investigated based on the results of single crystal X-ray structure determinations and cyclic voltammetry. The mechanism of the electron transfer for representative compound 4b was verified by density functional theory (DFT) calculations.

  20. Synthesis and Characterization of Hexagonal Boron Nitride (h- BN) Films

    Science.gov (United States)

    2014-01-09

    Synthesis 1. Diborane- ammonia (B2H6-NH3- gases): Early results with these precursors were published in 2012. 5 Briefly, LPCVD growth of h-BN in a hot-wall...Approved for public release; distribution is unlimited. Synthesis and Characterization of Hexagonal Boron Nitride (h- BN) Films. The views, opinions and...1 ABSTRACT Number of Papers published in peer-reviewed journals: Synthesis and Characterization of Hexagonal Boron Nitride (h-BN) Films. Report Title

  1. Synthesis, characterization and application of electrode materials

    Energy Technology Data Exchange (ETDEWEB)

    He, Lin [Iowa State Univ., Ames, IA (United States)

    1995-07-07

    It has been known that significant advances in electrochemistry really depend on improvements in the sensitivity, selectivity, convenience, and/or economy of working electrodes, especially through the development of new working electrode materials. The advancement of solid state chemistry and materials science makes it possible to provide the materials which may be required as satisfactory electrode materials. The combination of solid state techniques with electrochemistry expands the applications of solid state materials and leads to the improvement of electrocatalysis. The study of Ru-Ti4O7 and Pt-Ti4O7 microelectrode arrays as introduced in paper 1 and paper 4, respectively, focuses on their synthesis and characterization. The synthesis is described by high temperature techniques for Ru or Pt microelectrode arrays within a conductive Ti4O7ceramic matrix. The characterization is based on the data obtained by x-ray diffractometry, scanning electron microscopy, voltammetry and amperometry. These microelectrode arrays show significant enhancement in current densities in comparison to solid Ru and Pt electrodes. Electrocatalysis at pyrochlore oxide Bi2Ru2O7.3 and Bi2Ir2O7 electrodes are described in paper 2 and paper 3, respectively. Details are reported for the synthesis and characterization of composite Bi2Ru2O7.3 electrodes. Voltammetric data are examined for evidence that oxidation can occur with transfer of oxygen to the oxidation products in the potential region corresponding to anodic discharge of H2O with simultaneous evolution of O2. Paper 3 includes electrocatalytic activities of composite Bi2Ir2O7 disk electrodes for the oxidation of I- and the reduction of IO3-.

  2. Design, synthesis and characterization of novel nonlinear optical chromophores for electro-optical applications

    Science.gov (United States)

    Liu, Feng

    This dissertation involves the design, synthesis and characterization of second order nonlinear optical chromophores for electro-optic applications. The design concept, that poling efficiency and macroscopic nonlinearities can be improved by modifying a chromophore's shape, has been explored. Chapter 1 gives an introduction into theoretical background of nonlinear optics and electro-optic phenomenon in organic molecules and poled polymers. Chapter 2 involves the design and synthesis of GLD-2 and GLD-3 chromophores, both with bulky substituents on the ring-fused bridge. The optical studies and HRS measurement show that the two alkyl groups on the bridge blueshift the lambdamax in chloroform by 20 nm and decrease the beta values. DSC and TGA thermal analysis show Td of GLD-2 and GLD-3 over 240°C. The maximum achievable r33 of GLD-2/PMMA is 61 pm/V, compared to the 92.4 pm/V of GLD-1/PMMA. But GLD-2/APC shows r33 of 45.2pm/V, higher than GLD-1/APC due to the improved compatibility with APC. The optical loss of 13 wt% GLD-2/PMMA at 1.55mum is 1.4 dB compared to the 2.3 dB of 17 wt% GLD-1/PMMA. Optical loss studies prove that adding two bulky substituents on bridge help attenuate electrostatic interactions. GLD-3 show deteriorated solubility in common used organic solvents, probably due to the combination of two TBDMS and two lengthy alkyl groups. Chapter 3 presents synthesis of thiophene-based chromophores with variously positioned TBDMS groups. The optical studies of these chromophores show one TBDMSO substitution on the thiophene bridge yields little influence on the lambda max in chloroform. FTCDS chromophore with two TBDMS groups, one on donor and one on thiophene bridge, shows to be the best structure with regards the thermal stability and achievable maximum EO coefficient value, 65.9 pm/V, at only 24 wt% loading density at 1.3 mum. Chapter 4 deals with three novel bridges for NLO chromophores. Synthetic methodologies of the diketone precursor of rigidified

  3. Green synthesis and characterization of graphene nanosheets

    Energy Technology Data Exchange (ETDEWEB)

    Tavakoli, Farnosh [School of Chemistry, College of Science, University of Tehran, Tehran (Iran, Islamic Republic of); Salavati-Niasari, Masoud, E-mail: salavati@kashanu.ac.ir [Institute of Nano Science and Nano Technology, University of Kashan, Kashan, P. O. Box. 87317-51167, Islamic Republic of Iran (Iran, Islamic Republic of); Department of Inorganic Chemistry, Faculty of Chemistry, University of Kashan, Kashan, P. O. Box. 87317-51167, Islamic Republic of Iran (Iran, Islamic Republic of); Badiei, Alireza [School of Chemistry, College of Science, University of Tehran, Tehran (Iran, Islamic Republic of); Mohandes, Fatemeh [Department of Inorganic Chemistry, Faculty of Chemistry, University of Kashan, Kashan, P. O. Box. 87317-51167, Islamic Republic of Iran (Iran, Islamic Republic of)

    2015-03-15

    Highlights: • For the first time, we have synthesized graphene nanosheets in the presence of pomegranate juice. • Here pomegranate juice was used not only as reductant but also as capping agent. • FT-IR, XRD, SEM, EDS and TEM were used to characterize the samples. • According to TEM image, graphene nanosheet is individually exfoliated after stirring for 24 h. • As shown in the TEM image, graphene monolayer is obtained. - Abstract: For the first time, we have successfully synthesized graphene nanosheets in the presence of pomegranate juice. In this approach, pomegranate juice was used not only as reductant but also as capping agent to form graphene nanosheets. At first, the improved Hummer method to oxidize graphite for the synthesis of graphene oxide (GO) was applied, and then the as-produced graphene oxide was reduced by pomegranate juice to form graphene nanosheets. Fourier transformed infrared (FT-IR), X-ray powder diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectrometry (EDS), high resolution transmission electron microscopy (HRTEM), atomic force microscopy (AFM) and raman were used to characterize the samples. The results obtained from the characterization techniques proved high purity of the final products.

  4. Zeolite from fly ash: synthesis and characterization

    Indian Academy of Sciences (India)

    Keka Ojha; Narayan C Pradhan; Amar Nath Samanta

    2004-12-01

    Coal fly ash was used to synthesize X-type zeolite by alkali fusion followed by hydrothermal treatment. The synthesized zeolite was characterized using various techniques such as X-ray diffraction, scanning electron microscopy, Fourier transform infrared spectroscopy, BET method for surface area measurement etc. The synthesis conditions were optimized to obtain highly crystalline zeolite with maximum BET surface area. The maximum surface area of the product was found to be 383 m2/g with high purity. The crystallinity of the prepared zeolite was found to change with fusion temperature and a maximum value was obtained at 823 K. The cost of synthesized zeolite was estimated to be almost one-fifth of that of commercial 13X zeolite available in the market.

  5. Synthesis and characterization of anisotropic magnetic hydrogels

    Science.gov (United States)

    Hinrichs, Stephan; Nun, Nils; Fischer, Birgit

    2017-06-01

    Multiresponsive hydrogels are an interesting new class of materials. They offer the advantage, that they respond to different stimuli like temperature, pH and magnetic fields. By this they can change their properties which makes the hydrogels ideal candidates for many applications in the technical as well as medical field. Here we present the synthesis and characterization of hydrogels - micro- as well as macrogels - which consist of an iron oxide core, varying in phase and morphology, embedded in a thermoresponsive polymer, consisting of poly N-isopropylacrylamide. By using dynamic light scattering we investigated the thermoresponsive properties. In addition we were able to follow the formation of the macrogel by monitoring the shear viscosity.

  6. Synthesis, structural characterization, and magnetic properties of a copper-gadolinium complex derived from a hydroxybenzohydrazide ligand.

    Science.gov (United States)

    Costes, Jean-Pierre; Duhayon, Carine; Vendier, Laure

    2014-02-17

    The reaction of hydroxybenzohydrazide with o-vanillin yields 2-hydroxy-N'-[(2-hydroxy-3-methoxyphenyl)methylidene]benzohydrazide (LH3), a ligand that is able to give mononuclear and tetranuclear copper complexes but also to associate copper and gadolinium ions in a Cu2-Gd2 heterotetranuclear complex. This synthesis is successful if the Gd ions, which are acidic in protic solvents, are introduced in a basic methanol solution of the mononuclear copper complex. In the absence of piperidine, the addition of Gd ions to a methanol solution of the mononuclear copper complex only yields a tetranuclear cubane-type copper complex. This work reports on the first structural characterization of a copper-gadolinium complex involving a benzohydrazide ligand. The resulting complex consists of two Cu-Gd pairs linked by a dihydroxo Gd-Gd bridge, in which the Cu and Gd ions are bridged by a nonsymmetric phenoxo-hydroxo bridge. The magnetostructural correlation between the ferromagnetic coupling constant and the hinge angle observed in symmetrical double-phenoxo Cu-Gd bridges remains valid for dissymmetric Cu-Gd bridges and confirms the preponderance of the structural factor over the nature of the bridge. This tetranuclear complex corresponds to two S = 4 units linked through a dihydroxo bridge introducing a weak antiferromagnetic Gd-Gd interaction and impeding the existence of a S = 8 ground state.

  7. Synthesis, crystal structure and electrochemical and DNA binding studies of oxygen bridged-copper(II) carboxylate

    Science.gov (United States)

    Iqbal, Muhammad; Ali, Saqib; Tahir, Muhammad Nawaz; Muhammad, Niaz; Shah, Naseer Ali; Sohail, Manzar; Pandarinathan, Vedapriya

    2015-08-01

    A new binuclear O-bridged Cu(II) complex with 4-chlorophenyl acetate and 2,2‧-bipyridine has been synthesized and characterized using FT-IR, powder and single crystal XRD and electrochemical solution studies. The results revealed that the two penta-coordinated Cu(II) centers are linked by two carboxylate ligands in end-on bonding fashion. The coordination geometry is slightly distorted square pyramidal (SP) with bridging oxygen atoms occupying the apical position and other ligands lying in the equatorial plane. The striking difference in Cu-O bond distance of the bridging oxygen atom in the complex may be responsible for the SP geometry of Cu(II) ion. The complex gave rise to metal centered irreversible electro-activity where one electron Cu(II)/Cu(III) oxidation process and a single step two electron Cu(II)/Cu(0) reduction process was observed. The redox processes were found predominantly adsorption controlled. The values of diffusion coefficient and heterogeneous rate constant for oxidation process were 6.98 × 10-7 cm2 s-1 and 4.60 × 10-5 cm s-1 while the corresponding values for reduction were 5.30 × 10-8 cm2 s-1 and 5.41 × 10-6 cm s-1, respectively. The formal potential and charge transfer coefficient were also calculated. The DNA-binding ability was explored through cyclic voltammetry and UV-Visible spectroscopy. Diminution in the value of Do for oxidation indicated the binding of the complex with DNA corresponding to Kb = 8.58 × 104 M-1. UV-Visible spectroscopy yielded ε = 49 L mol-1 cm-1 and Kb = 2.96 × 104 M-1. The data of both techniques support each other. The self-induced redox activation of the complex, as indicated by cyclic voltammetry heralds its potential applications in redox catalysis and anticancer activity.

  8. Cable Supported Bridges

    DEFF Research Database (Denmark)

    Gimsing, Niels Jørgen

    Cable supported bridges in the form of suspension bridges and cable-stayed bridges are distinguished by their ability to overcome large spans.The book concentrates on the synthesis of cable supported bridges, covering both design and construction aspects. The analytical part covers simple methods...

  9. Design and construction of two rare aqua bridged copper (II) coordination polymers through mixed ligand strategy: Synthesis, characterization and single crystal X-ray structure determination of [Cu(2-iodobenzoate)2(β/γ-picoline)2(μ-H2O)]n

    Science.gov (United States)

    Kumar, Santosh; Sharma, Raj Pal; Saini, Anju; Venugopalan, Paloth; Ferretti, Valeria

    2015-03-01

    Reaction of hydrated copper (II) 2-iodobenzoate with β/γ-picoline in methanol:water mixture (4:1, v/v) yielded two rare aqua bridged zig-zag polymers [Cu(2-iodobenzoate)2(β-picoline)2(μ-H2O)]n; 1 and [Cu(2-iodobenzoate)2(γ-picoline)2(μ-H2O)]n; 2. The newly synthesized complexes have been characterized by elemental analysis, FT-IR spectroscopy, UV-Vis spectroscopy and single crystal X-ray structure determination. Complex 1 crystallized in monoclinic crystal system with C2/c space group, and complex 2 crystallized in triclinic crystal system with P 1 ‾ space group. X-ray structure determination revealed the presence of 1-dimensional chains of constituent molecules running along a-axis in both complexes. Water molecules act as bridges between constituent molecules and hence play a crucial role in 1-dimensional chain propagation in zig-zag manner. Empty channels have been observed between the zig-zag chains of complexes. Non-covalent interactions interactions such as O-H⋯O, C-H⋯O and C-H⋯π have been observed, which play a decisive role in the stabilization of crystal lattices in both complexes 1 and 2.

  10. synthesis, characterization, thermal behavior and antimicrobial ...

    African Journals Online (AJOL)

    The design and synthesis of ... The double distilled water was used for the preparation and chemical analyses. ... Synthesis of 3-methyl benzoate complexes of transition metal with hydrazine. Bull. Chem. Soc. ..... hinder the respiration process of the cell and thus block the synthesis of the proteins, restricting further growth of ...

  11. Bridging ligands in organometallic chemistry. II. Synthesis and reactivity of the green dimer of molybdenocene containing a bridging fulvalene ligand

    Energy Technology Data Exchange (ETDEWEB)

    Smart, J.C.; Curtis, C.J.

    1978-11-01

    Synthesis, precipitation, and isolation of dicyclopentadienyl(fulvalene)dihydridomolybdenum are described. The compound was used in reaction studies involving the addition of carbon monoxide and deprotonation with n-butyllithium. Data for elemental analysis, ir spectral and NMR(in toluene-d) spectral analysis are reported for the title compound and its reaction products.

  12. 草酰胺桥联异三核配合物Cu(NiL)2(ClO4)2的合成、光谱表征和晶体结构%Synthesis,Spectroscopic Characterization and Crystal Structure of A Novel Oxamido-Bridged Trinuclear Complex Cu(NiL)2(ClO4)2

    Institute of Scientific and Technical Information of China (English)

    周旭光; 王圆方; 李容芳; 王庆伦; 杨光明; 廖代正

    2004-01-01

    A novel oxamido-bridged trinuclear complex Cu(NiL)2(ClO4)2 (where H2L=2,3-dioxo-5,6,14,15-dibenzo-1,4,8,12-tetraazacyclo-pentadeca-7,3-dien) has been synthesized and characterized by elemental analysis, IR spectrum,UV-Visible spectrum and single crystal X-ray diffraction. It crystallizes in the monoclinic system, space group P21/n. The lattice parameters are: a=1.0524(6) nm, b=1.182 1(6) nm, c=1.586 2(9) nm, β=91.657(9)°, and V=1.972 6(19) nm3, Z=2. The results show that the coordination geometry around copper(Ⅱ) in the title complex is hexa-coordinated octahedron.

  13. Organic Ion Exchangers. Synthesis, Characterization and Applications

    Institute of Scientific and Technical Information of China (English)

    E. S. Dragan

    2005-01-01

    @@ 1Introduction Organic ion exchangers in beads form are the most widely utilized materials in the purification, concentration and separation processes of inorganic and organic ions in many fields of science and industry[1,2]. Some original contributions in the preparation and characterization of porous organic ion exchangers will be summarized first. The main types of synthetic ion exchangers were obtained by polymer-analogous reactions performed on porous styrene-divinylbenzene copolymers (S-DVB)[3,4] and porous acrylonitrile-DVB copolymers (AN-DVB) [5,6]. Porous S-DVB copolymers were used as substrate for the synthesis of weak and strong base anion exchangers by chloromethylation reaction followed by the reaction with secondary or tertiary amines.Different chloromethylation agents were employed. Weak base anion exchangers with tertiary or primary amine groups were prepared starting from AN-DVB copolymers by aminolyse-hydrolyse reaction with asymmetrical diamines or ethylenediamine (EDA), respectively. Strong base anion exchangers were obtained by quaternization reaction with alkyl halides of the tertiary amine groups. Chelating ion exchangers with iminodiacetic groups were prepared by the carboxymethylation reaction of the primary amine groups above mentioned and of those contained in a vinylamine-ethylacrylate-DVB copolymer, vinylamine units being generated by a Hofmann degradation reaction of the primary amide groups contained in the acrylamide-ethylacrylate-DVB copolymerp[7]. An amphoteric ion exchanger was prepared by the hydrolysis of the ester groups after the Hofmann degradation.

  14. Synthesis and characterization of novel nanothermometers

    Energy Technology Data Exchange (ETDEWEB)

    Baumert, Delphine [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Larsen, George [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Coopersmith, Kaitlin [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Schyck, Sarah [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Murph, Simona [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)

    2016-03-23

    A straightforward approach was developed for the synthesis of Pd, Pd-Fe2O3, Au-Fe2O3, and Au-Pd-Fe2O3 nanothermometers, using a single SL DNA. These NP-DNA conjugates were characterized using techniques including EDX measurements, ζ-potential of NPs before and after DNA functionalization, electron microscopy studies and fluorescence spectroscopy. The fluorescence studies of the NP-DNA demonstrate the interaction between the NP and the fluorophore, which is quenched in the case of Au-Pd-Fe2O3 NPs and is perhaps enhanced (when compared to AuNPs) in the case of Pd and Pd-Fe2O3 NPs. In order to achieve more accurate and reproducible measurements, designing a system that is able to hold the NP-DNA conjugates at a temperature for a longer period of time to allow them to 12 equilibrate is currently underway. Our studies show that Au-Pd-Fe2O3 NPs are the best candidate material to serve as nanothermometers when compared to Pd, Pd-Fe2O3, and Au-Fe2O3 materials.

  15. Synthesis Technique and Characterizations of Silver Nanostructures

    Science.gov (United States)

    Rajawat, Shweta; Qureshi, M. S.

    2015-06-01

    In this work, we report synthesis of nanostructures of silver nanoparticles using X-ray films. Exposed X-ray films, which consist of silver nanoparticles, are cut into small pieces of size 1 cm × 1 cm. These pieces were heated in distilled water at temperature 70°C. These nanoparticles, separated from heated films, are simultaneously collected through electrolytic deposition using copper and carbon rods. The carbon rod is wrapped over by Low density polyethylene (LDPE) sheet for easy extraction. This process was carried in two different environments (1) in broad daylight and (2) on a cloudy day. Characterization of the two samples was done using X-Ray Diffractometer (XRD), Transmission Electron Microscopy (TEM) and UV-Vis spectroscopy. XRD of the particles gave peaks well in accordance with JCPDS file 04-. This result confirms formation of highly pure silver nanoparticles. TEM revealed that the interaction of silver nanoparticles with sunlight gave chain like structures whereas in the absence of interaction with sunlight, cloudy day, nanoflowers were formed. Nanostructures were more prominent for bigger particles.

  16. Functionalized TUD-1: synthesis, characterization and (photo-)catalytic performance

    NARCIS (Netherlands)

    Hamdy M. Saad, M.S.

    2005-01-01

    The new mesoporous material; TUD-1 is chosen of which the synthesis, characterization, and functionalization for (photo)-catalytic performance are extensively investigated in this study. The synthesis of the new catalytic materials M TUD-1 (M = Ti, V, Cr, Mo, Fe, Co and Cu) is carried out through an

  17. Functionalized TUD-1: synthesis, characterization and (photo-)catalytic performance

    NARCIS (Netherlands)

    Hamdy M. Saad, M.S.

    2005-01-01

    The new mesoporous material; TUD-1 is chosen of which the synthesis, characterization, and functionalization for (photo)-catalytic performance are extensively investigated in this study. The synthesis of the new catalytic materials M TUD-1 (M = Ti, V, Cr, Mo, Fe, Co and Cu) is carried out through an

  18. Synthesis, Characterization, and Sensitivity Analysis of Urea Nitrate (UN)

    Science.gov (United States)

    2015-04-01

    ARL-TR-7250 ● APR 2015 US Army Research Laboratory Synthesis, Characterization, and Sensitivity Analysis of Urea Nitrate (UN...Characterization, and Sensitivity Analysis of Urea Nitrate (UN) by William M Sherrill Weapons and Materials Research Directorate...Characterization, and Sensitivity Analysis of Urea Nitrate (UN) 5a. CONTRACT NUMBER 5b. GRANT NUMBER 5c. PROGRAM ELEMENT NUMBER 6. AUTHOR(S

  19. Synthesis,Characterization,and Electrochemical Property of Nanometer Porphyrin Dimer

    Institute of Scientific and Technical Information of China (English)

    2008-01-01

    A nanometer porphyrin dimer was synthesized with fumaryl chloride as a bridge-linked reagent. The characterization was carried out with elemental analyses, 1H NMR, UV-Vis, and IR spectrometries, and then the electrochemical properties of the porphyrins were studied. The authors found that there was moderate electronic communication between the two porphyrin rings in the nanometer porphyrin dimer.

  20. Synthesis of novel redox calix[4]arene derivative with 1,3-substituted large conjugated ferrocene bridge

    Institute of Scientific and Technical Information of China (English)

    Bi Qiong Hong; Fa Fu Yang; Hong Yu Guo; Yan Hua Wang; Xian Feng Chai

    2009-01-01

    A novel redox calix[4]arene derivative with 1,3-substituted large conjugated ferrocene bridge was designed and synthesized in high yield.Its structure was characterized by element analysis,IR,ESI-MS,NMR spectrum,etc.The primary study of cyclic voltammetry showed it possessed excellent reversible electrochemistry response property.

  1. Synthesis, Characterization and Application of 2-Line and 6-Line ...

    African Journals Online (AJOL)

    Michael Horsfall

    Synthesis, Characterization and Application of 2-Line and 6-Line Ferrihydrite to Pb(II). Removal from Aqueous ... found applications in medicine, catalysis, electronic device and ..... thermodynamics of dyes onto acid activated low cost carbon.

  2. Synthesis, characterization, and catalysis of metal nanoparticles

    Science.gov (United States)

    Mott, Derrick M.

    The goal of the dissertation work is the understanding of the physical and chemical properties of materials in the nanoscale regime. As discussed in this dissertation, the goal is accomplished by specifically focusing on the investigation of the synthesis and characterization of metal nanoparticles and supported catalysts. The findings have provided us with new and important insights into the physical and chemical properties of metal nanoparticles and supported catalysts. Several new routes allowed us to synthesize copper, gold-platinum, core-shell nanoparticles with monodispersed sizes, controlled shapes and tunable surface properties. For example, we have demonstrated the ability to control the formation of copper nanorods with high monodispersity and ordering by controlled thermal processing. Another of our studies has focused on the exploitation of the synergistic properties of multimetallic nanoparticles by monitoring the CO adsorption on bimetallic gold-platinum nanoparticles using infrared spectroscopy. The size correlation between using different microscopic techniques such as TEM and AFM has been established for the size determination of nanoparticles. This correlation is important in understanding their physical or chemical properties of nanoparticles on different substrate surfaces. The quantitative correlation demonstrates the ability of AFM in determining sizes of nanoparticles, which has implications to the understanding of the relative radius of curvature of the tip vs. the particle sizes as well as the surface properties of the particles. The preliminary results using computational modeling to elucidate some of the surface binding and energy properties of nanoparticles provides some guidelines to experimental measurements, and also helps in the explanation of the complex experimental data. Overall, these findings and results have provided new insights into the fundamental factors governing the physical and chemical properties in the synthesis and

  3. Synthesis and characterization of new meso-substituted unsymmetrical metalloporphyrins

    Indian Academy of Sciences (India)

    Babasaheeb P Bandgar; Pradip B Gujarathi

    2008-03-01

    The synthesis and characterization of new meso-substituted unsymmetrical metalloporphyrins has been described. A new modified Adler method was used for the synthesis of two unsymmetrical porphyrins. Reactions of these unsymmetrical porphyrins with metal acetates afforded the corresponding metalloporphyrins in high yields with excellent purity. These porphyrins and their metal derivatives were characterized by spectroscopic methods. However, the copper complexes were further studied by ESR spectra and zinc complex by fluorescence spectrum.

  4. The Synthesis and Characterization of Several Corroles

    African Journals Online (AJOL)

    NICO

    Preliminary results towards the synthesis of a corrole-based vitamin B12 analogue are reported. The synthesis of ..... petroleum ether (1:4 v/v) containing 1 % triethylamine; ethyl acetate ... by column chromatography on flash silica gel with ethyl.

  5. The supramolecular interaction mediated chiral 1D cyanide-bridged metamagnet: synthesis, crystal structures and magnetic properties.

    Science.gov (United States)

    Zhang, Daopeng; Bian, Yongzhong; Qin, Jie; Wang, Ping; Chen, Xia

    2014-01-21

    Two cyanide-bridged enantiopure one-dimensional single chain complexes, [Mn((R,R)-Salcy)Fe(pcq)(CN)3]2n·1.5nDMF (1) and [Mn((S,S)-Salcy)Fe(pcq)(CN)3]2n·1.5nDMF (2), have been synthesized and structurally characterized. Systematically magnetic investigations show the antiferromagnetic coupling between the cyanide-bridged Mn(III)-Fe(III) centers and the interesting metamagnetic behavior at about 5.0 K resulted from the intermolecular π-π interaction.

  6. Synthesis, characterization and applications of graphene architectures

    Science.gov (United States)

    Thomas, Abhay Varghese

    Graphene, a two--dimensional sheet of sp2 hybridized carbon atoms arranged in a honeycomb lattice structure, has garnered tremendous interest from the scientific community for its unique combination of properties. It has interesting electrical, thermal, optical and mechanical properties that scientists and engineers are trying to understand and harness to improve current products as well as focus on disruptive technologies that can be made possible by this next generation material. In this thesis the synthesis, characterization and applications of various graphene architectures were explored from the context of a bottom--up and top--down synthesis approach. The work is divided into three main chapters and each one deals with a unique architecture of graphene as well as its properties and an application to a real world problem. In Chapter 2, we focus on bottom--up synthesis of graphene sheets by chemical vapor deposition. We then studied the wetting properties of graphene coated surfaces. More specifically the wetting properties of single and multilayer graphene films on flat and nanoscale rough surfaces are explored and the insights gained are used in improving heat transfer performance of copper surfaces. Single layer graphene, on certain flat surfaces, was shown to exhibit `wetting transparency' as a result of its sheer thinness and this property is of interest in various wetting related applications. Surface protection from corrosion and/or oxidation without change in wetting properties is tremendously useful in multiple fields and we looked to apply this property to dehumidification of copper surfaces. The short time scales results demonstrated that graphene indeed served to prevent oxidation of the surface which in turn promoted increased heat transfer co--efficients with respect to the oxidized copper surfaces. Closer inspection of the surface over long time scales however revealed that the oxide layer changed the wetting properties and this was detrimental

  7. Two-dimensional carbon fundamental properties, synthesis, characterization, and applications

    CERN Document Server

    Yihong, Wu; Ting, Yu

    2013-01-01

    After a brief introduction to the fundamental properties of graphene, this book focuses on synthesis, characterization and application of various types of two-dimensional (2D) nanocarbons ranging from single/few layer graphene to carbon nanowalls and graphene oxides. Three major synthesis techniques are covered: epitaxial growth of graphene on SiC, chemical synthesis of graphene on metal, and chemical vapor deposition of vertically aligned carbon nanosheets or nanowalls. One chapter is dedicated to characterization of 2D nanocarbon using Raman spectroscopy. It provides extensive coverage for a

  8. Novel metallomesogenic polyurethanes: Synthesis, characterization and properties

    Energy Technology Data Exchange (ETDEWEB)

    Senthilkumar, Natarajan, E-mail: nskumar77@yahoo.com [Production Technology Research Center, Samsung Cheil Industries, 62 Pyeongyeo-dong, Yeosu-si, JeonNam 555-210 (Korea, Republic of); Narasimhaswamy, Tanneru [Polymer Laboratory, Central Leather Research Institute, Chennai 600 020 (India); Kim, Il-Jin [Production Technology Research Center, Samsung Cheil Industries, 62 Pyeongyeo-dong, Yeosu-si, JeonNam 555-210 (Korea, Republic of)

    2012-12-01

    A series of tetradentate Schiff base metallomesogenic diols were synthesized from two simple dihydroxy benzenes. The metallomesogenic diol was constructed from three ring containing mesogen linked through ester and azomethine with terminal hydroxy group. This upon complexation with copper(II) formed metallomesogenic diol with varying terminal chain length. A series of metallomesogenic polyurethanes were synthesized using these metallomesogenic diols as chain extenders for the prepolymers based on polytetramethylene glycol (PTMG) of varying molecular weight (M{sub n} = 650, 2000) and 2,4-toluene diisocyanate (TDI), or 4,4 Prime -methylene bis(phenyl isocyanate) (MDI). The molar ratio of metallomesogenic diol and PTMG were varied in the polyurethane to find their role in liquid crystalline and mechanical properties. Extensive characterization of all metallomesogenic compounds and intermediates were carried out by FT-IR, {sup 1}H and {sup 13}C NMR, EPR, VSM, Mass (EI and FAB) and UV-visible spectroscopy. Hot stage polarizing microscope and differential scanning calorimetry were used to ensure the phase characteristics such as nature of phase, melting and clearing temperatures and phase range. The appearance of enantiotropic smectic A phases indicated high molecular polarizability of the core due to the metal ion. - Highlights: Black-Right-Pointing-Pointer Design and synthesis of metallomesogenic diols. Black-Right-Pointing-Pointer Metallomesogenic polyurethanes were prepared using these diols as chain extenders. Black-Right-Pointing-Pointer Liquid crystalline and mechanical properties were studied. Black-Right-Pointing-Pointer A square pyramidal structure for the copper(II) complexes have been proposed. Black-Right-Pointing-Pointer Polyurethanes exhibited enantiotropic smectic A phases.

  9. Hydrothermal synthesis of pyrochlores and their characterization

    Science.gov (United States)

    Redkin, Alexander F.; Ionov, Andrey M.; Kotova, Nataliya P.

    2013-10-01

    Pyrochlores, microlites, and U-betafites of pyrochlore group minerals were obtained from mixing experiments of the corresponding oxides and fluorides by hydrothermal synthesis at T = 800 °C and P = 200 MPa in the solution of 1.0 M NaF. The presence of U4+ in pyrochlore does not affect the cell parameter, which for the phases of pyrochlore-microlite series is 10.42 ± 0.01 Å. In a system with an excess of UO2, pyrochlores and microlites, containing uranium up to 0.2-0.3 atoms per formula unit (apfu), are formed. In the uranium-free system of betafites composition, perovskites and Ti-bearing pyrochlores are formed. U-pyrochlores of betafite series, containing 2Ti = Nb + Ta in moles, have cubic cell parameters of 10.26 ± 0.02 Å and U4+ isomorphic capacity of 0.4-0.5 apfu. In the pyrochlore structure, U4+ may substitute for Ca2+ and Na+ cations in the eightfold site. In pyrochlores of pyrochlore-microlite series, Ca2+ is replaced by U4+, while in pyrochlores of betafite series, U4+ replaces Na+. Phases with pyrochlore structure, containing U5+ and U6+ in the sixfold site, usually occupied by Nb5+, Ta5+, and Ti4+, are formed under oxidizing conditions (Cu-Cu2O buffer). They are characterized by low content of Nb5+, Ta5+ (<0.1 apfu), and anomalous behavior of the crystal lattice (compression, instead of expansion). Under natural conditions, the formation of pyrochlores containing a significant amount of U5+ and U6+ is unlikely.

  10. Ruthenium-catalyzed intramolecular metathesis of dienes and its application in the synthesis of bridged and spiro azabicycles

    Science.gov (United States)

    Kuznetsov, N. Yu; Bubnov, Yu N.

    2015-07-01

    The review presents a historical excursion into catalytic alkene metathesis, covering the problems of history of the discovery of this process, as well as investigations on the properties, structure and reactivity of the most popular ruthenium catalysts for metathesis, mechanism of their action and decomposition. The main part covers studies devoted to the syntheses of bridged azabicyclic and 1-azaspirocyclic compounds comprising the intramolecular metathesis of dienes as the key step. The formation of a bicyclic skeleton of a series of natural bridged (cocaine, ferruginine, calystegines, and anatoxin-a) and spiro (pinnaic acids, halichlorine, hystrionicotoxin, and cephalotaxine) azabicycles, as well as their analogues and compounds with larger rings is demonstrated. The methods for the synthesis of diene precursors and the conditions for final assembling of the bicyclic compounds are considered in detail. The generalization of the literature data allows one to efficiently carry out the mentioned process taking into account the most important features. The bibliography includes 129 references.

  11. Bisxantphos: stereoselective synthesis and coordination behaviour of a new class of cyclic double bridged diphosphines

    NARCIS (Netherlands)

    den Heeten, R.; Zuidema, E.; Lutz, M.; Spek, A.L.; van Leeuwen, P.W.N.M.; Kamer, P.C.J.

    2011-01-01

    A new class of cyclic double bridged diphosphine ligands was developed and the coordination properties are described. The reaction of 4,5-dilithioxanthene with dichlorophenylphosphine gave a cyclic double bridged diphosphine ligand based on two xanthene backbones (4) as a single stereoisomer. X-ray

  12. Synthesis and antitumor activity of iodo-bridged-binuclear platinum complex

    Institute of Scientific and Technical Information of China (English)

    2006-01-01

    Iodo-bridged binuclear platinum(II) com- plex[Pt((◇)-NH2)I2]2(BPA) has been synthesized and characterized by elemental analysis, conductivity, differential thermal analysis, IR, UV and 1HNMR spectra techniques. The cytotoxicity of the complex was tested by MTT and SRB assays. The results show that complex BPA demonstrates better cytotoxicity than that of the clinically established cisplatin against EJ, HCT-8, BGC-823, HL-60 and MCF-7 cell lines. The complex BPA at concentrations of 1.00 and 2.00 μmol/L induces G1 cell cycle arrest in HL-60 cells. The level of total platinum bound to DNA in HL-60 cells is significantly higher than that of cisplatin under the same experimental conditions. Acute toxicity experimental results indiacte that LD50 of BPA is 815.3 mg/kg by intraperitoneal administration. BPA at dose of 12 mg/kg significantly inhibits the growth of nude mice implanted by human A2780 and HCT-116 carcinomas, and inhibition rate is similar to that of cisplatin at dose of 4 mg/kg by intraperitoneal administration. BPA at dose of 20 mg/kg inhibits the growth of nude mice implanted by human A549 carcinomas, but there was no significant statistical difference.

  13. LADDER SUPERSTRUCTURE-DIRECTED SYNTHESIS OF A WELL-DEFINED m-PHENELENEDIIMINO-BRIDGED LADDER POLYMETHYLSILOXANE

    Institute of Scientific and Technical Information of China (English)

    Yin-sheng Lv; Zhong-jie Ren; You-zhi Wan; Ping Xie; Rong-ben Zhang

    2009-01-01

    A well-defined m-phenylenediimino-bridged ladder polymethylsiloxane (LP) was first synthesized through a well-defined ladder superstructure (LS) acting as synthetic template, which was self-assembled by concerted interaction of hydrogen bonding and aromatic π-π stacking of the monomer (M), N,N'-bis(phenyldichlorosilyl)-m-phenylenediamine. Some key characterization data of LP and, in particular, the extremely vulnerable LS with very unstable Si--Cl and Si-N groups were given. The molecular weights (Mn) of LS and LP are 5010 and 10480, corresponding to about 15 and 46 monomer units, respectively. To monitor the real in situ status of LS in solution the XRD measurements of special freeze-drying samples were performed, demonstrating two characteristic peaks of ladder structure. Most importantly, both LP and LS display exceedingly sharp resonance absorption peaks with a half peak width (△1/2) as small as < 0.3 of MeSi(NH)O2/2 moieties in 29Si-NMR spectra. It is well-known that the higher the regularity of the ladder polysiloxane, the narrower the resonance peak of the siloxane moiety on the ladder backbone, and the smaller the half peak width △1/2. Therefore, the very small values of △1/2 for both LS and LP confirm that both LS and LP possess well-defined ladder structures.

  14. Novel Green Synthesis and Characterization of Nanopolymer ...

    African Journals Online (AJOL)

    1King Abdullah Institute for Nanotechnology, 2Department of Chemical Engineering, ... Methods: Green synthesis of nano-polymer porous gold oxide nanoparticles ... UV (ultraviolet (UV) visible spectroscopy and dynamic light scattering (DLS) ...

  15. Experimental and numerical characterization of thermal bridges in prefabricated building walls

    Energy Technology Data Exchange (ETDEWEB)

    Zalewski, Laurent; Lassue, Stephane; Boukhalfa, Kamel [Univ Lille Nord de France, F-59000 Lille (France); UArtois, LGCgE, F-62400 Bethune (France); Rousse, Daniel [Department of Mechanical Engineering, Ecole de Technologie Superieure, Montreal (Canada)

    2010-12-15

    This work is a contribution to the characterization of the thermal efficiency of complex walls of buildings with respect to the ever increasing requirements in thermal insulation. The work specifically concerns the quantitative evaluation of heat losses by thermal bridges. The support of the study is the envelope of industrial light construction walls containing a metal framework, an insulating material inserted in between metal trusses, water and vapor barriers, and the internal and external facings. This article presents first the infrared thermography method which is used to visualize the thermal bridges as well as a genuine complementary experimental method allowing for the determination of the quantitative aspects of the heat losses through the envelope. Tangential-gradient heat fluxmeters, which create little disturbance in the measurements, are used in the context of laboratory and in full-scale insitu experiments. Then, the article presents a simple yet accurate prediction with a three-dimensional numerical method that could be used for the design of specific installations and parametric studies. (author)

  16. Synthesis and characterization of polymeric azido Zn(II) and Ni(II) complexes based on 3-hydroxypyridine

    Science.gov (United States)

    Mautner, Franz A.; Berger, Christian; Domian, Elisabeth; Fischer, Roland C.; Massoud, Salah S.

    2016-10-01

    The synthesis and structural characterization of two new complexes catena-[Ni(3-O-py)(3-HO-py)2(μ1,3-N3)(H2O)] (1) and catena-[Zn(μ-3-O-py)(μ1,1-N3)] (2), where 3-HO-py = 3-hydroxypyridine, are reported. The complexes were characterized by the elemental microanalyses, IR, and X-ray crystallography and by UV-Vis spectroscopy for complex 1. Single crystal X-ray crystallography revealed the polymeric nature of the complexes: 1 as 1D with a single EE azide bridging, and 2 as 2D with μ(O,O‧,N) bridging of the deprotonated 3-O-py anions and di-EO azide groups, respectively. In 1 the neutral and deprotonated 3-hydroxypyridine molecules act only as N-terminal ligands. The emission spectral properties of the Zn(II) complex were investigated.

  17. Synthesis, crystal structure and magnetic properties of a one-dimensional copper(II) polymer bridged by different double end-on azide bridges

    Science.gov (United States)

    Zhang, Li-Fang; Yu, Ming-Ming; Ni, Zhong-Hai; Cui, Ai-Li; Kou, Hui-Zhong

    2011-12-01

    A one-dimensional (1D) copper(II) complex [Cu 3(μ 1,1-N 3) 6(dmp) 2] n ( 1) has been synthesized and structurally characterized. The molecular structure of 1 is constructed by trimeric [Cu 3(μ 1,1-N 3) 6(dmp) 2] units formed through two double symmetric (basal-to-basal) end-on (EO) azide bridges and the trimeric units are connected further by double asymmetric (basal-to-apical) EO azide bridges, giving 1D chain-like structure. The chains of 1 are linked together by N-H⋯N azide hydrogen bonds and very weak Cu⋯N azide coordination interactions from μ-1,1,3,3-N 3 fashion to form two-dimensional (2D) supramolecular architecture. The magnetic structure can be considered as uniform 1D chain formed by linear trimeric Cu II-Cu II-Cu II units and the dominating magnetic coupling occurs within the trimeric Cu3II unit. The magnetic study shows that the compound exhibits ferromagnetic interactions with Jt = + 8.36(2) cm -1 and Jc = + 0.35(4) cm -1 for intratrimeric and intertrimeric Cu3II unit based on 1D magnetic model, respectively.

  18. Synthesis and characterization of Schiff's bases of sulfamethoxazole

    OpenAIRE

    Hussain, Zainab; Yousif, Emad; Ahmed, Ahmed; Altaie, Ali

    2014-01-01

    Background Schiff's bases are excellent ligands which are synthesized from the condensation of primary amines with carbonyl groups. Findings The classical reaction for the synthesis of Schiff's bases in an ethanolic solution and glacial acetic acid as a catalyst was followed in the synthesis of substituted sulfamethoxazole compounds. Conclusions Some Schiff's bases containing sulfamethoxazole nucleus have been synthesized and characterized. The present compounds are hoped to be applied in the...

  19. Synthesis, Characterization and In-vitro Evaluation

    African Journals Online (AJOL)

    Department of Chemistry, Tabriz Branch, Islamic Azad University, Tabriz, Iran ... Results: 1H-NMR and elemental analyses data for calculating mole composition of CMS polymers were relatively in good agreement. ... different processes as photo-sensitizers [15], ..... Babazadeh M. Design, synthesis and in vitro evaluation.

  20. The nonantibiotic small molecule cyslabdan enhances the potency of β-lactams against MRSA by inhibiting pentaglycine interpeptide bridge synthesis.

    Directory of Open Access Journals (Sweden)

    Nobuhiro Koyama

    Full Text Available The nonantibiotic small molecule cyslabdan, a labdan-type diterpene produced by Streptomyces sp. K04-0144, markedly potentiated the activity of the β-lactam drug imipenem against methicillin-resistant Staphylococcus aureus (MRSA. To study the mechanism of action of cyslabdan, the proteins that bind to cyslabdan were investigated in an MRSA lysate, which led to the identification of FemA, which is involved in the synthesis of the pentaglycine interpeptide bridge of the peptidoglycan of MRSA. Furthermore, binding assay of cyslabdan to FemB and FemX with the function similar to FemA revealed that cyslabdan had an affinity for FemB but not FemX. In an enzyme-based assay, cyslabdan inhibited FemA activity, where as did not affected FemX and FemB activities. Nonglycyl and monoglycyl murein monomers were accumulated by cyslabdan in the peptidoglycan of MRSA cell walls. These findings indicated that cyslabdan primarily inhibits FemA, thereby suppressing pentaglycine interpeptide bridge synthesis. This protein is a key factor in the determination of β-lactam resistance in MRSA, and our findings provide a new strategy for combating MRSA.

  1. Cyanide- and phenoxo-bridged heterobimetallic Fe(III)-Mn(III) complexes: Synthesis, crystal structures and magnetic properties

    Indian Academy of Sciences (India)

    Daopeng Zhang; Ping Wang; Kexun Chen; Xia Chen

    2014-11-01

    By employing two -tricyanidoiron(III) precursors [Ph4P][FeIII(pcq)(CN)3] and [Ph4P][FeIII (pzq)(CN)3] as building blocks and a salen-tpye Schiff-basemanganese (III) compound as assembling segment, two tetranuclear cyanide- and phenoxo- bridged heterobimetallic Fe(III)-Mn(III) complexes {[Mn(saltmen)] [Fe(pcq)(CN)3]}2·2CH3OH (1) and {[Mn(saltmen)] [Fe(pzq)(CN)3]}2·2CH3OH (2) (pcq = 8-(pyridine-2-carboxamido, pzq = 8-(pyrazine-2-carboxamido, saltmen2− = N,N′-(1,1,2,2-tetramethylethylene)bis(salicylideneaminato) dianion) have been synthesized and characterized by elemental analysis, IR spectroscopy and X-ray structure determination. Single x-ray analysis reveals their isostructural cyanide-bridged Fe(III)-Mn(III) binuclear structure. The binuclear entity is self-complementary through phenoxo oxygen from the neighbouring complex, giving cyanide- and phenoxo- bridged tetranuclear structure. Furthermore, under the help of the intermolecular - interaction, these two complexes can be constructed into 1D infinite chain supramolecular structure. Investigation over magnetic susceptibilities reveals the overall ferromagnetic coupling between the adjacent Fe(III) and Mn(III) ions bridged by cyanide group with = 5.34 cm-1 and 5.55 cm-1 for complexes 1 and 2, respectively.

  2. Synthesis of bridged β-cyclodextrin–polyethylene glycol and evaluation of its inhibition performance in oilfield wastewater

    Energy Technology Data Exchange (ETDEWEB)

    Zou, Changjun, E-mail: changjunzou@126.com; Liu, Yuan; Yan, Xueling; Qin, Yibie; Wang, Meng; Zhou, Lu

    2014-10-15

    The bridged β-cyclodextrin–polyethylene glycol (β-CD–PEG) is synthesized through reaction of β-CD with PEG, which has been characterized by Fourier transform infrared spectroscope. The inhibition efficiency of bridged β-CD–PEG on corrosion of Q235 carbon steel in 0.5 M HCl solution has been investigated by electrochemical impedance spectroscopy (EIS), potentiodynamic polarization and weight loss measurements. The results show that β-CD–PEG acted as a mixed-type inhibitor and performed excellent inhibiting effect for the corrosion of the Q235 carbon steel. The steel surface morphologies are analyzed using scanning electron microscopy (SEM) and energy dispersive X-ray analysis (EDX) and then an adsorption mechanism model is proposed. The high inhibitory efficiency of β-CD–PEG is related with the adsorption of polymer molecules at the steel surface and a protective film formation. Finally, these results present a novel corrosion inhibitor works in oil-gas field. - Highlights: • The bridged β-CD–PEG is synthesized by polyethylene glycol and cyclodextrin. • The bridged β-CD–PEG acts as an inhibitor for carbon steel in oilfield wastewater. • The high inhibitory efficiency is related with a protective film formation. • The adsorption of β-CD–PEG is well described by the Langmuir adsorption isotherm.

  3. Synthesis and characterization of acrylate-bridged dinuclear copper complex and acetate and 2,4,6-trimethylpyridine copper complex%Cu(Ⅱ))的丙烯酸桥联双核配合物及醋酸、2,4,6-三甲基吡啶三元配合物的合成与表征

    Institute of Scientific and Technical Information of China (English)

    钱永; 王建军

    2012-01-01

    在温和条件下合成了Cu(Ⅱ)的丙烯酸双核配合物[Cu2(C3H3O2)4].H2O和醋酸、2,4,6-三甲基吡啶三元配合物[Cu(C2H3O2)2(C8H11N)2]。通过元素分析、红外光谱、紫外光谱和核磁测试表征了该两种配合物的组成和结构,并用溶解度、电导率测试等物理化学手段对配合物的物理化学性质进行了初步研究。%The acrylate-bridged dinuclear copper complex [Cu2(C3H3O2)4]·H2O and acetate and 2,4,6-Trimethylpyridine copper complex [Cu(C2H3O2)2(C8H11N)2] were synthesized under tender conditions in this paper.The elemental components and structures of the two complexes were characterized and confirmed by elemental analyses,FT-IR,UV-Vis and 1H NMR.And the primary investigation on the physical and chemical characteristics of the two complexes has been carried out through some physical and chemical methods such as the solubility and molar conductivity in this work.

  4. Synthesis and Characterization of Novel Perylene Diimide

    Science.gov (United States)

    Yu, Zhen; Wang, Ying; Wang, Wen-Guang; Pu, Jia-Ling

    2016-05-01

    This paper designed and synthesized a new organic semiconductor material perylene diimide (PDI) derivative which taped into perylene tetracarboxylic anhydride as the starting material. The molecule belongs to the first synthesis which can enrich the varieties of PDI derivatives. And it can expectedly be used as one candidate of organic semiconductor materials. The structure of the target molecule was confirmed by 1HNMR, 13CNMR and HRMS.

  5. Synthesis and characterization of magnetite nanoparticles coated with lauric acid

    Energy Technology Data Exchange (ETDEWEB)

    Mamani, J.B., E-mail: javierbm@einstein.br [Instituto do Cérebro-InCe, Hospital Israelita Albert Einstein-HIAE, 05651-901 São Paulo (Brazil); Costa-Filho, A.J. [Faculdade de Filosofia, Ciências e Letras de Ribeirão Preto, Universidade de São Paulo, Ribeirão Preto (Brazil); Cornejo, D.R. [Instituto de Física Universidade de São Paulo, USP, São Paulo (Brazil); Vieira, E.D. [Instituto de Física, Universidade Federal de Goiás, Goiânia (Brazil); Gamarra, L.F. [Instituto do Cérebro-InCe, Hospital Israelita Albert Einstein-HIAE, 05651-901 São Paulo (Brazil)

    2013-07-15

    Understanding the process of synthesis of magnetic nanoparticles is important for its implementation in in vitro and in vivo studies. In this work we report the synthesis of magnetic nanoparticles made from ferrous oxide through coprecipitation chemical process. The nanostructured material was coated with lauric acid and dispersed in aqueous medium containing surfactant that yielded a stable colloidal suspension. The characterization of magnetic nanoparticles with distinct physico-chemical configurations is fundamental for biomedical applications. Therefore magnetic nanoparticles were characterized in terms of their morphology by means of TEM and DLS, which showed a polydispersed set of spherical nanoparticles (average diameter of ca. 9 nm) as a result of the protocol. The structural properties were characterized by using X-ray diffraction (XRD). XRD pattern showed the presence of peaks corresponding to the spinel phase of magnetite (Fe{sub 3}O{sub 4}). The relaxivities r{sub 2} and r{sub 2}* values were determined from the transverse relaxation times T{sub 2} and T{sub 2}* at 3 T. Magnetic characterization was performed using SQUID and FMR, which evidenced the superparamagnetic properties of the nanoparticles. Thermal characterization using DSC showed exothermic events associated with the oxidation of magnetite to maghemite. - Highlights: • Synthesis of magnetic nanoparticles coated with lauric acid • Characterization of magnetic nanoparticles • Morphological, structural, magnetic, calorimetric and relaxometric characterization.

  6. Synthesis of bright red-emissive dicyanoetheno-bridged hexa-peri-hexabenzocoronene dimers.

    Science.gov (United States)

    Oda, Kazuma; Hiroto, Satoru; Hisaki, Ichiro; Shinokubo, Hiroshi

    2017-02-07

    The introduction of a dicyanomethyl anion group to hexa-peri-hexabenzocoronene (HBC) substantially enhanced the emission properties of HBC due to a large perturbation of its electronic structure. In addition, dicyanoetheno-bridged HBC dimers obtained from oxidation of a dicyanomethyl HBC anion exhibited bright red emission in solution and solid states. Intramolecular charge transfer interactions between the HBC units and the dicyanoethene bridge induced solvatochromic behaviour in their emission spectra. Dicyanoetheno-bridged HBC dimers exhibited cis-trans photoisomerization behaviour in the solution, affording the mixture in cis-isomer dominance in the photostationary state. Theoretical calculations revealed that the cis-isomer is more thermodynamically stable than the trans-isomer.

  7. Synthesis and characterization of thermotropic liquid crystalline polyimides

    Indian Academy of Sciences (India)

    Sachin Mane; C R Rajan; Surendra Ponrathnam; Nayaku Chavan

    2015-10-01

    Non-symmetrical and linear dyad-based mesogens were synthesised containing imine or ester bridging group. In the present work, due to the absence of branching in diamine-based mesogen, the structure has—rigidity inversely imine/ester bridging groups between two benzene rings imparts—flexible property to the mesogen and consequently rigid–flexible property has been balanced. The synthesised mesogens were characterized by different techniques including nuclear magnetic resonance and Fourier transform infrared spectroscopy. Liquid crystalline polymers (LCPs) were synthesised using pyromellitic dianhydride and 4-[(4-aminobenzylidene)amino]aniline or 4-aminophenyl-4-aminobenzoate. Subsequently, thermotropic liquid crystalline polymers (TLCPs) have also been evaluated to obtain optical microscopy textures at different temperatures which demonstrated interesting and notable changes. It is worth noting that marble-like textures were observed upto 200 ° C.

  8. Synthesis and characterization of ester and amide derivatives of titanium(IV) carboxymethylphosphonate

    Science.gov (United States)

    Melánová, Klára; Beneš, Ludvík; Trchová, Miroslava; Svoboda, Jan; Zima, Vítězslav

    2013-06-01

    A set of layered ester and amide derivatives of titanium(IV) carboxymethylphosphonate was prepared by solvothermal treatment of amorphous titanium(IV) carboxymethylphosphonate with corresponding 1-alkanols, 1,ω-alkanediols, 1-aminoalkanes, 1,ω-diaminoalkanes and 1,ω-amino alcohols and characterized by powder X-ray diffraction, IR spectroscopy and thermogravimetric analysis. Whereas alkyl chains with one functional group form bilayers tilted to the layers, 1,ω-diaminoalkanes and most of 1,ω-alkanediols form bridges connecting the adjacent layers. In the case of amino alcohols, the alkyl chains form bilayer and either hydroxyl or amino group is used for bonding. This simple method for the synthesis of ester and amide derivatives does not require preparation of acid chloride derivative as a precursor or pre-intercalation with alkylamines and can be used also for the preparation of ester and amide derivatives of titanium carboxyethylphosphonate and zirconium carboxymethylphosphonate.

  9. Synthesis of L-cystine bridged bis(β-cyclodextrin) and its cooperative binding toward guest molecules

    Institute of Scientific and Technical Information of China (English)

    LI Li; LI Xiaoyun; LIU Yu

    2004-01-01

    A novel β-cyclodextrin derivative, L-cystine bridged bis(β-cyclodextrin) 1 has been synthesized and characterized by 1H NMR, 13C NMR, IR, Raman and combustion analyses. Spectrofluorometric titrations have been performed in aqueous phosphate buffer solution (pH=7.20) at 25℃ to give the complex stability constants (Ks) and Gibbs free energy changes (-△G°) for the stoichiometric 1︰1 inclusion complexation of 1 with four dyes. The binding abilities and molecular selectivities are discussed from the viewpoint of size/shape-fit and electrostatic interactions between hosts and guests. 2D ROESY investigation for the complexation between host and guest further confirms the cooperative binding of bridged cyclodextrin 1 with guest.

  10. The synthesis and characterization of iron nanoparticles

    Science.gov (United States)

    Bennett, Tyler

    Nanoparticle synthesis has garnered attention for technological applications for catalysts, industrial processing, and medical applications. The size ranges for these is in the particles nanostructural domain. Pure iron nanoparticles have been of particular interest for their reactivity and relative biological inertness. Applications include cancer treatment and carrying medicine to a relevant site. Unfortunately, because of their reactivity, pure iron nanoparticles have been difficult to study. This is because of their accelerated tendency to form oxides in air, due to the increased surface area to volume ratio. Using synthesis processes with polyphenols or long chain amines, air stable iron nanoparticles have been produced with a diameter size range of ~ 2 to about ~10 nm, but apparently have transformed due to internal pressure and crystallographic defects to the FCC phase. The FCC crystals have been seen to form icosahedral and decahedral shapes. This size is within the range for use as a catalyst for the growth of both carbon nanotubes and boron nitride nanotubes as well for biomedical applications. The advantages of these kinds of catalysts are that nanotube growth can be for the first time separated from the catalyst formation. Additionally, the catalyst size can be preselected for a certain size nanotube to grow. In summary: (1) we found the size distributions of nanoparticles for various synthesis processes, (2) we discovered the right size range for growth of nanotubes from the iron nanoparticles, (3) the nanoparticles are under a very high internal pressure, (4) the nanoparticles are in the FCC phase, (5) they appear to be in icosahedral and decahedral structures, (6) they undergo room temperature twinning, (7) the FCC crystals are distorted due to carbon in octahedral sites, (8) the iron nanoparticles are stable in air, (9) adding small amounts of copper make the iron nanoparticles smaller.

  11. Molybdenum oxide nanocubes: Synthesis and characterizations

    Energy Technology Data Exchange (ETDEWEB)

    Muthamizh, S.; Suresh, R.; Giribabu, K.; Manigandan, R.; Kumar, S. Praveen; Munusamy, S.; Narayanan, V., E-mail: vnnara@yahoo.co.in [Department of Inorganic Chemistry, University of Madras, Guindy Campus, Chennai -600025 (India); Stephen, A. [Department of Nuclear Physics, University of Madras, Guindy Campus, Chennai-600025 (India)

    2015-06-24

    Molybdenum oxide nanoparticles were prepared by Solid state synthesis. The MoO{sub 3} nanoparticles were synthesized by using commercially available ammonium heptamolybdate. The XRD pattern reveals that the synthesized MoO{sub 3} has orthorhombic structure. In addition, lattice parameter values were also calculated using XRD data. The Raman analysis confirm the presence of Mo-O in MoO{sub 3} nanoparticles. DRS-UV analysis shows that MoO{sub 3} has a band gap of 2.89 eV. FE-SEM analysis confirms the material morphology in cubes with nano scale.

  12. Molybdenum oxide nanocubes: Synthesis and characterizations

    Science.gov (United States)

    Muthamizh, S.; Suresh, R.; Giribabu, K.; Manigandan, R.; Kumar, S. Praveen; Munusamy, S.; Stephen, A.; Narayanan, V.

    2015-06-01

    Molybdenum oxide nanoparticles were prepared by Solid state synthesis. The MoO3 nanoparticles were synthesized by using commercially available ammonium heptamolybdate. The XRD pattern reveals that the synthesized MoO3 has orthorhombic structure. In addition, lattice parameter values were also calculated using XRD data. The Raman analysis confirm the presence of Mo-O in MoO3 nanoparticles. DRS-UV analysis shows that MoO3 has a band gap of 2.89 eV. FE-SEM analysis confirms the material morphology in cubes with nano scale.

  13. Synthesis, Characterization, and Surface Initiated Polymerization of Carbazole Functionalized Isocyanides

    NARCIS (Netherlands)

    Schwartz, Erik; Lim, Eunhee; Gowda, Chandrakala M.; Liscio, Andrea; Fenwick, Oliver; Tu, Guoli; Palermo, Vincenzo; Gelder, de Rene; Cornelissen, Jeroen J.L.M.; Eck, van Ernst R.H.; Kentgens, Arno P.M.; Cacialli, Franco; Nolte, Roeland J.M.; Samori, Paolo; Huck, Wilhelm T.S.; Rowan, Alan E.

    2010-01-01

    We describe the design and synthesis of carbazole functionalized isocyanides and the detailed investigation of their properties. Characterization by solid state NMR, CD, and IR spectroscopic techniques reveals that the polymer has a well-defined helical architecture. Surface-initiated polymerization

  14. Synthesis, characterization, and antiplasmodial activity of polymer-incorporated aminoquinolines

    CSIR Research Space (South Africa)

    Aderibigbe, BA

    2014-01-01

    Full Text Available Journal of Biomedical Materials Research Part A Vol. 102(A) Synthesis, characterization, and antiplasmodial activity of polymer-incorporated aminoquinolines B. A. Aderibigbe,1 E. W. Neuse,2 E. R. Sadiku,1 S. Shina Ray,3 P. J. Smith4 1Department...

  15. Synthesis, characterization and properties of some organozinc hydride complexes

    NARCIS (Netherlands)

    Koning, A.J. de; Boersma, J.; Kerk, G.J.M. van der

    1980-01-01

    The synthesis and characterization of the monopyridine complexes of ethylzinc hydride and phenylzinc hydride are described. On treatment with TMED these complexes are converted into R2Zn3H4. TMED species through a combination of ligand-exchange and disproportionation. The formation of organozinc hyd

  16. Polymer protected gold nanoparticles: synthesis, characterization and application in catalysis

    OpenAIRE

    Baygazieva, E. K.; Yesmurzayeva, N. N.; Tatykhanova, G. S.; Mun, G. A.; Khutoryanskiy, V. V.; Kudaibergenov, S. E.

    2014-01-01

    This review discusses the stabilization of gold nanoparticles (AuNPs) by nonionic, anionic, cationic and amphoteric polymers. The protocols used for synthesis of AuNPs in aqueous and organic solvents are described. Size, shape and morphology of AuNPs are characterized by various physicochemical methods. Application aspects of polymer-protected AuNPs in catalysis are outlined.

  17. Monolayer transition metal disulfide:Synthesis, characterization and applications

    Institute of Scientific and Technical Information of China (English)

    Qi Fu; Bin Xiang

    2016-01-01

    Two-dimensional transition metal dichalcogenides (2D TMDCs) has aroused tremendous attention in recent years, because of their remarkable properties originated from their unique structure. In this re-view we report the synthesis, characterization and applications of monolayer MoS2 and WS2.

  18. Poly/diphenylsiloxy/arylazines. I - Synthesis and characterization

    Science.gov (United States)

    Goldsberry, R. E.; Adamson, M. J.; Reinisch, R. F.

    1973-01-01

    A detailed description is presented for the synthesis of poly(diphenylsiloxy)arylazines by the melt polymerization of hydroxyarylazines and bis(anilino)diphenylsilane. The resulting polymers have been characterized by elemental analysis, gel-permeation chromatography, vapor-phase osmometry, and UV-VIS-IR optical spectroscopy.

  19. Identification and characterization of RBM44 as a novel intercellular bridge protein.

    Directory of Open Access Journals (Sweden)

    Tokuko Iwamori

    Full Text Available Intercellular bridges are evolutionarily conserved structures that connect differentiating germ cells. We previously reported the identification of TEX14 as the first essential intercellular bridge protein, the demonstration that intercellular bridges are required for male fertility, and the finding that intercellular bridges utilize components of the cytokinesis machinery to form. Herein, we report the identification of RNA binding motif protein 44 (RBM44 as a novel germ cell intercellular bridge protein. RBM44 was identified by proteomic analysis after intercellular bridge enrichment using TEX14 as a marker protein. RBM44 is highly conserved between mouse and human and contains an RNA recognition motif of unknown function. RBM44 mRNA is enriched in testis, and immunofluorescence confirms that RBM44 is an intercellular bridge component. However, RBM44 only partially localizes to TEX14-positive intercellular bridges. RBM44 is expressed most highly in pachytene and secondary spermatocytes, but disappears abruptly in spermatids. We discovered that RBM44 interacts with itself and TEX14 using yeast two-hybrid, mammalian two-hybrid, and immunoprecipitation. To define the in vivo function of RBM44, we generated a targeted deletion of Rbm44 in mice. Rbm44 null male mice produce somewhat increased sperm, and show enhanced fertility of unknown etiology. Thus, although RBM44 localizes to intercellular bridges during meiosis, RBM44 is not required for fertility in contrast to TEX14.

  20. Identification and Characterization of RBM44 as a Novel Intercellular Bridge Protein

    Science.gov (United States)

    Iwamori, Tokuko; Lin, Yi-Nan; Ma, Lang; Iwamori, Naoki; Matzuk, Martin M.

    2011-01-01

    Intercellular bridges are evolutionarily conserved structures that connect differentiating germ cells. We previously reported the identification of TEX14 as the first essential intercellular bridge protein, the demonstration that intercellular bridges are required for male fertility, and the finding that intercellular bridges utilize components of the cytokinesis machinery to form. Herein, we report the identification of RNA binding motif protein 44 (RBM44) as a novel germ cell intercellular bridge protein. RBM44 was identified by proteomic analysis after intercellular bridge enrichment using TEX14 as a marker protein. RBM44 is highly conserved between mouse and human and contains an RNA recognition motif of unknown function. RBM44 mRNA is enriched in testis, and immunofluorescence confirms that RBM44 is an intercellular bridge component. However, RBM44 only partially localizes to TEX14-positive intercellular bridges. RBM44 is expressed most highly in pachytene and secondary spermatocytes, but disappears abruptly in spermatids. We discovered that RBM44 interacts with itself and TEX14 using yeast two-hybrid, mammalian two-hybrid, and immunoprecipitation. To define the in vivo function of RBM44, we generated a targeted deletion of Rbm44 in mice. Rbm44 null male mice produce somewhat increased sperm, and show enhanced fertility of unknown etiology. Thus, although RBM44 localizes to intercellular bridges during meiosis, RBM44 is not required for fertility in contrast to TEX14. PMID:21364893

  1. Proficient magnesium nanoferrites: synthesis and characterization

    Energy Technology Data Exchange (ETDEWEB)

    Anis-ur-Rehman, M; Malik, Muhammad Ali; Akram, M [Applied Thermal Physics Laboratory, Department of Physics, COMSATS Institute of Information Technology, Islamabad 44000 (Pakistan); Khan, Kishwar; Maqsood, Asghari, E-mail: marehman@cosmsats.edu.pk [Thermal Transport Laboratory, School of Chemical and Materials Engineering (SCME), National University of Sciences and Technology, Islamabad (Pakistan)

    2011-01-15

    Ferrite materials are potential candidates for modern technological applications because of their tunable electrical and magnetic properties. The excellent combination of magnetic and dielectric properties of magnesium ferrites can be used to fulfill the future demand for high-frequency applications such as antennas. The electrical transport properties of these materials depend on the synthesis conditions such as sintering and composition. The aim of this work has been to correlate the synthesis conditions and induced electrical transport properties, so that these materials prepared in optimized conditions can be used for the miniaturization of high-frequency application devices. X-ray diffraction (XRD) patterns of samples prepared by the co-precipitation method confirmed the formation of a single spinel phase. The crystallite size, lattice parameters and porosity of the samples were calculated from XRD data. The scanning electron microscopy results showed the formation of rods in the case of the samples sintered at 950 {sup 0}C. All the electrical and dielectric properties showed strong dependence on structural properties. The dielectric constant, dielectric loss tangent and ac electrical conductivity of nanocrystalline Mg ferrites were investigated as a function of frequency and sintering temperature. Dielectric, ac electrical properties and the effect of sintering temperature are explained in accordance with the Maxwell-Wagner and the Koops models.

  2. Synthesis and structure characterization of diethyldiallylammonium chloride

    Institute of Scientific and Technical Information of China (English)

    刘立华; 龚竹青; 郑雅杰

    2003-01-01

    The unsaturated quaternary ammonium salt diethyldiallylammonium chloride(DEDAAC) was synthesized in a two-step synthetic method. The influences of the adding method of raw materials and temperature on the yields of diethylallylamine (DEAA), and drying and temperature on the synthesis of DEDAAC were investigated. The content of in-process product DEAA was determined by non-aqueous titration. The structure of product DEDAAC was identified with IR, 1 H NMR and elemental analysis. The results show that adding allyl chloride and sodium hydroxide alternately can increase the yield of DEAA and decrease by-products. In further synthesizing of DEDAAC from DEAA, the step of drying DEAA is very necessary. When DEAA is dried by solid sodium hydroxide, good columnar crystals with a high purity(mp 199.5-201.0 ℃) are obtained; when DEAA is undried or the content of water in DEAA is above 20%, only platelets with bad quality are obtained even without crystals. The suitable synthesis conditions for DEAA and DEDAAC are 35 ℃, 6 h and 40 ℃, 36 h, respectively, and their yields are 69.7% and 67.3%, respectively.

  3. Synthesis, Characterization and Antibacterial Evaluations of the ...

    African Journals Online (AJOL)

    MBI

    2014-06-05

    Jun 5, 2014 ... ... Ni(II) and Zn(II) were synthesized and characterized by molar conductance, FTIR, NMR, UV-Visible and elemental analysis. ... 10mmol) at room temperature and then refluxed for ..... Cytochrome P450 dependent metabolism.

  4. Synthesis and characterization of tantalum silsesquioxane complexes.

    Science.gov (United States)

    Guillo, Pascal; Fasulo, Meg E; Lipschutz, Michael I; Tilley, T Don

    2013-02-14

    Tantalum polyhedral oligosilsesquioxane (POSS) complexes have been synthesised and characterized. X-ray structures of these complexes revealed that the coordination number of the tantalum center greatly affects the cube-like silsesquioxane framework.

  5. Synthesis and Luminescent Properties of an Acetylide-Bridged Dinuclear Platinum(II) Terpyridyl Complex

    Institute of Scientific and Technical Information of China (English)

    WANG,You-Wei(王幼薇); YANG,Qing-Zheng(杨清正); WU,Li-Zhu(吴骊珠); ZHANG,Li-Ping(张丽萍); TUNG,Chen-Ho(佟振合)

    2004-01-01

    An acetylide-bridged dinuclear platinum(II) terpyridyl complex, [Pt(4'-p-tolyl-terpy)-≡-phenyl-≡-(4'-p-tolyl- terpy)Pt](ClO4)2 (1), has been successfully synthesized and its photophysical properties are reported.

  6. High-spin molecules: synthesis, X-ray characterization, and magnetic behavior of two new cyano-bridged Ni(II)(9)Mo(V)(6) and Ni(II)(9)W(V)(6) clusters with a S = 12 ground state.

    Science.gov (United States)

    Bonadio, Federica; Gross, Mathias; Stoeckli-Evans, Helen; Decurtins, Silvio

    2002-11-04

    The preparations, X-ray structures, and magnetic characterizations are presented for two new pentadecanuclear cluster compounds: [Ni(II)(Ni(II)(MeOH)(3))(8)(mu-CN)(30)(M(V)(CN)(3))(6)].xMeOH.yH(2)O (M(V) = Mo(V) (1) with x = 17, y = 1; M(V) = W(V) (2) with x = 15, y = 0). Both compounds crystallize in the monoclinic space group C2/c, with cell dimensions of a = 28.4957(18) A, b = 19.2583(10) A, c = 32.4279(17) A, beta = 113.155(6) degrees, and Z = 4 for 1 and a = 28.5278(16) A, b = 19.2008(18) A, c = 32.4072(17) A, beta = 113.727(6) degrees, and Z = 4 for 2. The structures of 1 and 2 consist of neutral cluster complexes comprising 15 metal ions, 9 Ni(II) and 6 M(V), all linked by mu-cyano ligands. Magnetic susceptibilities and magnetization measurements of compounds 1 and 2 in the crystalline and dissolved state indicate that these clusters have a S = 12 ground state, originating from intracluster ferromagnetic exchange interactions between the mu-cyano-bridged metal ions of the type Ni(II)-NC-M(V). Indeed, these data show clearly that the cluster molecules stay intact in solution. Ac magnetic susceptibility measurements reveal that the cluster compounds exhibit magnetic susceptibility relaxation phenomena at low temperatures since, with nonzero dc fields, chi"(M) has a nonzero value that is frequency dependent. However, there appears no out-of-phase (chi"(M)) signal in zero dc field down to 1.8 K, which excludes the expected signature for a single molecule magnet. This finding is confirmed with the small uniaxial magnetic anisotropy value for D of 0.015 cm(-1), deduced from the high-field, high-frequency EPR measurement, which distinctly reveals a positive sign in D. Obviously, the overall magnetic anisotropy of the compounds is too low, and this may be a consequence of a small single ion magnetic anisotropy combined with the highly symmetric arrangement of the metal ions in the cluster molecule.

  7. Synthesis and spectral and redox properties of three triply bridged complexes of ruthenium

    Science.gov (United States)

    Llobet, A.; Curry, M.E.; Evans, H.T.; Meyer, T.J.

    1989-01-01

    Syntheses are described for the ligand-bridged complexes [(tpm)RuIII(??-O)(??-L)2RuIII(tpm) n+ (L = O2P(O)(OH), n = 0 (1); L = O2CO, n = 0 (2); L = O2CCH3, n = 2 (3); tpm is the tridentate, facial ligand tris(1-pyrazolyl)methane. The X-ray crystal structure of [(tpm)Ru(??-O)(??-O2P(O)(OH))2Ru(tpm)]??8H 2O was determined from three-dimensional X-ray counter data. The complex crystallizes in the trigonal space group P3221 with three molecules in a cell of dimensions a = 18.759 (4) A?? and c = 9.970 (6) A??. The structure was refined to a weighted R factor of 0.042 based on 1480 independent reflections with I ??? 3??(I). The structure reveals that the complex consists of two six-coordinate ruthenium atoms that are joined by a ??-oxo bridge (rRU-O = 1.87 A??; ???RuORu = 124.6??) and two ??-hydrogen phosphato bridges (average rRu-O = 2.07 A??) which are capped by two tpm ligands. The results of cyclic voltammetric and coulometric experiments show that the complexes undergo both oxidative and reductive processes in solution. Upon reduction, the ligand-bridged structure is lost and the monomer [(tpm)Ru(H2O)3]2+ appears quantitatively. All three complexes are diamagnetic in solution. The diamagnetism is a consequence of strong electronic coupling between the low-spin d5 Ru(III) metal ions through the oxo bridge and the relatively small Ru-O-Ru angle. ?? 1989 American Chemical Society.

  8. NEW ROOM TEMPERATURE LIQUIDS: SYNTHESIS AND CHARACTERIZATION

    Directory of Open Access Journals (Sweden)

    Macaev Fliur

    2007-06-01

    Full Text Available Room temperature ionic liquids (ILs have been recognized as a new generation of solvents for “green chemistry” and represent remarkably promising classes of technologically useful and fundamentally interesting materials [1-6]. Most of them are quaternary imidazolium cations with inorganic counterions. Cation in these salts is appended to the organic group (usually saturated hydrocarbon fragments. However, some problems regarding the functionalization [2,7], coordination properties [4] of ILs still remain to be solved. It seems to us that functionalization of imidazoles by ethylcarbonitrile, allyl, 2,3-epoxypropyl fragments will lead to new properties of synthesized ILs. There are no literature data on use of 2-(1H-1-imidazolylethylcarbonitrile 4 for synthesis of imidazolium salts with ILs properties.

  9. Synthesis and Characterization of Two Danazol Derivatives

    Directory of Open Access Journals (Sweden)

    Lauro Figueroa-Valverde

    2010-01-01

    Full Text Available Two danazol derivatives were synthesized and characterized by spectral analyses. In order to characterize the structural and chemical requirements of danazol derivatives, several parameters such as logP, π, Rm and Vm were evaluated. The results showed an increase in the values of logP for the compound 6 in comparison with 3. The compound 3 showed an increase in the values of π, R Vm and V Vm with respect to 6. These data indicate a high degree of lipophilicity and a low steric impediment for compound 6 in comparison with 3.

  10. Anisotropic Gold Nanocrystals:. Synthesis and Characterization

    Science.gov (United States)

    Stiufiuc, R.; Toderas, F.; Iosin, M.; Stiufiuc, G.

    In this letter we report on successful preparation and characterization of anisotropic gold nanocrystals bio-synthesized by reduction of aqueous chloroaurate ions in pelargonium plant extract. The nanocrystals have been characterized by means of Transmission Electron Microscopy (TEM), UV-VIS absorption spectroscopy and tapping mode atomic force microscopy (TM-AFM). Using these investigation techniques, the successful formation of anisotropic single nanocrystals with the preferential growth direction along the gold (111) plane has been confirmed. The high detail phase images could give us an explanation concerning the growth mechanism of the nanocrystals.

  11. Pyrazole bridged dinuclear Cu(II) and Zn(II) complexes as phosphatase models: Synthesis and activity

    Science.gov (United States)

    Naik, Krishna; Nevrekar, Anupama; Kokare, Dhoolesh Gangaram; Kotian, Avinash; Kamat, Vinayak; Revankar, Vidyanand K.

    2016-12-01

    Present work describes synthesis of dibridged dinuclear [Cu2L2(μ2-NN pyr)(NO3)2(H2O)2] and [Zn2L(μ-OH)(μ-NNpyr)(H2O)2] complexes derived from a pyrazole based ligand bis(2-hydroxy-3-methoxybenzylidene)-1H-pyrazole-3,5-dicarbohydrazide. The ligand shows dimeric chelate behaviour towards copper against monomeric for zinc counterpart. Spectroscopic evidences affirm octahedral environment around the metal ions in solution state and non-electrolytic nature of the complexes. Both the complexes are active catalysts towards phosphomonoester hydrolysis with first order kcat values in the range of 2 × 10-3s-1. Zinc complex exhibited promising catalytic efficiency for the hydrolysis. The dinuclear complexes hydrolyse via Lewis acid activation, whereby the phosphate esters are preferentially bound in a bidentate bridging fashion and subsequent nucleophilic attack to release phosphate group.

  12. Radical aryl migration enables diversity-oriented synthesis of structurally diverse medium/macro- or bridged-rings

    Science.gov (United States)

    Li, Lei; Li, Zhong-Liang; Wang, Fu-Li; Guo, Zhen; Cheng, Yong-Feng; Wang, Na; Dong, Xiao-Wu; Fang, Chao; Liu, Jingjiang; Hou, Chunhui; Tan, Bin; Liu, Xin-Yuan

    2016-12-01

    Medium-sized and medium-bridged rings are attractive structural motifs in natural products and therapeutic agents. Due to the unfavourable entropic and/or enthalpic factors with these ring systems, their efficient construction remains a formidable challenge. To address this problem, we herein disclose a radical-based approach for diversity-oriented synthesis of various benzannulated carbon- and heteroatom-containing 8-11(14)-membered ketone libraries. This strategy involves 1,4- or 1,5-aryl migration triggered by radical azidation, trifluoromethylation, phosphonylation, sulfonylation, or perfluoroalkylation of unactivated alkenes followed by intramolecular ring expansion. Demonstration of this method as a highly flexible tool for the construction of 37 synthetically challenging medium-sized and macrocyclic ring scaffolds including bridged rings with diverse functionalities and skeletons is highlighted. Some of these products showed potent inhibitory activity against the cancer cell or derivative of human embryonic kidney line in preliminary biological studies. The mechanism of this novel strategy is investigated by control experiments and DFT calculations.

  13. Synthesis, Properties Characterization and Applications of Various Organobismuth Compounds

    Directory of Open Access Journals (Sweden)

    Jingfei Luan

    2011-05-01

    Full Text Available Organobismuth chemistry was emphasized in this review article due to the low price, low toxicity and low radioactivity characteristics of bismuth. As an environmentally-friendly class of organometallic compounds, different types of organobismuth compounds have been used in organic synthesis, catalysis, materials, etc. The synthesis and property characterization of many organobismuth compounds had been summarized. This review article also presented a survey of various applications of organobismuth compounds in organic transformations, as reagents or catalysts. The reactivity, reaction pathways and mechanisms of reactions with organobismuths were discussed. Less common and limiting aspects of organobismuth compounds were also briefly mentioned.

  14. Gaseous detonation synthesis and characterization of nano-oxide

    Science.gov (United States)

    Yan, Honghao; Wu, Linsong; Li, Xiaojie; Wang, Xiaohong

    2015-07-01

    Gaseous detonation is a new method of heating the precursor of nanomaterials into gas, and integrating it with combustible gas as mixture to be detonated for the synthesis of nanomaterials. In this paper, the mixed gas of oxygen and hydrogen is used as the source for detonation, to synthesize nano TiO2, nano SiO2 and nano SnO2 through gaseous detonation method, characterization and analysis of the products, it was found that the products from gaseous detonation method were of high purity, good dispersion, smaller particle size and even distribution. It also shows that for the synthesis of nano-oxides, gaseous detonation is universal.

  15. Facile synthesis of carbon nanofibers-bridged porous carbon nanosheets for high-performance supercapacitors

    Science.gov (United States)

    Jiang, Yuting; Yan, Jun; Wu, Xiaoliang; Shan, Dandan; Zhou, Qihang; Jiang, Lili; Yang, Deren; Fan, Zhuangjun

    2016-03-01

    A facile and one-step method is demonstrated to prepare carbon nanofibers (CNFs)-bridged porous carbon nanosheets (PCNs) through carbonization of the mixture of bacterial cellulose and potassium citrate. The CNFs bridge PCNs to form integrated porous carbon architecture with high specific surface area of 1037 m2 g-1, much higher than those of pure PCNs (381 m2 g-1) and CNFs (510 m2 g-1). As a consequence, the PCN/CNF composite displays high specific capacitance of 261 F g-1, excellent rate capability and outstanding cycling stability (97.6% of capacitance retention after 10000 cycles). Moreover, the assembled symmetric supercapacitor with PCN/CNF electrodes delivers an ultrahigh energy density of 20.4 Wh kg-1 and outstanding cycling life (94.8% capacitance retention after 10000 cycles) in an aqueous electrolyte.

  16. Synthesis and DFT Study of a Diphenylsilanone-Bridged Dimolybdenum Complex.

    Science.gov (United States)

    Alvarez, M Angeles; García, M Esther; García-Vivó, Daniel; Menéndez, Sonia; Ruiz, Miguel A

    2016-06-20

    Reaction of the 30-electron benzylidyne complex [Mo2 Cp2 (μ-CPh)(μ-PCy2 )(μ-CO)] with excess Ph2 SiH2 under visible-UV irradiation yields the silylene-bridged complex [Mo2 Cp2 (μ-CPh)(μ-PCy2 )(μ-SiPh2 )]. This compound undergoes selective oxidation with O2 to give the unsaturated complex [Mo2 Cp2 (μ-CPh)(μ-PCy2 )(μ-κ(1) :κ(1) -OSiPh2 )], which contains an unprecedented bridging diphenylsilanone ligand, as confirmed by X-ray diffraction analysis and DFT calculations. The bonding within the central Mo2 SiO ring of this complex approaches the extreme description of a dimetallacyclosiloxane according to the relevant solid-state bond lengths and theoretical calculations.

  17. Synthesis Array Topology Metrics in Location Characterization

    Science.gov (United States)

    Shanmugha Sundaram, GA

    2015-08-01

    Towards addressing some of the fundamental mysteries in physics at the micro- and macro-cosm level, that form the Key Science Projects (KSPs) for the Square Kilometer Array (SKA; such as Probing the Dark Ages and the Epoch of Reionization in the course of an Evolving Universe; Galaxy Evolution, Cosmology, and Dark Energy; and the Origin and evolution of Cosmic Magnetism) a suitable interfacing of these goals has to be achieved with its optimally designed array configuration, by means of a critical evaluation of the radio imagingcapabilities and metrics. Of the two forerunner sites, viz. Australia and South Africa, where pioneering advancements to state-of-the-art in synthesis array radio astronomy instrumentation are being attempted in the form of pathfinders to the SKA, for its eventual deployment, a diversity of site-dependent topology and design metrics exists. Here, the particular discussion involves those KSPs that relate to galactic morphology and evolution, and explores their suitability as a scientific research goal from the prespective of the location-driven instrument design specification. Relative merits and adaptability with regard to either site shall be presented from invoking well-founded and established array-design and optimization principles designed into a customized software tool.

  18. Synthesis and Characterization of Boehmite Nanofibers

    Directory of Open Access Journals (Sweden)

    Jing Yang

    2008-01-01

    Full Text Available Boehmite nanofibers of high quality were synthesized through a wet-gel conversion process without the use of a surfactant. The long nanofibers of boehmite with clear-cut edges were obtained by steaming the wet-gel precipitate at 170∘C for 2 days. Analytical techniques such as X-ray diffraction (XRD, scanning electron microscopy (SEM, infrared emission spectroscopy (IES, as well as Raman spectroscopy were used to characterize the products.

  19. Dynamic characterization and damage detection in the I-40 bridge over the Rio Grande

    Energy Technology Data Exchange (ETDEWEB)

    Farrar, C.R.; Baker, W.E.; Bell, T.M.; Cone, K.M.; Darling, T.W.; Duffey, T.A.; Eklund, A.; Migliori, A.

    1994-06-01

    In the 1960`s and 1970`s over 2500 bridges were built in the U.S. with a design similar to those on Interstate 40 over the Rio Grande in Albuquerque, New Mexico. These bridges were built without structural redundancy and typically have only two plate girders carrying the entire dead and live loads. Failure of either girder is assumed to produce catastrophic failure of the bridge, hence these bridges are referred to as fracture-critical bridges. The Federal Highway Administration (FHWA) and the National Science Foundation (NSF) have provided funds to New Mexico State University (NMSU) through the New Mexico State Highway and Transportation Department (NMSH&TD) and The Alliance For Transportation Research (ATR) for evaluation and testing of the existing fracture critical bridges over the Rio Grande. Because the 1-40 bridges over the Rio Grande were to be razed during the summer of 1993, the investigators were able to introduce simulated fatigue cracks, similar to those observed in the field, into the structure in order to test various damage identification methods and to observe the changes in load paths through the structure caused by the cracking. To support this research effort, NMSU contracted Los Alamos National Laboratory (LANL) to perform experimental modal analyses, and to develop experimentally verified numerical models of the bridge. Scientists from the LANL`s Condensed Matter and Thermal Physics Group (P-10) applied state-of-the-art sensors and data acquisition software to the modal tests. Engineers from the LANL`s Advanced Engineering Technology Group (MEE-13) conducted ambient and forced vibration tests to verify detailed and simplified finite element models of the bridge. Forced vibration testing was done in conjunction with engineers from Sandia National Laboratory (SNL) who provided and operated a hydraulic shaker.

  20. Synthesis and characterization of novel adsorbent fibers

    Science.gov (United States)

    Benak, Kelly Rene

    This thesis is devoted to the design and development of three novel fibrous systems where the unique properties of commercially available activated carbon fibers (ACFs) were used as a foundation. In the first system, sulfonated pyropolymeric fibers derived from phenol-formaldehyde resins serve as cationic exchangers. This system was characterized through elemental analysis (EA), diffuse reflectance infrared fourier transform spectroscopy, thermal gravimetric analysis, and nitrogen/carbon dioxide adsorption. Their performance as efficient ion exchange systems was evaluated through pressure drop, capacity and dynamic mode kinetic measurements. Total ion exchange capacities up to 19.5 meq/g were measured for the fibers with pressure drops less than half that of beads over a wide range of flow rates. The second system utilizes the activated carbon fiber as a template to prepare a high surface area zirconia fiber. Simultaneous differential thermal analysis/thermal gravimetric analysis, optical and scanning electron microscopy, X-ray diffraction, EA, and nitrogen adsorption were used to characterize the inorganic cloths. The information obtained provided fundamental materials properties used in the optimization of the inorganic fibers. The fibers possess surface areas of up to 101 m 2/g at 800°C. The final system took advantage of the ability to chemically modify an ACF surface to enhance the gas separation capability. The equilibrium adsorption of carbon dioxide and methane at standard temperature and pressure was used to calculate selectivity coefficients and thus measure the fiber's capacity to effectively separate the two gases. They were further characterized through EA and surface area. The separation coefficients obtained were compared against values reported in the literature for pillared clays, zeolites, and carbon molecular sieves. The chemically modified fibers exhibit selectivity factors as high as 4.03, which is better than values reported for pillared

  1. PLLA-HA composites: Synthesis and characterization

    Science.gov (United States)

    Gonzalez, Gema; Albano, Carmen; Palacios, Jordana

    2012-07-01

    A composite based on PLLA -HA was prepared by the solvent casting technique and characterized. An interaction between the polymer matrix and HA through the carbonyl and phosphate groups was obtained by FTIR . The several thermal transitions of PLLA were evaluated by DSC: the glass transition, crystallization, cold crystallization, melt-recrystallization and melting. The addition of HA to PLLA matrix increases its glass transition temperature and no major changes on the melting temperature and crystallinity were observed. The PLLA-HA composite showed better thermal stability than the neat polymer. The introduction of the nano-HA particles increased the decomposition temperature and the activation energy retarding the decomposition process.

  2. SYNTHESIS AND CHARACTERIZATION OF FULLY SOLUBLE POLYPHENYLENEVINYLENE

    Institute of Scientific and Technical Information of China (English)

    Jiang-qing Pan; Zi-kuan Chen; Yang Xiao; Wei Huang

    2000-01-01

    Fully soluble poly[2-methoxy-5-(2'-ethylhexyl)-oxy)-p-phenylenevinylene] (MEH-PPV) was synthesized by the addition of molecular weight modifiers (chain stopper, free radical scavengers) to a polymerization system containing monomer, catalyst and a solvent. These PPV products synthesized in this work were characterized by IR, NMR, UV-visible spectroscopy and GPC. Results show that the Mw of polyphenylvinylene (PPV) can be controlled by the addition of chain stopper (benzyl bromide) and radical inhibitor (2,6-di-tert-butyl-4-methyl phenol). The polymerization mechanism in the presence of these additives was also discussed. A dual mechanism involving carbene for PPV polymerization was proposed.

  3. Synthesis and Characterization of Glassy Carbon Nanowires

    Directory of Open Access Journals (Sweden)

    C. M. Lentz

    2011-01-01

    Full Text Available The advent of carbon-based micro- and nanoelectromechanical systems has revived the interest in glassy carbon, whose properties are relatively unknown at lower dimensions. In this paper, electrical conductivity of individual glassy carbon nanowires was measured as a function of microstructure (controlled by heat treatment temperature and ambient temperature. The semiconducting nanowires with average diameter of 150 nm were synthesized from polyfurfuryl alcohol precursors and characterized using transmission electron and Raman microscopy. DC electrical measurements made at 90 K to 450 K show very strong dependence of temperature, following mixed modes of activation energy and hopping-based conduction.

  4. Synthesis and Characterization of Electrodeposited Nanocrystalline Nickel

    Institute of Scientific and Technical Information of China (English)

    DAI Pin-qiang; YU Hui, LI Qiang

    2004-01-01

    Nanocrystalline nickel was synthesize d by direct current electrodeposition from a modified Watts-type bath. X-ray diffraction and transmission electron microscope were used to characterize the microstructure of nickel deposits. The results show that nanocrytalline nickel with grain sizes in the range 20~50nm can be synthesized from saccharin-containing Watts-type baths with current density range 5~30A/dm2. There existed preferred orientation in the deposits and it changed progressively from a (200) fibre texture to a (111) (200) double fibre texture as saccharin concentration increased. The hardness of the deposits increased prominently as grain size decreased to nanometer range.

  5. Synthesis and Characterization of Electrodeposited Nanocrystalline Nickel

    Institute of Scientific and Technical Information of China (English)

    DAIPin-qiang; YUHui; LIQiang

    2004-01-01

    Nanocrystalline nickel was synthesized by direct current electrodeposition from a modified Watts-type bath. X-ray diffraction and transmission electron microscope were used to characterize the microstructure of nickel deposits. The results show that nanocrytalline nickel with grain sizes in the range 20-50nm can be synthesized from saccharin-containing Watts-type baths with current density range 5-30A/dm2. There existed preferred orientation in the deposits and it changed progressively from a (200) fibre texture to a (111) (200) double fibre texture as saccharin concentration increased. The hardness of the deposits increased prominently as grain size decreased to nanometer range.

  6. Synthesis and characterization of Co nanoparticles

    Science.gov (United States)

    Singh, J.; Tripathi1, J.; Kaurav, N.

    2017-05-01

    Nanoparticles of Cobalt (Co) have attracted great interest in recent years because of their unique physical and optical properties that are of industrial importance. To understand their basic properties, Co nanoparticles were synthesized by Polyol method using Cobalt acetate and ethylene glycol in the presence of some pellets of sodium hydroxide. The synthesized powder was characterized X-ray diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FTIR). The average particle size and lattice parameter estimated by XRD were found to be ˜37.3 nm and 3.1653 Å respectively. The results suggest suitability of these nanoparticles as dopants in other materials such as polymer materials and oxides.

  7. PdCo/Pd-Hexacyanocobaltate Hybrid Nanoflowers: Cyanogel-Bridged One-Pot Synthesis and Their Enhanced Catalytic Performance.

    Science.gov (United States)

    Liu, Zhen-Yuan; Fu, Geng-Tao; Zhang, Lu; Yang, Xiao-Yu; Liu, Zhen-Qi; Sun, Dong-Mei; Xu, Lin; Tang, Ya-Wen

    2016-08-30

    Elaborate architectural manipulation of nanohybrids with multi-components into controllable 3D hierarchical structures is of great significance for both fundamental scientific interest and realization of various functionalities, yet remains a great challenge because different materials with distinct physical/chemical properties could hardly be incorporated simultaneously into the synthesis process. Here, we develop a novel one-pot cyanogel-bridged synthetic approach for the generation of 3D flower-like metal/Prussian blue analogue nanohybrids, namely PdCo/Pd-hexacyanocobaltate for the first time. The judicious introduction of polyethylene glycol (PEG) and the formation of cyanogel are prerequisite for the successful fabrication of such fascinating hierarchical nanostructures. Due to the unique 3D hierarchical structure and the synergistic effect between hybrid components, the as-prepared hybrid nanoflowers exhibit a remarkable catalytic activity and durability toward the reduction of Rhodamine B (RhB) by NaBH4. We expect that the obtained hybrid nanoflowers may hold great promises in water remediation field and beyond. Furthermore, the facile synthetic strategy presented here for synthesizing functional hybrid materials can be extendable for the synthesis of various functional hybrid nanomaterials owing to its versatility and feasibility.

  8. PdCo/Pd-Hexacyanocobaltate Hybrid Nanoflowers: Cyanogel-Bridged One-Pot Synthesis and Their Enhanced Catalytic Performance

    Science.gov (United States)

    Liu, Zhen-Yuan; Fu, Geng-Tao; Zhang, Lu; Yang, Xiao-Yu; Liu, Zhen-Qi; Sun, Dong-Mei; Xu, Lin; Tang, Ya-Wen

    2016-08-01

    Elaborate architectural manipulation of nanohybrids with multi-components into controllable 3D hierarchical structures is of great significance for both fundamental scientific interest and realization of various functionalities, yet remains a great challenge because different materials with distinct physical/chemical properties could hardly be incorporated simultaneously into the synthesis process. Here, we develop a novel one-pot cyanogel-bridged synthetic approach for the generation of 3D flower-like metal/Prussian blue analogue nanohybrids, namely PdCo/Pd-hexacyanocobaltate for the first time. The judicious introduction of polyethylene glycol (PEG) and the formation of cyanogel are prerequisite for the successful fabrication of such fascinating hierarchical nanostructures. Due to the unique 3D hierarchical structure and the synergistic effect between hybrid components, the as-prepared hybrid nanoflowers exhibit a remarkable catalytic activity and durability toward the reduction of Rhodamine B (RhB) by NaBH4. We expect that the obtained hybrid nanoflowers may hold great promises in water remediation field and beyond. Furthermore, the facile synthetic strategy presented here for synthesizing functional hybrid materials can be extendable for the synthesis of various functional hybrid nanomaterials owing to its versatility and feasibility.

  9. Recombinant expression, functional characterization of two scorpion venom toxins with three disulfide bridges from the Chinese scorpion Buthus martensii Karsch.

    Science.gov (United States)

    Lin, ShengGuo; Wang, XueLin; Hu, XueYao; Zhao, YongShan; Zhao, MingYi; Zhang, JingHai; Cui, Yong

    2017-01-17

    Scorpion venom contains a large variety of biologically active peptides. However, most of these peptides have not been identified and characterized. Peptides with three disulfide bridges, existing in the scorpion venom, have not been studied in detail and have been poorly characterized until now. Here, we report the recombinant expression and functional characterization of two kinds of venom peptides (BmKBTx and BmNaL-3SS2) with three disulfide bridges. This study adopted an effective E. coli system. The genes for BmKBTx and BmNaL-3SS2 were obtained by the Polymerase Chain Reaction method and finally cloned to the pSYPU-1b vector. After expression and purification, the two recombinant proteins underwent an analgesic activity assay in mice and whole-cell patch-clamp recording of hNav1.7-CHO cell lines. Functional tests showed that BmKBTx and BmNaL-3SS2 have analgesic activity in mice and can interact with the hNav1.7 subtype of the voltage-gated sodium channel (VGSC). Scorpion venom is rich in bioactive proteins, but most of their functions are unknown to us. This study has increased our knowledge of these novel disulfide-bridged peptides (DBPs) and their biological activities.

  10. Synthesis, characterization and optical properties of nanoparticles

    Science.gov (United States)

    Li, Shoutian

    ZnO, Si, silica, Ge, Ga oxide, W oxide and Mo oxide nanoparticles have been synthesized and characterized, and their optical properties have been investigated. These particles were synthesized by a Laser Vaporization and Controlled Condensation (LVCC) technique in a modified diffusion cloud chamber. The particles deposited on smooth substrates reveal highly organized web-like structures with uniform micrometer size pores. The effect of solvents on the web-like structures was also investigated. ZnO nanoparticles were also prepared by wet chemical methods such as the reversed micelle and sol solutions technique. The photoluminescence quantum yield is enhanced 10 times once the surfaces of the ZnO nanoparticles are coated with a layer of stearate molecules. Many techniques have been used to characterize the nanoparticles. SEM gives information about particle size and morphology; X-ray diffraction and Raman spectroscopy determine the crystallinity and crystal structure; XPS and FTIR reveal the surface chemical composition; UV-vis spectroscopy and photoluminescence measurements characterize the optical properties of nanoparticles. Silica nanoparticles, prepared in an amorphous phase, show bright blue photoluminescence upon irradiation with UV light, but the luminescence has a very short lifetime (less than 20 ns). Si nanoparticles, with a diamond-like crystal phase, acquire oxidized-surfaces on exposure to air. The surface-oxidized Si nanocrystals show a short- lived blue emission characteristic of the SiO2 coating and a longer-lived red emission at room temperature. The lifetime of the red emission depends on the emission wavelength. Some substituted benzene molecules and tungsten oxide nanoparticles can quench the red photoluminescence of the Si nanocrystals. Tungsten oxide and molybdenum oxide nanoparticles show photochromic properties: they change color to blue when irradiated. The photons drive a transition from one chemical state to another. The color change of

  11. Synthesis and characterization of tetraethylammonium tetrachlorocobaltate crystals

    Indian Academy of Sciences (India)

    M A Kandhaswamy; V Srinivasan

    2002-02-01

    Single crystals of tetraethylammonium tetrachlorocobaltate were grown by solution method and characterized through single crystal X-ray diffraction, thermogravimetric analysis (TGA), differential scanning calorimetric studies (DSC) and infrared spectroscopic technique (IR). The crystals were bright, transparent and blue coloured. The unit cell parameters were found to be = = 9.0363 Å and = 14.9879 Å and = = = 90°, showing tetragonal lattice from the XRD data. Thermogravimetric analysis showed a loss of weight at 683 K from which the decomposition reaction was formulated. Thermal anomalies were found for this crystal at temperatures 200 K, 220 K in the cooling cycle and at temperatures 200 K, 240 K in the heating cycle, respectively which showed that this crystal was associated with first order phase transition. All the vibrational frequencies corresponding to (TEA)+ ions and CoCl$^{2-}_4$ ions were assigned from the IR spectral data of this crystal.

  12. Synthesis and Electroluminescence Characterization of Cadmium Complex

    Directory of Open Access Journals (Sweden)

    Rahulkumar

    2011-01-01

    Full Text Available We have synthesized and characterized a new electroluminescence material,Cadmium [(2-(2-hydroxyphenylbenzoxazole(8-hydoxyquinoline] Cd(HPBq. The absorption spectra of this material show maxima at 378 nm. It may be attributed due to π° – π* transition. The photoluminescence showed peak at 520 nm. TGA data of the material shows stability up to 370 °C .Organic light emitting diode have been fabricated with this material and the fundamental structures of the device is ITO/α-NPD/ Cd(HPBq/BCP/Alq3/LiF/Al exhibited a luminescence peak at 550 nm. The maximum luminescence of the device was 295 cd/m2 with current density of 6687 A/m2 at 20 V. The maximum current efficiency of OLED was 1.01 cd/A at 17 V and power efficiency was 1.01 lm/w at 17 V.

  13. Organic nanomaterials: synthesis, characterization, and device applications

    CERN Document Server

    Torres, Tomas

    2013-01-01

    Recent developments in nanoscience and nanotechnology have given rise to a new generation of functional organic nanomaterials with controlled morphology and well-defined properties, which enable a broad range of useful applications. This book explores some of the most important of these organic nanomaterials, describing how they are synthesized and characterized. Moreover, the book explains how researchers have incorporated organic nanomaterials into devices for real-world applications.Featuring contributions from an international team of leading nanoscientists, Organic Nanomaterials is divided into five parts:Part One introduces the fundamentals of nanomaterials and self-assembled nanostructuresPart Two examines carbon nanostructures—from fullerenes to carbon nanotubes to graphene—reporting on properties, theoretical studies, and applicationsPart Three investigates key aspects of some inorganic materials, self-assembled monolayers,...

  14. Synthesis and characterization of carbonate hydroxyapatite.

    Science.gov (United States)

    Merry, J C; Gibson, I R; Best, S M; Bonfield, W

    1998-12-01

    Substituted apatite ceramics are of clinical interest as they offer the potential to improve the bioactive properties of implants. Carbonate hydroxyapatite (CHA) has been synthesized by an aqueous precipitation method and precipitates with two different levels of carbonate, processed as powders. Sintering experiments were performed to establish the influence of carbonate in significantly reducing the temperature required to prepare high-density ceramics when compared with stoichiometric hydroxyapatite (HA). High-temperature X-ray diffraction was used to characterize the phase stability of the apatites on sintering. Increasing carbonate content was shown to reduce the temperature at which decomposition occurred, to phases of CaO and beta-TCP. Mechanical testing, performed using biaxial flexure, showed that the CHA specimens had strengths similar to stoichiometric HA. Copyright 1998 Kluwer Academic Publishers

  15. Synthesis and characterization of mesoporous hydrocracking catalysts

    Science.gov (United States)

    Munir, D.; Usman, M. R.

    2016-08-01

    Mesoporous catalysts have shown great prospective for catalytic reactions due to their high surface area that aids better distribution of impregnated metal. They have been found to contain more adsorption sites and controlled pore diameter. Hydrocracking, in the presence of mesoporous catalyst is considered more efficient and higher conversion of larger molecules is observed as compared to the cracking reactions in smaller microporous cavities of traditional zeolites. In the present study, a number of silica-alumina based mesoporous catalysts are synthesized in the laboratory. The concentration and type of surfactants and quantities of silica and alumina sources are the variables studied in the preparation of catalyst supports. The supports prepared are well characterized using SEM, EDX, and N2-BET techniques. Finally, the catalysts are tested in a high pressure autoclave reactor to study the activity and selectivity of the catalysts for the hydrocracking of a model mixture of plastics comprising of LDPE, HDPE, PP, and PS.

  16. SYNTHESIS, CHARACTERIZATION AND BIOLOGICAL ACTIVITY OF POLYKETONES

    Institute of Scientific and Technical Information of China (English)

    Ismail A.Alkskas; Altaher M.Alhubge; Faizul Azam

    2013-01-01

    Polyketone resins have been prepared by the Friedel-Crafts polymerization of dithiophenylidenecyclopentanone (Ⅰ),dithiophenylidenecyclohexanone (Ⅱ) and dithiophenylideneacetone (Ⅲ) with adipoyl,sebacoyl and terephthaloyl dichlorides using boron trifluoride as catalyst and carbon disulphide as solvent.Polymers were characterized with IR,1H-NMR,and the results showed the presence of carbonyl of ketonic groups in the main chain.The polyketones have inherent viscosities of 0.40-0.70 dL/g.All the polymers are semicrystalline and most of them are partially soluble in most common organic solvents but freely soluble in aprotic solvents.The temperatures of 50% weight loss are as high as 185℃ to 280℃ in air,indicating that these aromatic polyketones have excellent thermal stability.All the polyketones were tested for their antimicrobial activity against bacteria and fungi.

  17. Synthesis and characterization of sodium alkoxides

    Indian Academy of Sciences (India)

    K Chandran; R Nithya; K Sankaran; A Gopalan; V Ganesan

    2006-04-01

    Alcohol route is being adopted for cleaning sodium from sodium-wetted small components of coolant circuits of fast reactors. For better understanding of sodium–alcohol reactions and their energetics, the data on thermo-chemical properties such as heats of sodium–alcohol reactions, heats of dissolution, heat capacities, thermal decomposition behaviour, etc of their end products are essential. In order to generate such data, high purity sodium alkoxides, viz. sodium methoxide, sodium ethoxide and sodium -propoxide, were prepared by reacting sodium metal with respective alcohol. These compounds were characterized using X-ray diffraction technique and IR spectroscopy. The elemental analysis was carried out by CHNS analyser and atomic emission spectroscopy. Normal chain sodium alkoxides were found to exhibit tetragonal crystal structure. Crystal structures of sodium ethoxide and sodium -propoxide are reported for the first time. The IR spectrum of sodium -propoxide is also reported for the first time.

  18. Synthesis and Characterization of Bimodal Mesoporous Silica

    Institute of Scientific and Technical Information of China (English)

    ZHANG Xiaofang; GUO Cuili; WANG Xiaoli; WU Yuanyuan

    2012-01-01

    Mesoporous silica with controllable bimodal pore size distribution was synthesized with cetyltrimethylammonium bromide (CTAB) as chemical template for small mesopores and silica gel as physical template for large mesopores.The structure of synthesized samples were characterized by Fourier transform infrared (FT-IR) spectroscopy,X-ray diffraction (XRD),scanning electron microscopy (SEM),transmission electron microscopy (TEM) and N2 adsorption-desorption measurements.The experimental results show that bimodal mesoporous silica consists of small mesopores of about 3 nm and large mesopores of about 45 nm.The small mesopores which were formed on the external surface and pore walls of the silica gel had similar characters with those of MCM-41,while large mesopores were inherited from parent silica gel material.The pore size distribution of the synthesized silica can be adjusted by changing the relative content of TEOS and silica gel or the feeding sequence of silica gel and NH4OH.

  19. Synthesis and electrochemical characterization of substituted indolizine carboxylates

    Directory of Open Access Journals (Sweden)

    Soare Maria-Laura

    2013-01-01

    Full Text Available This work is devoted to the synthesis and characterization of new indolizine derivatives. Particular attention was paid to the electrochemical investigations by cyclic voltammetry and differential pulse voltammetry. The redox processes for each compound were established, analyzed and assessed to the particular functional groups at which they take place. This assessment was based on detailed comparison between the electrochemical behaviour of the compounds, similarities in their structure, as well as substituent effects.

  20. Diradicals acting through diamagnetic phenylene vinylene bridges: Raman spectroscopy as a probe to characterize spin delocalization

    Energy Technology Data Exchange (ETDEWEB)

    González, Sandra Rodríguez; Nieto-Ortega, Belén; González Cano, Rafael C.; López Navarrete, Juan T., E-mail: vecianaj@icmab.es, E-mail: teodomiro@uma.es, E-mail: casado@uma.es; Casado, Juan, E-mail: vecianaj@icmab.es, E-mail: teodomiro@uma.es, E-mail: casado@uma.es [Department of Physical Chemistry, University of Málaga, Campus de Teatinos s/n, Málaga 29071 (Spain); Lloveras, Vega; Vidal-Gancedo, José; Rovira, Concepció; Veciana, Jaume, E-mail: vecianaj@icmab.es, E-mail: teodomiro@uma.es, E-mail: casado@uma.es [Department of Molecular Nanoscience and Organic Materials, Institut de Ciència de Materials de Barcelona (CSIC), Campus Universitari de Bellaterra, E-08193 Cerdanyola, Barcelona (Spain); NANOMOL group, Networking Research Center on Bioengineering, Biomaterials and Nanomedicine (CIBER-BBN), Campus Universitari de Bellaterra, E-08193 Cerdanyola, Barcelona (Spain); Novoa, Juan J.; Mota, Fernando [Dpt. de Química Física and IQTCUB, Fac. Química, Univ. de Barcelona, Av. Diagonal, 647, 08028-Barcelona (Spain); Corro, Elena del; Taravillo, Mercedes; Baonza, Valentín G. [MALTA-Consolider Team, Department of Physical Chemistry, University Complutense of Madrid, Madrid 28040 (Spain)

    2014-04-28

    We present a complete Raman spectroscopic study in two structurally well-defined diradical species of different lengths incorporating oligo p-phenylene vinylene bridges between two polychlorinated triphenylmethyl radical units, a disposition that allows sizeable conjugation between the two radicals through and with the bridge. The spectroscopic data are interpreted and supported by quantum chemical calculations. We focus the attention on the Raman frequency changes, interpretable in terms of: (i) bridge length (conjugation length); (ii) bridge conformational structure; and (iii) electronic coupling between the terminal radical units with the bridge and through the bridge, which could delineate through-bond spin polarization, or spin delocalization. These items are addressed by using the “oligomer approach” in conjunction with pressure and temperature dependent Raman spectroscopic data. In summary, we have attempted to translate the well-known strategy to study the electron (charge) structure of π−conjugated molecules by Raman spectroscopy to the case of electron (spin) interactions via the spin delocalization mechanism.

  1. Subsurface soil characterization using geoelectrical and geotechnical investigations at a bridge site in Uttarakhand Himalayan region

    Science.gov (United States)

    Devi, Anita; Israil, M.; Anbalagan, R.; Gupta, Pravin K.

    2017-09-01

    Geoelectrical characterization of subsurface soil has been done at a bridge foundation site on the banks of Bhagirathi River at Tehri reservoir site, Uttarakhand, India. For this purpose, the Electrical Resistivity Tomography (ERT) and the Standard Penetration Test (SPT) data, recorded at both banks of Bhagirathi River are analyzed. A total of six ERT profiles, recorded on both the West and East banks, were interpreted to determine an electrical resistivity image showing the resistivity variations with depth. The borehole data and geological inputs were used for lithological correlation and calibration of the resistivity values to the subsurface formation. Subsequently the electrical parameter (resistivity) for different subsurface lithological units has been inferred. Further, at selected points, the electrical resistivity sounding data, derived from the ERT, have been correlated with the Standard Penetration Test (SPT) data. This correlation results from the fact that in the subsurface soil both the electrical resistivity variations and the soil strength measured by SPT are controlled by the soil properties: grain size distribution, compactness, porosity and water saturation. It has been observed that the N-values smaller than 16 are unreliable and inconsistent. In the River Borne Material (RBM) on the West Bank it is due to the presence of coarse gravels while on the East Bank it is due to the boulders. The N-values greater than 16 mainly correspond to the weathered rock formation. For these values, there exists a linear relationship between N-values and resistivity with a correlation coefficient greater than 0.80. The coefficients of linear relationship at the two banks vary due to varying amount of clay content. Such a relationship is important for any site in tough Himalayan terrain because it can be used as an alternative to the SPT for determining soil strength parameters from ERT.

  2. Synthesis and characterization of thermoplastic polyphenoxyquinoxalines

    Science.gov (United States)

    Erdem, Haci Bayram

    This research was divided into two main parts. In the first part, a new facile route to relatively inexpensive thermoplastic polyphenoxyquinoxalines was developed. The synthetic route involves the aromatic nucleophilic substitution reaction of bisphenols with 2,3-dichloroquinoxaline. The dichloro monomer was prepared in two steps. In the first step, oxalic acid was condensed with o-phenylenediamine to give 2,3-dihydroxyquinoxaline. In the second step, 2,3-dihydroxyquinoxaline was treated with thionyl chloride to give 2,3-dichloroquinoxaline. This monomer was successfully polymerized with bisphenol-A, bisphenol-S, hexafluorobisphenol-A and 9,9-bis(4-hydroxyphenyl)fluorenone. Hydroquinone and biphenol, however, can not be polymerized to high molecular weight polymers because of the premature precipitation of crystalline oligomers. The glass transition temperatures of the high molecular weight polymers prepared from a series of bisphenols range from 191 °C to 279 °C, and their thermal decomposition temperatures are around 500 °C. The polymers are soluble in a wide range of solvents and can be solution-cast into thin films that are colorless and transparent. The polymers have tensile strengths ranging from 61 to 107 MPa, and tensile moduli ranging from 3.5 to 2.3 GPa. The synthesis of polymer obtained from 2,3-dichloroquinoxaline and bisphenol-A was scaled up to afford 500 g of material. This polymer is a thermoplastic with a melt-viscosity less than 1000 Pa.s. at 300 °C. The notched Izod impact strength of injection-molded samples of this polymer is 40.7 J/m. In the second part of this research, the synthetic method has been modified to allow the preparation of quinoxaline containing polyimides. Thus, 2,3-dichloroquinoxaline was treated either with p-nitrophenol followed by reduction of nitro groups, or with p-aminophenols to directly obtain the desired 2,3-(4-aminophenoxy)quinoxaline. This diamine was polymerized with 3,3',4,4'-biphenyldianhydride, 4

  3. Synthesis and photochromic behavior of mono-,and biphotochromic system linked by p-phenylene bridge

    Institute of Scientific and Technical Information of China (English)

    N.O.Mahmoodi; K.Tabatabaeian; A.Ghavidast

    2010-01-01

    The synthesis of mono- and bis-1,3-diazabicyclo[3.1.0]hex-3-ene derivatives with indole ring and p-phenylene spacer,which behave as photochromic materials,is reported.The structure-photochromic behavior relationship (SPBR) of the synthesized compounds has been analyzed.

  4. Hydrothermal Synthesis, Characterization, and Visible Light-Driven Photocatalytic Properties of Bi2WO6 Nanoplates

    Directory of Open Access Journals (Sweden)

    Anukorn Phuruangrat

    2014-01-01

    Full Text Available In this research, the effects on reaction temperature and length of time on Bi2WO6 nanoplates by hydrothermal synthesis on morphologies and photocatalytic properties were studied. The products obtained at different reaction temperature and reaction time were characterized by XRD, Raman, FTIR, SEM, and TEM techniques. The photocatalytic properties of the samples were measured by decomposing the rhodamine-B organic dye. XRD pattern was specified as pure orthorhombic well-crystallized Bi2WO6 phase for the 180°C and 20 h synthesis. Its FTIR spectrum shows main absorption bands at 400–1000 cm−1, assigned to Bi–O stretching, W–O stretching, and W–O–W bridging stretching modes. SEM and TEM analyses show that the product was composed of nanoplates. Photocatalytic activity of Bi2WO6 nanoplates shows the 98.24% degradation of rhodamine-B under the Xe light irradiation within 100 min.

  5. Polypeptide Grafted Hyaluronan: Synthesis and Characterization

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Xiaojun [ORNL; Messman, Jamie M [ORNL; Mays, Jimmy [ORNL; Baskaran, Durairaj [University of Tennessee, Knoxville (UTK)

    2010-01-01

    Poly(L-leucine) grafted hyaluronan (HA-g-PLeu) has been synthesized via a Michael addition reaction between primary amine terminated poly(L-leucine) and acrylate-functionalized HA (TBAHA-acrylate). The precursor hyaluronan was first functionalized with acrylate groups by reaction with acryloyl chloride in the presence of triethylamine in N,N-dimethylformamide. 1H NMR analysis of the resulting product indicated that an increase in the concentration of acryloylchoride with respect to hydroxyl groups on HA has only a moderate effect on functionalization efficiency, f. A precise control of stoichiometry was not achieved, which could be attributed to partial solubility of intermolecular aggregates and the hygroscopic nature of HA. Michael addition at high [PLeu- NH2]/[acrylate]TBAHA ratios gave a molar grafting ratio of only 0.20 with respect to the repeat unit of HA, indicating grafting limitation due to insolubility of the grafted HA-g-PLeu. Soluble HA-g-PLeu graft copolymers were obtained for low grafting ratios (<0.039) with <8.6% by mass of PLeu and were characterized thoroughly using light scattering, 1H NMR, FT-IR, and AFM techniques. Light scattering experiments showed a strong hydrophobic interaction between PLeu chains, resulting in aggregates with segregated nongrafted HA segments. This yields local networks of aggregates, as demonstrated by atomic force microscopy. Circular dichroism spectroscopy showed a -sheet conformation for aggregates of poly(L-leucine).

  6. Synthesis and characterization of organosoluble aromatic copolyimids

    Institute of Scientific and Technical Information of China (English)

    YANG Jintian; HUANG Wei; ZHOU Yongfeng; YAN Deyue

    2007-01-01

    A series of aromatic copolyimides was success fully synthesized from the commercial pyromellitic dianhy dride (PMDA) with a commercial diamine p-phenyldiamine (PDA) and a diamine 4,4'-methylenebis-(2-tert-butylaniline)(MBTBA) specially designed by the authors.The copoly imides were characterized by Infra-red (IR),Nuclear Magnetic Resonance (NMR),Gel Permeation Chromato graphy (GPC),Ultraviolet Visual (UV-Vis),Thermogra vimetic Analysis (TGA) and Dynamic Mechanical Analysis (DMA).The copolyimide was precipitated in m-cresol in the polymerization process when the molar ratio of MBTBA and PDA was lower than 6/4.The number-average molecular weight of the soluble copolyimides measured by GPC was larger than 4.0 x 104,and the polydispersity index was higher than 1.5.Only one glass transition temperature of these copolyimdies was detected around 360℃ by DMA.The copolyimides did not show appreciable decomposition up to 500℃ under N2,and the thermal stability of the copolyimide increased a little with the introduction of PDA into the polyimide main chain.

  7. Synthesis and characterization of hematite nanopowders

    Science.gov (United States)

    Sharmila Justus, J.; Dharma Roy, S. Dawn; Ezhil Raj, A. Moses

    2016-10-01

    A facile solution approach was employed to synthesize hematite (α-Fe2O3) nanoparticles by using starting precursor iron (III) chloride (FeCl3) and sodium hydroxide (NaOH) as reducing agent without templates at low temperature. The growth and solubility of iron oxide particle was controlled by adjusting the pH of the solution using ammonium hydroxide. As-prepared powders were subsequently calcined in air for 3 h at three different temperatures ranging from 400 to 800 °C. The precursor and the synthesized particles were characterized using TGA-DTA thermal analysis to study the decomposition pattern. X-ray diffraction (XRD) technique confirmed the nanocrystal formation of α-Fe2O3 and Fourier transform infra-red (FTIR) spectral information identified the metal-oxide phase formation. Scanning electron microscope (SEM) was engaged to study the morphology and the purity of the sample was evaluated from the energy dispersive spectrum (EDS). The optical band gap of the particles and its variations with calcination temperature (2.32-2.49 eV) was obtained from the constructed Tauc plot using the optical absorption data. The electrical parameters of the samples were obtained from two probe measuring technique and the effect of temperature on the electrical properties of α-Fe2O3 was discussed.

  8. Synthesis and characterization of luminescence magnetic nanocomposite

    Energy Technology Data Exchange (ETDEWEB)

    Kiplagat, Ayabei [DST/Mintek Nanotechnology Innovation Centre, Department of Chemistry, University of the Western Cape, Private Bag X17, Bellville (South Africa); Onani, Martin O., E-mail: monani@uwc.ac.za [DST/Mintek Nanotechnology Innovation Centre, Department of Chemistry, University of the Western Cape, Private Bag X17, Bellville (South Africa); Meyer, Mervin [DST/Mintek Nanotechnology Innovation Centre, Department of Biotechnology, University of the Western Cape, Private Bag X17, Bellville (South Africa); Akenga, Teresa A. [Department of Chemistry, University of Eldoret, P.O. Box 1125, Eldoret (Kenya); Dejene, Francis B. [Department of Physics, University of the Free State, QwaQwa Campus, Private Bag X13, Phuthadithaba 9866 (South Africa)

    2016-01-01

    We report a new type of indium based quantum dots which were conjugated to the magnetic Fe{sub 2}O{sub 3} nanoparticles. They were characterized by photoluminescence (PL), high resolution transmission electron microscopy (HRTEM), superconducting quantum interference device (SQUID) and fourier transform infra-red (FTIR). The photoluminescence characteristics of the coupled and uncoupled indium based quantum dots were investigated to determine whether the fluorescing property could be retained in the bifunctional system. Generally, the PL intensity of the quantum dots was observed to reduce significantly and with huge red shift most probably due to quenching effects for the MNPs. The average size of the coupled nanoparticles were found to range between 4 and 5 nm for the quantum dots and range of 6–13 nm for the Fe{sub 2}O{sub 3} magnetic nanoparticles as revealed by both HRTEM and XRD. The highest magnetic saturation reached for both bare and functionalized magnetic nanoparticles was 68.58 emu/g. The FTIR data revealed that the postulated functional groups were actually present in both the bare and functionalized nanoparticles. For instance, Fe–O was observed at around 580 cm{sup −1}, O–H at 3432 cm{sup −1} and thiol group at 2929 cm{sup −1} for meso-2,3-dimercaptosuccinic acid capped Fe{sub 2}O{sub 3} magnetic nanoparticles. The energy dispersive spectroscopy (EDS) also confirmed that all the elements of the nanocomposite were actually present in the designed material.

  9. Synthesis, characterization, and applications of nanocomposite membranes

    Science.gov (United States)

    Kizilel, Riza

    In the present work polymer nanocomposites (PCN) derived from synthetic lithium hectorite clay (SLH) and polyethylene oxide (PEO) have been prepared and characterized for use as polymer electrolytes in lithium ion secondary batteries and as catalytic membranes for fuel cell applications. PCNs are prepared by intercalating polyethylene oxide in the clay layers of SLH. The resulting films are physically and electrochemically evaluated. In situ small-angle X-ray scattering (SAXS) studies have been conducted to monitor the structural changes of polymer nanocomposites upon heating. These nanocomposites are made of different mass ratios of PEO and SLH. On the basis of the in situ SAXS results, it was found that the polymer matrix losses its crystallinity at about 60°C and the composite is stable up to 150°C. Conductivity values, activation energies, and lithium transference numbers indicate that the PCNs are single ion conductors with transference numbers close to unity. The activation energies are in the range of 0.02 eV, two orders of magnitude higher than the conventional polymer electrolytes. A synthetic hectorite was also ion-exchanged with Pt(II) and suspended in a solution containing PEO for the fuel cell applications. The resulting membrane was subsequently reduced under H2 at 200°C for 2--3 hr. The final membrane contains Pt(0) at 2.4 wt% loading levels. XRD shows development of Pt(0) by the appearance of crystalline peaks upon reduction. A lineshape analysis using the Scherrer equation of the (220) peak shows Pt(0) particles of 3.8 nm or 7.5 nm depending upon processing conditions. These values are confirmed by TEM, and a high dispersion of the metal is evident. XRD and TGA confirm that PEO is stable to the processing conditions. In situ SAXS measurements of the reduction process were also performed. Under a reducing atmosphere, the shape of the scattering curves visually changes between 100--120°C. Analysis of the scattering curves using the general

  10. A maurotoxin with constrained standard disulfide bridging: innovative strategy of chemical synthesis, pharmacology, and docking on K+ channels.

    Science.gov (United States)

    M'Barek, Sarrah; Lopez-Gonzalez, Ignacio; Andreotti, Nicolas; di Luccio, Eric; Visan, Violeta; Grissmer, Stephan; Judge, Susan; El Ayeb, Mohamed; Darbon, Hervé; Rochat, Hervé; Sampieri, François; Béraud, Evelyne; Fajloun, Ziad; De Waard, Michel; Sabatier, Jean-Marc

    2003-08-15

    Maurotoxin (MTX) is a 34-residue toxin that has been isolated initially from the venom of the scorpion Scorpio maurus palmatus. It presents a large number of pharmacological targets, including small conductance Ca2+-activated and voltage-gated K+ channels. Contrary to other toxins of the alpha-KTx6 family (Pi1, Pi4, Pi7, and HsTx1), MTX exhibits a unique disulfide bridge organization of the type C1-C5, C2-C6, C3-C4, and C7-C8 (instead of the conventional C1-C5, C2-C6, C3-C7, and C4-C8, herein referred to as Pi1-like) that does not prevent its folding along the classic alpha/beta scaffold of scorpion toxins. Here, we developed an innovative strategy of chemical peptide synthesis to produce an MTX variant (MTXPi1) with a conventional pattern of disulfide bridging without any alteration of the toxin chemical structure. This strategy was used solely to address the impact of half-cystine pairings on MTX structural properties and pharmacology. The data indicate that MTXPi1 displays some marked changes in affinities toward the target K+ channels. Computed docking analyses using molecular models of both MTXPi1 and the various voltage-gated K+ channel subtypes (Shaker B, Kv1.2, and Kv1.3) were found to correlate with MTXPi1 pharmacology. A functional map detailing the interaction between MTXPi1 and Shaker B channel was generated in line with docking experiments.

  11. Flame synthesis and characterization of nanocrystalline titania powders

    Directory of Open Access Journals (Sweden)

    Bhaskaran Manjith Kumar

    2012-09-01

    Full Text Available Flame reactors are considered to be one of the most promising and versatile synthesis routes for the largescale production of submicron and nanosized particles. An annular co-flow type oxy-gas diffusion burner was designed for its application in a modular flame reactor for the synthesis of nanocrystalline oxide ceramics. The burner consisted of multiple ports for the individually regulated flow of a precursor vapour, inert gas, fuel gas and oxidizer. The nanopowders formed during flame synthesis in the reaction chamber were collected by a suitable set of filters. In the present study, TTIP was used as the precursor for the synthesis of nanocrystalline TiO2 and helium was used to carry the precursor vapour to the burner head. Methane and oxygen were used as fuel and oxidizer respectively. The operating conditions were varied by systematically changing the flow rates of the gases involved. The synthesized powders were characterized using standard techniques such as XRD, SEM, TEM, BET etc., in order to determine the crystallite size, phase content, morphology, particle size and degree of agglomeration. The influences of gas flow rates on the powder characteristics are discussed.

  12. Green synthesis of multi metal- citrate complexes and their characterization

    Science.gov (United States)

    Raju, Usha; Warkar, Sudhir G.; Kumar, Anil

    2017-04-01

    Four new multi metal-citrate complexes have been synthesized through green synthetic pathways. Their synthesis by hydrothermal route in the present research is decorated with features such as, a simple one pot synthesis, cost effectiveness, easy to scale up for commercial production, efficient synthesis conditions like mild temperature and shorter duration which further rules out the possibility of forming byproducts which may cause damage to the environment and being environmental benign as it eliminates the use and recovery of harmful organic solvents such as N, N- dimethyl formamide and N, N- diethyl formamide, used by the researchers in the past during the synthesis of similar metal- organic framework complexes. All four complexes are well defined crystalline materials with polynuclear multi metal-citrate framework having cubic crystal structure as indicated by their Powder X-ray Diffraction patterns. These complexes have been characterized by Fourier Transform Infrared Spectroscopy, Scanning Electron Microscopy, Energy Dispersive X-ray Spectroscopy, Thermogravimetric analysis and Powder XRD techniques.

  13. Bio-mediated synthesis, characterization and cytotoxicity of gold nanoparticles.

    Science.gov (United States)

    Klekotko, Magdalena; Matczyszyn, Katarzyna; Siednienko, Jakub; Olesiak-Banska, Joanna; Pawlik, Krzysztof; Samoc, Marek

    2015-11-21

    We report here a "green" approach for the synthesis of gold nanoparticles (GNPs) in which the Mentha piperita extract was applied for the bioreduction of chloroauric acid and the stabilization of the formed nanostructures. The obtained GNPs were characterized by UV-Vis absorption spectroscopy and transmission electron microscopy (TEM). The reduction of gold ions with the plant extract leads to the production of nanoparticles with various shapes (spherical, triangular and hexagonal) and sizes (from 10 to 300 nm). The kinetics of the reaction was monitored and various conditions of the synthesis were investigated. As a result, we established protocols optimized towards the synthesis of nanospheres and nanoprisms of gold. The cytotoxic effect of the obtained gold nanoparticles was studied by performing MTT assay, which showed lower cytotoxicity of the biosynthesized GNPs compared to gold nanorods synthesized using the usual seed-mediated growth. The results suggest that the synthesis using plant extracts may be a useful method to produce gold nanostructures for various biological and medical applications.

  14. Synthesis and Complexation Studies of Calix[4]crown Telomers Intermolecularly Bridged with Calixarene Segments

    Institute of Scientific and Technical Information of China (English)

    LI Haibing; TIAN Demei; CHEN Yuanyin; GAO Zhinong

    2009-01-01

    Three derivatived calix[4]crowns were condensed with calixarene segments: 2,6-bis(bromomethyl)-4-methyl-anisole (BBA) to afford their telomers TCA[4] in rational yields. The binding sites may complex metal ions or amino acids selectively. The telomers shows different metal ions selectivity in comparison with their monomers, which suggests that calixarene segment bridges play an important role in ion-binding. The liquid-liquid extraction experiment showed that telomer TCA[4]-Ⅲ was excellent receptor for zwitterionic a-amino acids and soft cations Ag+ and Pb2+. The extraction percentage of tryptophan and histidine was as high as 87.9% and 91.5%, respec-tively.

  15. Coinage metal complexes with bridging hybrid phosphine-NHC ligands: synthesis of di- and tetra-nuclear complexes.

    Science.gov (United States)

    Simler, Thomas; Braunstein, Pierre; Danopoulos, Andreas A

    2016-03-28

    A series of P-NHC-type hybrid ligands containing both PR2 and N-heterocyclic carbene (NHC) donors on meta-bis-substituted phenylene backbones, L(Cy), L(tBu) and L(Ph) (R = Cy, tBu, Ph, respectively), was accessed through a modular synthesis from a common precursor, and their coordination chemistry with coinage metals was explored and compared. Metallation of L(Ph)·n(HBr) (n = 1, 2) with Ag2O gave the pseudo-cubane [Ag4Br4(L(Ph))2], isostructural to [Ag4Br4(L(R))2] (R = Cy, tBu) (T. Simler, P. Braunstein and A. A. Danopoulos, Angew. Chem., Int. Ed., 2015, 54, 13691), whereas metallation of ·HBF4 (R = Ph, tBu) led to the dinuclear complexes [Ag2(L(R))2](BF4)2 which, in the solid state, feature heteroleptic Ag centres and a 'head-to-tail' (HT) arrangement of the bridging ligands. In solution, interconversion with the homoleptic 'head-to-head' (HH) isomers is facilitated by ligand fluxionality. 'Head-to-tail' [Cu2Br2(L(R))2] (R = Cy, tBu) dinuclear complexes were obtained from L(R)·HBr and [Cu5(Mes)5], Mes = 2,4,6-trimethylphenyl, which also feature bridging ligands and heteroleptic Cu centres. Although the various ligands L(R)l ed to structurally analogous complexes for R = Cy, tBu and Ph, the rates of dynamic processes occurring in solution are dependent on R, with faster rates for R = Ph. Transmetallation of both NHC and P donor groups from [Ag4Br4(L(tBu))2] to AuI by reaction with [AuCl(THT)] (THT = tetrahydrothiophene) led to L(tBu) transfer and to the dinuclear complex [Au2Cl2L(tBu)] with one L(tBu) ligand bridging the two Au centres. Except for the silver pseudo-cubanes, all other complexes do not exhibit metallophilic interactions.

  16. Synthesis and Evaluation of New Generation Cross-Bridged Bifunctional Chelator for (64)Cu Radiotracers.

    Science.gov (United States)

    Dale, Ajit V; An, Gwang Il; Pandya, Darpan N; Ha, Yeong Su; Bhatt, Nikunj; Soni, Nisarg; Lee, Hochun; Ahn, Heesu; Sarkar, Swarbhanu; Lee, Woonghee; Huynh, Phuong Tu; Kim, Jung Young; Gwon, Mi-Ri; Kim, Sung Hong; Park, Jae Gyu; Yoon, Young-Ran; Yoo, Jeongsoo

    2015-09-08

    Bifunctional chelators have been successfully used to construct (64)Cu-labeled radiopharmaceuticals. Previously reported chelators with cross-bridged cyclam backbones have various essential features such as high stability of the copper(II) complex, high efficiency of radiolabeling at room temperature, and good biological inertness of the radiolabeled complex, along with rapid body clearance. Here, we report a new generation propylene-cross-bridged chelator with hybrid acetate/phosphonate pendant groups (PCB-TE1A1P) developed with the aim of combining these key properties in a single chelator. The PCB-TE1A1P was synthesized from cyclam with good overall yield. The Cu(II) complex of our chelator showed good robustness in kinetic stability evaluation experiments, such as acidic decomplexation and cyclic voltammetry studies. The Cu(II) complex of PCB-TE1A1P remained intact under highly acidic conditions (12 M HCl, 90 °C) for 8 d and showed quasi-reversible reduction/oxidation peaks at -0.77 V in electrochemical studies. PCB-TE1A1P was successfully radiolabeled with (64)Cu ions in an acetate buffer at 60 °C within 60 min. The electrophoresis study revealed that the (64)Cu-PCB-TE1A1P complex has net negative charge in aqueous solution. The biodistribution and in vivo stability study profiles of (64)Cu-PCB-TE1A1P indicated that the radioactive complex was stable under physiological conditions and cleared rapidly from the body. A whole body positron emission tomography (PET) imaging study further confirmed high in vivo stability and fast clearance of the complex in mouse models. In conclusion, PCB-TE1A1P has good potential as a bifunctional chelator for (64)Cu-based radiopharmaceuticals, especially those involving peptides.

  17. Synthesis and Characterization of Colloidal Metal and Photovoltaic Semiconductor Nanocrystals

    KAUST Repository

    Abulikemu, Mutalifu

    2014-11-05

    Metal and semiconducting nanocrystals have received a great deal of attention from fundamental scientists and application-oriented researchers due to their physical and chemical properties, which differ from those of bulk materials. Nanocrystals are essential building blocks in the development of nanostructured devices for energy conversion. Colloidal metals and metal chalcogenides have been developed for use as nanocrystal inks to produce efficient solar cells with lower costs. All high-performing photovoltaic nanocrystals contain toxic elements, such as Pb, or scarce elements, such as In; thus, the production of solution-processable nanocrystals from earth-abundant materials using environmentally benign synthesis and processing methods has become a major challenge for the inorganic semiconductor-based solar field. This dissertation, divided into two parts, addresses several aspects of these emerging challenges. The first portion of the thesis describes the synthesis and characterization of nanocrystals of antimony sulfide, which is composed of non-scarce and non-toxic elements, and examines their performance in photovoltaic devices. The effect of various synthetic parameters on the final morphology is explored. The structural, optical and morphological properties of the nanocrystals were investigated, and Sb2S3 nanocrystal-based solid-state semiconductor-sensitized solar cells were fabricated using different deposition processes. We achieved promising power conversion efficiencies of 1.48%. The second part of the thesis demonstrates a novel method for the in situ synthesis and patterning of nanocrystals via reactive inkjet printing. The use of low-cost manufacturing approaches for the synthesis of nanocrystals is critical for many applications, including photonics and electronics. In this work, a simple, low-cost method for the synthesis of nanocrystals with minimum size variation and waste using reactive inkjet printing is introduced. As a proof of concept, the

  18. Nanoscale Synthesis and Characterization Laboratory Annual Report 2007

    Energy Technology Data Exchange (ETDEWEB)

    Hamza, A V

    2008-04-07

    The Nanoscale Synthesis and Characterization Laboratory's (NSCL) primary mission is to create and advance interdisciplinary research and development opportunities in nanoscience and technology. The NSCL is delivering on its mission providing Laboratory programs with scientific solutions through the use of nanoscale synthesis and characterization. While this annual report summarizes 2007 activities, we have focused on nanoporous materials, advanced high strength, nanostructured metals, novel 3-dimensional lithography and characterization at the nanoscale for the past 3 years. In these three years we have synthesized the first monolithic nanoporous metal foams with less than 10% relative density; we have produced ultrasmooth nanocrystalline diamond inertial confinement fusion capsules; we have synthesized 3-dimensional graded density structures from full density to 5% relative density using nanolithography; and we have established ultrasmall angle x-ray scattering as a non-destructive tool to determine the structure on the sub 300nm scale. The NSCL also has a mission to recruit and to train personnel for Lab programs. The NSCL continues to attract talented scientists to the Laboratory. Andrew Detor from Massachusetts Institute of Technology, Sutapa Ghosal from the University of California, Irvine, Xiang Ying Wang from Shanghai Institute of Technology, and Arne Wittstock from University of Bremen joined the NSCL this year. The NSCL is pursuing four science and technology themes: nanoporous materials, advanced nanocrystalline materials, novel three-dimensional nanofabrication technologies, and nondestructive characterization at the mesoscale. The NSCL is also pursuing building new facilities for science and technology such as nanorobotics and atomic layer deposition.

  19. Lanthanide phosphonates: Synthesis, thermal stability and magnetic characterization

    Energy Technology Data Exchange (ETDEWEB)

    Amghouz, Z., E-mail: amghouz.uo@uniovi.es [Departamentos de Quimica Fisica y Analitica y Quimica Organica e Inorganica, Universidad de Oviedo - CINN, 33006 Oviedo (Spain); Garcia, J.R.; Garcia-Granda, S. [Departamentos de Quimica Fisica y Analitica y Quimica Organica e Inorganica, Universidad de Oviedo - CINN, 33006 Oviedo (Spain); Clearfield, A. [Department of Chemistry, Texas A and M University, College Station, TX 77842-3012 (United States); Rodriguez Fernandez, J.; Pedro, I. de [CITIMAC, Facultad de Ciencias, Universidad de Cantabria, 39005 Santander (Spain); Blanco, J.A. [Departamento de Fisica, Universidad de Oviedo, 33007 Oviedo (Spain)

    2012-09-25

    Highlights: Black-Right-Pointing-Pointer Report of the complete series of lanthanide 1,4-phenylbis(phosphonate). Black-Right-Pointing-Pointer Synthesis under conventional hydrothermal synthesis or microwave-assisted hydrothermal synthesis. Black-Right-Pointing-Pointer Cation size is the key factor for the structural and particles size variations. Black-Right-Pointing-Pointer Thermal behaviour is characterized by unusual very high thermal stability. - Abstract: Series of novel organic-inorganic hybrids materials based on trivalent lanthanides (Ln = Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu) and 1,4-phenylbis(phosphonate) obtained under hydrothermal conditions either by oven heat or microwave irradiation. The anhydrous compounds containing La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, and Ho, are isostructural. However, the compounds based on Y, Er, Tm, Yb, and Lu are hydrated and their structures have not yet been solved. The series of compounds are characterized by PXRD, TEM, SEM-EDX and thermal analyses (TG-MS and DSC). TEM study show a variable particles size with a minimum mean-particle size of ca. 30 nm. These compounds exhibit unusual very high thermal stability. The size of particles and the thermal stability are depending on lanthanide(III) cation features. All the investigated materials show paramagnetic behaviour. The magnetic susceptibility data follow a Curie-Weiss laws with paramagnetic effective moments in good agreement with those expected for Ln{sup 3+} free ions.

  20. Synthesis and Characterization of Functionalized Metal-organic Frameworks

    Science.gov (United States)

    Karagiaridi, Olga; Bury, Wojciech; Sarjeant, Amy A.; Hupp, Joseph T.; Farha, Omar K.

    2014-01-01

    Metal-organic frameworks have attracted extraordinary amounts of research attention, as they are attractive candidates for numerous industrial and technological applications. Their signature property is their ultrahigh porosity, which however imparts a series of challenges when it comes to both constructing them and working with them. Securing desired MOF chemical and physical functionality by linker/node assembly into a highly porous framework of choice can pose difficulties, as less porous and more thermodynamically stable congeners (e.g., other crystalline polymorphs, catenated analogues) are often preferentially obtained by conventional synthesis methods. Once the desired product is obtained, its characterization often requires specialized techniques that address complications potentially arising from, for example, guest-molecule loss or preferential orientation of microcrystallites. Finally, accessing the large voids inside the MOFs for use in applications that involve gases can be problematic, as frameworks may be subject to collapse during removal of solvent molecules (remnants of solvothermal synthesis). In this paper, we describe synthesis and characterization methods routinely utilized in our lab either to solve or circumvent these issues. The methods include solvent-assisted linker exchange, powder X-ray diffraction in capillaries, and materials activation (cavity evacuation) by supercritical CO2 drying. Finally, we provide a protocol for determining a suitable pressure region for applying the Brunauer-Emmett-Teller analysis to nitrogen isotherms, so as to estimate surface area of MOFs with good accuracy. PMID:25225784

  1. Synthesis of doubly ethyl-bridged bis(p-sulfonatocalix[4]arene) and its supramolecular polymerization with viologen dimer.

    Science.gov (United States)

    Wang, Kun-Peng; Guo, Dong-Sheng; Zhao, Hong-Xia; Liu, Yu

    2014-04-01

    A water-soluble supramolecular polymer with a high degree of polymerization and viscosity has been constructed based on the strong host-guest interaction between p-sulfonatocalix[4]arenes (SC4As) and viologen. A homoditopic doubly ethyl-bridged bis(p-sulfonatocalix[4]arene) (d-SC4A) was prepared and its binding behavior towards methyl viologen compared with the singly ethyl-bridged bis(p-sulfonatocalix[4]arene) (s-SC4A) by NMR spectroscopy and isothermal titration calorimetry. By employing a viologen dimer (bisMV(4+)) as the homoditopic guest, two linear AA/BB-type supramolecular polymers, d-SC4A⊃bisMV(4+) and s-SC4A⊃bisMV(4+), were successfully constructed. Compared with s-SC4A⊃bisMV(4+), d-SC4A⊃bisMV(4+) shows much higher solubility and viscosity, and has also been characterized by viscosity, diffusion-ordered NMR spectroscopy, dynamic light scattering, and atomic force microscopy measurements. Furthermore, the polymer is responsive to electrostimulus as viologen is electroactive, which was studied by cyclic voltammetry. This study represents a proof-of-principle as the polymer can potentially be applied as a self-healing and degradable polymeric material.

  2. Structural and functional characterization of the conserved salt bridge in mammalian paneth cell alpha-defensins

    DEFF Research Database (Denmark)

    Rosengren, K Johan; Daly, Norelle L; Fornander, Liselotte M;

    2006-01-01

    )-Crp4 peptide, in which a conserved Glu(15) residue was replaced by Asp. Structural analysis of the two peptides confirms the involvement of this Glu in a conserved salt bridge that is removed in the mutant because of the shortened side chain. Despite disruption of this structural feature, the peptide...... variant retains a well defined native fold because of a rearrangement of side chains, which result in compensating favorable interactions. Furthermore, salt bridge-deficient Crp4 mutants were tested for bactericidal effects and resistance to proteolytic degradation, and all of the variants had similar...

  3. Corrigendum to "Synthesis, crystal structure and electrochemical and DNA binding studies of oxygen bridged-copper(II) carboxylate" [J. Mol. Struct. 1093 (2015) 135-143

    Science.gov (United States)

    Iqbal, Muhammad; Ali, Saqib; Tahir, Muhammad Nawaz; Muhammad, Niaz; Shah, Naseer Ali; Sohail, Manzar; Pandarinathan, Vedapriya

    2017-04-01

    The authors regret to inform that Scheme 1 in the article titled 'Synthesis, crystal structure and electrochemical and DNA binding studies of oxygen bridged-copper(II) carboxylate' in vol. 1093 of the Journal of Molecular Structure is incorrect. The corrected scheme is as shown in this correction. This is purely a copy error. The error does not affect the conclusion in paper. The authors would like to apologize for any inconvenience caused.

  4. Synthesis and characterization of MWCNT/CdS nanocomposite

    Directory of Open Access Journals (Sweden)

    M R Khanlary

    2014-12-01

    Full Text Available In this work we report the synthesis and characterization of hybrid nanostructures of multiwall carbon nanotubes (MWCNT and cadmium sulphide (CdS nanoparticles. In a solution of thioacetamide and cadmium sulphide, purified MWCNT are added to prepare the CNT/CdS hetrostructure. XRD diagrams, SEM images, and also photoluminescence spectra of the prepared samples are analyzed. SEM images show the CdS nanoparticles of 17nm size coated on the CNTs. Visible photoluminescence with peaks at 435 nm and 535 nm, obtained from the prepared CNT/CdS, is discussed. The synthesis technique can be simply extended to other luminescent dopants, and the possibility of making optoelectronic devises based on the CNTs is confirmed by this method

  5. New Synthesis of TATB. Scaleup and Product Characterization

    Energy Technology Data Exchange (ETDEWEB)

    Schmidt, R.D.; Mitchell, A.R.; Lee, G.S.; Pagoria, P.F.; Coburn, M.D.; Quinlan, W.T.; Thorpe, R.; Cates, M.

    2000-03-15

    At the 29th International Annual Conference of ICT (1998), the authors described the results of laboratory-scale process development studies for a new synthesis of 1,3,5-triamino-2,4,6-trinitrobenzene (TATB). This new synthesis approach--which uses vicarious nucleophilic substitution (VNS) methodology--converts picramide to TATB in high yield, and potentially at lower cost and with few environmental effects than existing synthetic approaches. In this report they describe results of their work on producing TATB by the VNS method at the pilot plant scale. They will discuss structure and control of impurities, changes in yield/quality with reaction conditions, choice of solvents, workup and product isolation, safety, and environmental considerations. Product characterization (particle size, DSC, HPLC, etc.) as well as small-scale safety and performance testing is also discussed.

  6. A new cadmium(II) complex with bridging dithiolate ligand: Synthesis, crystal structure and antifungal activity study

    Science.gov (United States)

    Singh, Mahesh Kumar; Sutradhar, Sanjit; Paul, Bijaya; Adhikari, Suman; Laskar, Folguni; Butcher, Raymond J.; Acharya, Sandeep; Das, Arijit

    2017-07-01

    A new polymeric complex of Cd(II) with 1,1-dicyanoethylene- 2,2-dithiolate [ i-MNT2- = {S2C:C(CN)2}2- ] as a bridging ligand has been synthesized and characterized on the basis of spectroscopy and single-crystal X-ray diffraction analysis. Single crystal X-ray diffraction analysis reveals that the Cadmium (II) complex is six coordinated 1D polymeric in nature. Biological screening effects in vitro of the synthesized polymeric complex has been tested against five fungi Synchitrium endobioticum, Pyricularia oryzae, Helminthosporium oryzae, Candida albicans(ATCC10231), Trichophyton mentagrophytes by the disc diffusion method. In vitro antifungal screening indicates that the complex exhibits fungistatic and fungicidal antifungal activity whereas K2i-MNT.H2O became silent on Synchitrium endobioticum, Pyricularia oryzae, Helminthosporium oryzae, Candida albicans (ATCC10231), Trichophyton mentagrophytes.

  7. H-Bonding Self-assembled Template-directed Synthesis of a Reactive Amide-bridged Ladder Polyvinylsiloxane

    Institute of Scientific and Technical Information of China (English)

    You Zhi WAN; Ying Hua LIU; Ping XIE; Rong Ben ZHANG

    2006-01-01

    A novel, reactive amide-bridged ladder polyvinylsiloxane (abbr. LP) with Mn = 2.4×104was synthesized for the first time by means of aryl amide H-bonding self-assembled template.The regularity of LP was characterized by the XRD, 29Si NMR and DSC methods. XRD analysis demonstrated the ladder width w = 9.09 A and the ladder thickness t = 3.89 A, respectively, which are approximately consistent with the molecular simulation-calculated ones: w'= 10.60 A and t'=3.06 A. 29Si NMR displayed a resonance peak with small half peak width, △1/2 ~ 4 ppm, for the moiety [=Si(Vi)O2/2-]n of LP. Besides, as a collateral evidence, DSC measurement revealed a high glass transition temperature Tg = 225℃, suggesting high stiffness of the ladder main chain of LP.

  8. Functional Metal Oxide Nanostructures: Their Synthesis, Characterization, and Energy Applications

    Science.gov (United States)

    Iyer, Aparna

    This research focuses on studying metal oxides (MnO 2, Co3O4, MgO, Y2O3) for various applications including water oxidation and photocatalytic oxidation, developing different synthesis methodologies, and presenting detailed characterization studies of these metal oxides. This research consists of three major parts. The first part is studying novel applications and developing a synthesis method for manganese oxide nanomaterials. Manganese oxide materials were studied for renewable energy applications by using them as catalysts for water oxidation reactions. In this study, various crystallographic forms of manganese oxides (amorphous, 2D layered, 1D 2 x 2 tunnel structures) were evaluated for water oxidation catalysis. Amorphous manganese oxides (AMO) were found to be catalytically active for chemical and photochemical water oxidation compared to cryptomelane type tunnel manganese oxides (2 x 2 tunnels; OMS2) or layered birnessite (OL-1) materials. Detailed characterization was done to establish a correlation between the properties of the manganese oxide materials and their catalytic activities in water oxidation. The gas phase photocatalytic oxidation of 2-propanol under visible light was studied using manganese oxide 2 x 2 tunnel structures (OMS-2) as catalysts (Chapter 3). The reaction is 100% selective to acetone. As suggested by the photocatalytic and characterization data, important factors for the design of active OMS-2 photocatalysts are synthesis methodology, morphology, mixed valency and the release of oxygen from the OMS-2 structure. Manganese oxide octahedral molecular sieves (2 x 2 tunnels; OMS-2) with self-assembled dense or hollow sphere morphologies were fabricated via a room temperature ultrasonic atomization assisted synthesis (Chapter 4). The properties and catalytic activities of these newly developed materials were compared with that of OMS-2 synthesized by conventional reflux route. These materials exhibit exceptionally high catalytic activities

  9. Boron bridging of rhamnogalacturonan-II, monitored by gel electrophoresis, occurs during polysaccharide synthesis and secretion but not post-secretion.

    Science.gov (United States)

    Chormova, Dimitra; Messenger, David J; Fry, Stephen C

    2014-02-01

    The cell-wall pectic domain rhamnogalacturonan-II (RG-II) is cross-linked via borate diester bridges, which influence the expansion, thickness and porosity of the wall. Previously, little was known about the mechanism or subcellular site of this cross-linking. Using polyacrylamide gel electrophoresis (PAGE) to separate monomeric from dimeric (boron-bridged) RG-II, we confirmed that Pb(2+) promotes H3 BO3 -dependent dimerisation in vitro. H3 BO3 concentrations as high as 50 mm did not prevent cross-linking. For in-vivo experiments, we successfully cultured 'Paul's Scarlet' rose (Rosa sp.) cells in boron-free medium: their wall-bound pectin contained monomeric RG-II domains but no detectable dimers. Thus pectins containing RG-II domains can be held in the wall other than via boron bridges. Re-addition of H3 BO3 to 3.3 μm triggered a gradual appearance of RG-II dimer over 24 h but without detectable loss of existing monomers, suggesting that only newly synthesised RG-II was amenable to boron bridging. In agreement with this, Rosa cultures whose polysaccharide biosynthetic machinery had been compromised (by carbon starvation, respiratory inhibitors, anaerobiosis, freezing or boiling) lost the ability to generate RG-II dimers. We conclude that RG-II normally becomes boron-bridged during synthesis or secretion but not post-secretion. Supporting this conclusion, exogenous [(3) H]RG-II was neither dimerised in the medium nor cross-linked to existing wall-associated RG-II domains when added to Rosa cultures. In conclusion, in cultured Rosa cells RG-II domains have a brief window of opportunity for boron-bridging intraprotoplasmically or during secretion, but secretion into the apoplast is a point of no return beyond which additional boron-bridging does not readily occur.

  10. Synthesis and characterization of energetic thermoplastic elastomers for propellant formulations

    Directory of Open Access Journals (Sweden)

    Aparecida M. Kawamoto

    2009-01-01

    Full Text Available Synthesis and characterization of energetic ABA-type thermoplastic elastomers for propellant formulations has been carried out. Following the working plan elaborated, the synthesis and characterization of Poly 3- bromomethyl-3-methyl oxetane (PolyBrMMO, Poly 3- azidomethyl-3-methyl oxetane (PolyAMMO, Poly 3,3-bis-azidomethyl oxetane (PolyBAMO and Copolymer PolyBAMO/AMMO (by TDI end capping has been successfully performed. The thermoplastic elastomers (TPEs were synthesized using the chain elongation process PolyAMMO, GAP and PolyBAMO by diisocyanates. In this method 2.4-toluene diisocyanate (TDI is used to link block A (hard and mono- functional to B (soft and di-functional. For the hard A-block we used PolyBAMO and for the soft B-block we used PolyAMMO or GAP.This is a joint project set up, some years ago, between the Chemistry Division of the Institute of Aeronautics and Space (IAE - subordinated to the Brazilian Ministry of Defense - and the Fraunhofer Institut Chemische Technologie (ICT, in Germany. The products were characterized by different techniques as IR- and (1H,13CNMR spectroscopies, elemental and thermal analyses. New methodologies based on FT-IR analysis have been developed as an alternative for the determination of the molecular weight and CHNO content of the energetic polymers.

  11. Synthesis and characterization of zinc oxide nanostructures for piezoelectric applications

    Science.gov (United States)

    Hughes, William L.

    Union between top-down and bottom-up assembly is inevitable when scaling down physical, chemical, and biological sensors and probes. Current sensor/probe-based technologies are firmly founded on top-down manufacturing, with limitations in cost of production, manufacturing methods, and material constraints. As an alternative to such limitations, contemporary synthesis techniques for one-dimensional nanostructures have been combined with established methods of micro-fabrication for the development of novel tools and techniques for nanotechnology. More specifically, this dissertation is a systematic study of the synthesis and characterization of ZnO nanostructures for piezoelectric applications. Within this study the following goals have been achieved: (1) rational design and control of a diversity of novel ZnO nanostructures, (2) improved understanding of polar-surface-dominated (PSD) phenomena among Wurtzite crystal structures, (3) confirmation of Tasker's Rule via the synthesis, characterization, and modeling of polar-surface-dominated nanostructures, (4) measurement of the surface-charge density for real polar surfaces of ZnO, (5) confirmation of the electrostatic polar-charge model used to describe polar-surface-dominated phenomena, (6) dispersion of ZnO nanobelts onto the selective layers of surface acoustic wave (SAW) devices for gas sensing applications, (7) manipulation of ZnO nanostructures using an atomic force microscope (AFM) for the development of piezoelectric devices, (8) fabrication of bulk acoustic resonator (BAR) and film bulk acoustic resonator (FBAR) devices based on the integrity of individual ZnO belts, (9) electrical characterization of a ZnO belt BAR device, (10) prediction and confirmation of the electrical response from a BAR device using a one-dimensional Krimholt-Leedom-Matthaei (KLM) model, and (11) development of a finite element model (FEM) to accurately predict the electrical response from ZnO belt BAR and FBAR devices in 3D.

  12. Schiff base functionalized Organopropylsilatranes: Synthesis and structural characterization

    Indian Academy of Sciences (India)

    Gurjaspreet Singh; Promila; Amandeep Saroa; Jandeep Singh; Raj Pal Sharm; V Ferretti

    2016-02-01

    Synthesis of Schiff bases linked to organopropylsilatranes were performed by condensation reaction of post-functionalized silatranes such as aminopropylsilatrane (4), aminopropyl-3,7,10-trimethylsilatrane (5) and N-substituted aminopropylsilatrane (10) with two different aldehydes viz. pyrrole-2-carboxaldehyde and 2-hydroxy-1-napthaldehyde. The resulting Schiff base substituted silatranes were well characterized by elemental analysis, spectroscopic studies [IR, (1H, 13C) NMR, and MS]. The structures of two silatranes were confirmed by single crystal X-ray diffraction analysis.

  13. Synthesis and characterization of the polyaniline dopant Schiff base

    Directory of Open Access Journals (Sweden)

    Mirian Y. Matsumoto

    2012-06-01

    Full Text Available The Schiff base, N-salicilidenoanilina was used as dopant to induce polymerization of aniline and thus preparing polyaniline (PAni. The different conditions of preparation, including Schiff base structure, and the dosage of acidity reaction medium, were investigated to discuss the influence of these conditions relative conductivity of the resulting samples. The products were also characterized by Fourier transform infrared (FTIR, ultraviolet-visible (UV-Vis, electrochemical impedance spectroscopy (EIE. The results showed the synthesis conditions play an important in the formation and the final properties of the polyaniline

  14. Synthesis and Characterization of Boron Trifluoride Doped High Performance Polyaniline

    Directory of Open Access Journals (Sweden)

    K. Basavaiah

    2012-01-01

    Full Text Available We report simple synthesis of boron trifluoride (BF3 doped defect free high performance polyaniline (HPPANI in two step method. Firstly, HPPANI was prepared via self-stabilization dispersion polymerization method in a heterogeneous reaction medium. Second step involves doping of emeraldine base form of HPPANI with boron trifluoride under reduced vacuum. The resultants BF3 doped HPPANI have been well characterized by using UV-Visible spectroscopy, Fourier transform infrared spectroscopy (FTIR, scanning electron microscopy (SEM and thermogravimetry. The spectroscopic data indicated that the interaction between HPPANI and BF3.Thermogravimetry studies revealed that the BF3 doping improved the thermal stability of defects free PANI.

  15. Synthesis and biophysical characterization of chlorambucil anticancer ether lipid prodrugs.

    Science.gov (United States)

    Pedersen, Palle J; Christensen, Mikkel S; Ruysschaert, Tristan; Linderoth, Lars; Andresen, Thomas L; Melander, Fredrik; Mouritsen, Ole G; Madsen, Robert; Clausen, Mads H

    2009-05-28

    The synthesis and biophysical characterization of four prodrug ether phospholipid conjugates are described. The lipids are prepared from the anticancer drug chlorambucil and have C16 and C18 ether chains with phosphatidylcholine or phosphatidylglycerol headgroups. All four prodrugs have the ability to form unilamellar liposomes (86-125 nm) and are hydrolyzed by phospholipase A(2), resulting in chlorambucil release. Liposomal formulations of prodrug lipids displayed cytotoxicity toward HT-29, MT-3, and ES-2 cancer cell lines in the presence of phospholipase A(2), with IC(50) values in the 8-36 microM range.

  16. Synthesis and Biophysical Characterization of Chlorambucil Anticancer Ether Lipid Prodrugs

    DEFF Research Database (Denmark)

    Pedersen, Palle Jacob; Christensen, Mikkel Stochkendahl; Ruysschaert, Tristan

    2009-01-01

    The synthesis and biophysical characterization of four prodrug ether phospholipid conjugates are described. The lipids are prepared from the anticancer drug chlorambucil and have C16 and C18 ether chains with phosphatidylcholine or phosphatidylglycerol headgroups. All four prodrugs have the ability...... to form unilamellar liposomes (86-125 nm) and are hydrolyzed by phospholipase A2, resulting in chlorambucil release. Liposomal formulations of prodrug lipids displayed cytotoxicity toward HT-29, MT-3, and ES-2 cancer cell lines in the presence of phospholipase A2, with IC50 values in the 8-36 μM range....

  17. Controllable synthesis and characterization of alumina/MWNT nanocomposites

    Energy Technology Data Exchange (ETDEWEB)

    Nemeth, Zoltan; Hernadi, Klara [Department of Applied and Environmental Chemistry, University of Szeged, Rerrich Bela ter 1, 6720 Szeged (Hungary); Marko, Kata; Erdohelyi, Andras [Department of Physical Chemistry and Material Science, University of Szeged, Aradi ter 2, 6720 Szeged (Hungary); Forro, Laszlo [Laboratory of Physics of Complex Matter, IPMC, EPFL, 1026 Ecublens (Switzerland)

    2011-11-15

    The aim of this work is to develop a controllable synthesis pathway which produces a stable alumina layer on the surface of carbon nanotubes by impregnation method. Precursor compounds such as aluminium isopropoxide and aluminium-acetyl-acetonate were used to cover the surface of multiwalled carbon nanotubes (MWNTs) under different solvent conditions. As-prepared alumina coverages were characterized by TEM, SEM, SEM-EDX, TG and X-ray diffraction techniques. Results revealed that homogeneous coverage can be achieved in a controllable way. (Copyright copyright 2011 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  18. Texas Barrier Islands Region ecological characterization: environmental synthesis papers

    Energy Technology Data Exchange (ETDEWEB)

    Shew, D.M.; Baumann, R.H.; Fritts, T.H.; Dunn, L.S.

    1981-09-01

    This report is a synthesis of selected environmental literature for the Texas Barrier Islands Region and is a part of the Texas Barrier Islands Region Ecological Characterization Study. The Texas Barrier Islands Region is defined to include the coastal counties and extends 64 km inland and offshore to the State-Federal demarcation. These papers deal with six drainage basins along the Texas coast: Galveston, Matagorda-Brazos, San Antonio, Copano-Aransas, Corpus Christi and Laguna Madre; as well as the marine system offshore. The papers address the geology, climate, hydrology and hydrography, and the biology of each basin.

  19. SYNTHESIS AND CHARACTERIZATION OF HETEROAROMATIC POLYMERS CONTAINING PYRIDINE MOIETIES

    Institute of Scientific and Technical Information of China (English)

    LI Yanfeng; WANG Xiaolong; ZHANG Shujiang

    2006-01-01

    The progress on the molecular design, synthesis and characterizations of some kinds of pyridine-containing heteroaromatic polymers in main chain were reviewed in this paper, they would include polyimides (PIs), polypyrrolones (PPYs), poly(pyrrolone-imide)s (PPIs), and poly(pyrrolone-benzimidazone)s (PPBs) containing pyrldine moieties. The pyridine-containing polymers reported all exhibit good processability, excellent thermal properties and mechanical properties. However, the contribution of pyridine ring to polymers properties is still need to research further, the heteroarornatic polymers containing pyridine moieties have focused by more and more researchers.

  20. Synthesis and characterization of nanoscale magnetic drug-inorganic composites

    Institute of Scientific and Technical Information of China (English)

    SUN Hui; ZHANG Hui; David G. Evans; DUAN Xue

    2005-01-01

    The synthesis by direct coprecipitation and characterization of captopril (Cpl) and 5-aminosalicylic acid (5-ASA) intercalated ZnAl layered double hydroxides coated on MgFe2O4 magnetic core particles are reported. Powder XRD analysis shows the well-defined crystallite structure of the composites. TEM and XPS results reveal that a core-shell structure involving a drug-LDHs layer coated on MgFe2O4 particles is formed through Zn-O-Mg and/or Al-O-Mg linkages. VSM measurements demonstrate that the novel magnetic drug-inorganic composites possess considerable magnetization.

  1. Synthesis and characterization of metal oxide nanorod brushes

    Indian Academy of Sciences (India)

    Kalyan Raidongia; M Eswaramoorthy

    2008-02-01

    Nanorod brushes of -Al2O3, MoO3 and ZnO have been synthesized using amorphous carbon nanotube (-CNT) brushes as the starting material. The brushes of -Al2O3 and MoO3 are made up of single crystalline nanorods. In the case of ZnO brushes, the nanorod bristles are made by the fusion of 15–25 nm size nanoparticles and are porous in nature. Metal oxide nanorod brushes thus obtained have been characterized by XRD, FESEM, TEM and Raman spectroscopy. Single crystalline ruby nanorods were obtained by introducing chromium ions during the synthesis of alumina rods.

  2. DISY. The direct synthesis of hydrogen peroxide, a bridge for innovative applications

    Energy Technology Data Exchange (ETDEWEB)

    Buzzoni, R.; Perego, C. [Eni S.p.A., Novara (Italy). Research Center for Non-Conventional Energies

    2011-07-01

    Hydrogen peroxide is largely recognized as the green oxidant of choice for future sustainable processes. The current industrial production still goes through the old anthraquinone process, a complex, two-step process suffering from a low specific productivity. Following the development of TS-1/H{sub 2}O{sub 2} based selective oxidation processes e.g. propylene epoxidation, cyclohexanone ammoximation and the new benzene direct oxidation to phenol, there has been an incentive for the development of a new technology, simpler and with better economics. DISY process, based on direct synthesis of hydrogen peroxide from hydrogen and oxygen, is highly suitable to the design of integrated selective oxidation processes as well as for production of commercial-grade high concentration aqueous hydrogen peroxide solutions. Catalyst and process development up to pilot scale are described. (orig.)

  3. Sol - Gel synthesis and characterization of magnesium peroxide nanoparticles

    Science.gov (United States)

    Jaison, J.; Ashok raja, C.; Balakumar, S.; Chan, Y. S.

    2015-04-01

    Magnesium peroxide is an excellent source of oxygen in agriculture applications, for instance it is used in waste management as a material for soil bioremediation to remove contaminants from polluted underground water, biological wastes treatment to break down hydrocarbon, etc. In the present study, sol-gel synthesis of magnesium peroxide (MgO2) nanoparticles is reported. Magnesium peroxide is odourless; fine peroxide which releases oxygen when reacts with water. During the sol-gel synthesis, the magnesium malonate intermediate is formed which was then calcinated to obtain MgO2 nanoparticles. The synthesized nanoparticles were characterized using Thermo gravimetric -Differential Thermal Analysis (TG- DTA), X-Ray Diffraction studies (XRD) and High Resolution Transmission Electron Microscope (HRTEM). Our study provides a clear insight that the formation of magnesium malonate during the synthesis was due to the reaction between magnesium acetate, oxalic acid and ethanol. In our study, we can conclude that the calcination temperature has a strong influence on particle size, morphology, monodispersity and the chemistry of the particles.

  4. Synthesis and characterization of novel cellulose ether sulfates.

    Science.gov (United States)

    Rohowsky, Juta; Heise, Katja; Fischer, Steffen; Hettrich, Kay

    2016-05-20

    The synthesis and characterization of novel cellulose sulfate derivatives was reported. Various cellulose ethers were prepared in a homogeneous reaction with common sulfating agents. The received product possess different properties in dependence on the reaction conditions like sulfating agent, solvent, reaction time and reaction temperature. The cellulose ether sulfates are all soluble in water, they rheological behavior could be determined by viscosity measurements and the determination of the sulfur content by elemental analysis lead to a resulting degree of substitution ascribed to sulfate groups (DSSul) of the product. A wide range of products from DSSul 0.1 to DSSul 2.7 will be obtained. Furthermore the cellulose sulfate ethers could be characterized by Raman spectroscopy.

  5. Electrochemical synthesis and characterization of copper (I oxide

    Directory of Open Access Journals (Sweden)

    Bugarinović Sanja J.

    2009-01-01

    Full Text Available The quest and need for clean and economical energy sources have increased interest in the development of thin film cells technologies. Electrochemical deposition is an attractive method for synthesis of thin films. It offers the advantages of low synthesis temperature, low cost and high purity. Copper (I oxide or cuprous oxide is an oxide semiconductor which is used as the anodic material in the form of thin film in lithium batteries and solar cells. The cathodic process of synthesis of cuprous oxide thin film is carried out in a potentiostatic mode from the organic electrolyte. The process parameters are chosen in that way to accomplish maximum difference between the potentials at which Cu2O and CuO are obtained. The electrochemical characterization was carried out by cyclic voltammetry. The electrodeposition techniques are particularly well suited for the deposition of single elements but it is also possible to carry out simultaneous depositions of several elements and syntheses of well-defined alternating layers of metals and oxides with thicknesses down to a few nm. Nanomaterials exhibit novel physical properties and play an important role in fundamental research. In addition, cuprous oxide is commonly used as a pigment, a fungicide, and an antifouling agent for marine paints. It is insoluble in water and organic solvents. This work presents the examinations of the influence of bath, temperature, pH and current density on the characteristics of electrochemically synthesized cuprous oxide. In the 'classic' process of synthesis, which is carried out under galvanostatic conditions on the anode, the grain size of the powder decreases with the increase in current density while the grain colour becomes lighter. The best commercial quality of the Cu2O (grain size, colour, content of choride was obtained at the temperature of 80°C, concentration of NaCl of 3 mol/dm3 and current density of 400 A/m2.

  6. In-service performance and behavior characterization of the hybrid composite bridge system - a case study

    CERN Document Server

    Civitillo, John M; Gheitasi, Amir; Saliba, Mark; Kassner, Bernard L

    2014-01-01

    The Hybrid Composite Beam (HCB) system is an innovative structural technology that has been recently used in bridge construction within the U.S. transportation network. In this system, the superstructure consists of a conventional reinforced concrete deck supported by Hybrid Composite Beams. Each beam is comprised of a glassfiber reinforced polymer (FRP) box shell containing a tied parabolic concrete arch. Inclined stirrups provide shear integrity and enforce composite action between the HCBs and the concrete deck. This paper focuses on evaluating the in-service performance of a newly constructed HCB bridge superstructure located on Route 205 in Colonial Beach, Virginia. A live load test was conducted using tandem axle dump trucks under both quasi-static and dynamic conditions. Results obtained from the experimental investigation were used to determine three key behavior characteristics. Dynamic amplification and lateral load distribution were found to be reasonable in comparison to the assumed design values....

  7. Characterizing Arctic sea ice topography using high-resolution IceBridge data

    OpenAIRE

    Petty, Alek A.; Tsamados, Michel C.; Kurtz, Nathan T.; Farrell, Sinead L.; Newman, Thomas; Harbeck, Jeremy P.; FELTHAM, DANIEL L.; Richter-Menge, Jackie A.

    2015-01-01

    We present an analysis of Arctic sea ice topography using high resolution, three-dimensional, surface elevation data from the Airborne Topographic Mapper, flown as part of NASA's Operation IceBridge mission. Surface features in the sea ice cover are detected using a newly developed surface feature picking algorithm. We derive information regarding the height, volume and geometry of surface features from 2009–2014 within the Beaufort/Chukchi and Central Arcti...

  8. Synthesis, structure characterization and catalytic activity of nickel tungstate nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Pourmortazavi, Seied Mahdi, E-mail: pourmortazavi@yahoo.com [Faculty of Material and Manufacturing Technologies, Malek Ashtar University of Technology, Tehran (Iran, Islamic Republic of); Rahimi-Nasrabadi, Mehdi, E-mail: rahiminasrabadi@gmail.com [Department of Chemistry, Imam Hossein University, Tehran (Iran, Islamic Republic of); Khalilian-Shalamzari, Morteza [Department of Chemistry, Imam Hossein University, Tehran (Iran, Islamic Republic of); Zahedi, Mir Mahdi; Hajimirsadeghi, Seiedeh Somayyeh [Islamic Azad University, Varamin Pishva Branch, Varamin (Iran, Islamic Republic of); Omrani, Ismail [Department of Chemistry, Imam Hossein University, Tehran (Iran, Islamic Republic of)

    2012-12-15

    Graphical abstract: NiWO{sub 4} nanoparticles were prepared via precipitation technique. Experimental parameters of procedure were optimized statistically. Highlights: Black-Right-Pointing-Pointer NiWO{sub 4} spherical nanoparticles were synthesized via direct precipitation method. Black-Right-Pointing-Pointer Taguchi robust design was used for optimization of synthesis reaction parameters. Black-Right-Pointing-Pointer Composition and structural properties of NiWO{sub 4} nanoparticles were characterized. Black-Right-Pointing-Pointer EDAX, XRD, SEM, FT-IR, UV-vis and photoluminescence techniques were employed. Black-Right-Pointing-Pointer Catalytic activity of the product in a cyclo-addition reaction was investigated. - Abstract: Taguchi robust design was applied to optimize experimental parameters for controllable, simple and fast synthesis of nickel tungstate nanoparticles. NiWO{sub 4} nanoparticles were synthesized by precipitation reaction involving addition of nickel ion solution to the tungstate aqueous reagent and then formation of nickel tungstate nucleolus which are insoluble in aqueous media. Effects of various parameters such as nickel and tungstate concentrations, flow rate of reagent addition and reactor temperature on diameter of synthesized nickel tungstate nanoparticles were investigated experimentally by the aid of orthogonal array design. The results for analysis of variance (ANOVA) showed that particle size of nickel tungstate can be effectively tuned by controlling significant variables involving nickel and tungstate concentrations and flow rate; while, temperature of the reactor has a no considerable effect on the size of NiWO{sub 4} particles. The ANOVA results proposed the optimum conditions for synthesis of nickel tungstate nanoparticles via this technique. Also, under optimum condition nanoparticles of NiWO{sub 4} were prepared and their structure and chemical composition were characterized by means of EDAX, XRD, SEM, FT-IR spectroscopy, UV

  9. Synthesis and characterization of five-coordinated indium amidinates

    Energy Technology Data Exchange (ETDEWEB)

    Riahi, Yasaman

    2016-07-29

    The focus of this work is synthesis, characterization and exploring the reactivity of new indium amidinate compounds of the type R{sub 2}InX (R = R''NCR'NR''; R' = Ph, R'' = SiMe{sub 3}, iPr, dipp; X = Br, Cl) with the coordination number of five and R{sub 3}In (R = Me{sub 3}SiNCPhNSiMe{sub 3}) with the coordination number of six. By using amidinates as chelating ligands the electron deficiency of indium atom will be resolved. Additionally, by using different substituents the study of the different synthesized indium amidinates has become possible. The selected method for the synthesis allows the carbodiimides to react with organolithium compounds to get the corresponding lithium amidinates. Afterwards the resulting lithium amidinates take part in transmetalation reactions with InBr{sub 3} and InCl{sub 3}. The study of the reactivity of indium amidinate complexes including nucleophilic reactions as well as their reduction were also examined. Beside crystal structure analysis, nuclear magnetic resonance spectroscopy as well as elemental analysis has been applied to characterize the compounds.

  10. Synthesis of novel polymethacrylates with siloxyl bridging perfluoroalkyl side-chains for hydrophobic application on cotton fabrics

    Energy Technology Data Exchange (ETDEWEB)

    Cai, Lu; Dai, Li; Yuan, Yanhua; Liu, Anqi [College of Textile and Clothing Engineering, Soochow University, Suzhou 215021 (China); National Engineering Laboratory for Modern Silk, Suzhou 215123 (China); Zhanxiong, Li, E-mail: lizhanxiong@suda.edu.cn [College of Textile and Clothing Engineering, Soochow University, Suzhou 215021 (China); National Engineering Laboratory for Modern Silk, Suzhou 215123 (China)

    2016-05-15

    Highlights: • Novel polymethacrylates with multi-perfluoroalkyl groups were reported. • TFSMA monomer in the polymer contributed much to the lower surface free energy. • PSD and TEM showed a broader size distribution with the increasing fluorine content. • EDS and XPS revealed migration of perfluoroalkyl chains under high temperature. - Abstract: Three novel fluorinated methacrylate monomers with siloxyl bridging perfluoroalkyl groups were synthesized and characterized. Afterwards, the corresponding polymethacrylate latexes, namely monofluoroalkylsiloxyl polymethacrylate (PMFSMA), bisfluoroalkylsiloxyl polymethacrylate (PBFSMA) and trisfluoroalkylsiloxyl polymethacrylate (PTFSMA), were prepared and coated onto cotton fabrics to make them water-repellent. Particle size, particle size distribution, zeta potential and high-resolution transmission electron microscope (TEM) were tested to assess the emulsion stability and particle morphology. Thermal properties of PTFSMA were evaluated by thermal-gravimetric analysis (TGA). Surface properties of the coated cotton fabrics were characterized by Fourier transform infrared spectroscopy (FT-IR), scanning electron microscope (SEM), water contact angle (WCA), adhesive force and X-ray photoelectron spectroscopy (XPS). It was found that the incorporation of more perfluoroalkyl chains and the annealing process could decrease the surface free energy of polymer film to 13.7 mN/m. Furthermore, the EDS spectra of PTFSMA film after annealing showed an enrichment of fluorine in the film-air interface.

  11. Synthesis of novel polymethacrylates with siloxyl bridging perfluoroalkyl side-chains for hydrophobic application on cotton fabrics

    Science.gov (United States)

    Cai, Lu; Dai, Li; Yuan, Yanhua; Liu, Anqi; Zhanxiong, Li

    2016-05-01

    Three novel fluorinated methacrylate monomers with siloxyl bridging perfluoroalkyl groups were synthesized and characterized. Afterwards, the corresponding polymethacrylate latexes, namely monofluoroalkylsiloxyl polymethacrylate (PMFSMA), bisfluoroalkylsiloxyl polymethacrylate (PBFSMA) and trisfluoroalkylsiloxyl polymethacrylate (PTFSMA), were prepared and coated onto cotton fabrics to make them water-repellent. Particle size, particle size distribution, zeta potential and high-resolution transmission electron microscope (TEM) were tested to assess the emulsion stability and particle morphology. Thermal properties of PTFSMA were evaluated by thermal-gravimetric analysis (TGA). Surface properties of the coated cotton fabrics were characterized by Fourier transform infrared spectroscopy (FT-IR), scanning electron microscope (SEM), water contact angle (WCA), adhesive force and X-ray photoelectron spectroscopy (XPS). It was found that the incorporation of more perfluoroalkyl chains and the annealing process could decrease the surface free energy of polymer film to 13.7 mN/m. Furthermore, the EDS spectra of PTFSMA film after annealing showed an enrichment of fluorine in the film-air interface.

  12. Synthesis and thermal decomposition of a pyridylene-bridged bis-beta-diketiminate magnesium hydride cluster

    NARCIS (Netherlands)

    Harder, Sjoerd; Spielmann, Jan; Intemann, Julia

    2014-01-01

    Reaction of PYR-(MgnBu)(2), in which PYR is 2,6-[(DIPP)NC(Me)CHC(Me)N-]2-pyridine and DIPP is 2,6-iPr(2)-phenyl, with (DIPP)NH2BH3 gave PYR-[MgNH(DIPP)BH3](2) (56%) which was characterized by crystal structure determination. Addition of THF resulted in beta-H elimination and formation of PYR-[MgNH(D

  13. Synthesis and thermal decomposition of a pyridylene-bridged bis-beta-diketiminate magnesium hydride cluster

    NARCIS (Netherlands)

    Harder, Sjoerd; Spielmann, Jan; Intemann, Julia

    2014-01-01

    Reaction of PYR-(MgnBu)(2), in which PYR is 2,6-[(DIPP)NC(Me)CHC(Me)N-]2-pyridine and DIPP is 2,6-iPr(2)-phenyl, with (DIPP)NH2BH3 gave PYR-[MgNH(DIPP)BH3](2) (56%) which was characterized by crystal structure determination. Addition of THF resulted in beta-H elimination and formation of PYR-[MgNH(D

  14. Synthesis, Characterization and Thermal Decomposition Mechanism of Cetyltrimethyl Ammonium Tetrathiotungstate

    Institute of Scientific and Technical Information of China (English)

    Gaojun An; Yunqi Liu; Yongming Chai; Hongyan Shang; Chenguang Liu

    2006-01-01

    The synthesis, characterization and thermal decomposition mechanism of cetyltrimethyl ammonium tetrathiotungstate (CTriMATT) were studied herein. The as-synthesized CTriMATT was characterized by Elemental analysis, X-ray diffraction (XRD), Fourier transform infrared (FT-IR), Ultraviolet visible (UV-Vis) spectra. The results showed that the as-synthesized CTriMATT had high purity and good crystallinity. The introduction of alkyl groups induced a shift of the stretching vibration band of W-S bond to lower wavenumber, while it had no influence on the position of WS2-4. Thermogravimetric analysis (TG), differential thermal analysis (DTA) and in situ XRD characterizations revealed that CTriMATT began to decompose at 423 K in nitrogen and was converted to WS2 eventually. In addition,the decomposition product of CTriMATT at 673 K in nitrogen was characterized by N2 adsorption (BET)and scanning electron microscopy (SEM). The results demonstrated that WS2 with higher specific surface area, and pore volume could be obtained from the thermal decomposition of CTriMATT in nitrogen.

  15. Design, Synthesis and Evaluation of Organic Non-linear Optical Chromophores with Configurationally and Conformationally Locked Polyene Bridges

    Science.gov (United States)

    2007-11-02

    A modular, synthetic scheme was developed for versatile variation of donors, acceptors and polyene bridge length of NLO-chromophores. Configurational...and conformational rigidity of the polyene bridges were realized by making each set of adjacent double and single bond pair part of a fused...cylohexene ring. Substituent effects on the reactions leading to the establishment of the donor, elongation of the fused polyene bridge and the final

  16. Design and Characterization of a Peptide Mimotope of the HIV-1 gp120 Bridging Sheet

    Directory of Open Access Journals (Sweden)

    Guido Poli

    2012-05-01

    Full Text Available The Bridging Sheet domain of HIV-1 gp120 is highly conserved among the HIV-1 strains and allows HIV-1 binding to host cells via the HIV-1 coreceptors. Further, the bridging sheet domain is a major target to neutralize HIV-1 infection. We rationally designed four linear peptide epitopes that mimic the three-dimensional structure of bridging sheet by using molecular modeling. Chemically synthesized peptides BS3 and BS4 showed a fair degree of antigenicity when tested in ELISA with IgG purified from HIV+ broadly neutralizing sera while the production of synthetic peptides BS1 and BS2 failed due to their high degree of hydrophobicity. To overcome this limitation, we linked all four BS peptides to the COOH-terminus of GST protein to test both their antigenicity and immunogenicity. Only the BS1 peptide showed good antigenicity; however, no envelope specific antibodies were elicited upon mice immunization. Therefore we performed further analyses by linking BS1 peptide to the NH2-terminus of the E2 scaffold from the Geobacillus Stearothermophylus PDH complex. The E2-BS1 fusion peptide showed good antigenic results, however only one immunized rabbit elicited good antibody titers towards both the monomeric and oligomeric viral envelope glycoprotein (Env. In addition, moderate neutralizing antibodies response was elicited against two HIV-1 clade B and one clade C primary isolates. These preliminary data validate the peptide mimotope approach as a promising tool to obtain an effective HIV-1 vaccine.

  17. Synthesis and Structure of Novel Double Flexible Spacer BridgedBiscalix [4] arenes

    Institute of Scientific and Technical Information of China (English)

    ZENG, Xian-Shun; WENG, Lin-Hong; CHEN,Lang-Xing; JU, Hong-Fang; LENG, Xue-Bing; HE, Xi-Wen

    2001-01-01

    25,25′ ,27,27′-Bis ( 1,3-dioxypropane ) -bis (5,11,17,23-tetratert-butylcalix[4]arene-26,28-diol) (4) and 25,25′,27,27′-bis( 1, 4-dioxybutane)-bis (5, 11, 17, 23-tetra-tert-butylcalix[4]arene-26,28-diol) (5) were synthesized by the reaction of p-tert-butylcalix[4]arene (1) with preorganized 25,27-bis(3-bromoproxyl)calix[4]arene-26,27-diol (2) and 25,27-bis(3-bromobutoxyl)calix[4]arene-26,27-diol (3) in the presence of K2CO3 and KI. Compounds 4 and 5 were characterized with X-ray analysis and the selectivity of 4 and 5 to ward K + over other alkali metal ions, alkaline metal ions as well as NH4 + were investigated with an ion-selective electrode.

  18. Synthesis and Characterization of Highly Intercalated Graphite Bisulfate

    Science.gov (United States)

    Salvatore, Marcella; Carotenuto, Gianfranco; De Nicola, Sergio; Camerlingo, Carlo; Ambrogi, Veronica; Carfagna, Cosimo

    2017-03-01

    Different chemical formulations for the synthesis of highly intercalated graphite bisulfate have been tested. In particular, nitric acid, potassium nitrate, potassium dichromate, potassium permanganate, sodium periodate, sodium chlorate, and hydrogen peroxide have been used in this synthesis scheme as the auxiliary reagent (oxidizing agent). In order to evaluate the presence of delamination, and pre-expansion phenomena, and the achieved intercalation degree in the prepared samples, the obtained graphite intercalation compounds have been characterized by scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), X-ray powder diffraction (XRD), infrared spectroscopy (FT-IR), micro-Raman spectroscopy ( μ-RS), and thermal analysis (TGA). Delamination and pre-expansion phenomena were observed only for nitric acid, sodium chlorate, and hydrogen peroxide, while the presence of strong oxidizers (KMnO4, K2Cr2O7) led to stable graphite intercalation compounds. The largest content of intercalated bisulfate is achieved in the intercalated compounds obtained from NaIO4 and NaClO3.

  19. Characterization and sonochemical synthesis of black phosphorus from red phosphorus

    Science.gov (United States)

    Aldave, Sandra H.; Yogeesh, Maruthi N.; Zhu, Weinan; Kim, Joonseok; Sonde, Sushant S.; Nayak, Avinash P.; Akinwande, Deji

    2016-03-01

    Phosphorene is a new two-dimensional material which is commonly prepared by exfoliation from black phosphorus bulk crystals that historically have been synthesized from white phosphorus under high-pressure conditions. The few layers of phosphorene have a direct band gap in the range of 0.3-2 eV and high mobility at room temperature comparable to epitaxial graphene. These characteristics can be used for the design of high speed digital circuits, radio frequency circuits, flexible and printed systems, and optoelectronic devices. In this work, we synthesized black phosphorus from red phosphorus, which is a safer solid precursor, using sonochemistry. Furthermore, via a variety of microscopy and spectroscopy techniques, we report characterization results of the sonochemically synthesized black phosphorus in addition to the commercial black phosphorus. Finally, we describe the air stability of black phosphors and the crystalline structure of the synthesized material. This is the first result of sonochemical or solution-based synthesis of black phosphorus based on readily available low-cost red phosphorus. This solution-based synthesis of black phosphorus is suitable for printable applications of nanomaterial.

  20. Synthesis, structure characterization and catalytic activity of nickel tungstate nanoparticles

    Science.gov (United States)

    Pourmortazavi, Seied Mahdi; Rahimi-Nasrabadi, Mehdi; Khalilian-Shalamzari, Morteza; Zahedi, Mir Mahdi; Hajimirsadeghi, Seiedeh Somayyeh; Omrani, Ismail

    2012-12-01

    Taguchi robust design was applied to optimize experimental parameters for controllable, simple and fast synthesis of nickel tungstate nanoparticles. NiWO4 nanoparticles were synthesized by precipitation reaction involving addition of nickel ion solution to the tungstate aqueous reagent and then formation of nickel tungstate nucleolus which are insoluble in aqueous media. Effects of various parameters such as nickel and tungstate concentrations, flow rate of reagent addition and reactor temperature on diameter of synthesized nickel tungstate nanoparticles were investigated experimentally by the aid of orthogonal array design. The results for analysis of variance (ANOVA) showed that particle size of nickel tungstate can be effectively tuned by controlling significant variables involving nickel and tungstate concentrations and flow rate; while, temperature of the reactor has a no considerable effect on the size of NiWO4 particles. The ANOVA results proposed the optimum conditions for synthesis of nickel tungstate nanoparticles via this technique. Also, under optimum condition nanoparticles of NiWO4 were prepared and their structure and chemical composition were characterized by means of EDAX, XRD, SEM, FT-IR spectroscopy, UV-vis spectroscopy, and photoluminescence. Finally, catalytic activity of the nanoparticles in a cycloaddition reaction was examined.

  1. Synthesis and characterization of related substances of Azilsartan Kamedoxomil

    Directory of Open Access Journals (Sweden)

    Maddi N. V. D. Harikiran

    2017-03-01

    Full Text Available Azilsartan Kamedoxomil is an AT1-subtype angiotensin II receptor blocker (ARB. During the laboratory synthesis of Azilsartan Kamedoxomil, four related substances of Azilsartan Kamedoxomil were observed and identified. These were 2-Ethoxy-3-[[4-[2- [4-[(5-methyl-2-oxo-1,3-dioxol-4-ylmethyl]-5-oxo-1,2,4-oxadiazol-3-yl]phenyl]phenyl] methyl] benzimidazole-4-carboxylic acid (azilsartan N-medoxomil, 9, (5-methyl-2-oxo- 1,3-dioxol-4-ylmethyl 2-ethoxy-3-[[4-[2-[4-[(5-methyl-2-oxo-1,3-dioxol-4-ylmethyl]-5- oxo-1,2,4-oxadiazol-3-yl]phenyl]phenyl] methyl] benzimidazole-4-carboxylate (azilsartan dimedoxomil, 10, (5-methyl-2-oxo-1,3-dioxo-4-ylmethyl 1-[2’-(4,5-dihydro-5-oxo-4H- 1,2,4-oxadiazol-3-ylbiphenyl-4-yl]methyl]-2-methoxy-1H-benzimidazole-7-carboxylate (methoxy analogue of azilsartan medoxomil, 11, Methyl 1-((2’-amidobiphenyl-4-yl methyl-2-ethoxy-1H-benzo[d]imidazole-7-carboxylate (amide methyl ester, 12. The present work describes the origin, synthesis and characterization of these related substances.

  2. Synthesis, characterization, and antimicrobial properties of copper nanoparticles

    Directory of Open Access Journals (Sweden)

    Usman MS

    2013-11-01

    Full Text Available Muhammad Sani Usman,1 Mohamed Ezzat El Zowalaty,2,5 Kamyar Shameli,1,3 Norhazlin Zainuddin,1 Mohamed Salama,4 Nor Azowa Ibrahim1 1Department of Chemistry, Faculty of Science, 2Laboratory of Vaccines and Immunotherapeutics, Institute of Bioscience, Universiti Putra Malaysia, Selangor, Malaysia; 3Materials and Energy, Research Center, Karaj, Iran; 4Faculty of Pharmacy, UiTM, Puncak Alam, Selangor, Malaysia; 5Department of Environmental Health, Faculty of Public Health and Tropical Medicine, Jazan University, Jazan, Kingdom of Saudi Arabia Abstract: Copper nanoparticle synthesis has been gaining attention due to its availability. However, factors such as agglomeration and rapid oxidation have made it a difficult research area. In the present work, pure copper nanoparticles were prepared in the presence of a chitosan stabilizer through chemical means. The purity of the nanoparticles was authenticated using different characterization techniques, including ultraviolet visible spectroscopy, transmission electron microscopy, X-ray diffraction, Fourier transform infrared spectroscopy, and field emission scanning electron microscopy. The antibacterial as well as antifungal activity of the nanoparticles were investigated using several microorganisms of interest, including methicillin-resistant Staphylococcus aureus, Bacillus subtilis, Pseudomonas aeruginosa, Salmonella choleraesuis, and Candida albicans. The effect of a chitosan medium on growth of the microorganism was studied, and this was found to influence growth rate. The size of the copper nanoparticles obtained was in the range of 2–350 nm, depending on the concentration of the chitosan stabilizer. Keywords: chitosan, copper nanoparticles, antimicrobial activity, chemical synthesis, aqueous medium

  3. Synthesis and characterization of oxovanadium (IV) dithiocarbamates with pyridine

    Energy Technology Data Exchange (ETDEWEB)

    Doadrio, Antonio L.; Sotelo, Jose; Fernandez-Ruano, Ana [Universidad Complutense, Madrid (Spain). Facultad de Farmacia. Dept. de Quimica Inorganica y Bioinorganica]. E-mail: antoniov@farm.ucm.es

    2002-07-01

    We report the synthesis and study of a new series of oxovanadium (IV) dithiocarbamate adducts and derivatives with pyridine and cyclohexyl, di-iso-butyl, di-n-propyl, aniline, morpholine, piperidine and di-iso-propyl amines. The complexes have been characterized by analytical, magneto chemical, IR, visible-UV spectral and thermal studies, and are assigned the formulas [VO(L){sub 2}].py, where L=cyclohexyl, di-iso-butyl, di-n-propyl, aniline dithiocarbamate and [VO(OH)(L)(py){sub 2}] OH.H{sub 2}O (L=morpholine, piperidine and di-iso-propyl dithiocarbamate). The effect of the adduct formation on the p{sub V=0} bound is discussed in terms of the IR (V=O, V-S and V-N stretching frequencies) and electronic spectra (d-d transitions). (author)

  4. SYNTHESIS AND CHARACTERIZATION OF N-(1-NAPHTHYL) SUCCINIMIDE

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    In this paper a modified two-step procedure for synthesis of N-(1-naphthyl) succinimide (NaS) was developed, and the molecular structure of NaS was properly characterized by XRD, FT-IR, 1H NMR, DSC, etc. The results show that the melting point of our product is 159℃~160.5 ℃, and the characteristic infrared absorption band of carbonyl group splits into two peaks (1705cm-1/1779cm-1), which are found to be quite different from the documented data (mp 147℃~149℃;IR C=O,~1700cm-1). Besides, photophysical spectroscopy was found to be powerful to study the molecular structure and crystal morphology of NaS compound.

  5. Synthesis and characterization of carbon cryogel/zeolite composites

    Directory of Open Access Journals (Sweden)

    Biljana Babić

    2011-06-01

    Full Text Available A novel method for synthesis of carbon cryogel/zeolite composites was obtained. Method considers forming of carbon cryogel from the sol-gel polycondenzation of resorcinol and formaldehyde, followed by freeze drying, and subsequent pyrolysis in presence of different amount of zeolite. Characterization of composite materials by nitrogen adsorption shows that samples are micro- and mesoporous and that specific surface area decrease with increasing the amount of zeolite in samples. XRD method confirms amorphous structure of carbon cryogel and crystalline structure of zeolite, i.e. structure of zeolite has not been destroyed by carbonization process. SEM and EDX analyses reveal homogenous distribution of zeolite through out carbon cryogel and corresponding composition.

  6. Synthesis and Spectroscopic Characterization of Two Tetrasubstituted Cationic Porphyrin Derivatives

    Directory of Open Access Journals (Sweden)

    Newton M. Barbosa Neto

    2011-07-01

    Full Text Available An imidazolium tetrasubstituted cationic porphyrin derivative (the free base and its Zn(II complex with five-membered heterocyclic groups in the meso-positions were synthesized using microwave irradiation, and the compounds obtained characterized by 1H-NMR and mass spectrometry. We observed that under microwave irradiation the yield is similar to when the synthesis is performed under conventional heating, however, the time required to prepare the porphyrins decreases enormously. In order to investigate the electronic state of these compounds, we employed UV-Vis and fluorescence spectroscopy combined with quantum chemical calculations. The results reveal the presence, in both compounds, of a large number of electronic states involving the association between the Soret and a blue-shifted band. The Soret band in both compounds also shows a considerable solvent dependence. As for emission, these compounds present low quantum yield at room temperature and no solvent influence on the fluorescence spectra was observed.

  7. Synthesis, characterization, and antimicrobial properties of copper nanoparticles

    Science.gov (United States)

    Usman, Muhammad Sani; Zowalaty, Mohamed Ezzat El; Shameli, Kamyar; Zainuddin, Norhazlin; Salama, Mohamed; Ibrahim, Nor Azowa

    2013-01-01

    Copper nanoparticle synthesis has been gaining attention due to its availability. However, factors such as agglomeration and rapid oxidation have made it a difficult research area. In the present work, pure copper nanoparticles were prepared in the presence of a chitosan stabilizer through chemical means. The purity of the nanoparticles was authenticated using different characterization techniques, including ultraviolet visible spectroscopy, transmission electron microscopy, X-ray diffraction, Fourier transform infrared spectroscopy, and field emission scanning electron microscopy. The antibacterial as well as antifungal activity of the nanoparticles were investigated using several microorganisms of interest, including methicillin-resistant Staphylococcus aureus, Bacillus subtilis, Pseudomonas aeruginosa, Salmonella choleraesuis, and Candida albicans. The effect of a chitosan medium on growth of the microorganism was studied, and this was found to influence growth rate. The size of the copper nanoparticles obtained was in the range of 2–350 nm, depending on the concentration of the chitosan stabilizer. PMID:24293998

  8. Synthesis, characterization and application of soluble fullerenat ed polymer materials

    Institute of Scientific and Technical Information of China (English)

    CHEN, Yu; CAI, Rui-Fang; HUANG, Zu-En; WANG, Jing-Xia

    2000-01-01

    This article only deals with the topic of intense interest to us and to a considerable extent of our own experimental results on the synthesis, characterization and application of C60-con taining functional polymers such as poly (N-vinylcarbazole), polyrene and polyacrylonitrne-based fullerene polymers. The results demonstrate that [60] fullerene can be directly in corporated into a variety of functional polymers by copolymer ization or grafting, but also can be used to modify or improve the electronic, optiical and physicochemical properties of poly mers. Both the stereo-electroniceffect and the steric hindrance of C60 have an important influence on the structu-e and physicochemical properties of the parent polymer.

  9. Synthesis, Characterization, and Thermokinetic Analysis of New Epoxy Sugar Derivative

    Directory of Open Access Journals (Sweden)

    Selinay Y. Erişkin

    2014-01-01

    Full Text Available The synthesis of 5,6-O-isopropylidene-1,2-O-(R-trichloroethylidene-α-D-glucofuranose (compound 1 and 5,6-O-isopropylidene-1,2-O-(R-trichloroethylidene-3-O-(2′,3′-epoxypropan-1′-yl-α-D-glucofuranose (compound 2 was carried out. The synthesized compounds 1 and 2 were characterized by nuclear magnetic resonance (1H-NMR, Fourier transform infrared spectroscopy (FTIR, and thermogravimetric analysis (TG. The FTIR and 1H NMR spectra showed that the epoxy group in compound 2 was attached by means of a nucleophilic substitution reaction. The activation energies for thermal degradation of compounds 1 and 2 were calculated from their TG data by using the Kissinger-Akahira-Sunose (KAS and Tang methods.

  10. Synthesis and characterization of yttrium aluminium garnet (YAG powders

    Directory of Open Access Journals (Sweden)

    Magdalena Zarzecka-Napierala

    2007-12-01

    Full Text Available In this paper synthesis and characterization of YAG powders, prepared by a process based on complexing properties of citric acid, was reported. Influence of citric acid estrification induced by 2-propanol or ethylene glycol on the system homogeneity was investigated. These reagents were introduced to aqueous solution of yttrium and aluminium nitrates. A variety of powders from Al2O3-Y2O3 system with different phase composition were obtained by altering the citrate to nitrate ratio. Evolution of the powders phase composition vs. temperature was investigated using DTA/TG, XRD, and FT-IR methods. The most interesting results were observed in case of the citric acid–propanol–relative nitrates system. The mole ratio of these reagents equal to 1:2.5:2.5 (nitrates (Al,Y:citric acid:2-propanol allowed to synthesize pure YAG phase powders at temperature as low as 950°C.

  11. Synthesis and characterization of oxovanadium (IV dithiocarbamates with pyridine

    Directory of Open Access Journals (Sweden)

    Antonio L. Doadrio

    2002-07-01

    Full Text Available We report the synthesis and study of a new series of oxovanadium (IV dithiocarbamate adducts and derivatives with pyridine and cyclohexyl, di-iso-butyl, di-n-propyl, anilin, morpholin, piperidin and di-iso-propyl amines. The complexes have been characterized by analytical, magnetochemical, IR, visible-UV spectral and thermal studies, and are assigned the formulas [VO(L2].py, where L=cyclohexyl, di-iso-butyl, di-n-propyl, anilin dithiocarbamate and [VO(OH(L(py2]OH.H2O (L=morpholin, piperidin and di-iso-propyl dithiocarbamate. The effect of the adduct formation on the pV=0 bound is discussed in terms of the IR (V=O, V-S and V-N stretching frequencies and electronic spectra (d-d transitions.

  12. Synthesis and Characterization of Compatibilizer TLCP-b-PC

    Institute of Scientific and Technical Information of China (English)

    XIAO Ru; JIN Shu-wen; ZHANG Yue-ting; WU Cheng-xun

    2002-01-01

    The compatibilizer (TLCP-b-PC) of 60PHB/PET thermotropic liquid crystal polymer (TLCP) and polycarbonate (PC) blend system was prepared. The synthesis and characterization of the compatibilizer as well as its effects on the microscopic morphology and the mechanical properties of the TLCP/PC blend system were studied with a series of analysis ways, such as Soxhlet extraction, infrared absorption spectroscopy,electron microscopy, etc. It is shown that the ideal reaction condition for preparing the compatibilizer is:the reaction temperature of 275℃, the reaction time of 20minutes and without catalyst. And the compatibilizer can improve the compatibility of the blending system of 60PHB/PET and PC.

  13. SYNTHESIS AND CHARACTERIZATION OF N-(1-NAPHTHYL) SUCCINIMIDE

    Institute of Scientific and Technical Information of China (English)

    LI Hexian; YANG Hailong; LIU Kun; WANG Ying; YUAN Jialong; WANG Guochang

    2007-01-01

    In this paper a modified two-step procedure for synthesis of N-(1-naphthyl) succinimide (NaS) was developed, and the molecular structure of NaS was properly characterized by XRD, FT-IR,1H NMR, DSC, etc. The results show that the melting point of our product is 159 ℃~160.5 ℃, and the characteristic infrared absorption band of carbonyl group splits into two peaks (1705cm-1/1779cm-1),which are found to be quite different from the documented data (mp 147 ℃~149 ℃; IR C=O,~1700cm-1 ). Besides, photophysical spectroscopy was found to be powerful to study the molecular structure and crystal morphology of NaS compound.

  14. Antibacterial gold nanoparticles-biomass assisted synthesis and characterization.

    Science.gov (United States)

    Badwaik, Vivek D; Willis, Chad B; Pender, Dillon S; Paripelly, Rammohan; Shah, Monic; Kherde, Yogesh A; Vangala, Lakshmisri M; Gonzalez, Matthew S; Dakshinamurthy, Rajalingam

    2013-10-01

    Xylose is a natural monosaccharide found in biomass such as straw, pecan shells, cottonseed hulls, and corncobs. Using this monosaccharide, we report the facile, green synthesis and characterization of stable xylose encapsulated gold nanoparticles (Xyl-GNPs) with potent antibacterial activity. Xyl-GNPs were synthesized using the reduction property of xylose in an aqueous solution containing choloraurate anions carried out at room temperature and atmospheric pressure. These nanoparticles were stable and near spherical in shape with an average diameter of 15 +/- 5 nm. Microbiological assay results showed the concentration dependent antibacterial activity of these particles against both Gram-negative (Escherichia coli) and Gram-positive (Staphylococcus epidermidis) bacteria. Thus the facile, environmentally friendly Xyl-GNPs have many potential applications in chemical and biomedical industries, particularly in the development of antibacterial agents in the field of biomedicine.

  15. Optimization of amine-terminated polyacrylonitrile synthesis and characterization

    Directory of Open Access Journals (Sweden)

    Mohamed H. El-Newehy

    2014-04-01

    Full Text Available Amine-terminated PANs were prepared in two steps. The first step includes free radical polymerization of acrylonitrile (AN using initiator pair of ammonium persulfate and sodium thiosulfate as redox system. In the second step, the amino groups were introduced through the reaction of polyacrylonitrile with excess of different diamines (10-fold including ethylenediamine (EDA, hexamethylenediamine (HMDA and octamethylenediamine (OMDA, to yield PAN–EDA, PAN–HMDA and PAN–OMDA, respectively. Optimization of the amine-terminated PANs synthesis was carried out at different temperatures (30–90 °C and different time intervals (4–24 h. In addition, the introduction of the amino group was followed by the piperidine test and recording of the FT-IR spectra. All polymers were characterized by, 1H NMR spectra, thermogravimetric analysis (TGA, and FT-IR spectra.

  16. Single step synthesis and characterization of thermoresponsive hyaluronan hydrogels.

    Science.gov (United States)

    D'Este, Matteo; Alini, Mauro; Eglin, David

    2012-10-15

    An efficient and scale-up ready single-step synthesis for the conjugation of thermoresponsive polymers to hyaluronic acid (HA) was established. Jeffamines(®) (JFM) and poly(N-isopropylacrylamide) (PNIPAM) were grafted to HA via direct amidation mediated by 1,1'-carbonyldiimidazole activation. The temperature-induced gelation of the semi-synthetic co-polymers was characterized by rheology as a function of the temperature and by differential scanning calorimetry (DSC). A HA-JFM conjugate with sol-gel transition in a physiologically relevant temperature range was identified. The grafting of PNIPAM resulted in the drastic change of the main rheological properties of native HA, revealing the hydrophobic non-covalent nature of the interactions between the thermoresponsive brushes in the gel state. Owing to the reversibility of these interactions and the sharpness of the transition, the HA-PNIPAM conjugates are suitable candidates for the incorporation of drugs, cells or ceramic materials for different biomedical applications.

  17. Hexamethylenetetramine carboxyborane: synthesis, structural characterization and CO releasing properties.

    Science.gov (United States)

    Ayudhya, T I; Raymond, C C; Dingra, N N

    2017-01-17

    Carbon monoxide, although widely known as a toxic gas, has received great attention in the past few decades due to its promising role as a medical gas. Several classes of carbon monoxide releasing molecules (CORMs) have been synthesised with many of them having pharmacological activities under physiological conditions. Herein, we report the synthesis and structural characterization of the first example of amine carboxyborane that releases CO under physiological conditions without the aid of inducers. A representative compound hexamethylenetetramine carboxyborane (HMTA-CB) described here has a half-life of 2.7 days and gradually releases CO with the rate constant of 3.0 × 10(-6) s(-1). Its ability to promote cell growth shows the beneficial effect of slow CO release to supplement CO in small amounts over time.

  18. Nanoscale Synthesis and Characterization Laboratory Annual Report 2005

    Energy Technology Data Exchange (ETDEWEB)

    Hamza, A V; Lesuer, D R

    2006-01-03

    The Nanoscale Synthesis and Characterization Laboratory's (NSCL) primary mission is to create and advance interdisciplinary research and development opportunities in nanoscience and technology. The initial emphasis of the NSCL has been on development of scientific solutions in support of target fabrication for the NIF laser and other stockpile stewardship experimental platforms. Particular emphasis has been placed on the design and development of innovative new materials and structures for use in these targets. Projects range from the development of new high strength nanocrystalline alloys to graded density materials to high Z nanoporous structures. The NSCL also has a mission to recruit and train personnel for Lab programs such as the National Ignition Facility (NIF), Defense and Nuclear Technologies (DNT), and Nonproliferation, Arms control and International security (NAI). The NSCL continues to attract talented scientists to the Laboratory.

  19. Synthesis of highly phosphonic acid functionalized benzene-bridged periodic mesoporous organosilicas for use as efficient dye adsorbents.

    Science.gov (United States)

    Deka, Juti Rani; Liu, Chia-Ling; Wang, Tzu-Hua; Chang, Wei-Chieh; Kao, Hsien-Ming

    2014-08-15

    Periodic mesoporous organosilicas (PMOs) with benzene bridging groups in the silica wall were functionalized with a tunable content of phosphonic acid groups. These bifunctional materials were synthesized by co-condensation of two different organosilane precursors, that is, 1,4-bis(triethoxysilyl)benzene (BTEB) and sodium 3-(trihydroxysilyl)propyl methyl phosphate (SPMP), under acidic conditions using nonionic surfactant Brij-S10 as template. The materials exhibited well-ordered mesostructures and were characterized by X-ray diffraction, nitrogen sorption, TEM, TGA, FTIR, and solid-state NMR measurements. The materials thus obtained were employed as adsorbents to remove different types of dyes, for example, cationic dyes methylene blue and phenosafranine, anionic orange II, and amphoteric rhodamine B, from aqueous solutions. The materials exhibited a remarkably high adsorption capacity than activated carbon due to their ordered mesostructures, a large number of phosphonic acid groups, and high surface areas. The adsorption was mainly governed by electrostatic interaction, but also involved π-π stacking interaction as well as hydrogen bonding. The adsorption kinetics can be better fitted by the pseudo-second order model. The adsorption process was controlled by the mechanisms of external mass transfer and intraparticle diffusion. The materials retained more than 97% dye removal efficiency after use for five consecutive cycles.

  20. Exogenous bridging and nonbridging in Cu(II) complexes of Mannich base ligands: Synthesis and physical properties

    Indian Academy of Sciences (India)

    S Sujatha; T M Rajendiran; R Kannappan; R Venkatesan; P Sambasiva Rao

    2000-12-01

    Preparation of pentadentate ligands L1, L2, L3 and L4, where L1=4-chloro-3-methyl-2[(prolin-1-yl)methyl]-6-[N-phenyl piperazin-1-yl)methyl]phenol, L2= 4-ethyl-2-[(prolin-1-yl)methyl]-6-[(N-phenyl piperazin-1-yl)methyl]phenol, L3 =4-chloro-3-methyl-2-[(prolin-1-yl)methyl]-6-[N-methyl piperazin-1-yl]methyl phenol, L4 = 4-methoxy-2-[(prolin-1-yl)methyl]-6-[(N-phenyl piperazin-1-yl)methyl]phenol is described together with that of the corresponding Cu(II) complexes with various bridging motifs like OH, OAc and NO2. The complexes are characterized by elemental analysis, electrochemical and electron paramagnetic spectral studies. Redox properties of the complexes in acetonitrile are highly quasireversible due to the chemical or/and stereochemical changes subsequent to electron transfer. The complexes show resolved copper hyperfine EPR at room temperature, indicating the presence of weak antiferromagnetic coupling between the copper atoms. Strengths of the antiferromagnetic interactions are in the order NO2 > OAc > OH.

  1. Synthesis and Crystal Structure of a Dinuclear Cu(II) Complex with Tridentate Schiff Base and Azido Bridge

    Institute of Scientific and Technical Information of China (English)

    LIN Hong; FENG Yun Long; GAO Shan

    2005-01-01

    A new dinuclear copper(II) complex ([Cu(C12H17N2O)(N3)]2, C24H34Cu2N10O2) has been synthesized and characterized by X-ray structure determination. It crystallizes in the monoclinic system, space group P21/c with a = 18.529(4), b = 10.933(2), c = 14.534(3)(A),β = 111.07(3)(A), V = 2748(1)(A)3, Z = 4, Mr = 621.69, F(000) = 1288, Dc = 1.503 g/cm3 and μ(MoKα) = 1.590 mm(1. The structure was refined to R = 0.0647 and wR = 0.1846 for 4406 observed reflections (I > 2σ(I)). The asymmetric unit comprises two halfmolecules. The complex is a centrosymmetric dimmer in which the copper atoms are penta-coordinated by three coordination atoms from the corresponding tridentate Schiff base ligand and two bridging azide anions. The Cu(II)…Cu(II) average distance is 3.350(1)(A).

  2. Characterization of Individuals with Sacroiliac Joint Bridging in a Skeletal Population: Analysis of Degenerative Changes in Spinal Vertebrae

    Directory of Open Access Journals (Sweden)

    Takeshi Imamura

    2014-01-01

    Full Text Available The aim of this study was to characterize the individuals with sacroiliac joint bridging (SIB by analyzing the degenerative changes in their whole vertebral column and comparing them with the controls. A total of 291 modern Japanese male skeletons, with an average age at death of 60.8 years, were examined macroscopically. They were divided into two groups: individuals with SIB and those without bridging (Non-SIB. The degenerative changes in their whole vertebral column were evaluated, and marginal osteophyte scores (MOS of the vertebral bodies and degenerative joint scores in zygapophyseal joints were calculated. SIB was recognized in 30 individuals from a total of 291 males (10.3%. The average of age at death in SIB group was significantly higher than that in Non-SIB group. The values of MOS in the thoracic spines, particularly in the anterior part of the vertebral bodies, were consecutively higher in SIB group than in Non-SIB group. Incidence of fused vertebral bodies intervertebral levels was obviously higher in SIB group than in Non-SIB group. SIB and marginal osteophyte formation in vertebral bodies could coexist in a skeletal population of men. Some systemic factors might act on these degenerative changes simultaneously both in sacroiliac joint and in vertebral column.

  3. Synthesis, structural characterization and antitumor activity of a Ca(II) coordination polymer based on 4-formyl-1,3-benzenedisulfonate-2-furoic acid hydrazide ligands

    Science.gov (United States)

    Tai, Xi-Shi; Wang, Xin

    2017-03-01

    A new Ca(II) coordination polymer, {[CaL(H2O)4] · (H2O)4} n (L = 4-formyl-1,3-benzenedisulfonate-2-furoic acid hydrazide) has been prepared by one-pot synthesis method. And it was characterized by elemental analysis, IR and thermal analysis. The result of X-ray single-crystal diffraction analysis shows that the Ca(II) complex molecules form one-dimensional chain structure by the bridging oxygen atoms. The anti-tumor activity of L ligand and the Ca(II) coordination polymer has also been studied.

  4. Characterization of semiconductor bridges (SCB) igniters for use in thermal batteries

    Energy Technology Data Exchange (ETDEWEB)

    Bickes, R.W.; Guidotti, R.A. [Sandia National Labs., Albuquerque, NM (United States); McCampbell, C.B. [SCB Technologies, Inc., Albuquerque, NM (United States)

    1996-05-01

    Semiconductor bridges (SCB) igniters were evaluated as possible replacements for conventional hot-wire igniters for use in thermal batteries. The all-fire and no-fire characteristics were determined using an up-down scheme; the Neyer/SENSIT program was used to analyze the data. The SCB igniters functioned with a higher no-fire level, relative to a hot-wire igniter, for a given all-fire level. This makes the SCB igniter safer and more reliable than its hot-wire counterpart. The SCB is very resistant to electrostatic discharge and does not require a sensitization mixture for ignition of the primary pyrotechnic charge. These factors, along with its amenability to large-scale production, make the SCB igniter ideally suited for use in thermal batteries.

  5. Preparation and Characterization of Single-handed Helical Carbonaceous Nanoifbers using 1,4-Phenylene Bridged Polybissilsesquioxanes

    Institute of Scientific and Technical Information of China (English)

    XIAO Zeli; GUO Yongmin; LI Baozong; LI Yi

    2016-01-01

    Single-handed helical carbonaceous materials attracted much attention for varieties of potential applications. Herein, single-handed helical 1, 4-phenylene bridged polybissilsesquioxane nanoifbers were prepared through a supramolecular templating approach using a pair of enantiomers. After carbonization at 700℃ for 2.0 h and removal of silica using HF aqueous solution, single-handed helical carbonaceous nanoifbers were obtained. The obtained samples were characterized using the ifeld-emission scanning electron microscopy, transmission electron microscopy, N2 sorptions, X-ray diffraction, Raman spectroscopy and diffuse relfectance circular dichroism (DRCD). The Raman spectrum indicated that the carbon was amorphous. The DRCD spectra indicated that the carbonaceous nanoifbers exhibited optical activity. The surface area of the left-handed helical carbonaceous nanoifbers was 907 m2/g. Such material has potential applications as chirality sensor and supercapacitor electrode.

  6. Synthesis and characterization of N-doped zinc oxide nanotetrapods

    Science.gov (United States)

    Al Rifai, S. A.; Kulnitskiy, B. A.

    2016-05-01

    Nitrogen-doped (N-doped) self-assembled nanotetrapods ZnO were synthesized via chemical vapor deposition process using N2O as a dopant source via vapor-solid (VS) growth. The decomposition of N2O gas giving NO and NO2 during the synthesis provided successful N-doping of the sample. All samples (N-doped and undoped) were characterized by XRD, SEM, TEM, EDX, photoluminescence (PL), Fourier transform infrared (FT-IR), and diffuse reflection spectra. After nitrogen-doping process, N-doped ZnO samples show the change in structural and optical properties. The detailed structure and the growth mechanism of individual ZnO tetrapod is characterized by TEM and SEM investigations. The TEM study gives the direct assumption about the formation of zincblende (sphalerite) structure on the initial stage of growth of N-doped tetrapods. Besides, SEM observation indicated that tetrapods have perfect tetrahedral symmetry. N-Doped ZnO samples exhibit a broad orange-red PL emission band, peaking near 2.1 eV, in good agreement with the deep-acceptor model for the nitrogen impurity. An IR absorption peak at 3146 cm-1 at room temperature was observed for N-doped sample. This peak has been unambiguously assigned to N-H complex.

  7. Gold complexes with benzimidazole derivatives: synthesis, characterization and biological studies.

    Science.gov (United States)

    Mota, Vinicius Zamprogno; de Carvalho, Gustavo Senra Gonçalves; da Silva, Adilson David; Costa, Luiz Antônio Sodré; de Almeida Machado, Patrícia; Coimbra, Elaine Soares; Ferreira, Carmen Veríssima; Shishido, Silvia Mika; Cuin, Alexandre

    2014-02-01

    Synthesis, characterization, DFT studies and biological assays of new gold(I) and gold(III) complexes of benzimidazole are reported. Molecular and structural characterizations of the compounds were based on elemental (C, H and N) and thermal (TG-DTA) analyses, and FT-IR and UV-Visible spectroscopic measurements. The structures of complexes were proposed based DFT calculations. The benzimidazole compounds (Lig1 and Lig2) and the gold complexes were tested against three Leishmania species related to cutaneous manifestations of leishmaniasis. The free benzimidazole compounds showed no leishmanicidal activity. On the other hand, the gold(I and III) complexes have shown to possess significant activity against Leishmania in both stages of parasite, and the gold(III) complex with Lig2 exhibited expressive leishmanicidal activity with IC50 values below 5.7 μM. Also, the gold complexes showed high leishmania selectivity. The gold(I) complex with Lig1, for example, is almost 50 times more toxic for the parasite than for macrophages. Besides the leishmanicidal activity, all complexes exhibited toxic effect against SK-Mel 103 and Balb/c 3T3, cancer cells.

  8. Synthesis and characterization of anodized titanium-oxide nanotube arrays

    Energy Technology Data Exchange (ETDEWEB)

    Hu, Michael Z. [ORNL; Lai, Peng [University of Cincinnati; Bhuiyan, Md S [ORNL; Tsouris, Costas [ORNL; Gu, Baohua [ORNL; Paranthaman, Mariappan Parans [ORNL; Gabitto, Jorge [Prairie View A& M University; Harrison, L. D. [Prairie View A& M University

    2009-01-01

    Anodized titanium-oxide containing highly ordered, vertically oriented TiO2 nanotube arrays is a nanomaterial architecture that shows promise for diverse applications. In this paper, an anodization synthesis using HF-free aqueous solution is described. The anodized TiO2 film samples (amorphous, anatase, and rutile) on titanium foils were characterized with scanning electron microscopy, X-ray diffraction, and Raman spectroscopy. Additional characterization in terms of photocurrent generated by an anode consisting of a titanium foil coated by TiO2 nanotubes was performed using an electrochemical cell. A platinum cathode was used in the electrochemical cell. Results were analyzed in terms of the efficiency of the current generated, defined as the ratio of the difference between the electrical energy output and the electrical energy input divided by the input radiation energy, with the goal of determining which phase of TiO2 nanotubes leads to more efficient hydrogen production. It was determined that the anatase crystalline structure converts light into current more efficiently and is therefore a better photocatalytic material for hydrogen production via photoelectrochemical splitting of water.

  9. Gamma radiation-induced synthesis and characterization of Polyvinylpyrrolidone nanogels

    Science.gov (United States)

    Ges, A. A.; Viltres, H.; Borja, R.; Rapado, M.; Aguilera, Y.

    2017-01-01

    Due to the importance of bioactive peptides, proteins and drug for pharmaceutical purpose, there is a growing interest for suitable delivery systems, able to increase their bioavailability and to target them to the desired location. Some of the most studied delivery systems involve encapsulation or entrapment of drugs into biocompatible polymeric devices. A multitude of techniques have been described for the synthesis of nanomaterials from polymers, however, the use of ionizing radiation (γ, e-), to obtain nano- and microgels polymer is characterized by the possibility of obtaining products with a high degree of purity. Although, in the world, electronic radiation is used for this purpose, gamma radiation has not been utilized for these purposes. In this paper is developed the formulation the formulation of Polyvinylpyrrolidone (PVP) nanogels synthesized by gamma radiation techniques, for their evaluation as potential system of drug delivery. Experiments were performed in absence of oxygen using aqueous solutions of PVP (0.05% -1%). Crosslinking reactions were carried out at 25° C in a gamma irradiation chamber with a 60Co source (MPX-γ 30). The Viscosimetry, Light Scattering, X-Ray Diffraction and Transmission Electron Microscopy (TEM), were used as characterization techniques.

  10. Synthesis and characterization of thermoplastic polyurethane/nanoclay composites

    Energy Technology Data Exchange (ETDEWEB)

    Pizzatto, Leandro [Autotravi Borrachas e Plasticos Ltda, Caxias do Sul (Brazil); Lizot, Analice; Fiorio, Rudinei [Departamento de Engenharia Quimica, Universidade de Caxias do Sul, Caxias do Sul (Brazil); Amorim, Cintia L.; Machado, Giovanna [Programa de Pos-Graduacao em Materiais, Universidade de Caxias do Sul, Caxias do Sul (Brazil); Giovanela, Marcelo [Departamento de Fisica e Quimica, Universidade de Caxias do Sul, Caxias do Sul (Brazil); Zattera, Ademir J. [Departamento de Engenharia Quimica, Universidade de Caxias do Sul, Caxias do Sul (Brazil); Crespo, Janaina S. [Grupo de Materiais Elastomericos, Universidade de Caxias do Sul, Caxias do Sul (Brazil)], E-mail: jscrespo@ucs.br

    2009-03-01

    In this study thermoplastic polyurethane (TPU) composites were obtained with different nanoclay contents (0, 1, 3 for all cases and 10 wt.% in some cases). The nanoclay Cloisite (registered) 30B (C30B) was dispersed in the TPU matrix by melt processing (twin-screw extruder; TPU-E composites) and during bulk polymerization (TPU-S composites). The synthesis method involved the two-step bulk polymerization of polyesterpolyol (molecular weight 2000 g mol{sup -1}) and diphenylmethanediisocyanate (MDI) with 1,4-butanediol as the chain extender. The dispersion state of the nanoclay particles and its effect on the mechanical properties of the composites, before and after ageing, was investigated. The characterization of TPU/nanoclay composites was carried out by means of scanning electron microscopy (SEM) and X-ray diffraction (XRD). The mechanical characterization was performed through determination of the tensile and tear strengths. The TPU-E 3 wt.% composite showed the best improvement with increases in stress and strain at break (28% and 35%, respectively) and energy (88%), compared to the TPU-E (sample without nanoclay)

  11. Synthesis and characterization of porous hydroxyapatite and hydroxyapatite coatings

    Energy Technology Data Exchange (ETDEWEB)

    Nieh, T G; Choi, B W; Jankowski, A F

    2000-10-25

    A technique is developed to construct bulk hydroxyapatite (HAp) with different cellular structures. The technique involves the initial synthesis of nanocrystalline hydroxyapatite powder from an aqueous solution using water-soluble compounds and then followed by spray drying into agglomerated granules. The granules were further cold pressed and sintered into bulks at elevated temperatures. The sintering behavior of the HAp granules was characterized and compared with those previously reported. Resulting from the fact that the starting HAp powders were extremely fine, a relatively low activation energy for sintering was obtained. In the present study, both porous and dense structures were produced by varying powder morphology and sintering parameters. Porous structures consisting of open cells were constructed. Sintered structures were characterized using scanning electron microscopy and x-ray tomography. In the present paper, hydroxyapatite coatings produced by magnetron sputtering on silicon and titanium substrates will also be presented. The mechanical properties of the coatings were measured using nanoindentation techniques and microstructures examined using transmission electron microscopy.

  12. Pyrazine-based organometallic complex: synthesis, characterization, and supramolecular chemistry.

    Science.gov (United States)

    Bhowmick, Sourav; Chakraborty, Sourav; Das, Atanu; Rajamohanan, P R; Das, Neeladri

    2015-03-16

    The design, synthesis, and characterization of a new pyrazine-based ditopic platinum(II) organometallic complex are reported. The molecular structure of the organoplatinum pyrazine dipod was determined by single-crystal X-ray crystallography. The potential utility of this organometallic ditopic acceptor as a building block in the construction of neutral metallasupramolecular macrocycles containing the pyrazine motif was explored. Pyrazine motifs containing supramolecules were characterized by multinuclear NMR (including (1)H DOSY), mass spectrometry, and elemental analysis. The geometry of each supramolecular framework was optimized by employing the PM6 semiempirical molecular orbital method to predict its shape and size. The ability of the pyrazine-based organoplatinum complex to act as a host for nitroaromatic guest (2,4-dinitrotoluene and PA) molecules was explored by isothermal titration calorimetry (ITC). The binding stoichiometry and thermodynamic parameters of these host-guest complexation reactions were evaluated using ITC. Theoretical calculations were performed to obtain insight into the binding pattern between the organometallic host and nitroaromatic guests. The preferable binding propensity of the binding sites of complex 1 for both nitroaromatics (PA and 2,4-dinitrotoluene) determined by molecular simulation studies corroborates well with the experimental results as obtained by ITC experiments.

  13. Mechanochemical synthesis and characterization of pure Co$_2$B nanocrystals

    Indian Academy of Sciences (India)

    MUSTAFA BARIS; TUNCAY SIMSEK; ADNAN AKKURT

    2016-08-01

    Cobalt boride (Co$_2$B) is a significant transition metal boride having a wide range of usage area due to its high oxidation, abrasion and corrosion resistance as well as its superior electrochemical, magnetic and anisotropicproperties. In this study, pure Co2B nanocrystals were synthesized with Co, B$_2$O$_3$ and Mg as starting materials via the mechanochemical synthesis (MCS) method by high-energy planetary ball mill in a hardened steel vial withhardened steel balls. All the experiments were conducted under Ar atmosphere at different rotational speeds and at 20:1–30:1–40:1 ball-to-powder ratios. Leaching of Co$_2$B $+$ MgO powder mixtures occurred after milling andpurified with acetic acid and pure Co$_2$B nanocrystals were obtained in solid form. The Co2Bs were characterized through X-ray diffraction, scanning electronmicroscopy, vibrating samplemagnetometer, Brunauer–Emmett–Tellerand specific density analyses, and effects of synthesis parameters on product properties were revealed. Surface areas of the powders synthesized at 40:1 ball-to-powder ratio at different rotational speeds were measured as 21.14,40.36 and 52.33 m$^2$ g$^{−1}$, respectively. Crystallite sizes of Co$_2$B nanocrystals were between 7.27 and 9.84 nm and their specific density varied between 7.61 and 7.78 g cm$^{−3}$. It was determined that all samples were saturated and exhibited hysteresis and ferromagnetic behaviours, and saturation magnetization was between 35 and 50 emu g$^{−1}$.

  14. Nanocrystalline hydroxyapatite doped with magnesium and zinc: Synthesis and characterization

    Energy Technology Data Exchange (ETDEWEB)

    Kalita, Samar J. [Department of Mechanical, Materials and Aerospace Engineering, University of Central Florida, Orlando, FL 32816-2450 (United States)]. E-mail: samar@mail.ucf.edu; Bhatt, Himesh A. [Department of Mechanical, Materials and Aerospace Engineering, University of Central Florida, Orlando, FL 32816-2450 (United States)

    2007-05-16

    During recent years, there have been efforts in developing nanocrystalline bioceramics, to enhance their mechanical and biological properties for use in tissue engineering applications. In this research, we made an attempt to synthesize nanocrystalline bioactive hydroxyapatite (Ca{sub 10}(PO{sub 4}){sub 6}(OH){sub 2}, HAp) ceramic powder in the lower-end of nano-range (2-10 nm), using a simple low-temperature sol-gel technique and studied its densification behavior. We further studied the effects of metal ion dopants during synthesis on powder morphology, and the properties of the sintered structures. Calcium nitrate and triethyl phosphite were used as precursors for calcium and phosphorous, respectively, for sol-gel synthesis. Calculated quantities of magnesium oxide and zinc oxide were incorporated as dopants into amorphous dried powder, prior to calcination at 250-550 {sup o}C. The synthesized powders were analyzed for their phases using X-ray diffraction technique and characterized for powder morphology and particle size using transmission electron microscopy (TEM). TEM analysis showed that the average particle size of the synthesized powders were in the range of 2-10 nm. The synthesized nano-powders were uniaxially compacted and then sintered at 1250 {sup o}C and 1300 {sup o}C for 6 h, separately, in air. A maximum average sintered density of 3.29 g/cm{sup 3} was achieved in structures sintered at 1300 {sup o}C, developed from nano-powder doped with magnesium. Vickers hardness testing was performed to determine the hardness of the sintered structures. Uniaxial compression tests were performed to evaluate the mechanical properties. Bioactivity and biodegradation behavior of the sintered structures were assessed in simulated body fluid (SBF) and maintained in a dynamic state.

  15. Hydrothermal synthesis and characterization of zirconia based catalysts

    Energy Technology Data Exchange (ETDEWEB)

    Caillot, T., E-mail: Thierry.caillot@ircelyon.univ-lyon1.fr; Salama, Z.; Chanut, N.; Cadete Santos Aires, F.J.; Bennici, S.; Auroux, A.

    2013-07-15

    In this work, three equimolar mixed oxides ZrO{sub 2}/CeO{sub 2}, ZrO{sub 2}/TiO{sub 2}, ZrO{sub 2}/La{sub 2}O{sub 3} and a reference ZrO{sub 2} have been synthesized by hydrothermal method. The structural and surface properties of these materials have been fully characterized by X-ray diffraction, transmission electron microscopy, surface area measurement, chemical analysis, XPS, infrared spectroscopy after adsorption of pyridine and adsorption microcalorimetry of NH{sub 3} and SO{sub 2} probe molecules. All investigated mixed oxides are amphoteric and possess redox centers on their surface. Moreover, hydrothermal synthesis leads to catalysts with higher surface area and with better acid–base properties than classical coprecipitation method. Both Lewis and Brønsted acid sites are present on the surface of the mixed oxides. Compared to the other samples, the ZrO{sub 2}/TiO{sub 2} material appears to be the best candidate for further application in acid–base catalysis. - Graphical abstract: Mesoporous amorphous phase with a high surface area of titania zirconia mixed oxide obtained by hydrothermal preparation. - Highlights: • Three zirconia based catalysts and a reference were prepared by hydrothermal synthesis. • Mixed oxides present larger surface areas than the reference ZrO{sub 2}. • ZrO{sub 2}/TiO{sub 2} catalyst presents a mesoporous structure with high surface area. • ZrO{sub 2}/TiO{sub 2} catalyst presents simultaneously strong acidic and basic properties.

  16. Railroad Bridges

    Data.gov (United States)

    Department of Homeland Security — Bridges-Rail in the United States According to The National Bridge Inspection Standards published in the Code of Federal Regulations (23 CFR 650.3), a bridge isA...

  17. Chemically bonded hybrid systems from functionalized hydroxypyridine molecular bridge: characterization and photophysical properties.

    Science.gov (United States)

    Yan, Bing; Qian, Kai

    2009-01-01

    A series of novel photoactive hybrid materials with organic parts covalently linked to inorganic parts via the acylamino group have been assembled by sol-gel process. The organic parts as molecular bridge derive from alpha-hydroxypyridine (HP) functionalized by 3-(triethoxysilyl)-propyl isocyanate (TESPIC). Finally homogeneous, molecular-based hybrid materials with different microstructure (uniform spherical or clubbed) are obtained, in which no phase separation is observed. This may be ascribed as the different coordination behavior of metal ions (Eu3+ (Tb3+) or Zn2+). Red emission of Eu-HP-Si, green emission of Tb-HP-Si and violet-blue luminescence of Zn-HP-Si hybrids can be achieved within these molecular-based hybrid materials. Besides, both Eu(Tb) and Zn are introduced into the same hybrid systems (Eu(Zn)-HP-Si or Tb(Zn)-HP-Si) through the covalent Si-O bond, whose sphere particle size can be modified. Especially the photoluminescence behavior can be enhanced, suggesting that intramolecular energy transfer takes place between inert Zn2+ and Eu3+ (Tb3+) in the covalently bonded hybrid systems.

  18. Nanoparticle additives for multiphase systems: Synthesis, formulation and characterization

    Science.gov (United States)

    Kanniah, Vinod

    Study on nanoparticle additives in multiphase systems (liquid, polymer) are of immense interest in developing new product applications. Critical challenges for nanoparticle additives include their synthesis, formulation and characterization. These challenges are addressed in three application areas: nanofluids for engine lubrication, ultrathin nanocomposites for optical devices, and nanoparticle size distribution characterization. Nanoparticle additives in oligomer mixtures can be used to develop extended temperature range motor oils. A model system includes poly(alpha-olefin) based oligomers with a modest fraction of poly(dimethylsiloxane) oligomers along with graphite as nanoparticle additive. Partition coefficients of each oligomer are determined since the oligomer mixture phase separated at temperatures less than -15 °C. Also, the surface of graphite additive is quantitatively analyzed and modified via silanization for each oligomer. Thus, upon separation of the oligomer mixture, each functionalized graphite additive migrates to its preferred oligomers and forms a uniform dispersion. Similarly, nanoparticle additives in polymer matrices can be used to develop new low haze ultrathin film optical coatings. A model system included an acrylate monomer as the continuous phase with monodisperse or bidisperse mixtures of silica nanoparticles deposited on glass and polycarbonate substrates. Surface (root mean squared roughness, Wenzel's contact angle) and optical properties (haze) of these self assembled experimental surfaces were compared to simulated surface structures. Manipulating the size ratios of silica nanoparticle mixtures varied the average surface roughness and the height distributions, producing multimodal structures with different packing fractions. In both nanofluid and nanocomposite applications, nanoparticle additives tend to aggregate/agglomerate depending on various factors including the state of nanoparticles (powder, dispersion). A set of well-characterized

  19. Synthesis and characterization of zeolites prepared from industrial fly ash.

    Science.gov (United States)

    Franus, Wojciech; Wdowin, Magdalena; Franus, Małgorzata

    2014-09-01

    In this paper, we present the possibility of using fly ash to produce synthetic zeolites. The synthesis class F fly ash from the Stalowa Wola SA heat and power plant was subjected to 24 h hydrothermal reaction with sodium hydroxide. Depending on the reaction conditions, three types of synthetic zeolites were formed: Na-X (20 g fly ash, 0.5 dm(3) of 3 mol · dm(-3) NaOH, 75 °C), Na-P1 (20 g fly ash, 0.5 dm(3) of 3 mol · dm(-3) NaOH, 95 °C), and sodalite (20 g fly ash, 0.8 dm(3) of 5 mol · dm(-3) NaOH + 0.4 dm(3) of 3 mol · dm(-3) NaCl, 95 °C). As synthesized materials were characterized to obtain mineral composition (X-ray diffractometry, Scanning electron microscopy-energy dispersive spectrometry), adsorption properties (Brunauer-Emmett-Teller surface area, N2 isotherm adsorption/desorption), and ion exchange capacity. The most effective reaction for zeolite preparation was when sodalite was formed and the quantitative content of zeolite from X-ray diffractometry was 90 wt%, compared with 70 wt% for the Na-X and 75 wt% for the Na-P1. Residues from each synthesis reaction were the following: mullite, quartz, and the remains of amorphous aluminosilicate glass. The best zeolitic material as characterized by highest specific surface area was Na-X at almost 166 m(2) · g(-1), while for the Na-P1 and sodalite it was 71 and 33 m(2) · g(-1), respectively. The ion exchange capacity decreased in the following order: Na-X at 1.8 meq · g(-1), Na-P1 at 0.72 meq · g(-1), and sodalite at 0.56 meq · g(-1). The resulting zeolites are competitive for commercially available materials and are used as ion exchangers in industrial wastewater and soil decontamination.

  20. Design, synthesis, insecticidal activity, and structure-activity relationship (SAR): studies of novel triazone derivatives containing a urea bridge group based on transient receptor potential (TRP) channels.

    Science.gov (United States)

    Yang, Yan; Liu, Yuxiu; Song, Hongjian; Li, Yongqiang; Wang, Qingmin

    2016-11-01

    Numerous compounds containing urea bridge and biurea moieties are used in a variety of fields, especially as drugs and pesticides. To search for novel, environmentally benign and ecologically safe pesticides with unique modes of action, four series of novel triazone analogues containing urea, thiourea, biurea, and thiobiurea bridge, respectively, were designed and synthesized, according to various calcium ion channel inhibitors which act on transient receptor potential protein. Their structures were characterized by [Formula: see text] NMR, [Formula: see text] NMR, and HRMS. The insecticidal activities of the new compounds were obtained. The bioassay results indicated that compounds containing a thiourea bridge and a thiobiurea bridge exhibited excellent insecticidal activities against bean aphid. Specifically, compounds [Formula: see text], [Formula: see text], and [Formula: see text] exhibited 85, 90, and 95 % activities, respectively, at 10 mg/kg. Compounds [Formula: see text] (30 %), [Formula: see text] (35 %), [Formula: see text] (30 %), and [Formula: see text] (40 %) exhibited the approximate aphicidal activity of pymetrozine (30 %) at 5 mg/kg. In addition, some target compounds exhibited insecticidal activities against lepidopteran pests. From a molecular design standpoint, the information obtained in this study could help in the further design of new derivatives with improved insecticidal activities.

  1. Synthesis and characterization of covalently bound benzocaine graphite oxide derivative

    Science.gov (United States)

    Kabbani, Ahmad; Kabbani, Mohamad; Safadi, Khadija

    2015-09-01

    Graphite oxide (GO) derived materials include chemically functionalize or reduced graphene oxide (exfoliated from GO) sheets, assembled paper-like forms , and graphene-based composites GO consists of intact graphitic regions interspersed with sp3-hybridized carbons containing hydroxyl and epoxide functional groups on the top and bottom surfaces of each sheet and sp2-hybridized carbons containing carboxyl and carbonyl groups mostly at the sheet edges. Hence, GO is hydrophilic and readily disperses in water to form stable colloidal suspensions Due to the attached oxygen functional groups, GO was used to prepare different derivatives which result in some physical and chemical properties that are dramatically different from their bulk counterparts .The present work discusses the covalent cross linking of graphite oxide to benzocaine or ethyl ester of para-aminobenzoic acid,structure I,used in many over-the-counter ointment drug.Synthesis is done via diazotization of the amino group.The product is characterized via IR,Raman, X-ray photoelectron spectroscopy as well as electron microscopy.

  2. Encapsulated Nanoparticle Synthesis and Characterization for Improved Storage Fluids: Preprint

    Energy Technology Data Exchange (ETDEWEB)

    Glatzmaier, G. C.; Pradhan, S.; Kang, J.; Curtis, C.; Blake, D.

    2010-10-01

    Nanoparticles are typically composed of 50--500 atoms and exhibit properties that are significantly different from the properties of larger, macroscale particles that have the same composition. The addition of these particles to traditional fluids may improve the fluids' thermophysical properties. As an example, the addition of a nanoparticle or set of nanoparticles to a storage fluid may double its heat capacity. This increase in heat capacity would allow a sensible thermal energy storage system to store the same amount of thermal energy in half the amount of storage fluid. The benefit is lower costs for the storage fluid and the storage tanks, resulting in lower-cost electricity. The goal of this long-term research is to create a new class of fluids that enable concentrating solar power plants to operate with greater efficiency and lower electricity costs. Initial research on this topic developed molecular dynamic models that predicted the energy states and transition temperatures for these particles. Recent research has extended the modeling work, along with initiating the synthesis and characterization of bare metal nanoparticles and metal nanoparticles that are encapsulated with inert silica coatings. These particles possess properties that make them excellent candidates for enhancing the heat capacity of storage fluids.

  3. Synthesis and characterization of Ni-Zn ferrite nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Shahane, G.S., E-mail: shahanegs@yahoo.co [Department of Electronics, DBF Dayanand College of Arts and Science, Solapur 413002, Maharashtra (India); Kumar, Ashok; Arora, Manju; Pant, R.P.; Lal, Krishan [National Physical Laboratory, New Delhi (India)

    2010-04-15

    Nickel zinc ferrite nanoparticles Ni{sub x}Zn{sub 1-x}Fe{sub 2}O{sub 4} (x=0.1, 0.3, 0.5) have been synthesized by a chemical co-precipitation method. The samples were characterized by X-ray diffraction, Fourier transform infrared spectroscopy, electron paramagnetic resonance, dc magnetization and ac susceptibility measurements. The X-ray diffraction patterns confirm the synthesis of single crystalline Ni{sub x}Zn{sub 1-x}Fe{sub 2}O{sub 4} nanoparticles. The lattice parameter decreases with increase in Ni content resulting in a reduction in lattice strain. Similarly crystallite size increases with the concentration of Ni. The magnetic measurements show the superparamagnetic nature of the samples for x=0.1 and 0.3 whereas for x=0.5 the material is ferromagnetic. The saturation magnetization is 23.95 emu/g and increases with increase in Ni content. The superparamagnetic nature of the samples is supported by the EPR and ac susceptibility measurement studies. The blocking temperature increases with Ni concentration. The increase in blocking temperature is explained by the redistribution of the cations on tetrahedral (A) and octahedral (B) sites.

  4. Synthesis and characterization of phosphorescent platinum complexes containing phenylpyridazine

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Sang Jin; Kang, Seok; Lee, Seung Hee; Hwang, Kwang Jin; Park, Noh Kil; Kim, Young Sik

    2004-01-05

    Synthesis and characterization of a series of square planar Pt(II)-phenylpyridazine complexes are reported. The complexes have the general structure of (C-N)Pt(O-O), where HC-N is 3-phenyl-pyridazine (ppdz), 3-(3'-trifluoromethylphenyl)pyridazine (3'tfmppdz), 3-(3'-methoxyphenyl)-pyridazine (3'meoppdz), 3-(4'-methoxyphenyl)pyridazine (4'meoppdz), or 3-phenyl-6-chloro-pyridazine (6Clppdz) and HO-O is acetylacetone (Hacac). Reaction of K{sub 2}PtCl{sub 4} with a HC-N ligand forms the dimer, (C-N)Pt({mu}-Cl){sub 2}Pt(C-N), which is cleaved with Hacac to give the corresponding monomer, (C-N)Pt(O-O). The emission characteristics of these complexes are governed by the substituents of the cyclometalating ligands, showing emission {lambda}{sub max} values from 508 to 610 nm. Strong spin-orbit coupling of the platinum atom allows for the formally forbidden mixing of the {sup 1}MLCT with the {sup 3}MCLT and {sup 3}({pi}-{pi}*) states.

  5. Synthesis and Characterization of Metal Phosphates for Photocatalytic Applications

    KAUST Repository

    Al-Sabban, Bedour

    2012-07-01

    Solar energy is the most abundant efficient and important source of renewable energy. The objective of this study is to develop highly efficient visible light responsive photocatalysts for overall water splitting. This is done by using silver or copper containing materials. Phosphate compounds have caught much attention due to their rigid structure, thermal stability and resistance to chemical attacks. Solid phosphates can be prepared by direct solid-state reaction between metal cations and phosphate anions at high temperatures. Double metal phosphates of the Nasion-type structure had shown further technological importance. It has been reported that well-crystallized double metal phosphate particles have excellent ordering and cationic conduction channels in the Nasicon framework. In this study, several Nasion-type structured materials have been synthesized by solid-state method (e.g. CuTi2(PO4)3 and AgTi2(PO4)3) heated up under different temperatures (400–1100C) in N2 or air atmosphere. These materials were characterized by XRD, SEM, DR-UV-Vis spectroscopy and tested for photocatalytic applications. A new method for direct synthesis of photoelectrode on Ti Plate had been demonstrated. Further investigations on controlling the size and morphology for better performance of single and double metal phosphates will be done.

  6. Zinc impregnated cellulose nanocomposites: Synthesis, characterization and applications

    Science.gov (United States)

    Ali, Attarad; Ambreen, Sidra; Maqbool, Qaisar; Naz, Sania; Shams, Muhammad Fahad; Ahmad, Madiha; Phull, Abdul Rehman; Zia, Muhammad

    2016-11-01

    Nanocomposite materials have broad applicability due to synergistic effect of combined components. In present investigation, cellulose isolated from citrus peel waste is used as a supporting material; impregnation of zinc oxide nanoparticles via co-precipitation method. The characterization of nano composite is carried out through Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD) analysis, scanning electron microscopy (SEM) and Thermo-gravimetric analysis (TGA) resulting less than 10 μm cellulose fiber and approx. 50 nm ZnO NPs. Zinc oxide impregnated cellulose (ZnO-Cel) exhibited significant bacterial devastation property when compared to ZnO NPs or Cellulose via disc diffusion and colony forming unit methods. In addition, the ZnO-Cel exhibited significant total antioxidant, and minor DPPH free radical scavenging and total reducing power activities. The nano composite also showed time dependent increase in photocatalytic by effectively degrading methylene blue dye up to 69.5% under sunlight irradiation within 90 min. The results suggest effective utilization of cellulose obtained from citrus waste and synthesis of pharmacologically important nano-composites that can be exploited in wound dressing; defence against microbial attack and healing due to antioxidative property, furthermore can also be used for waste water treatment.

  7. Synthesis, characterization and gas sensing performance of aluminosilicate azide cancrinite

    Indian Academy of Sciences (India)

    A V BORHADE; T A KSHIRSAGAR; S G WAKCHAURE; A G DHOLI

    2016-10-01

    The present investigation deals with synthesis and gas sensing performance of Na$_8$[AlSiO$_4$]$_6$(N$_3$)$_{2.4}$(H$_2$O)$_{4.6}$ cancrinite-based thick film. The product obtained was characterized by Fourier transform infrared spectroscopy, X-ray diffraction, scanning electron microscope, thermogravimetric analysis and magic-angle spin nuclear magneticresonance (MAS NMR). The crystal structure of the product was determined from X-ray powder diffraction data by applying Rietveld refinement. Refinement showed that azide cancrinite crystallize in the space group P6$_3$. Alternate arrangement of Si and Al atoms was confirmed by single intense peak of MAS NMR analysis. For the first time, this study reports the gas sensing performance of aluminosilicate azide cancrinite. The effect of annealing andoperating temperature on gas sensing characteristic of azide cancrinite thick film is investigated systematically for various gases at different operating temperatures. This sensor was observed to be highly sensitive and selective toammonia gas.

  8. Synthesis and characterization of novel Schiff bases containing pyrimidine unit

    Directory of Open Access Journals (Sweden)

    Jumbad H. Tomma

    2014-01-01

    Full Text Available The work involves synthesis of novel Schiff base derivatives containing a pyrimidine unit starting with chalcones. 4-Aminoacetophenone was reacted with 4-nitrobenzaldehyde or 4-chlorobenzaldehyde in basic medium giving chalcones, [I]a and [I]b, respectively, by Claisen-Schemidt reaction. The chalcones [I]a and [I]b were reacted with urea in HCl medium giving oxopyrimidines, [II]a and [II]b. They were also reacted with thiourea in basic medium to give thioxopyrimidines, [III]a and [III]b. The novel mono and bis Schiff bases, [VIII]na, [VIII]nb, [IX]na, [IX]nb, [X]na, [X]nb, [XI]na, and [XI]nb were synthesized by the reaction of pyrimidine derivatives; oxopyrimdines, [II]a and [II]b and thioxopyrimidines, [III]a and [III]b with 4-(4′-n-alkoxybenzoloxybenzaldehyde [VI] and polymethylene-α,ω-bis-4-oxybenzaldehydes [VII]m, respectively, in dry benzene using drops of glacial acetic acid as a catalyst. The synthesized compounds were characterized by melting points, elemental analysis, FTIR, and 1H NMR spectroscopy.

  9. Synthesis and characterization of furazan energetics ADAAF and DOATF

    Energy Technology Data Exchange (ETDEWEB)

    Veauthier, Jaqueline M [Los Alamos National Laboratory; Chavez, David E [Los Alamos National Laboratory; Tappan, Bryce C [Los Alamos National Laboratory; Parrish, Damon [Los Alamos National Laboratory

    2009-01-01

    The synthesis and structural characterization of bis[4-aminofurazanyl-3-azoxy]azofurazan (ADAAF) and 3,4:7,8:11,12:15,16-tetrafurazano-1,2,5,6,9,10,13,14-octaazacyclohexadeca-1,3,5,7,9,11,13,15-octaene-1,10-dioxide (DOATF) are described. Explosive sensitivity properties of both materials were determined. The heat of formation of ADAAF was measured to be 300 kcal/mol while the detonation velocity and pressure of ADAAF were measured to be 7.88 km/s and 299 kbar, respectively at 94% theoretical maximum density. We also investigated the burning rate characteristics of ADAAF. We have reported two new synthetic procedures and the first X-ray crystal structures for the azoxyfurazan compounds ADAAF (4) and DOATF (5). These new energetic materials were found to be significantly more sensitive to mechanical initiation than DAAF (3) and the heat of formation of 4 was found to be nearly three times that of 3. The detonation velocity and pressure for 4 are comparable to 2 while its burning rate characteristics are similar to HMX. Further studies to elucidate sensitivity behavior are ongoing.

  10. Synthesis, characterization and physiological activity of some novel isoxazoles.

    Directory of Open Access Journals (Sweden)

    NITIN G. GHODILE

    2012-07-01

    Full Text Available Hushare VJ, Rajput PR, Malpani MO, Ghodile NG. 2012. Synthesis, characterization and physiological activity of some novel isoxazoles. Nusantara Bioscience 4: 81-85. A series of chlorosubstituted 4-aroylisoxazoles have been synthesized by refluxing chlorosubstituted-3-aroylflavones and 3-alkoylchromone with hydroxylamine hydrochloride in dioxane medium containing 0.5 mL piperidine. Chlorosubstituted-3-aroylflavones and chlorosubstituted-3-alkoylchromone were prepared by refluxing them separately with iodine crystal in ethanol. Initially chlorosubstituted-3-aroylflavanones and 3-alkoylchromanone were prepared by the interaction of different aromatic and aliphatic aldehydes with 1-(2’-hydroxy-3’,5’-dichlorophenyl-3-phenyl-1,3-propanedione. Constitutions of synthesized compounds were confirmed on the basis of elemental analysis, molecular weight determination, UV-Visible, I.R. and 1H-NMR spectral data. The titled compounds were evaluated for their growth promoting activity on some flowering plants viz. Papaver rhoeas, Calendula officinalise, Gladiola tristis, Gaillardia aristata, Dianthus chinensis, and Iberis sp. (candytuft. The results indicate that applicated plants had higher shoots and more number of leaves.

  11. Synthesis and Characterization of Mixed Metal Oxide Nanocomposite Energetic Materials

    Energy Technology Data Exchange (ETDEWEB)

    Gash, A; Pantoya, M; Jr., J S; Zhao, L; Shea, K; Simpson, R; Clapsaddle, B

    2003-11-18

    In the field of composite energetic materials, properties such as ingredient distribution, particle size, and morphology, affect both sensitivity and performance. Since the reaction kinetics of composite energetic materials are typically controlled by the mass transport rates between reactants, one would anticipate new and potentially exceptional performance from energetic nanocomposites. We have developed a new method of making nanostructured energetic materials, specifically explosives, propellants, and pyrotechnics, using sol-gel chemistry. A novel sol-gel approach has proven successful in preparing metal oxide/silicon oxide nanocomposites in which the metal oxide is the major component. Two of the metal oxides are tungsten trioxide and iron(III) oxide, both of which are of interest in the field of energetic materials. Furthermore, due to the large availability of organically functionalized silanes, the silicon oxide phase can be used as a unique way of introducing organic additives into the bulk metal oxide materials. As a result, the desired organic functionality is well dispersed throughout the composite material on the nanoscale. By introducing a fuel metal into the metal oxide/silicon oxide matrix, energetic materials based on thermite reactions can be fabricated. The resulting nanoscale distribution of all the ingredients displays energetic properties not seen in its microscale counterparts due to the expected increase of mass transport rates between the reactants. The synthesis and characterization of these metal oxide/silicon oxide nanocomposites and their performance as energetic materials will be discussed.

  12. Synthesis and Characterization of Molybdenum Disulfide Nanoflowers and Nanosheets: Nanotribology

    Directory of Open Access Journals (Sweden)

    S. V. Prabhakar Vattikuti

    2015-01-01

    Full Text Available This paper reports the solvothermal synthesis of MoS2 nanoflowers and nanosheets. The nanoflowers have a mean diameter of about 100 nm and were obtained using thioacetamide (C2H5NS as a sulfur source. The few layered nanosheets were obtained using thiourea (CH4N2S as a sulfur source. The obtained powders were characterized using powder X-ray diffraction (XRD, scanning electron microscopy (SEM with energy dispersive spectroscopy (EDS, and transmission electron microscopy (TEM. The lubricating effect of MoS2 nanoflowers and nanosheets were analyzed using four-ball test, the topography of the wear scar was analyzed using SEM, EDS, and 3D surface profilometry. The relationship between the tribological properties and morphology of the materials was determined. It is observed that the engine oil containing the MoS2 nanomaterials penetrated more easily into the interface space, and it formed a continuous film on the interface surface. The tribological performance showed that the synthesized nanosheets had superior antiwear and friction-reducing properties as a lubrication additive compared with nanoflowers. Also, the wear scar of balls lubricated with nanoflowers revealed a larger diameter compared to nanosheets. In conclusion, nanosheets dispensed in oil have better tribological performance compared to nanoflowers oil in terms of capability to reduce friction.

  13. Synthesis and characterization of MoS2 nanosheets.

    Science.gov (United States)

    Deokar, G; Vignaud, D; Arenal, R; Louette, P; Colomer, J-F

    2016-02-19

    Here, we report on the synthesis of MoS2 nanosheets using a simple two-step additive-free growth technique. The as-synthesized nanosheets were characterized to determine their structure and composition, as well as their optical properties. The MoS2 nanosheets were analyzed by scanning electron microscopy, transmission electron microscopy (TEM), including high-resolution scanning TEM imaging and energy-dispersive x-ray spectroscopy, x-ray photoelectron spectroscopy (XPS), Raman spectroscopy and photoluminescence (PL). The as-produced MoS2 nanosheets are vertically aligned with curved edges and are densely populated. The TEM measurements confirmed that the nanosheets have the 2H-MoS2 crystal structure in agreement with the Raman results. The XPS results revealed the presence of high purity MoS2. Moreover, a prominent PL similar to mechanically exfoliated few and mono-layer MoS2 was observed for the as-grown nanosheets. For the thin (≤50 nm) nanosheets, the PL feature was observed at the same energy as that for a direct band-gap monolayer MoS2 (1.83 eV). Thus, the as-produced high-quality, large-area, MoS2 nanosheets could be potentially useful for various optoelectronic and catalysis applications.

  14. Synthesis, physicochemical, structural and rheological characterizations of carboxymethyl xanthan derivatives.

    Science.gov (United States)

    Yahoum, Madiha M; Moulai-Mostefa, Nadji; Le Cerf, Didier

    2016-12-10

    The aim of this work was to synthesize a carboxymethylated xanthan (CMXG) via an etherification reaction between different ratios (2, 4, and 6) of xanthan gum (XG) and monochloroacetic acid (MCAA) using the Williamson synthesis method. The synthetized products were characterized in terms of their physico-chemical and rheological properties. Both FTIR and proton nuclear magnetic resonance (H(1) NMR) analyses confirmed the grafting of carboxymethyl groups on xanthan hydroxyl groups. The obtained results demonstrated that the degree of substitution was proportional to the chloroacetic acid and xanthan gum ratios. The obtained carboxymethyl derivatives presented greater hydrophilicity and lower molecular weights with increasing degrees of substitution than native xanthan gum. The rheological study revealed that the viscosity of the CMXG derivatives decreased with the degree of substitution and with the conservation of the shear-thinning and weak gel behaviours. The flow curves suggested the existence of two different populations of particles consisting of CMXG particles with a smaller average size and a second population formed by the residual fractions of native XG particles. It was also found that the elastic modulus of XG was largely higher than that of the CMXG derivatives and decreased with increasing DS. For the CMXG derivatives, two regions of viscoelastic behaviour were observed, which were separated by a crossover point corresponding to the critical frequency and relaxation time, i.e., the time required for stress relaxation.

  15. Microwave Synthesis, Characterization, and Photoluminescence Properties of Nanocrystalline Zirconia

    Directory of Open Access Journals (Sweden)

    A. K. Singh

    2014-01-01

    Full Text Available We report synthesis of ZrO2 nanoparticles (NPs using microwave assisted chemical method at 80°C temperature. Synthesized ZrO2 NPs were calcinated at 400°C under air atmosphere and characterized using FTIR, XRD, SEM, TEM, BET, and EDS for their formation, structure, morphology, size, and elemental composition. XRD results revealed the formation of mixed phase monoclinic and tetragonal ZrO2 phases having crystallite size of the order 8.8 nm from most intense XRD peak as obtained using Scherrer formula. Electron microscope analysis shows that the NPs were less than 10 nm and highly uniform in size having spherical morphology. BET surface area of ZrO2 NPs was found to be 65.85 m2/g with corresponding particle size of 16 nm. The band gap of synthesized NPs was found to be 2.49 eV and PL spectra of ZrO2 synthesized NPs showed strong peak at 414 nm, which corresponds to near band edge emission (UV emission and a relatively weak peak at 475 and 562 nm.

  16. Microwave Synthesis, Characterization, and Photoluminescence Properties of Nanocrystalline Zirconia

    Science.gov (United States)

    Singh, A. K.; Nakate, Umesh T.

    2014-01-01

    We report synthesis of ZrO2 nanoparticles (NPs) using microwave assisted chemical method at 80°C temperature. Synthesized ZrO2 NPs were calcinated at 400°C under air atmosphere and characterized using FTIR, XRD, SEM, TEM, BET, and EDS for their formation, structure, morphology, size, and elemental composition. XRD results revealed the formation of mixed phase monoclinic and tetragonal ZrO2 phases having crystallite size of the order 8.8 nm from most intense XRD peak as obtained using Scherrer formula. Electron microscope analysis shows that the NPs were less than 10 nm and highly uniform in size having spherical morphology. BET surface area of ZrO2 NPs was found to be 65.85 m2/g with corresponding particle size of 16 nm. The band gap of synthesized NPs was found to be 2.49 eV and PL spectra of ZrO2 synthesized NPs showed strong peak at 414 nm, which corresponds to near band edge emission (UV emission) and a relatively weak peak at 475 and 562 nm. PMID:24578628

  17. Synthesis and characterization of molybdenum incorporated mesoporous aluminophosphate

    Science.gov (United States)

    Ho, Li-Ngee; Ikegawa, Tasuku; Nishiguchi, Hiroyasu; Nagaoka, Katsutoshi; Takita, Yusaku

    2006-07-01

    A synthesis of molybdenum incorporated mesoporous aluminophosphate with long-chain n-alkylamine as template material had been prepared under non-aqueous condition. These materials were extensively characterized by using X-ray diffraction (XRD), nitrogen sorption isotherms, nuclear magnetic resonance of 27Al and 31P (NMR), inductive coupled plasma (ICP), electron spin resonance (ESR), Fourier transform infrared (FTIR) and thermogravimetric-differential thermal analysis (TG-DTA). Morphology of the materials had been observed by using transmission electron microscope (TEM) that revealed the mesoporous materials possessed wormhole-like structures. Alkaline solvent extraction using n-butylamine/ethanol had been efficiently removed the n-alkylamine from the mesoporous samples which yielded BET surface areas around 550-730 m 2/g. BJH analysis showed a narrow pore size distribution which increased with increasing of the carbon chain length of alkylamine (template). Valence state and coordination of the molybdenum in the obtained samples were investigated by using ESR and FTIR where it was found that Mo 4+ and Mo 6+ molybdenum species existed in the molybdenum incorporated mesoporous aluminophosphate in tetrahedral coordination.

  18. Synthesis, characterization and in vivo evaluation of biocompatible ferrogels

    Science.gov (United States)

    Lopez-Lopez, M. T.; Rodriguez, I. A.; Rodriguez-Arco, L.; Carriel, V.; Bonhome-Espinosa, A. B.; Campos, F.; Zubarev, A.; Duran, J. D. G.

    2017-06-01

    A hydrogel is a 3-D network of polymer chains in which water is the dispersion medium. Hydrogels have found extensive applications in the biomedical field due to their resemblance to living tissues. Furthermore, hydrogels can be endowed with exceptional properties by addition of synthetic materials. For example, magnetic field-sensitive gels, called ferrogels, are obtained by embedding magnetic particles in the polymer network. Novel living tissues with unique magnetic field-sensitive properties were recently prepared by 3-D cell culture in biocompatible ferrogels. This paper critically reviews the most recent progress and perspectives in their synthesis, characterization and biocompatibility evaluation. Optimization of ferrogels for this novel application requires low-density, strongly magnetic, multi-domain particles. Interestingly, the rheological properties of the resulting ferrogels in the absence of field were largely enhanced with respect to nonmagnetic hydrogels, which can only be explained by the additional cross-linking imparted by the embedded magnetic particles. Remarkably, rheological measurements under an applied magnetic field demonstrated that ferrogels presented reversibly tunable mechanical properties, which constitutes a unique advantage with respect to nonmagnetic hydrogels. In vivo evaluation of ferrogels showed good biocompatibility, with only some local inflammatory response, and no particle migration or damage to distant organs.

  19. Synthesis and Characterization of Binuclear Schiff Base Complexes of Nickel, Copper, and Manganese.

    Science.gov (United States)

    1983-11-04

    D-Ri35 493 SYNTHESIS AND CHRACTERILATION OF BINUCLEAR SCHIFF BASE i/i COMPLEXES OF NICK-.U) ROCHESTER UNIV NV DEPT OF CHEMISTRY B C WHITMIORE ET AL...RESEARCH Contract NOO014-83-K-0154 fl Task No. NR 634-742 TECHNICAL REPORT NO. 1 ,Z Synthesis and Characterization of Binuclear Schiff Base Complexes

  20. Characterization of Spermatogonial Stem Cells Lacking Intercellular Bridges and Genetic Replacement of a Mutation in Spermatogonial Stem Cells

    OpenAIRE

    2012-01-01

    Stem cells have a potential of gene therapy for regenerative medicine. Among various stem cells, spermatogonial stem cells have a unique characteristic in which neighboring cells can be connected by intercellular bridges. However, the roles of intercellular bridges for stem cell self-renewal, differentiation, and proliferation remain to be elucidated. Here, we show not only the characteristics of testis-expressed gene 14 (TEX14) null spermatogonial stem cells lacking intercellular bridges but...

  1. Synthesis, crystal structure and Thermogravimetry of ortho-phthalic acid bridged coordination polymer of Copper(II)

    Indian Academy of Sciences (India)

    BABITA SARMA; SAURAV BHARALI; DIGANTA KUMAR DAS

    2016-06-01

    Coordination polymer of Cu(II) bridged by o-phthalic acid alone is not known. The reaction of$CuCl_{2}.2H_{2}O$ with (2-butoxycarbonyl)benzoic acid yielded three dimensional coordination polymer bridged byo-phthalic acid. X-ray crystal structure shows structure with monoclinic P21/c space group. o-Phthalic acidmolecules act as bridge between two Cu(II), one carboxylate binds to one Cu(II) as bidentate while the othercarboxylate binds to another Cu(II) as monodentate. The four planar co-ordination positions of Cu(II) aresatisfied by two chelated carboxylates while fifth and sixth co-ordination positions are satisfied by monodentatecarboxylates. EPR and TGA of the coordination polymer are also reported.

  2. Synthesis and Characterization of Composite UPR/Fe3O4 for Its Use as Electromagnetic Wave Absorber

    Science.gov (United States)

    Yusmaniar; Adi, W. A.; Taryana, Y.; Muzaki, R.

    2017-05-01

    Synthesis and characterization of UPR/Fe3O4 composite were performed to evaluate its potency as a electromagnet absorbent. The composite was prepared from the mixture of unsaturated polyester resin and magnetite powder of iron oxide. Fe3O4 was used as filler and unsaturated polyester resins (UPR) was used as a matrix. Fe3O4 magnetite was synthesized from iron objects using electro synthesis method. The raw material was blended in the beaker glass for 120 min and then pressed at temperature of 60 °C for 30 min. The composite is in a semi-crystalline form that consists of amorphous matrix and the various crystalline fillers. The functional group’s analysis of the composite showed that crosslink (bridges) was formed between the chains of individual polymer and between Fe3O4 magnetite filler and UPR matrix. The performance of microwave absorbent measured by VNA method showed the highest RL at the frequency of 10.44 GHz and 11.74 dB. This value was achieved with a composition of 10wt% Fe3O4 and 90wt% UPR. We concluded that the composite of UPR/Fe3O4 has been successfully demonstrated as an electromagnetic wave absorber.

  3. Synthesis and Characterization of Chemically Etched Nanostructured Silicon

    KAUST Repository

    Mughal, Asad Jahangir

    2012-05-01

    Silicon is an essential element in today’s modern world. Nanostructured Si is a more recently studied variant, which has currently garnered much attention. When its spatial dimensions are confined below a certain limit, its optical properties change dramatically. It transforms from an indirect bandgap material that does not absorb or emit light efficiently into one which can emit visible light at room temperatures. Although much work has been conducted in understanding the properties of nanostructured Si, in particular porous Si surfaces, a clear understanding of the origin of photoluminescence has not yet been produced. Typical synthesis approaches used to produce nanostructured Si, in particular porous Si and nanocrystalline Si have involved complex preparations used at high temperatures, pressures, or currents. The purpose of this thesis is to develop an easier synthesis approach to produce nanostructured Si as well as arrive at a clearer understanding of the origin of photoluminescence in these systems. We used a simple chemical etching technique followed by sonication to produce nanostructured Si suspensions. The etching process involved producing pores on the surface of a Si substrate in a solution containing hydrofluoric acid and an oxidant. Nanocrystalline Si as well as nanoscale amorphous porous Si suspensions were successfully synthesized using this process. We probed into the phase, composition, and origin of photoluminescence in these materials, through the use of several characterization techniques. TEM and SEM were used to determine morphology and phase. FT-IR and XPS were employed to study chemical compositions, and steady state and time resolved optical spectroscopy techniques were applied to resolve their photoluminescent properties. Our work has revealed that the type of oxidant utilized during etching had a significant impact on the final product. When using nitric acid as the oxidant, we formed nanocrystalline Si suspensions composed of

  4. Synthesis and Characterization of Polymer-Templated Magnetic Nanoparticles

    Science.gov (United States)

    Tamakloe, Beatrice

    This research reports on the investigation into the synthesis and stabilization of iron oxide nanoparticles for theranostic applications using amine-epoxide polymers. Although theranostic agents such as magnetic nanoparticles have been designed and developed for a few decades, there is still more work that needs to be done with the type of materials that can be used to stabilize or functionalize these particles if they are to be used for applications such as drug delivery, imaging and hyperthermia. For in-vivo applications, it is crucial that organic coatings enclose the nanoparticles in order to prevent aggregation and facilitate efficient removal from the body as well as protect the body from toxic material. The objective of this thesis is to design polymer coated magnetite nanoparticles with polymers that are biocompatible and can stabilize the iron oxide nanoparticle to help create mono-dispersed particles in solution. It is desirable to also have these nanoparticles possess high magnetic susceptibility in response to an applied magnetic field. The co-precipitation method was selected because it is probably the simplest and most efficient chemical pathway to obtain magnetic nanoparticles. In literature, cationic polymers such as Polyethylenimine (PEI), which is the industry standard, have been used to stabilize IONPs because they can be used in magnetofections to deliver DNA or RNA. PEI however is known to interact very strongly with proteins and is cytotoxic, so as mentioned previously the Iron Oxide nanoparticles (IONPs) synthesized in this study were stabilized with amine-epoxide polymers because of the limitations of PEI. Four different amine-epoxide polymers which have good water solubility, biodegradability and less toxic than PEI were synthesized and used in the synthesis and stabilization of the magnetic nanoparticles and compared to PEI templated IONPs. These polymer-templated magnetic nanoparticles were also characterized by size, surface charge, Iron

  5. Synthesis and characterization of environmentally friendly fluorescent particle tracers

    Science.gov (United States)

    Tauro, Flavia; Porfiri, Maurizio; Rapiti, Emiliano; Grimaldi, Salvatore

    2013-04-01

    Tracers are widely used in experimental fluid mechanics and hydrology to investigate complex flows and water cycle processes. Commonly used tracers include dyes, artificial tracers, naturally occurring isotopes and chemicals, microorganisms, and DNA-based systems. Tracers should be characterized by low detection limits and high accuracy in following water paths and flow structures. For natural studies, tracers are also expected to be nontoxic and with low sorption affinity to natural substrates to minimize losses in the environment. In this context, while isotopes are completely natural, their use in field studies is limited by their ubiquity and, therefore, by the high uncertainty in data processing methodologies. Further, the use of dyes and artificial tracers can be hampered by extremely low detection limits due to dilution in natural streams and microorganisms, while DNA-based system may require physical sampling and time-consuming functionalization and detection procedures. In this work, we present the synthesis and characterization of fluorescent beads incorporating an eco-compatible fluorophore for environmental and laboratory applications. The particles are synthesized from natural beeswax through an inexpensive thermal procedure and can be engineered to present variable densities and diameters. A thorough characterization of their surface morphology at the nanoscale, crystal structure and size, chemical composition, and dye incorporation into the beeswax matrix is described by using a wide array of microscopy techniques. In addition, the particle fluorescence response is studied by performing excitation and emission scans on melted beeswax bead samples. The feasibility of using the synthesized particles in environmental settings is assessed through the design of ad-hoc weathering agent experiments where the beads are exposed to high energy radiation and hot water. Further, a proof of concept test is described to understand the particles' potential as a

  6. Synthesis, characterization, and reactivity of sulfided hexanuclear molybdenum cluster compounds

    Energy Technology Data Exchange (ETDEWEB)

    Spink, D.

    1990-09-21

    Hexanuclear molybdenum clusters with mixed chloride and sulfide bridging ligands were prepared by reacting {alpha}-MoCl{sub 2} with sodium hydrosulfide in the presence of sodium butoxide. The resulting species, Mo{sub 6}Cl{sub (8-x)}S{sub x}{center dot}npy(x {congruent} 3.6, n {congruent} 4, py = pyridine), was pyrophoric and insoluble. The mixed sulfide chloride cluster species Mo{sub 6}S{sub 4}Cl{sub 4}{center dot}6OPEt{sub 3} and Mo{sub 6}S{sub {approximately}5}Cl{sub {approximately}3}{center dot}6PEt{sub 3} and Mo{sub 6}S{sub 8}{center dot}6PEt{sub 3} were isolated and characterized. Phosphorus-31 nuclear magnetic resonance, electron paramagnetic resonance, and UV/visible spectra were obtained for each fraction. The completely sulfided cluster, Mo{sub 6}S{sub 8}{center dot}6PEt{sub 3}, was prepared similarly and used in various experiments as a possible precursor to Chevrel phase materials of the type Mo{sub 6}S{sub 8}or M{sub n}Mo{sub 6}S{sub 8}. With the goal of removing all of the triethylphosphine ligands, Mo{sub 6}S{sub 8}{center dot}6PEt{sub 3} was reacted with the transition metal carbonyls molybdenum hexacarbonyl and dicobalt octacarbonyl. Reaction on the molecular sulfide cluster with copper(I) chloride in toluene gave a completely insoluble product. The reaction of Mo{sub 6}S{sub 8}{center dot}6PEt{sub 3} with propylene sulfide gave a product whose infrared spectra showed only very weak peaks associated with coordinated triethylphosphine. The elemental analysis of this product fit the formula Mo{sub 6}S{sub 8}{center dot}5SPEt{sub 3}. Reactivity of the outer ligands of the Mo{sub 6}S{sub 8}{center dot}npy and Mo{sub 6}S{sub 8}{center dot}(6{minus}x)PrNH{sub x} clusters were investigated. Crystalline Mo{sub 6}S{sub 8}{center dot}6THT was recovered from the reaction of the n-propylamine derivative with THT. A crystal structure determination was done. 87 refs., 12 fig., 15 tabs.

  7. Nobel metal-TiO2 nanocomposites : synthesis, characterization and catalytic activity

    OpenAIRE

    Nascimento, Ana Cláudia Lobão do

    2016-01-01

    The work presented in this thesis is focused on the synthesis, characterization and catalytic activity of gold-TiO2 composites. We wanted to take advantage of the experience of the Colloid Chemistry Group, whose activity is strongly focused on the synthesis, characterization and evaluation of the formation mechanism of metal nanocrystals (mainly gold and silver) with size and shape control, which allows a fine-tuning of the optical response of these colloids in the UV-vis-NIR spectral range. ...

  8. Synthesis and Characterization of Organic Impurities in Bortezomib Anhydride Produced by a Convergent Technology

    Science.gov (United States)

    Ivanov, Andrey S.; Shishkov, Sergey V.; Zhalnina, Anna A.

    2012-01-01

    A profile of impurities in bortezomib anhydride, produced by a recently developed convergent technology, has been characterized. HPLC-MS analysis of the drug essence revealed three impurities: an epimer of bortezomib, resulting from partial racemization of l-phenylalanine’s stereogenic center during the chemical synthesis, and two epimeric products of oxidative degradation of bortezomib, in which boron is replaced by the OH group. The impurities were obtained by chemical synthesis and characterized by physical methods. PMID:22396904

  9. Design, Synthesis, and Characterization of High Performance Polymer Electrolytes for Printed Electronics and Energy Storage

    Science.gov (United States)

    2016-03-31

    linked in a second annealing step, thereby providing greatly enhanced toughness. The ABA triblock was a poly(styrene-b- ethylene oxide -b-styrene...AFRL-AFOSR-VA-TR-2016-0168 Design, Synthesis , and Characterization of High Performance Polymer Electrolytes for Printed Electronics and Energy...Sep 2015 4. TITLE AND SUBTITLE Design, Synthesis , and Characterization of High Performance Polymer Electrolytes for Printed Electronics and Energy

  10. Synthesis and spectra of a kind of novel longer-wavelength benzoxazole indole styryl cyanine dye with a carbazole-bridged chain.

    Science.gov (United States)

    Fei, Xuening; Gu, Yingchun; Li, Chao; Liu, Yuru; Yu, Lu

    2013-01-01

    Based on cyanine dye probe oxazole yellow (YO) and Cy(3), a series of novel styryl cyanine dyes were designed and synthesized. Carbazole was inserted into the structures of YO and Cy(3) to act as a bridge to link the benzoxazole and indole group. This modification resulted in a novel kind of benzoxazole indole styryl cyanine dye with a carbazole-bridged chain. The dyes were characterized by (1)HNMR and MS. The spectra of the novel dyes were also performed and the results showed that the maximum emission wavelength of the carbazole styryl cyanine dye was shifted red, the Stokes shift increased and the fluorescence intensity enhanced compared with those of YO and Cy(3). These results indicated that the novel dye could be used as an excellent fluorescent probe in biological labeling.

  11. Study on the Synthesis and Spectra of a Novel Kind of Carbozole Benzothiazole Indole Styryl Cyanine Dye with a Carbazole Bridged Chain.

    Science.gov (United States)

    Fei, Xuening; Hao, Yachao; Gu, Yingchun; Li, Chao; Yu, Lu

    2014-03-01

    Based on the frequently-used cyanine dye probe thiazole orange (TO) and Cy3, a novel kind of styryl cyanine dye was designed and synthesized. Carbazole was inserted into the structures of two cyanine dyes, TO and Cy3, to act as a bridge to link the benzothiazole and indole. This modification resulted in a novel kind of carbozole benzothiazole indole cyanine dye with a carbazole-bridged chain. The dyes were characterized by HNMR and MS. The spectra of the novel dyes were also studied and the results showed that the fluorescence wavelength of novel carbazole benzothiazole indole cyanine dye shifted red, the Stokes shift and Fluorescence quantum yields increased and the fluorescence intensity was enhanced compared to that of TO. These results indicated that the novel dye could be used as an excellent fluorescent probe in biological labeling.

  12. Synthesis and Characterization of Silver Nanoparticles for an Undergraduate Laboratory

    Science.gov (United States)

    Orbaek, Alvin W.; McHale, Mary M.; Barron, Andrew R.

    2015-01-01

    The aim of this simple, quick, and safe laboratory exercise is to provide undergraduate students an introduction to nanotechnology using nanoparticle (NP) synthesis. Students are provided two procedures that allow for the synthesis of different yet controlled sizes of silver NPs. After preparing the NPs, the students perform UV-visible…

  13. Synthesis and Characterization of Silver Nanoparticles for an Undergraduate Laboratory

    Science.gov (United States)

    Orbaek, Alvin W.; McHale, Mary M.; Barron, Andrew R.

    2015-01-01

    The aim of this simple, quick, and safe laboratory exercise is to provide undergraduate students an introduction to nanotechnology using nanoparticle (NP) synthesis. Students are provided two procedures that allow for the synthesis of different yet controlled sizes of silver NPs. After preparing the NPs, the students perform UV-visible…

  14. Synthesis and Characterization of DNase 1-Stabilized Gold Nanoclusters

    Science.gov (United States)

    2014-10-01

    biomolecule , and toxic synthesis protocols. For example, organic dyes such as fluorescein isothiocyanate (FITC) green and diamidino-2-phenylindole (DAPI...we present a new approach for biomolecule mediated synthesis of AuNCs. We have for the first time used DNase 1 to synthesize AuNCs of multiple

  15. 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)

    2015-09-30

    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

  16. Synthesis, crystal structure and magnetic properties of terephthalate-isophthalete- and phthalate-bridged copper (II) dinuclear complexes

    Energy Technology Data Exchange (ETDEWEB)

    Cano, J.; De Munno, G.; Sanz, J.L.; Ruiz, R.; Lloret, F.; Faus, J.; Julve, M.

    1997-09-01

    The ability of the dianions of the terephthalic (H{sub 2}ta), isophthalic (H{sub 2} ita) and phthalic (H{sub 2} phta) acids both to act as bridges between copper (II) ions and to mediate intramolecular exchange interactions has been investigated by single crystal X-ray diffraction and variable-temperature magnetic susceptibility measurements. (Author) 31 refs.

  17. Synthesis, crystal structure and magnetic properties of an oxalato-bridged Re(IV)Mo(VI) heterobimetallic complex.

    Science.gov (United States)

    Martínez-Lillo, José; Armentano, Donatella; De Munno, Giovanni; Lloret, Francesc; Julve, Miguel; Faus, Juan

    2011-05-14

    The Re(IV)-Mo(VI) compound of formula (PPh(4))(2)[ReCl(4)(μ-ox)MoO(2)Cl(2)] (1) constitutes the first example of a heterodinuclear oxalato-bridged complex in the coordination chemistry of molybdenum.

  18. Liquid-phase synthesis of bridged peptides using olefin metathesis of a protected peptide with a long aliphatic chain anchor.

    Science.gov (United States)

    Aihara, Keisuke; Komiya, Chiaki; Shigenaga, Akira; Inokuma, Tsubasa; Takahashi, Daisuke; Otaka, Akira

    2015-02-01

    Bridged peptides including stapled peptides are attractive tools for regulating protein-protein interactions (PPIs). An effective synthetic methodology in a heterogeneous system for the preparation of these peptides using olefin metathesis and hydrogenation of protected peptides with a long aliphatic chain anchor is reported.

  19. Synthesis and Luminescent Properties of Two New Triphenylamine-based Compounds with Heterocyclic Ring as Conjugation Bridge

    Institute of Scientific and Technical Information of China (English)

    LI,Qian-Qian; DI,Chong-An; YU,Gui; LIU,Yun-Qi; LI,Zhen; QIN,Jin-Gui

    2008-01-01

    Two new "D-π-D" type triphenylamine-based compounds with a heterocyclic ring,furan or thiophene,as a conjugation bridge were synthesized through a normal Wittig reaction which exhibited good thermal stability and strong luminescence.The preliminary light-emitting diode results indicate that they are promising candidates for the practical application.

  20. Synthesis, characterizations, and applications of carbon nanotubes and silicon nanowires

    Science.gov (United States)

    Xiong, Guangyong

    Carbon nanotubes (CNTs) have received great attention because of their unique structure and promising applications in microelectronic devices such as field electron emitters. Silicon nanowires (SiNWs) are also very popular because Si is a well established electronic material. This thesis will present my effort on synthesis, characterizations, and applications of CNTs and SiNWs by thermal chemical vapor deposition (CVD) method. For CNTs growth, block copolymer micelles were used as a template to create large area arrays of metal nanoclusters as catalysts for patterned arrays, and Fe/Al/Fe sandwich film on single crystal magnesium oxide (MgO) substrate was used as the catalyst for growth of long length aligned CNTs by CVD. The factors that affect the structure and length of CNTs have been investigated. CNTs were also grown on etched Si substrate by PECVD method. Continuous dropwise condensation was achieved on a biomimetic two-tier texture with short CNTs deposited on micromachined pillars. Superhydrophobic condensation model was studied. For SiNWs growth, hydrogen gold tetrachloride was uniformly mixed into the salt and decomposed into gold nanoparticles at the growth temperature and acted as the catalyst particles to start the growth of Si nanowires. The as-grown Si nanowires are about 70--90 nm in diameter and up to 200 micrometers long. The salt was completely removed by water rinse after growth. Field emission of aligned CNTs grown on Si substrates and SiNWs on Si substrates and carbon clothes has been studied. A post growth annealing procedure has been found to drastically improve the field emission performance of these CNTs and SiNWs.

  1. Synthesis and spectroscopic characterization of copper zinc aluminum nanoferrite particles

    Science.gov (United States)

    Lakshmi Reddy, S.; Ravindra Reddy, T.; Roy, Nivya; Philip, Reji; Montero, Ovidio Almanza; Endo, Tamio; Frost, Ray L.

    2014-06-01

    Copper doped zinc aluminum ferrites CuxZn1-x.(AlxFe2-x)O4 are synthesized by the solid-state reaction route and characterized by XRD, TEM, EPR and non linear optical spectroscopy techniques. The average particle size is found to be from 35 to 90 nm and the unit cell parameter “a” is calculated as from 8.39 to 8.89 Å. The cation distributions are estimated from X-ray diffraction intensities of various planes. The XRD studies have verified the quality of the synthesis of compounds and have shown the differences in the positions of the diffraction peaks due to the change in concentration of copper ions. TEM pictures clearly indicating that fundamental unit is composed of octahedral and tetrahedral blocks and joined strongly. The selected area electron diffraction (SAED) of the ferrite system shows best crystallinity is obtained when Cu content is very. Some of the d-plane spacings are exactly coinciding with XRD values. EPR spectra is compositional dependent at lower Al/Cu concentration EPR spectra is due to Fe3+ and at a higher content of Al/Cu the EPR spectra is due to Cu2+. Absence of EPR spectra at room temperature indicates that the sample is perfectly ferromagnetic. EPR results at low temperature indicate that the sample is paramagnetic, and that copper is placed in the tetragonal elongation (B) site with magnetically non-equivalent ions in the unit cell having strong exchange coupling between them. This property is useful in industrial applications. Nonlinear optical properties of the samples studied using 5 ns laser pulses at 532 nm employing the open aperture z-scan technique indicate that these ferrites are potential candidates for optical limiting applications.

  2. Synthesis and characterization of nanoparticles capped with medicinal plant extracts

    Science.gov (United States)

    Rekulapally, Sujith R.

    In this study, synthesis, characterization and biological application of series nanometal (silver, Ag) and nanometal oxide (titania, TiO2) were carried out. These nanomaterials were prepared using wet-chemistry method and then coated using natural plant extract. Three medicinal plants, namely Zingiber officinale (Ginger), Allium sativum (Garlic) and Capsicum annuum (Chili) were chosen as grafting agent to decrease the side-effects and increase the efficiency of NPs towards living organism. Extraction conditions were controlled under 60-100 °C for 8 hrs. Ag and TiO2 NPs were fabricated using colloidal chemistry and variables were controlled at ambient condition. The band gap of TiO2 NPs used as disinfectant was also modified through coating the medicinal plant extracts. The medicinal plant extracts and coated NPs were measured using spectroscopic methods. Ultraviolet-visible spectra indicated the Ag NPs were formed. The peak at 410 nm resulted from the electrons transferred from their ground to the excited state. The broadened full width at half maximum (FWHM) suggested the ultrafine particles were obtained. The lipid soluble compounds, phenols, tri-terpenoids, flavanoids, capsaicinoids, flavonoids, carotenoids, steroids steroidal glycosides, and vitamins were determined from the high performance liquid chromatographical analyses. X-ray powder diffraction indicated that the face-centered cubic Ag (PDF: 00-004-0783, a = 4.0862A, a = 90°) and anatase TiO2 (PDF: 01-08-1285, a = 3.7845, c = 9.5143A, a = 90°) were obtained using colloidal chemistry. Bactericidal activity indicated that these core-shelled TiO 2 were effective (MBC=0.6 ppm, within 30 mins) at inactivating Gram-positive and Gram-negative bacteria. It is proposed that the medicinal extracts enhanced the potency of NPs against bacteria. From our previous study, the Ag NPs were highly effective at inactivating both bacteria.

  3. Synthesis and characterization of polymers for light waveguide applications

    Science.gov (United States)

    Li, Bo

    The overall goal of this research was to prepare organo- soluble polymers that display low birefringence, low optical loss, and high thermal stability for use in light waveguide devices. Thus, two series of thermally stable polymers, i.e., aromatic polyimides and perfluorocyclobutane-containing poly(aryl ethers), were synthesized and characterized. The approach to the aromatic polyimides involved the synthesis of a new series of 4,4'-(9- fluorenylidene)dianilines containing large polarizable substituents. The diamines were polymerized with 2,2'-bis[4-(3,4- dicarboxyphenoxy)phenyl]propane dianhydride (BisA-DA) and 2,2'-bis(3,4- dicarboxyphenyl)hexafluoropropane dianhydride (6FDA) in refluxing m-cresol containing a catalytic amount of isoquinoline. The polyimides were soluble in common organic solvents such as N-methyl-2- pyrrolidinone (NMP), tetrahydrofuran (THF), chloroform (CHCl3), and cyclopentanone and could be solution cast into tough films. Thin films of the new cardo polyimides displayed birefringences that ranged from -0.0042 to 0.0074. In the second part of this work, a series of new difunctional and trifunctional trifluorovinylether-containing monomers was synthesized and polymerized via the thermal cyclodimerization of the vinyl groups. The number of carbon-hydrogen bonds was minimized in these systems in order to minimize the optical loss. A tough, transparent film was made from a polymer prepared from a trifunctional monomer, 1,1,1- trifluoro-2,2,2-tris(4-trifluorovinyloxyphenyl)ethane, which had a birefringence of 0.0008. The film showed negligible absorption at 1550 nm in the near-IR region. The polymer was also very thermally stable. Most of the linear polymers were soluble in common organic solvents such as NMP, THF, chloroform and cyclopentanone and could be solution cast into thin films, which displayed birefringences that ranged from -0.0005 to 0.0048.

  4. Synthesis and Characterization of Mixed Metal Oxide Nanocomposite Energetic Materials

    Energy Technology Data Exchange (ETDEWEB)

    Clapsaddle, B; Gash, A; Plantier, K; Pantoya, M; Jr., J S; Simpson, R

    2004-04-27

    In the field of composite energetic materials, properties such as ingredient distribution, particle size, and morphology affect both sensitivity and performance. Since the reaction kinetics of composite energetic materials are typically controlled by the mass transport rates between reactants, one would anticipate new and potentially exceptional performance from energetic nanocomposites. We have developed a new method of making nanostructured energetic materials, specifically explosives, propellants, and pyrotechnics, using sol-gel chemistry. A novel sol-gel approach has proven successful in preparing metal oxide/silicon oxide nanocomposites in which the metal oxide is the major component. By introducing a fuel metal, such as aluminum, into the metal oxide/silicon oxide matrix, energetic materials based on thermite reactions can be fabricated. Two of the metal oxides are tungsten trioxide and iron(III) oxide, both of which are of interest in the field of energetic materials. In addition, due to the large availability of organically functionalized silanes, the silicon oxide phase can be used as a unique way of introducing organic additives into the bulk metal oxide materials. These organic additives can cause the generation of gas upon ignition of the materials, therefore resulting in a composite material that can perform pressure/volume work. Furthermore, the desired organic functionality is well dispersed throughout the composite material on the nanoscale with the other components, and is therefore subject to the same increased reaction kinetics. The resulting nanoscale distribution of all the ingredients displays energetic properties not seen in its microscale counterparts due to the expected increase of mass transport rates between the reactants. The synthesis and characterization of iron(III) oxide/organosilicon oxide nanocomposites and their performance as energetic materials will be discussed.

  5. Synthesis and characterization of magnetite/PLGA/chitosan nanoparticles

    Science.gov (United States)

    Ibarra, Jaime; Melendres, Julio; Almada, Mario; Burboa, María G.; Taboada, Pablo; Juárez, Josué; Valdez, Miguel A.

    2015-09-01

    In this work, we report the synthesis and characterization of a new hybrid nanoparticles system performed by magnetite nanoparticles, loaded in a PLGA matrix, and stabilized by different concentrations of chitosan. Magnetite nanoparticles were hydrophobized with oleic acid and entrapped in a PLGA matrix by the emulsion solvent evaporation method, after that, magnetite/PLGA/chitosan nanoparticles were obtained by adding dropwise magnetite/PLGA nanoparticles in chitosan solutions. Magnetite/PLGA nanoparticles produced with different molar ratios did not show significant differences in size and the 3:1 molar ratio showed best spherical shapes as well as uniform particle size. Isothermal titration calorimetry studies demonstrated that the first stage of PLGA-chitosan interaction is mostly regulated by electrostatic forces. Based on a single set of identical sites model, we obtained for the average number of binding sites a value of 3.4, which can be considered as the number of chitosan chains per nanoparticle. This value was confirmed by using a model based on the DLVO theory and fitting zeta potential measurements of magnetite/PLGA/chitosan nanoparticles. From the adjusted parameters, we found that an average number of chitosan molecules of 3.6 per nanoparticle are attached onto the surface of the PLGA matrix. Finally, we evaluated the effect of surface charge of nanoparticles on a membrane model of endothelial cells performed by a mixture of three phospholipids at the air-water interface. Different isotherms and adsorption curves show that cationic surface of charged nanoparticles strongly interact with the phospholipids mixture and these results can be the basis of future experiments to understand the nanoparticles- cell membrane interaction.

  6. Two BN isosteres of anthracene: synthesis and characterization.

    Science.gov (United States)

    Ishibashi, Jacob S A; Marshall, Jonathan L; Mazière, Audrey; Lovinger, Gabriel J; Li, Bo; Zakharov, Lev N; Dargelos, Alain; Graciaa, Alain; Chrostowska, Anna; Liu, Shih-Yuan

    2014-10-29

    The synthesis of two parental BN anthracenes, 1 and 2, was developed, and their electronic structure and reactivity behavior were characterized in direct comparison with all-carbon anthracene. Gas-phase UV-photoelecton spectroscopy studies revealed the following HOMO energy trend: anthracene, -7.4 eV; BN anthracene 1, -7.7 eV; bis-BN anthracene 2, -8.0 eV. The λmax of the lower energy band in the UV-vis absorption spectrum is as follows: anthracene, 356 nm; BN anthracene 1, 359 nm; bis-BN anthracene 2, 357 nm. Thus, although the HOMO is stabilized with increasing BN incorporation, the HOMO-LUMO band gap remains unchanged across the anthracene series. The emission λmax values for the three investigated anthracene compounds are at 403 nm. The pKa values of the N-H proton for BN anthracene 1 and bis-BN anthracene 2 were determined to be approximately 26. BN anthracenes 1 and 2 do not undergo heat- or light-induced cycloaddition reactions or Friedel-Crafts acylations. Electrophilic bromination of BN anthracene 1 with Br2, however, occurs regioselectively at the 9-position. The reactivity behavior and regioselectivity of bromination of BN anthracenes are consistent with the electronic structure of these compounds; i.e., (1) the lower HOMO energy levels for BN anthracenes stabilize the molecules against cycloaddition and Friedel-Crafts reactions, and (2) the HOMO orbital coefficients are consistent with the observed bromination regioselectivity. Overall, this work demonstrates that BN/CC isosterism can be used as a molecular design strategy to stabilize the HOMO of acene-type structures while the optical band gap is maintained.

  7. Synthesis and Characterization of Elastomeric Heptablock Terpolymers Structured by Crystallization

    Energy Technology Data Exchange (ETDEWEB)

    Alfonzo, C.Guillermo; Fleury, Guillaume; Chaffin, Kimberly A.; Bates, Frank S. (UMM); (Medtronic)

    2010-12-07

    We report the synthesis and characterization of fully saturated hydrocarbon block copolymer thermoplastic elastomers with competitive mechanical properties and attractive processing features. Block copolymers containing glassy poly(cyclohexylethylene) (C), elastomeric poly(ethylene-alt-propylene) (P), and semicrystalline poly(ethylene) (E) were produced in a CEC-P-CEC heptablock architecture, denoted XPX, by anionic polymerization and catalytic hydrogenation. The X blocks contain equal volume fractions of C and E, totaling 40%-60% of the material overall. All the XPX polymers are disordered above the melt temperature for E (T{sub m,E} {approx_equal} 95 C) as evidenced by SAXS and dynamic mechanical spectroscopy measurements. Cooling below T{sub m,E} results in crystallization of the E blocks, which induces microphase segregation of E, C, and P into a complex morphology with a continuous rubbery domain and randomly arranged hard domains as shown by TEM. This mechanism of segregation decouples the processing temperature from the XPX molecular weight up to a limiting value. Tensile mechanical testing (simple extension and cyclic loading) demonstrates that the tensile strength (ca. 30 MPa) and strain at break (>500%) are comparable to the behavior of CPC triblock thermoplastic elastomers of similar molecular weight and glass content. However, in the CPC materials, processability is constrained by the order-disorder transition temperature, limiting the applications of these materials. Elastic recovery of the XPX materials following seven cycles of tensile deformation is correlated with the fraction of X in the heptablock copolymer, and the residual strain approaches that of CPC when the fraction of hard blocks f{sub X} {le} 0.39.

  8. Synthesis and characterization of oleophobic fluorinated polyester films

    Science.gov (United States)

    Demir, Tugba

    The study presented in this dissertation is dedicated to the synthesis and characterization of oleophobic fluorinated polyester films. Specifically, the blending of oleophilic polyethylene terephthalate (PET) with low surface energy materials such as fluorinated polyesters has been used in order to fabricate oleophobic PET films. First, fluorinated polyesters (P(PF-oate-R)) possessing different end-groups (-COOH, -OH and -CF3) are synthesized via polycondensation reaction of isophthaloyl chloride with perfluoro ether alcohols. Then, they are solvent-blended with PET at various concentrations to obtain oleophobic polyester films of different compositions. In addition, the films are annealed to investigate the effect of annealing on surface properties of the films. The results show that the obtained PET/P(PF-oate-R) polyester films demonstrate low wettability that depended on the polyester end-groups, film compositions, and annealing. It is found that PET blended with fluorinated polyesters terminated with CF3 groups exhibit higher contact angle (CA) with water and oils than other polyesters. In addition, CA increases with increasing P(PF-oate-R) polyester content in blends. To facilitate the oleophobicity of PET films, the fluorinated polyesters terminated with -CF3 groups with two different Mw were synthesized and blended with PET. The results reveal that at low concentrations, low molecular weight polyesters migrate to the surface easily, resulting in higher surface coverage. Thus, it leads to higher water and oil repellency. On the other hand, when they are used at high concentrations, higher molecular weight polyesters in blends reduce the wettability of the surface to the higher level. It is found that the wettability of the PET film surface depends on not only the Mw of polyesters, but also on annealing protocol. To this end, the effects of the annealing temperature on surface wettability are also examined.

  9. Synthesis and characterization of Ti–Ta–Nb–Mn foams

    Energy Technology Data Exchange (ETDEWEB)

    Aguilar, C., E-mail: claudio.aguilar@usm.cl [Departamento de Ingeniería Metalúrgica y Materiales, Universidad Técnica Federico Santa María, Av. España 1680, Valparaíso (Chile); Guerra, C. [Departamento de Ingeniería Metalúrgica y Materiales, Universidad Técnica Federico Santa María, Av. España 1680, Valparaíso (Chile); Lascano, S. [Departamento de Ingeniería Mecánica, Universidad Técnica Federico Santa María, Av. España 1680, Valparaíso (Chile); Guzman, D. [Departamento de Metalurgia, Universidad de Atacama, Av. Copayapu 485, Copiapó (Chile); Rojas, P.A. [Escuela de Ingeniería Mecánica, Facultad de Ingeniería, Pontificia Universidad Católica de Valparaíso, Av. Los Carrera, 01567 Quilpué (Chile); Thirumurugan, M. [Departamento de Ingeniería Metalúrgica y Materiales, Universidad Técnica Federico Santa María, Av. España 1680, Valparaíso (Chile); Bejar, L.; Medina, A. [Universidad Michoacana de San Nicolás de Hidalgo, Ciudad Universitaria, Morelia, Michoacán (Mexico)

    2016-01-01

    The unprecedented increase in human life expectancy have produced profound changes in the prevailing patterns of disease, like the observed increased in degenerative disc diseases, which cause degradation of the bones. Ti–Nb–Ta alloys are promising materials to replace the damaged bone due to their excellent mechanical and corrosion resistance properties. In general metallic foams are widely used for medical application due to their lower elastic moduli compare to bulk materials. In this work we studied the synthesis of 34Nb–29Ta–xMn (x: 2, 4 and 6 wt.% Mn) alloy foams (50% v/v) using ammonium hydrogen carbonate as a space holder. Alloys were produced through mechanical alloying in a planetary mill for 50 h. Green compacts were obtained by applying 430 MPa pressure. To remove the space holder from the matrix the green compacts were heated to 180 °C for 1.5 h and after sintered at 1300 °C for 3 h. Foams were characterized by x-ray diffraction, scanning, transmission electron microscopy and optical microscopy. The elastic modulus of the foam was measured as ~ 30 GPa, and the values are almost equal to the values predicted using various theoretical models. - Highlights: • Metallic foams of Ti–34Nb–29Ta–xMn (x: 2, 4 and 6 wt.% Mn) alloys were synthetized. • The macro and micro pore produced have sizes smaller than 600 and 20 μm, respectively. • The macro and micro pores shows good characteristics to cell adhesion and bone ingrowth. • Elastic properties were comparable to that exhibited by cortical bone.

  10. Phase II Characterization Survey of the USNS Bridge (T-AOE 10), Military Sealift Fleet Support Command, Naval Station, Norfolk, Virginia

    Energy Technology Data Exchange (ETDEWEB)

    ALTIC, NICK A

    2012-08-30

    In March 2011, the USNS Bridge was deployed off northeastern Honshu, Japan with the carrier USS Ronald Reagan to assist with relief efforts after the 2011 Tōhoku earthquake and tsunami. During that time, the Bridge was exposed to air-borne radioactive materials leaking from the damaged Fukushima I Nuclear Power Plant. The proximity of the Bridge to the air-borne impacted area resulted in the contamination of the ship’s air-handling systems and the associated components, as well as potential contamination of other ship surfaces due to either direct intake/deposition or inadvertent spread from crew/operational activities. Preliminary surveys in the weeks after the event confirmed low-level contamination within the heating, ventilation, and air conditioning (HVAC) ductwork and systems, and engine and other auxiliary air intake systems. Some partial decontamination was performed at that time. In response to the airborne contamination event, Military Sealift Fleet Support Command (MSFSC) contracted Oak Ridge Associated Universities (ORAU), under provisions of the Oak Ridge Institute for Science and Education (ORISE) contract, to assess the radiological condition of the Bridge. Phase I identified contamination within the CPS filters, ventilation systems, miscellaneous equipment, and other suspect locations that could not accessed at that time (ORAU 2011b). Because the Bridge was underway during the characterization, all the potentially impacted systems/spaces could not be investigated. As a result, MSFSC contracted with ORAU to perform Phase II of the characterization, specifically to survey systems/spaces previously inaccessible. During Phase II of the characterization, the ship was in port to perform routine maintenance operations, allowing access to the previously inaccessible systems/spaces.

  11. Synthesis, characterization and application of functional carbon nano materials

    Science.gov (United States)

    Chu, Jin

    The synthesis, characterizations and applications of carbon nanomaterials, including carbon nanorods, carbon nanosheets, carbon nanohoneycombs and carbon nanotubes were demonstrated. Different growth techniques such as pulsed laser deposition, DC/RF sputtering, hot filament physical vapour deposition, evaporative casting and vacuum filtration methods were introduced or applied for synthesizing carbon nanomaterials. The morphology, chemical compositions, bond structures, electronic, mechanical and sensing properties of the obtained samples were investigated. Tilted well-aligned carbon micro- and nano- hybrid rods were fabricated on Si at different substrate temperatures and incident angles of carbon source beam using the hot filament physical vapour deposition technique. The morphologic surfaces and bond structures of the oblique carbon rod-like structures were investigated by scanning electron microscopy, field emission scanning electron microscopy, transmission electron diffraction and Raman scattering spectroscopy. The field emission behaviour of the fabricated samples was also tested. Carbon nanosheets and nanohoneycombs were also synthesized on Si substrates using a hot filament physical vapor deposition technique under methane ambient and vacuum, respectively. The four-point Au electrodes are then sputtered on the surface of the nanostructured carbon films to form prototypical humidity sensors. The sensing properties of prototypical sensors at different temperature, humidity, direct current, and alternative current voltage were characterized. Linear sensing response of sensors to relative humidity ranging from 11% to 95% is observed at room temperature. Experimental data indicate that the carbon nanosheets based sensors exhibit an excellent reversible behavior and long-term stability. It also has higher response than that of the humidity sensor with carbon nanohoneycombs materials. Conducting composite films containing carbon nanotubes (CNTs) were prepared in

  12. Synthesis and characterization of nanostructured palladium-based alloy electrocatalysts

    Science.gov (United States)

    Sarkar, Arindam

    Low temperature fuel cells like proton exchange membrane fuel cells (PEMFC) are expected to play a crucial role in the future hydrogen economy, especially for transportation applications. These electrochemical devices offer significantly higher efficiency compared to conventional heat engines. However, use of exotic and expensive platinum as the electrocatalyst poses serious problems for commercial viability. In this regard, there is an urgent need to develop low-platinum or non-platinum electrocatalysts with electrocatalytic activity for the oxygen reduction reaction (ORR) superior or comparable to that of platinum. This dissertation first investigates non-platinum, palladium-based alloy electrocatalysts for ORR. Particularly, Pd-M (M = Mo and W) alloys are synthesized by a novel thermal decomposition of organo-metallic precursors. The carbon-supported Pd-M (M = Mo, W) electrocatalyts are then heat treated up to 900°C in H2 atmosphere and investigated for their phase behavior. Cyclic voltammetry (CV) and rotating disk electrode (RDE) measurements reveal that the alloying of Pd with Mo or W significantly enhances the catalytic activity for ORR as well as the stability (durability) of the electrocatalysts. Additionally, both the alloy systems exhibit high tolerance to methanol, which is particularly advantageous for direct methanol fuel cells (DMFC). The dissertation then focuses on one-pot synthesis of carbon-supported multi-metallic Pt-Pd-Co nanoalloys by a rapid microwave-assisted solvothermal (MW-ST) method. The multi-metallic alloy compositions synthesized by the MW-ST method show much higher catalytic activity for ORR compared to their counterparts synthesized by the conventional borohydride reduction method. Additionally, a series of Pt encapsulated Pd-Co nanoparticle electrocatalysts are synthesized by the MW-ST method and characterized to understand their phase behavior, surface composition, and electrocatalytic activity for ORR. Finally, the dissertation

  13. Synthesis, Characterization, and Electrochemical Properties of Polyaniline Thin Films

    Science.gov (United States)

    Rami, Soukaina

    Conjugated polymers have been used in various applications (battery, supercapacitor, electromagnetic shielding, chemical sensor, biosensor, nanocomposite, light-emitting-diode, electrochromic display etc.) due to their excellent conductivity, electrochemical and optical properties, and low cost. Polyaniline has attracted the researchers from all disciplines of science, engineering, and industry due to its redox properties, environmental stability, conductivity, and optical properties. Moreover, it is a polymer with fast electroactive switching and reversible properties displayed at low potential, which is an important feature in many applications. The thin oriented polyaniline films have been fabricated using self-assembly, Langmuir-Blodgett, in-situ self-assembly, layer-by-layer, and electrochemical technique. The focus of this thesis is to synthesize and characterize polyaniline thin films with and without dyes. Also, the purpose of this thesis is to find the fastest electroactive switching PANI electrode in different electrolytic medium by studying their electrochemical properties. These films were fabricated using two deposition techniques: in-situ self-assembly and electrochemical deposition. The characterization of these films was done using techniques such as Fourier Transform Infrared Spectroscopy (FTIR), UV-spectroscopy, Scanning Electron Microscope (SEM), and X-Ray Diffraction (XRD). FTIR and UV-spectroscopy showed similar results in the structure of the polyaniline films. However, for the dye incorporated films, since there was an addition in the synthesis of the material, peak locations shifted, and new peaks corresponding to these materials appeared. The 1 layer PANI showed compact film morphology, comparing to other PANI films, which displayed a fiber-like structure. Finally, the electrochemical properties of these thin films were studied using cyclic voltammetry (CV), chronoamperometry (CA), and electrochemical impedance spectroscopy (EIS) in

  14. Synthesis and characterization of GAP/BAMO copolymers applied at high energetic composite propellants

    Directory of Open Access Journals (Sweden)

    Paul Bernt Kempa

    2010-09-01

    Full Text Available The main objective of these studies was the synthesis and characterization of new energetic binders and their use in some propellant formulations. Following the working plan elaborated, the synthesis and characterization of the following compounds has been done successfully:• GAP;• energetic Monomer BAMO;• energetic Binders;• copolymer GAP/PolyBAMO.The scale up for the synthesis of copolymer GAP/PolyBAMO and PolyBAMO using GAP as initiator has been done and they were fully characterized by IR, (¹H, ¹³C NMR-spectroscopy, GPC, elemental analysis, OH-functionality, differential scanning calorimetry (DSC and sensitivity tests (friction, impact. For this two scale up synthesis some propellant formulations were carried out and the results of mechanical and burning properties have been compared with GAP propellants.

  15. Microwave Assisted Synthesis and Characterization of Perovskite Oxides

    OpenAIRE

    Prado-Gonjal, Jesus; Schmidt, Rainer; Moran, Emilio

    2014-01-01

    The use of microwave irradiation is a promising alternative heat source for the synthesis of inorganic materials such as perovskite oxides. The method offers massive energy and time savings as compared to the traditional ceramic method. In this work we review the basic principles of the microwave heating mechanism based on interactions between dipoles in the material and the electromagnetic microwave. Furthermore, we comment on and classify all different sub-types of microwave synthesis such ...

  16. Synthesis and Characterization of 5- and 6- Coordinated Alkali Pertechnetates

    Energy Technology Data Exchange (ETDEWEB)

    Weaver, Jamie; Soderquist, Chuck; Gassman, Paul; Walter, Eric; Lukens, Wayne; McCloy, John S.

    2017-01-01

    The local chemistry of technetium-99 (99Tc) in oxide glasses is important for understanding the incorporation and long-term release of Tc from nuclear waste glasses, both those for legacy defense wastes and fuel reprocessing wastes. Tc preferably forms Tc(VII), Tc(IV), or Tc(0) in glass, depending on the level of reduction of the melt. Tc(VII) in oxide glasses is normally assumed to be isolated pertechnetate TcO4-anions surrounded by alkali, but can occasionally precipitate as alkali pertechnetate salts such as KTcO4and NaTcO4when Tc concentration is high. In these cases, Tc(VII) is 4-coordinated by oxygen. A reinvestigation of the chemistry of alkali-technetium-oxides formed under oxidizing conditions and at temperatures used to prepare nuclear waste glasses showed that higher coordinated alkali Tc(VII) oxide species had been reported, including those with the TcO5-and TcO6-anions. The chemistry of alkali Tc(VII) and other alkali-Tc-oxides is reviewed, along with relevant synthesis conditions.

    Additionally, we report attempts to make 5- and 6-coordinate pertechnetate compounds of K, Na, and Li, i.e. TcO5-and TcO6-. It was found that higher coordinated species are very sensitive to water, and easily decompose into their respective pertechnetates. It was difficult to obtain pure compounds, but mixtures of the pertechnetate and other phase(s) were frequently found, as evidenced by x-ray absorption spectroscopy (XAS), neutron diffraction (ND), and Raman spectroscopy. Low temperature electron paramagnetic resonance (EPR) measurements showed the possibility of Tc(IV) and Tc(VI) in Na3TcO5and Na5TcO6compounds.

    It was hypothesized that the smaller counter cation would result in more stable pertechnetates. To confirm the synthesis method, LiReO4and Li5

  17. Synthesis and Characterization of 2-Phenylimidazo[1,2-a]pyridine: A Privileged Structure for Medicinal Chemistry

    Science.gov (United States)

    Santaniello, Brandi S.; Price, Matthew J.; Murray, James K., Jr.

    2017-01-01

    A straightforward synthesis of 2-phenylimidazo[1,2-a]pyridine is described. The reaction is designed to demonstrate to students the preparation of a bridged N-heterocycle, in which the heteroatom occupies a bridgehead position. The product is obtained in moderate to high yield and is highly crystalline. The compound can be purified either by…

  18. The Synthesis and Characterization of Some Fluoride Perovskites: An Undergraduate Experiment in Solid State Chemistry.

    Science.gov (United States)

    Langley, Richard H.; And Others

    1984-01-01

    Describes a senior-level experiment dealing with the synthesis and characterization of a perovskite. Since most perovskites are cubic, their characterization by x-ray diffraction is simplified. In addition, magnetic ordering may be observed and the effects of a Jahn-Teller distortion seen. (JN)

  19. Synthesis, characterization and antibacterial studies of 2-chloro-5-fluoro-N-[dibenzyl carbamothioyl] benzamide thiourea

    Energy Technology Data Exchange (ETDEWEB)

    Sapari, Suhaila; Yamin, Bohari M.; Hasbullah, Aishah; Ibrahim, Nazlina [School of Chemical Science and Food Technology, Faculty of Science and Technology, The National University of Malaysia, 43600, Bangi, Selangor (Malaysia)

    2014-09-03

    Synthesis, characterization and antibacterial studies of 2-chloro-5-fluoro-N-[dibenzyl carbamothioyl] benzamide thiourea has been reported. The compound characterized by using elementary analysis CHNS, IR, {sup 1}H NMR and {sup 13}C NMR spectroscopies. The compounds have been screened for their antibacterial studies.

  20. Fixation of CO2 in air: Synthesis and crystal structure of a 3-CO3-bridged tricopper(II) compound

    Indian Academy of Sciences (India)

    Jhumpa Mukherjee; V Balamurugan; Maninder Singh Hundal; Rabindranath Mukherjee

    2005-03-01

    A novel trinuclear copper(II) compound [{(L3)Cu(OClO3)}3(3-OCO2)][ClO4] has been synthesised using an N-tridentate symmetrical pyridylalkylamine ligand, N-methyl-N,N-bis(2-pyridylmethyl)amine (L3). The structure of the complex has been determined by X-ray crystallography; it is found to crystallise in the hexagonal space group 63/ with = 13.936(2), = 13.936(2), = 14.895(3) Å, = = 90°, = 120°. The complex possesses a $\\bar{6}$ - symmetry axis passing through the carbon atom of the triply bridging carbonate ion, with the three symmetry related copper ions connected to one another through the oxygen atoms from the bridging carbonato group, giving an equilateral triangular array of copper centres. Each copper ion has distorted square pyramidal environment with the basal plane formed by three nitrogen atoms of the ligand L3 and the oxygen atom of the bridging carbonato group. The apical position at each copper is provided by the weak oxygen coordination from the perchlorate ion.

  1. The Synthesis, Characterization and Catalytic Reaction Studies of Monodisperse Platinum Nanoparticles in Mesoporous Oxide Materials

    Energy Technology Data Exchange (ETDEWEB)

    Rioux, Robert M. [Univ. of California, Berkeley, CA (United States)

    2006-01-01

    A catalyst design program was implemented in which Pt nanoparticles, either of monodisperse size and/or shape were synthesized, characterized and studied in a number of hydrocarbon conversion reactions. The novel preparation of these materials enables exquisite control over their physical and chemical properties that could be controlled (and therefore rationally tuned) during synthesis. The ability to synthesize rather than prepare catalysts followed by thorough characterization enable accurate structure-function relationships to be elucidated. This thesis emphasizes all three aspects of catalyst design: synthesis, characterization and reactivity studies. The precise control of metal nanoparticle size, surface structure and composition may enable the development of highly active and selective heterogeneous catalysts.

  2. Synthesis, characterization, and biosensing application of novel hybrid nanomaterials

    Science.gov (United States)

    Mao, Shun

    Hybrid nanomaterials consisting of nanoparticles (NPs) distributed on the surface of the carbon nanotube (CNT)/graphene represent a new class of materials. These materials could potentially display not only the unique properties of NPs and those of the CNT/graphene, but also additional novel properties due to the interaction between the NP and the CNT/graphene. This thesis entails the synthesis and characterization of NP-CNT/graphene hybrid nanomaterials and the demonstration of their use for biosensors. A simple method that combines an electrospray technique with electrostatic force directed assembly (ESFDA) was developed for successful functionalization of the CNT/thermally-reduced graphene oxide (TRGO) with NPs. Colloidal CdSe NPs, Au NPs, and Au NP-antibody conjugates were electrosprayed and assembled onto random CNTs, vertically-aligned CNT arrays, and TRGO sheets in a controlled manner. CNT and TRGO field-effect transistors (FETs) were fabricated; and novel electronic protein biosensors based on the CNTFET/TRGO FET and Au NP-antibody conjugates were demonstrated. The electrical detection of the protein binding was accomplished by the introduction of Au NP-antibody conjugates in the CNTFET/TRGO FET, in which the Au-coated CNT/TRGO serves as the electrical conducting channel. Antibody (anti-horseradish peroxidase/anti-Immunoglobulin G) and antigen (horseradish peroxidase/Immunoglobulin G) binding events led to the change in the CNT/TRGO conductivity, which was sensitively detected by FET and direct current (dc) measurements. The CNTFET biosensor had a detection limit of 0.2 mg/ml (˜4.5 microM, horseradish peroxidase) while the TRGO FET biosensor exhibited a detection limit of 2 ng/ml (˜13 pM, Immunoglobulin G), which is among the best of carbon nanomaterial (e.g., CNT, graphene, GO)-based protein sensors. The dependence of the sensor response on the TRGO resistance and the antibody areal density on the TRGO sheet was systematically studied, and the sensor

  3. Synthesis and characterization of TEP-EDTA-regulated bioactive hydroxyapatite

    Science.gov (United States)

    Haders, Daniel Joseph, II

    Hydroxyapatite (HA), Ca10(PO4)6(OH) 2, the stoichiometric equivalent of the ceramic phase of bone, is the preferred material for hard tissue replacement due to its bioactivity. However, bioinert metals are utilized in load-bearing orthopedic applications due to the poor mechanical properties of HA. Consequently, attention has been given to HA coatings for metallic orthopedic implants to take advantage of the bioactivity of HA and the mechanical properties of metals. Commercially, the plasma spray process (PS-HA) is the method most often used to deposit HA films on metallic implants. Since its introduction in the 1980's, however, concerns have been raised about the consequences of PS-HA's low crystallinity, lack of phase purity, lack of film-substrate chemical adhesion, passivation properties, and difficulty in coating complex geometries. Thus, there is a need to develop inexpensive reproducible next-generation HA film deposition techniques, which deposit high crystallinity, phase pure, adhesive, passivating, conformal HA films on clinical metallic substrates. The aim of this dissertation was to intelligently synthesize and characterize the material and biological properties of HA films on metallic substrates synthesized by hydrothermal crystallization, using thermodynamic phase diagrams as the starting point. In three overlapping interdisciplinary studies the potential of using ethylenediamine-tetraacetic acid/triethyl phosphate (EDTA/TEP) doubly regulated hydrothermal crystallization to deposit HA films, the TEP-regulated, time-and-temperature-dependent process by which films were deposited, and the bioactivity of crystallographically engineered films were investigated. Films were crystallized in a 0.232 molal Ca(NO3)2-0.232 molal EDTA-0.187 molal TEP-1.852 molal KOH-H2O chemical system at 200°C. Thermodynamic phase diagrams demonstrated that the chosen conditions were expected to produce Ca-P phase pure HA, which was experimentally confirmed. EDTA regulation of

  4. Synthesis and characterization of polymer matrix nanocomposites and their components

    Science.gov (United States)

    Burnside, Shelly Dawn

    Herein we present synthesis schemes and characterization results for polymer matrix nanocomposite reinforced with organically modified layered silicates. These host materials with ultrafine dimensions are promising candidates for polymer and have been previously shown to yield substantial property enhancements at low silicate loadings due to their extreme geometry. Siloxane nanocomposites with a variety of nanostructures were formed. Thermal stability, solvent uptake and moduli of the nanocomposites were explores. Exfoliated nanocomposites displayed enhanced properties when compared to unreinforced siloxanes, and at lower volume fraction filler than in conventional composites. Large amounts of bound polymer, polymer affected by the silicate, were found in exfoliated nanocomposites as a result of the extreme geometry of the layered silicate. This bound polymer was related to the dramatic property enhancements in the nanocomposites. The behavior of these nanocomposites is compared to behavior expected from traditional models developed for conventional composites and model elastomeric networks. A lightly brominated polymer has been intercalated into a single crystal of organically exchanged vermiculite. The intercalation was followed using x-ray diffraction by monitoring the gallery height of the vermiculite host. Rutherford Backscattering Spectroscopy, used to confirm polymer intercalation, showed a constant bromine content in the direction normal to the layers. Atomic Force Microscopy images of a cleaved polymer-intercalated crystal showed raised hemispheres on an otherwise flat background. The hemispheres consist of single chains or aggregates of 3-40 polymer chains resulting from relaxations following cleaving. Three component or Hansen solubility parameters (delta) of organically modified layered silicates, the reinforcing agent in polymer matrix nanocomposites presented herein, have been determined. Two experimental techniques, temporal turbidimetry and

  5. Material Synthesis and Characterization on Low-Dimensional Cobaltates

    Science.gov (United States)

    Sha, Hao

    In this thesis, results of the investigation of a new low-dimensional cobaltates Ba2-xSrxCoO 4 are presented. The synthesis of both polycrystalline and single crystalline compounds using the methods of conventional solid state chemical reaction and floating-zone optical furnace is first introduced. Besides making polycrystalline powders, we successfully, for the first time, synthesized large single crystals of Ba2CoO4. Single crystals were also obtained for Sr doped Ba2-xSrxCoO 4. Powder and single crystal x-ray diffraction results indicate that pure Ba2CoO4 has a monoclinic structure at room temperature. With Sr doping, the lattice structure changes to orthorhombic when x ≥ 0.5 and to tetragonal when x = 2.0. In addition, Ba2CoO4 and Sr2CoO4, have completely different basic building blocks in the structure. One is CoO4 tetrahedron and the later is CoO6 octahedron, respectively. Electronic and magnetic properties were characterized and discussed. The magnetic susceptibility, specific heat and thermal conductivity show that Ba2CoO4 has an antiferromagnetic (AF) ground state with an AF ordering temperature TN = 25 K. However, the magnitude of the Neel temperature TN is significantly lower than the Curie-Weiss temperature (|theta| ˜ 110 K), suggesting either reduced-dimensional magnetic interactions and/or the existence of magnetic frustration. The AF interaction persists in all the samples with different doping concentrations. The Neel temperature doesn't vary much in the monoclinic structure regime but decreases when the system enters orthorhombic. Magnetically, Ba2CoO4 has an AF insulating ground state while Sr2CoO4 has a ferromagnetic (FM) metallic ground state. Neutron powder refinement results indicate a magnetic structure with the spin mostly aligned along the a-axis. The result from a mu-spin rotation/relaxation (mu+SR) experiment agrees with our refinement. It confirms the AF order in the ab -plane. We also studied the spin dynamics and its anisotropy in

  6. Synthesis and characterization of novel fullerenes and carbon nanotubes

    Science.gov (United States)

    Piskoti, Charles Richard

    Since the discovery of Buckminsterfullerene, the soccerball shaped carbon-caged molecule consisting of 60 carbon atoms, there has been much speculation about the stability of other "fullerenes" with less than 60 carbon atoms. Although several fullerenes with greater than 60 carbon atoms have since been isolated in bulk, the only evidence of lower fullerenes has come from minute-quantity gas phase experiments. This thesis presents work on the first ever bulk synthesis, extraction and characterization of a lower fullerene: C36. By exploring the parameter space of the Kratschmer-Huffman graphite arc-discharge method, C36 was produced in milligram quantities. This new material which was extracted with pyridine was found by electron diffraction to form a covalently bonded solid with a d-spacing of 6.68 A. This material is electrically insulating in its pure form but it becomes conducting upon intercalation with alkali metals. The resistance vs temperature behavior of the alkali intercalated samples is consistent with variable range hopping. From microwave-loss measurements and current vs. voltage data, there are preliminary results that may indicate the presence of a very small superconducting fraction in these alkali doped samples. This result would be consistent with predictions by Grossman, Cote, Cohen and Louie that a certain isomer of C 36 with D6h symmetry has an exceptionally strong electron-phonon coupling constant. Other developments described in this thesis include a method of synthesizing multi-walled carbon nanotubes in high yield at an accelerated rate using a low pressure mixture of nitrogen and helium as the buffer gas. Also, a simple technique has been developed for synthesizing magnetic nickel-iron clusters that are coated with both electrical insulators and electrical conductors. These clusters may have a variety of applications in the fields of magnetic recording and biochemistry where magnetic manipulation of cells is important. Finally, a

  7. Solvothermal synthesis and characterization of monodisperse superparamagnetic iron oxide nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Li, Shichuan; Zhang, Tonglai; Tang, Runze; Qiu, Hao [State Key Laboratory of Explosion Science and Technology, Beijing Institute of Technology, Beijing 100081 (China); Wang, Caiqin [Shandong Special Industry Group Co., Ltd, Shandong 255201 (China); Zhou, Zunning [State Key Laboratory of Explosion Science and Technology, Beijing Institute of Technology, Beijing 100081 (China)

    2015-04-01

    A series of magnetic iron oxide nanoparticle clusters with different structure guide agents were synthesized by a modified solvothermal method and characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), thermogravimetric analyses (TG), a vibrating sample magnetometer (VSM) and Fourier transform infrared spectroscopy (FTIR). It is found that the superparamagnetic nanoparticles guided by NaCit (sodium citrate) have high saturation magnetization (M{sub s}) of 69.641 emu/g and low retentivity (M{sub r}) of 0.8 emu/g. Guiding to form superparamagnetic clusters with size range of 80–110 nm, the adherent small-molecule citrate groups on the surface prevent the prefabricated ferrite crystals growing further. In contrast, the primary small crystal guided and stabilized by the PVP long-chain molecules assemble freely to larger ones and stop growing in size range of 100–150 nm, which has saturation magnetization (M{sub s}) of 97.979 emu/g and retentivity (M{sub r}) of 46.323 emu/g. The relevant formation mechanisms of the two types of samples are proposed at the end. The superparamagnetic ferrite clusters guided by sodium citrate are expected to be used for movement controlling of passive interference particles to avoid aggregation and the sample guided by PVP will be a candidate of nanometer wave absorbing material. - Highlights: • A facile synthesis of two kinds of monodisperse iron oxide nano-particle clusters was performed via a modified one-step solvothermal method in this work. • The NaCit and PVP as different guiding agents are used to control the formation and aggregation of nano-crystals during reacting and the ripening processes. • The superparamagnetic NaCit–Fe{sub 3}O{sub 4} samples have high saturation magnetization (M{sub s}) of 69.641 emu/g and low retentivity (M{sub r}) of 0.8 emu/g. • The relevant formation mechanisms of the two types of samples are proposed.

  8. Synthesis, characterization and mechanistic insights of mycogenic iron oxide nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Bhargava, Arpit; Jain, Navin; Manju Barathi L [Birla Institute of Technology and Science, Centre for Biotechnology, Department of Biological Sciences (India); Akhtar, Mohd Sayeed [Jimma University, Department of Applied Microbiology, College of Natural Sciences (Ethiopia); Yun, Yeoung-Sang [Chonbuk National University, Division of Environmental and Chemical Engineering (Korea, Republic of); Panwar, Jitendra, E-mail: drjitendrapanwar@yahoo.co.in [Birla Institute of Technology and Science, Centre for Biotechnology, Department of Biological Sciences (India)

    2013-11-15

    In the present study, extracellular synthesis of iron oxide nanoparticles (IONPs) was achieved using Aspergillus japonicus isolate AJP01. The isolate demonstrated its ability to hydrolyze the precursor salt solution, a mixture of iron cyanide complexes, under ambient conditions. Hydrolysis of these complexes released ferric and ferrous ions, which underwent protein-mediated coprecipitation and controlled nucleation resulting in the formation of IONPs. Transmission electron microscopy, selected area electron diffraction pattern, energy dispersive spectroscopy and grazing incidence X-ray diffraction analysis confirmed the mycosynthesis of IONPs. The synthesized particles were cubic in shape with a size range of 60–70 nm with crystal structure corresponding to magnetite. Scanning electron microscopy analysis revealed the absence of IONPs on fungal biomass surface, indicating the extracellular nature of synthesis. Fourier transform infrared spectroscopy confirmed the presence of proteins on as-synthesised IONPs, which may confer their stability. Preliminary investigation indicated the role of proteins in the synthesis and stabilization of IONPs. On the basis of present findings, a probable mechanism for synthesis of IONPs is suggested. The simplicity and versatility of the present approach can be utilized for the synthesis of other nanomaterials.

  9. Template-Assisted Synthesis and Characterization of Passivated Nickel Nanoparticles

    Directory of Open Access Journals (Sweden)

    Al-Omari IA

    2010-01-01

    Full Text Available Abstract Potential applications of nickel nanoparticles demand the synthesis of self-protected nickel nanoparticles by different synthesis techniques. A novel and simple technique for the synthesis of self-protected nickel nanoparticles is realized by the inter-matrix synthesis of nickel nanoparticles by cation exchange reduction in two types of resins. Two different polymer templates namely strongly acidic cation exchange resins and weakly acidic cation exchange resins provided with cation exchange sites which can anchor metal cations by the ion exchange process are used. The nickel ions which are held at the cation exchange sites by ion fixation can be subsequently reduced to metal nanoparticles by using sodium borohydride as the reducing agent. The composites are cycled repeating the loading reduction cycle involved in the synthesis procedure. X-Ray Diffraction, Scanning Electron Microscopy, Transmission Electron microscopy, Energy Dispersive Spectrum, and Inductively Coupled Plasma Analysis are effectively utilized to investigate the different structural characteristics of the nanocomposites. The hysteresis loop parameters namely saturation magnetization and coercivity are measured using Vibrating Sample Magnetometer. The thermomagnetization study is also conducted to evaluate the Curie temperature values of the composites. The effect of cycling on the structural and magnetic characteristics of the two composites are dealt in detail. A comparison between the different characteristics of the two nanocomposites is also provided.

  10. Metal oxide and mercuric sulfide nanoparticles synthesis and characterization

    Science.gov (United States)

    Xu, Xin

    Commercially available and laboratory-synthesized metal based nanoparticles (NPs), iron oxide (Fe2O3), copper oxide (CuO), titanium dioxide (TiO2), zinc oxide (ZnO) and mercuric sulfide (HgS) were studied by comprehensive characterizations methods. The general synthesis process was modified sol-gel method. The size and morphology of NPs could be influenced by temperature, sonication, calcination, precursor concentration, pH and types of reaction media. All types of the laboratory-synthesized or commercially available NPs were characterized by physical and chemical processes. One characteristic of NP that can lead to ambiguous toxicity test results was the effect of agglomeration of primary nano-sized particles. Laser light scattering was used to measure the aggregated and particle size distribution. Aggregation effects were apparent and often extensive in some synthesis approaches. Electron microscopy (SEM and TEM) gave the images of those laboratory-synthesized particles and aggregation. The average single particle was about 5-20 nm of ZnO; 20-40 nm of CuO; 10-20 nm of TiO2; 20-35 nm of Fe2O3; 10-15 nm of HgS, while the aggregate size was in the range of a hundred nanometers or more. These five types of NPs were obtained with spherical and oblong formation and the agglomeration of ZnO, CuO, HgS and TiO2 was random, but Fe2O3 has web-like aggregation. Other measurements performed on the particles and aggregates include bandgap energies, surface composition, surface area, hydrodynamic radius, and particle surface charge. In aqueous environment, NPs are subject to processes such as solubilization and aggregation. These processes can be controlling factors in the fate of nanomaterials in environmental settings, including bioavailability to organisms. This study has focused primarily on measurement of the solubility in aqueous media of varying composition (pH, ionic strength, and organic carbon), sedimentation and stability. The aggregate size distribution was

  11. An efficient synthesis of 3-OBn-6β,14-epoxy-bridged opiates from naltrexone and identification of a related dual MOR inverse agonist/KOR agonist.

    Science.gov (United States)

    Martin, David J; FitzMorris, Paul E; Li, Bo; Ayestas, Mario; Sally, Ellicott J; Dersch, Christina M; Rothman, Richard B; Deveau, Amy M

    2012-11-15

    In an effort to better understand the conformational preferences that inform the biological activity of naltrexone and related naltrexol derivatives, a new synthesis of the restricted analog 3-OBn-6β,14-epoxymorphinan 4 is described. 4 was synthesized starting from naltrexone in 50% overall yield, proceeding through the OBn-6α-triflate intermediate 8. Key steps to the synthesis include benzylation (96% yield), reduction (90% yield, α:β:3:2), followed by a one-pot triflation/displacement sequence (96% yield) to yield the desired bridged epoxy derivative 4. X-ray crystallographic analysis of intermediate 3-OBn-6α-naltrexol 7a supports population of the key boat conformation required for the epoxy ring closure. We also report that the 6β-mesylate 10-a high affinity opioid receptor ligand, the epimeric derivative of 11, and an analog of 12-functions as an inverse agonist at the mu opioid receptor using herkinorin pre-conditioned cells and an agonist at the kappa opioid receptor when evaluated in independent in vitro [(35)S]-GTP-γ-S assays.

  12. Chiral cyanide-bridged 1D FeⅢ-MnⅢ heterobimetallic chains: Synthesis,structures and magnetic properties%Chiral cyanide-bridged 1D FeⅢ-MnⅢ heterobimetallic chains:Synthesis,structures and magnetic properties

    Institute of Scientific and Technical Information of China (English)

    YAO MinXia; ZHENG Qi; GAO Feng; LI YiZhi; ZUO JingLin

    2012-01-01

    Two couples of enantiomerically pure chiral cyano-bridged heterobimetallic one-dimensional(1D)chain complexes:[Mn((R,R)-Salphen)Fe(Tp)(CN)3]n(1)and[Mn((S,S)-Salphen)Te(Tp)(CN)3]n(2)(Salphen =N,N1-I,2-diphenyl ethylenebis(salicylideneiminato)dianion,Tp =tris(pyrazolyl)hydroborate),[Mn((R,R)-Salphen)Fe(Tp*)(CN)3·2H2O]n(3)and[Mn((S,S)-Salphen)Fe(Tp*)(CN)3.2H2O]n(4)(Tp* =hydridotris(3,5-dimethylpyrazol- l-yl)borate),have been successfully synthesized by the reactions of MnⅢ schiff-base complexes with the tricyanometalate building block,[(LTp)Fe(CN)3]-(LTp =Tp or Tp*).All complexes are made up of neutral cyano-bridged zigzag double chains with(-Fe-C≡ N-Mn-N≡C-)n as the repeating unit.Circular dichroism(CD)spectra confirm the enantiomeric nature of the optically active complexes.Magnetic studies demonstrate that ferromagnetic interactions are operative in these complexes.The ferromagnetic couplings become weak in the chains with the bending of the Mn-N ≡C angles.

  13. Synthesis and characterization of a linker for primary amines used in the solid phase organic synthesis of spermidine

    Energy Technology Data Exchange (ETDEWEB)

    Silva, Emerson T. da; San Gil, Rosane A.S.; Lima, Edson L.S. [Universidade Federal do Rio de Janeiro (IQ/UFRJ), RJ (Brazil). Inst. de Quimica; Caldarelli, Stefano [Aix-Marseille Univ., Marseille (France). Campus de Saint Jerome; Ziarelli, Fabio [Aix-Marseille Universite Spectropole - Federation de Sciences Chimiques de Marseille, Campus de Saint Jerome (France)

    2011-07-01

    A linker resin for the synthesis of functionalized spermidine in good yield is described, along with its characterization by infrared (IR), {sup 13}C solid-state nuclear magnetic resonance with cross polarization and magic angle spinning ({sup 13}C CPMAS NMR) and {sup 1}H high resolution magic angle spinning nuclear magnetic resonance ({sup 1}H HRMAS NMR). This linker has been regenerated after cleavage of spermidine and re-used without loss of efficiency. (author)

  14. Characterizing the mechanism(s) of heavy element synthesis reactions

    Science.gov (United States)

    Loveland, Walter

    2016-12-01

    A review of the current state of our understanding of complete fusion reaction mechanisms is presented, from the perspective of an experimentalist. For complete fusion reactions, the overall uncertainties in predicting heavy element synthesis cross sections are examined in terms of the uncertainties associated with the calculations of capture cross sections, fusion probabilities and survival probabilities.

  15. SYNTHESIS, CHARACTERIZATION AND BIOACTIVITY Zn2+, Cu2+ ...

    African Journals Online (AJOL)

    ray powder diffraction analysis of complexes (2) and (3) indicate that the ... wastewater and catalytic processes [15]. furthermore, azo compounds have an increased ...... Dong Koo, K.; Lee, C.S.; Sung Koh, J.; Kim, G.T. Design and synthesis of ...

  16. Synthesis and characterization of zwitterionic carbon dioxide fixing reagents

    DEFF Research Database (Denmark)

    Mikkelsen, Mette; Jørgensen, Mikkel; Krebs, Frederik C

    2010-01-01

    The synthesis of three amine-based carbon dioxide fixing reagents is presented. The reagents were designed so that they would be able to bind CO2 reversibly through the formation of the well known carbamates that was stabilized through forming a zwitterion. CO2 fixing experiments were performed...

  17. Synthesis of an Albendazole Metabolite: Characterization and HPLC Determination

    Science.gov (United States)

    Mahler, Graciela; Davyt, Danilo; Gordon, Sandra; Incerti, Marcelo; Nunez, Ivana; Pezaroglo, Horacio; Scarone, Laura; Serra, Gloria; Silvera, Mauricio; Manta, Eduardo

    2008-01-01

    In this laboratory activity, students are introduced to the synthesis of an albendazole metabolite obtained by a sulfide oxidation reaction. Albendazole as well as its metabolite, albendazole sulfoxide, are used as anthelmintic drugs. The oxidation reagent is H[subscript 2]O[subscript 2] in acetic acid. The reaction is environmental friendly,…

  18. Synthesis and photonic bandgap characterization of polymer inverse opals

    Energy Technology Data Exchange (ETDEWEB)

    Miguez, H.; Meseguer, F.; Lopez, C. [Consejo Superior de Investigaciones Cientificas, Madrid (Spain). Inst. de Ciencia de Materiales; Universidad Politecnica de Valencia (Spain). Centro Tecnologico de Ondas; Lopez-Tejeira, F.; Sanchez-Dehesa, J. [Universidad Autonoma de Madrid (Spain). Dept. de Fisica Teorica de la Materia Condensada

    2001-03-16

    Polymer inverse opals with long-range order have been fabricated and their photonic crystal behavior examined. Good agreement between band structure calculations and experiment is found. It is envisaged that these inverse opals could be used for the modification of the electronic properties of incorporated luminescent materials and as matrices for the synthesis of spherical colloidal particles. (orig.)

  19. The synthesis and characterization of 2-mercaptoethyl methacrylate

    Directory of Open Access Journals (Sweden)

    Knežević Marija

    2005-01-01

    Full Text Available The synthesis of 2-mercaptoethyl methacrylate from methacrylic acid and 2-mercaptoethanol by etherification using acetyl chloride as catalyst was optimized. The purity of the obtained product was controlled by gas chromatography and its identity confirmed by H-NMR and FTIR spectroscopy. 2-Mercapto-ethyl methacrylate could find application as a chain transfer agent in radical polymerizations.

  20. Synthesis of an Albendazole Metabolite: Characterization and HPLC Determination

    Science.gov (United States)

    Mahler, Graciela; Davyt, Danilo; Gordon, Sandra; Incerti, Marcelo; Nunez, Ivana; Pezaroglo, Horacio; Scarone, Laura; Serra, Gloria; Silvera, Mauricio; Manta, Eduardo

    2008-01-01

    In this laboratory activity, students are introduced to the synthesis of an albendazole metabolite obtained by a sulfide oxidation reaction. Albendazole as well as its metabolite, albendazole sulfoxide, are used as anthelmintic drugs. The oxidation reagent is H[subscript 2]O[subscript 2] in acetic acid. The reaction is environmental friendly,…

  1. Advances in acrylic-alkyd hybrid synthesis and characterization

    Science.gov (United States)

    Dziczkowski, Jamie

    2008-10-01

    performance. Reversible-addition fragmentation polymerization techniques were employed to create a new class of acrylic-alkyd hybrid materials. Medium and long oil alkyds made from the monoglyceride process using soybean oil, glycerol, and phthalic anhydride were modified with a RAFT chain transfer agent. The alkyd macro-RAFT agents were reached by end-capping a medium oil soya-based alkyd with a carboxy-functional trithiocarbonate. The alkyd macro-RAFT agents were then used to create acrylic-alkyd block structures by polymerizing different acrylic monomers, including both acrylates and methacrylates in the presence of the macro-RAFT agent and 2, 2'-azobisisobutyronitrile (AIBN). Co-acrylic segments were reached by complete polymerization of one monomer followed by the addition of a second monomer and additional free radical initiator. The alkyds, macro-RAFT agents and, acrylic-alkyd blocks were characterized by size-exclusion chromatography (SEC), FTIR, and 1H-NMR. Pseudo-first-order kinetics behavior and conversion vs. molecular weight plots show that the RAFT-mediated reaction afforded a more controlled process for the synthesis of acrylated-alkyd materials. Preliminary coatings tests showed that material properties of acrylated-alkyds achieved by RAFT polymerization exhibit good overall coatings properties including adhesion, gloss, hardness, and impact resistance.

  2. Synthesis and characterization of aminated perfluoro polymer electrolytes

    Science.gov (United States)

    Page-Belknap, Zachary Stephan Glenn

    Polymer electrolytes have been developed for use in anion exchange membrane fuel cells for years. However, due to the highly corrosive environment within these fuel cells, poor chemical stability of the polymers and low ion conductivity have led to high development costs and thus prevention from widespread commercialization. The work in this study aims to provide a solution to these problems through the synthesis and characterization of a novel polymer electrolyte. The 800 EW 3M PFSA sulfonyl fluoride precursor was aminated with 3-(dimethylamino)-1-propylamine to yield a functional polymer electrolyte following quaternization, referred to in this work as PFSa-PTMa. 1 M solutions of LiPF6, HCL, KOH, NaOH, CsOH, NaHCO3 and Na2CO3 were used to exchange the polymer to alternate counterion forms. Chemical structure analysis was performed using both FT and ATR infrared spectroscopy to confirm sulfonyl fluoride replacement and the absence of sulfonic acid sites. Mechanical testing of the polymer, following counterion exchange with KOH, at saturated conditions and 60 ºC exhibited a tensile strength of 13 +/- 2.0 MPa, a Young's modulus of 87 +/- 16 MPa and a degree of elongation reaching 75% +/- 9.1%, which indicated no mechanical degradation following exposure to a highly basic environment. Conductivities of the polymer in the Cl- and OH- counterion forms at saturated conditions and 90 ºC were observed at 26 +/- 8.0 mS cm-1 and 1.1 +/- 0.1 mS cm-1, respectively. OH- conductivities were slightly above those observed for CO32- and HCO 3- counterions at the same conditions, 0.63 +/- 0.18 and 0.66 +/- 0.21 mS cm-1 respectively. The ion exchange capacity (IEC) of the polymer in the Cl- counterion form was measured via titration at 0.57 meq g-1 which correlated to 11.2 +/- 0.10 water molecules per ion site when at 60ºC and 95% relative humidity. The IEC of the polymer in the OH- counterion form following titration expressed nearly negligible charge density, less than 0.01 meq

  3. Characterization of spermatogonial stem cells lacking intercellular bridges and genetic replacement of a mutation in spermatogonial stem cells.

    Directory of Open Access Journals (Sweden)

    Naoki Iwamori

    Full Text Available Stem cells have a potential of gene therapy for regenerative medicine. Among various stem cells, spermatogonial stem cells have a unique characteristic in which neighboring cells can be connected by intercellular bridges. However, the roles of intercellular bridges for stem cell self-renewal, differentiation, and proliferation remain to be elucidated. Here, we show not only the characteristics of testis-expressed gene 14 (TEX14 null spermatogonial stem cells lacking intercellular bridges but also a trial application of genetic correction of a mutation in spermatogonial stem cells as a model for future gene therapy. In TEX14 null testes, some genes important for undifferentiated spermatogonia as well as some differentiation-related genes were activated. TEX14 null spermatogonial stem cells, surprisingly, could form chain-like structures even though they do not form stable intercellular bridges. TEX14 null spermatogonial stem cells in culture possessed both characteristics of undifferentiated and differentiated spermatogonia. Long-term culture of TEX14 null spermatogonial stem cells could not be established likely secondary to up-regulation of CDK4 inhibitors and down-regulation of cyclin E. These results suggest that intercellular bridges are essential for both maintenance of spermatogonial stem cells and their proliferation. Lastly, a mutation in Tex14(+/- spermatogonial stem cells was successfully replaced by homologous recombination in vitro. Our study provides a therapeutic potential of spermatogonial stem cells for reproductive medicine if they can be cultured long-term.

  4. Characterization of Spermatogonial Stem Cells Lacking Intercellular Bridges and Genetic Replacement of a Mutation in Spermatogonial Stem Cells

    Science.gov (United States)

    Iwamori, Naoki; Iwamori, Tokuko; Matzuk, Martin M.

    2012-01-01

    Stem cells have a potential of gene therapy for regenerative medicine. Among various stem cells, spermatogonial stem cells have a unique characteristic in which neighboring cells can be connected by intercellular bridges. However, the roles of intercellular bridges for stem cell self-renewal, differentiation, and proliferation remain to be elucidated. Here, we show not only the characteristics of testis-expressed gene 14 (TEX14) null spermatogonial stem cells lacking intercellular bridges but also a trial application of genetic correction of a mutation in spermatogonial stem cells as a model for future gene therapy. In TEX14 null testes, some genes important for undifferentiated spermatogonia as well as some differentiation-related genes were activated. TEX14 null spermatogonial stem cells, surprisingly, could form chain-like structures even though they do not form stable intercellular bridges. TEX14 null spermatogonial stem cells in culture possessed both characteristics of undifferentiated and differentiated spermatogonia. Long-term culture of TEX14 null spermatogonial stem cells could not be established likely secondary to up-regulation of CDK4 inhibitors and down-regulation of cyclin E. These results suggest that intercellular bridges are essential for both maintenance of spermatogonial stem cells and their proliferation. Lastly, a mutation in Tex14+/− spermatogonial stem cells was successfully replaced by homologous recombination in vitro. Our study provides a therapeutic potential of spermatogonial stem cells for reproductive medicine if they can be cultured long-term. PMID:22719986

  5. Synthesis, Characterization and Applications in Catalysis of Polyoxometalate/Zeolite Composites

    Directory of Open Access Journals (Sweden)

    Frédéric Lefebvre

    2016-05-01

    Full Text Available An overview of the synthesis, characterization and catalytic applications of polyoxometalates/zeolites composites is given. The solids obtained by direct synthesis of the polyoxometalate in the presence of the zeolite are first described with their applications in catalysis. Those obtained by a direct mixing of the two components are then reviewed. In all cases, special care is taken in the localization of the polyoxometalate, inside the zeolite crystal, in mesopores or at the external surface of the crystals, as deduced from the characterization methods.

  6. Synthesis and Characterization of Two New p-tert-Butylcalix[4]-arene Schiff Bases

    OpenAIRE

    Saeed Taghvaee Ganjali; Karim Akbari Dilmaghani; Behrouz Shaabani; Abdol Ali Alemi

    2001-01-01

    Synthesis and characterization of two new Schiff bases of p-tertbuthylcalix[4]arene (H2L1 and HL2) is described. The synthesis of H2L1 and HL2 has been achieved by the condensation of salicylaldehyde with the amine group of upper rim monoamine p-tert-butylcalix[4]arene in ethanol. These compounds have been characterized on the basis of elemental analysis and spectral data. Solvatochromicity and fluorescence properties were observed and measured for H2L1 and HL2. Solvatochromicity of these lig...

  7. Synthesis and Characterization of Two New p-tert-Butylcalix[4]-arene Schiff Bases

    Directory of Open Access Journals (Sweden)

    Saeed Taghvaee Ganjali

    2001-03-01

    Full Text Available Synthesis and characterization of two new Schiff bases of p-tertbuthylcalix[4]arene (H2L1 and HL2 is described. The synthesis of H2L1 and HL2 has been achieved by the condensation of salicylaldehyde with the amine group of upper rim monoamine p-tert-butylcalix[4]arene in ethanol. These compounds have been characterized on the basis of elemental analysis and spectral data. Solvatochromicity and fluorescence properties were observed and measured for H2L1 and HL2. Solvatochromicity of these ligands indicates their potential for NLO applications.

  8. [Synthesis and Characterization of a Sugar Based Electrolyte for Thin-film Polymer Batteries

    Science.gov (United States)

    1998-01-01

    The work performed during the current renewal period, March 1,1998 focused primarily on the synthesis and characterization of a sugar based electrolyte for thin-film polymer batteries. The initial phase of the project involved developing a suitable sugar to use as the monomer in the polymeric electrolyte synthesis. The monomer has been synthesized and characterized completely. Overall the yield of this material is high and it can be produced in relatively large quantity easily and in high purity. The scheme used for the preparation of the monomer is outlined along with pertinent yields.

  9. Controlling Magnetic and Ferroelectric Order Through Geometry: Synthesis, Ab Initio Theory, Characterization of New Multi-Ferric Fluoride Materials

    Energy Technology Data Exchange (ETDEWEB)

    Halasyamani, Shiv [Univ. of Houston, TX (United States); Fennie, Craig [Cornell Univ., Ithaca, NY (United States)

    2016-11-03

    We have focused on the synthesis, characterization, and ab initio theory on multi-functional mixed-metal fluorides. With funding from the DOE, we have successfully synthesized and characterized a variety of mixed metal fluoride materials.

  10. Preliminary Synthesis and Characterization of Mesoporous Nanocrystalline Zirconia

    Institute of Scientific and Technical Information of China (English)

    Xinmei Liu; Gaoqing Lu; Zifeng Yan

    2003-01-01

    A novel method to prepare mesoporous nano-zirconia was developed. The synthesis was carried out in the presence of PEO surfactants via a solid-state reaction. The materials exhibit a strong diffraction peak at low 2θ angle and their nitrogen adsorption/desorption isotherms are typical of type Ⅳ with H1 hysteresis loops. The pore structure imaged by TEM can be described as wormhole domains.The tetragonal zirconia nanocrystals are uniform in size (around 1.5 nm) and their mesopores focus on around 4.6 nm. The zirconia nanocrystal growth is tentatively postulated to be the result of an aggregation mechanism. This study also reveals that the PEO surfactants can interact with the Zr-O-Zr framework to reinforce the thermal stability of zirconia. The ratio of NaOH to ZrOC12, crystallization and calcination temperature play an important role in the synthesis of mesoporous nano-zirconia.

  11. Unprecedented copper(I) bifluoride complexes: synthesis, characterization and reactivity.

    Science.gov (United States)

    Vergote, Thomas; Nahra, Fady; Welle, Alexandre; Luhmer, Michel; Wouters, Johan; Mager, Nathalie; Riant, Olivier; Leyssens, Tom

    2012-01-16

    To be or not to bifluoride: Two synthetic pathways to unprecedented N-heterocyclic carbene copper(I) bifluoride complexes have been developed. Catalytic tests demonstrated that copper(I) bifluorides are very efficient catalysts, which do not require any additional activating agent. The first Cu-catalyzed diastereoselective allylation of (R)-N-tert-butanesulfinyl aldimines was also established. The method enables efficient, simple and general synthesis of enantiomerically enriched homoallylic amines at room temperature in high yields.

  12. Synthesis, characterization and functionalization of vertically aligned carbon nanotube arrays

    OpenAIRE

    2012-01-01

    Ankara : The Materials Science and Nanotechnology Program of the Graduate School of Engineering and Sciences of Bilkent University, 2012. Thesis (Ph. D.) -- Bilkent University, 2012. Includes bibliographical refences. In the last decade, there has been an increased interest on carbon nanotubes (CNTs) for various applications due to their unique structural, electronic, mechanical and chemical properties. Synthesis of CNTs is no more a challenge with the enhancements and diver...

  13. Synthesis of Telechelic Polyisobutylenes and Polyethers and Their Characterization

    Institute of Scientific and Technical Information of China (English)

    Sándor Kéki; Miklós Nagy; Gy(o)rgy Deák; László Orosz; Miklós Zsuga

    2005-01-01

    @@ 1Introduction Telechelic polymers have attained great consideration as building blocks in the synthesis of block copolymers and networks. Telechelic polymers with various endgroups are also widely used materials for the preparation of polymeric prodrugs. Several methods have been reported to obtain functionalized polymers from the corresponding polyisobutylene (PIB) and polyether derivatives. In this presentation, we will demonstrate very versatile and powerful synthetic methods to obtain telechelic polymers.

  14. Characterization and synthesis of carbon aggregates in high temperature environment

    OpenAIRE

    2013-01-01

    Carbon materials in all its forms, from the natural carbon solid materials, as coal and graphite, to the synthesized carbon materials, as carbon black, pitch fibers, fullerenes, carbon nanotubes, etc,. have been object of many studies regarding their characteristics and behaviour due to their importance in the energy and industrial sectors. Recently, most of the research efforts have been focused on the synthesis of new carbon materials and in particular on their physico-chemical propertie...

  15. Synthesis, characterization, and reactivity of furan- and thiophene-functionalized bis(n-heterocyclic carbene) complexes of iron(II)

    KAUST Repository

    Rieb, Julia

    2014-09-15

    The synthesis of iron(II) complexes bearing new heteroatom-functionalized methylene-bridged bis(N-heterocyclic carbene) ligands is reported. All complexes are characterized by single-crystal X-ray diffraction (SC-XRD), nuclear magnetic resonance (NMR) spectroscopy, and elemental analysis. Tetrakis(acetonitrile)-cis-[bis(o-imidazol-2-ylidenefuran)methane]iron(II) hexafluorophosphate (2a) and tetrakis(acetonitrile)-cis-[bis(o-imidazol-2-ylidenethiophene)methane]iron(II) hexafluorophosphate (2b) were obtained by aminolysis of [Fe{N(SiMe3)2}2(THF)] with furan- and thiophene-functionalized bis(imidazolium) salts 1a and 1b in acetonitrile. The SC-XRD structures of 2a and 2b show coordination of the bis(carbene) ligand in a bidentate fashion instead of a possible tetradentate coordination. The four other coordination sites of these distorted octahedral complexes are occupied by acetonitrile ligands. Crystallization of 2a in an acetone solution by the slow diffusion of Et2O led to the formation of cisdiacetonitriledi[ bis(o-imidazol-2-ylidenefuran)methane]iron(II) hexafluorophosphate (3a) with two bis(carbene) ligands coordinated in a bidentate manner and two cis-positioned acetonitrile molecules. Compounds 2a and 2b are the first reported iron(II) carbene complexes with four coordination sites occupied by solvent molecules, and it was demonstrated that those solvent ligands can undergo ligand-exchange reactions.

  16. Synthesis, Crystal Structure and Magnetic Properties of a Novel Azide-bridged Copper(Ⅱ) Coordination Polymers Containing Nitroxy Nitroxide

    Institute of Scientific and Technical Information of China (English)

    WANG Yu-Fang; ZHANG Yong-Hua; WANG Li-Ya

    2011-01-01

    A novel azide-bridged copper(Ⅱ) coordination polymer, [Cu3(NITpPy)4(N3)6]n (NITpPy = 4-pyridyl-4,4,5,5-tetramethylimidazline-3-oxide-1-oxyl), was structurally and magnetically characterized. It crystallizes in the triclinic space group P with a = 7.6932(10), b = 14.5556(19), c = 16.122(2) , α = 108.443(2), β = 95.251(2), γ = 104.236(2)°, V = 1631.7(4) 3, C48H64Cu3N30O8, Mr = 1379.87, Z = 1, Dc = 1.404 g/cm3, μ(MoKα) = 1.041 mm-1, F(000) = 713, the R = 0.0510 and wR = 0.1185 for 4285 observed reflections with I 2σ(I). X-ray analysis reveals that the Cu(Ⅱ) ions are linked by nitrogen atom of μ1,1 azido ligands to form a Cu-Cu-Cu unit. The units are linked by μ1,3 azido ligands through a bridging style to form a one-dimensional coordination polymer. The variable-temperature magnetic susceptibility data of the complex show ferromagnetic interactions in the complex.

  17. Synthesis and Crystal Structure of a New One-dimensional Zn(II) Nitronyl Nitroxide Complex Bridged by Pyridine-2,4-dicarboxylate Anion

    Institute of Scientific and Technical Information of China (English)

    GAO Dong-Zhao; LI Li-Cun; LIAO Dai-Zheng; JIANG Zong-Hui; YAN Shi-Ping

    2006-01-01

    A new one-dimensional (1-D) Zn(II) nitronyl nitroxide complex bridged by pyri- dine-2,4-dicarboxylate anion, [Zn(NIT4Py)(2,4-PDA)(H2O)2]n (NIT4Py = 2-(4'-pyridyl)-4,4,5,5- tetramethylimidazoline-1-oxyl-3-oxide and 2,4-PDA = pyridine-2,4-dicarboxylate anion), has been synthesized and structurally characterized by X-ray diffraction. It crystallizes in monoclinic, space group P21/c with a = 16.834(2), b = 7.4376(10), c = 18.295(3) (A), β = 102.848(2)°, V = 2233.2(5)(A)3, C19H23N4O8Zn, Mr = 500.78, Dc = 1.489 g/cm3, μ(MoKα) = 1.152 mm-1, F(000) = 1036, Z = 4, the final R = 0.0390 and wR = 0.0915 for 3234 observed reflections. In the complex, each zinc(II) ion is six-coordinated by one nitrogen atom of the radical ligand (NIT4Py), one nitrogen atom and two oxygen atoms of two 2,4-PDA anions and two oxygen atoms of two water molecules. Each 2,4-PDA anion bridges two Zn(II) ions via a tridentate mode into a 1-D chain, and these 1-D chains are further linked into a 2-D network via hydrogen-bonding interactions.

  18. Synthesis and properties of the chain-like polymeric copper(Ⅱ)complexes bridged by bis(diphenylphosphino oxide)ethane

    Institute of Scientific and Technical Information of China (English)

    YANG, Rui-Na(杨瑞娜); HOU, Yi-Min(侯益民); HU, Xiao-Yuan(胡晓院); SUN, Yu-An(孙雨安); JIN, Dou-Man(金斗满)

    2000-01-01

    At room temperature, the chain-like polymeric copper(Ⅱ)complexes bridged by bis(diphenylphosphino oxide) ethane (dppeO2), [Cu(dppeO2)X2]n[X= Cl(1), Br(2)] have been prepared and characterized by elemental analysis, 31P NMR,TG-DTA X-ray analysis for [CuBr2(dppeO2)]n. The chain is composed of subunits containing tetrahedron coordinated copper(Ⅱ) atoms. The four-coordinated copper(Ⅱ)atom is ligated to another four-coordinated copper(Ⅱ) atom through dppeO2. The coordination sphere of copper(Ⅱ) atom is completed by two monodentate bromide and two oxygen atoms from bridging dppeO2. Crystal data are as follows: C26-H24CuP2Br2O2, 0.50 mm×0.40 mm×0.40 mm, monoclinic, space group: C2/c, λ=0.07107(Mo Kα), a=1.2286(2) mm, b =2.0555(8) nm, c = 1.0652(2) nm, β=97.366(9)°, V=2.668 nm3, Z=4, Dcalc=1.628g.cm-3,R =0.066; Rw= 0.091.

  19. Synthesis and characterization of nanoparticles of CZTSe by microwave-assited chemical synthesis

    Science.gov (United States)

    Reyes Vallejo, O.; Sánchez, Mónica; Pal, Mou; Espinal, R.; Llorca, Jordi; Sebastian, P. J.

    2016-12-01

    In this study we present the synthesis of Cu2ZnSnSe4 (CZTSe) nanoparticles by microwave-assisted chemical synthesis employing organic solvents. The effect of reaction time, reactant concentration, solvent and additives (inorganic material) was studied on the structural and optical properties of the nanomaterials. The powder samples were analyzed by x-ray diffraction, Raman spectroscopy, x-ray energy dispersive spectroscopy and x-ray photoelectron spectroscopy. The results show that the synthesis performed with triethanolamine and deionized water is better than others solvents, producing nanocrystals of quaternary phase (CZTSe) with stoichiometric relations similar to the reported research in the literature, which falls in the range of Cu/(Zn+Sn): 0.8-1.0, Zn/Sn: 1.0-1.20. The nanoparticles of CZTSe synthesized in this study present desirable properties in order to use them in solar cell and photoelectrochemical cell applications.

  20. Synthesis, molecular structure, computational study and in vitro anticancer activity of dinuclear thiolato-bridged pentamethylcyclopentadienyl Rh(III) and Ir(III) complexes.

    Science.gov (United States)

    Gupta, Gajendra; Garci, Amine; Murray, Benjamin S; Dyson, Paul J; Fabre, Gabin; Trouillas, Patrick; Giannini, Federico; Furrer, Julien; Süss-Fink, Georg; Therrien, Bruno

    2013-11-21

    Neutral dinuclear dithiolato-bridged pentamethylcyclopentadienyl Rh(III) complexes of the type (C5Me5)2Rh2(μ-SR)2Cl2 (R = CH2Ph, 1; R = CH2CH2Ph, 2) and cationic dinuclear trithiolato-bridged pentamethylcyclopentadienyl Rh(III) and Ir(III) complexes of the type [(C5Me5)2M2(μ-SR)3](+) (M = Rh, R = CH2Ph, 3; M = Rh, R = CH2CH2Ph, 5; M = Rh, R = CH2C6H4-p-(t)Bu, 7: M = Ir, R = CH2Ph, 4; M = Ir, R = CH2CH2Ph, 6; M = Ir, R = CH2C6H4-p-(t)Bu, 8) have been synthesized from the chloro-bridged pentamethylcyclopentadienyl Rh(III) and Ir(III) dimers (C5Me5)2M2(μ-Cl)2Cl2 by reaction with the corresponding thiol derivative (RSH). Complexes 3-8 were isolated as chloride salts. All complexes were obtained in good yield and were fully characterized by spectroscopic methods. The molecular structures of the neutral complexes (1 and 2) show interesting features: the two rhodium atoms are bridged by two thiolato ligands with no metal-metal bonds and the pentamethylcyclopentadienyl and chlorido ligands are oriented syn to each other, an uncommon conformation for such dinuclear complexes. These structural features were rationalized using DFT calculations. Additionally, the antiproliferative activity of the complexes was evaluated against the cancerous A2780 (cisplatin sensitive) and A2780cisR (cisplatin resistant) human ovarian cell lines and on the noncancerous HEK293 human embryonic kidney cells. All complexes were found to be active and the cationic iridium complexes , and are particularly cytotoxic, with IC50 values in the nanomolar range (IC50 < 0.1 μM). The catalytic activity of the complexes for the oxidation of glutathione (GSH) to GSSG was evaluated by NMR spectroscopy.

  1. Role of a salt bridge in the model protein crambin explored by chemical protein synthesis: X-ray structure of a unique protein analogue, [V15A]crambin-alpha-carboxamide.

    Science.gov (United States)

    Bang, Duhee; Tereshko, Valentina; Kossiakoff, Anthony A; Kent, Stephen B H

    2009-07-01

    We have used total chemical synthesis to prepare [V15A]crambin-alpha-carboxamide, a unique protein analogue that eliminates a salt bridge between the delta-guanidinium of the Arg(10) side chain and the alpha-carboxylate of Asn(46) at the C-terminus of the polypeptide chain. This salt bridge is thought to be important for the folding and stability of the crambin protein molecule. Folding, with concomitant disulfide bond formation, of the fully reduced [V15A]crambin-alpha-carboxamide polypeptide was less efficient than folding/disulfide formation for the [V15A]crambin polypeptide under a standard set of conditions. To probe the origin of this less efficient folding/disulfide bond formation, we separately crystallized purified synthetic [V15A]crambin-alpha-carboxamide and chemically synthesized [V15A]crambin and solved their X-ray structures. The crystal structure of [V15A]crambin-alpha-carboxamide showed that elimination of the Arg(10)-Asn(46) salt bridge caused disorder of the C-terminal region of the polypeptide chain and affected the overall 'tightness' of the structure of the protein molecule. These studies, enabled by chemical protein synthesis, strongly suggest that in native crambin the Arg(10)-Asn(46) salt bridge contributes to efficient formation of correct disulfide bonds and also to the well-ordered structure of the protein molecule.

  2. Myocardial Bridging

    Directory of Open Access Journals (Sweden)

    Shi-Min Yuan

    2016-02-01

    Full Text Available Abstract Myocardial bridging is rare. Myocardial bridges are most commonly localized in the middle segment of the left anterior descending coronary artery. The anatomic features of the bridges vary significantly. Alterations of the endothelial morphology and the vasoactive agents impact on the progression of atherosclerosis of myocardial bridging. Patients may present with chest pain, myocardial infarction, arrhythmia and even sudden death. Patients who respond poorly to the medical treatment with β-blockers warrant a surgical intervention. Myotomy is a preferred surgical procedure for the symptomatic patients. Coronary stent deployment has been in limited use due to the unsatisfactory long-term results.

  3. Bridging Classroom Language Ethnography

    OpenAIRE

    GRENFELL, MICHAEL JAMES

    2012-01-01

    PUBLISHED Paper #5: Bridging Classroom Language Ethnography, New Literacy Studies and Bourdieu?s Social Philosophy: Principles and Practice The purpose of this paper is to analyze and synthesize the various ways that classroom language ethnography, NLS, and Bourdieu?s social philosophy, were integrated. The goal of the analysis and synthesis is to provide a fresh perspective and fruitful insights on literacy in all its manifestations that provides the foundations for a more robust...

  4. Synthesis and electrochemical characterization of stabilized nickel nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Dominguez-Crespo, M.A.; Ramirez-Meneses, E.; Torres Huerta, A.M. [Centro de Investigacion en Ciencia Aplicada y Tecnologia Avanzada, CICATA-IPN Unidad Altamira, Carretera Tampico-Puerto Industrial, C.P. 89600 Altamira, Tamaulipas (Mexico); Montiel-Palma, V. [Centro de Investigaciones Quimicas, Universidad Autonoma del Estado de Morelos, Av. Universidad 1001, Colonia Chamilpa, C.P.62201 Cuernavaca, Morelos (Mexico); Dorantes Rosales, H. [Departamento de Metalurgia, Escuela Superior de Ingenieria Quimica e Industrias Extractivas - IPN, C.P. 07300, D.F. (Mexico)

    2009-02-15

    Nickel stabilized nanoparticles produced by an organometallic approach (Chaudret's method) starting from the complex Ni(1,5-COD){sub 2} were used as electrode materials for hydrogen evolution in NaOH at two temperatures (298 and 323 K). The synthesis of the nickel nanoparticles was performed in the presence of two different stabilizers, 1,3-diaminopropane (DAP) and anthranilic acid (AA), by varying the molar ratios (1:1, 1:2 and 1:5 metal:ligand) in order to evaluate their influence on the shape, dispersion, size and electrocatalytic activity of the metallic particles. The presence of an appropriate amount of stabilizer is an effective alternative to the synthesis of small monodispersed metal nanoparticles with diameters around 5 and 8 nm for DAP and AA, respectively. The results are discussed in terms of morphology and the surface state of the nanoparticles. The importance of developing a well-controlled synthetic method which results in higher performances of the resulting nanoparticles is highlighted. Herein we found that the performance with respect to the HER of the Ni electrodes dispersed on a carbon black Vulcan substrate is active and comparable to that reported in the literature for the state-of-the-art electrocatalysts. Appreciable cathodic current densities of {proportional_to}240 mA cm{sup -2} were measured with highly dispersed nickel particles (Ni-5{sub DAP}). This work demonstrates that the aforementioned method can be extended to the preparation of highly active stabilized metal particles without inhibiting the electron transfer for the HER reaction, and it could also be applied to the synthesis of bimetallic nanoparticles. (author)

  5. Solution combustion synthesis and characterization of nanosized bismuth ferrite

    Science.gov (United States)

    Sai Kumar, V. Sesha; Rao, K. Venkateswara; Krishnaveni, T.; Kishore Goud, A. Shiva; Reddy, P. Ranjith

    2012-06-01

    The present paper describes a simple method of nanosized BiFeO3 by the solution combustion synthesis using bismuth and iron nitrates as oxidizers and the combination fuel of citric acid and ammonium hydroxide, with fuel to oxidizer ratio (Ψ = 1) one. The X-ray Diffraction results indicated rhombohedral phase (R3m) with JCPDS data card no: 72-2035. The ferroelectric transition of the sample at 8310C was detected by differential thermal analysis. Thermal analysis was done by Thermal gravimetric-Differential thermal analyzer and obtained results were presented in this paper.

  6. Plasma synthesis and characterization of ultrafine SiC

    Energy Technology Data Exchange (ETDEWEB)

    Vogt, G.J.; Phillips, D.S.; Taylor, T.N.

    1986-01-01

    Ultrafine SiC powders have been prepared by gas phase synthesis from silane and methane in an argon thermal rf-plasma. Bulk properties of the powders were determined by elemental analysis, x-ray diffractin, helium pycnometry, and BET surface area measurements. The near-surface composition and structure of the particles were examined by x-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM). In addition to free silicon and carbon particles in the powders, free carbon and various silicon/carbon/oxygen species were found on the surface of the SiC particles.

  7. Aqueous combustion synthesis and characterization of zirconia-alumina nanocomposites

    Energy Technology Data Exchange (ETDEWEB)

    Kishan, J.; Mangam, Venu; Reddy, B.S.B.; Das, Siddhartha [Department of Metallurgical and Materials Engineering, Indian Institute of Technology, Kharagpur, West Bengal 721302 (India); Das, Karabi, E-mail: karabi@metal.iitkgp.ernet.i [Department of Metallurgical and Materials Engineering, Indian Institute of Technology, Kharagpur, West Bengal 721302 (India)

    2010-02-04

    The zirconia-alumina nanocomposite powders with 3-48 mol% of alumina are prepared by aqueous combustion synthesis technique using stoichiometric amounts of aluminium nitrate, zirconyl nitrate and glycine. The nanopowders are compacted uniaxially and sintered at 1000 {sup o}C temperature in a muffle furnace. Thermodynamic modeling of the combustion reaction shows that, as the alumina content increases, the amount of gases produced increases with a decrease in the adiabatic flame temperature. The green and sintered densities of cold press composite powders decrease with an increase in the mol% of alumina.

  8. Synthesis, Characterization and Testing of Novel Anode and Cathode Materials for Li-Ion Batteries

    Energy Technology Data Exchange (ETDEWEB)

    White, Ralph E.; Popov, Branko N.

    2002-10-31

    During this program we have synthesized and characterized several novel cathode and anode materials for application in Li-ion batteries. Novel synthesis routes like chemical doping, electroless deposition and sol-gel method have been used and techniques like impedance, cyclic voltammetry and charge-discharge cycling have been used to characterize these materials. Mathematical models have also been developed to fit the experimental result, thus helping in understanding the mechanisms of these materials.

  9. Nano-/micro metallic wire synthesis on Si substrate and their characterization

    Energy Technology Data Exchange (ETDEWEB)

    Kaur, Jaskiran, E-mail: kaur.jaskiran@gmail.com; Kaur, Harmanmeet, E-mail: kaur.jaskiran@gmail.com; Singh, Surinder, E-mail: kaur.jaskiran@gmail.com [Department of Physics, Guru Nanak Dev University, Amritsar-143005 (India); Kanjilal, Dinakar [Inter-University Accelerator Centre, New Delhi-110067 (India); Chakarvarti, Shiv Kumar [Manav Rachna International University, Faridabad-121003 (India)

    2014-04-24

    Nano-/micro wires of copper are grown on semiconducting Si substrate using the template method. It involves the irradiation of 8 um thick polymeric layer coated on Si with150 MeV Ni ion beam at a fluence of 2E8. Later, by using the simple technique of electrodeposition, copper nano-/micro wires were grown via template synthesis. Synthesized wires were morphologically characterized using SEM and electrical characterization was carried out by finding I-V plot.

  10. Synthesis and Characterization of Impurities in the Production Process of Lopinavir.

    Science.gov (United States)

    Raghava Reddy, Ambati V; Garaga, Srinivas; Takshinamoorthy, Chandiran; Naidu, Andra

    2015-01-01

    Lopinavir is an antiretroviral drug used for the inhibition of HIV protease. Four related substances of lopinavir were observed during the manufacturing process of lopinavir in the laboratory and they were identified. The present work describes the origin, synthesis, characterization, and control of these related substances.

  11. Synthesis and Characterization of Star-like Liquid Crystals Centered by Silicon

    Institute of Scientific and Technical Information of China (English)

    Jian Qiang LIU; Qi Zhen ZHANG; Jing Zhi ZHANG

    2004-01-01

    The synthesis and characterization of two new star-like liquid crystals are reported.They are made of a silicon core and four alkoxyazobenzene monomers in the periphery. Their phase behaviors and the structures are determined by infrared absorption spectroscopy (IR),nuclear magnetic resonance spectroscopy (NMR), elemental analysis (EA), polarizing optical microscope (POM) and differential scanning calorimetry (DSC).

  12. Synthesis and Characterization of Process-Related Impurities of Antihypertensive Drug Olmesartan Medoxomil

    OpenAIRE

    Venkanna, G.; Madhusudhan, G.; K. Mukkanti; A. Sankar; Sampath Kumar, Y.; G. Venakata Narayana

    2013-01-01

    Olmesartan medoxomil (1) is the latest angiotensin receptor antagonist approved by the FDA for the treatment of hypertension. During the process development of olmesartan medoxomil, three process-related impurities were observed along with the final API. These impurities were identified as isopropyl olmesartan (12), dimedoxomil olmesartan (19), dibiphenyl olmesartan (17). The present work describes the synthesis and characterization of all these three impurities.

  13. Synthesis and characterization of long perylenediimide polymer fibers: from bulk to the single-molecule level

    NARCIS (Netherlands)

    de Witte, Pieter A.J.; Hernando Campos, J.; Neuteboom, Edda E.; van Dijk, E.M.H.P.; Meskers, Stefan C.J.; Janssen, Rene A.J.; van Hulst, N.F.; Nolte, Roeland J.M.; Garcia Parajo, M.F.; Rowan, Alan E.

    2006-01-01

    The synthesis and characterization of perylenediimide polyisocyanides is reported. In addition to short oligomers, our synthetic approach results in the formation of extremely long, well-defined, and rigid perylenediimide polymers. Ordering and close-packing of the chromophores in these long

  14. Synthesis and characterization of covalent diphenylalanine nanotube-folic acid conjugates

    DEFF Research Database (Denmark)

    León, John Jairo Castillo; Rindzevicius, Tomas; Wu, Kaiyu

    2014-01-01

    Herein, we describe the synthesis and characterization of a covalent nanoscale assembly formed between diphenylalanine micro/nanotubes (PNT) and folic acid (FA). The conjugate was obtained via chemical functionalization through coupling of amine groups of PNTs and carboxylic groups of FA. The sur...

  15. Tunable Hydrophobicity in DNA Micelles : Design, Synthesis, and Characterization of a New Family of DNA Amphiphiles

    NARCIS (Netherlands)

    Anaya, Milena; Kwak, Minseok; Musser, Andrew J.; Muellen, Klaus; Herrmann, Andreas; Müllen, Klaus

    2010-01-01

    This work describes the synthesis and characterization of a new family of DNA amphiphiles containing modified nucleobases. The hydrophobicity was imparted by the introduction of a dodec-1-yne chain at the 5-position of the uracil base, which allowed precise and simple tuning of the hydrophobic

  16. Synthesis and Characterization of Long Perylenediimide Polymer Fibers: From Bulk to the Single-Molecule Level

    NARCIS (Netherlands)

    Witte, de Pieter A.J.; Hernando, Jordi; Neuteboom, Edda E.; Dijk, van Erik M.H.P.; Meskers, Stefan C.J.; Janssen, Rene A.J.; Hulst, van Niek F.; Nolte, Roeland J.M.; Garcia-Parajo, Maria F.; Rowan, Alan E.

    2006-01-01

    The synthesis and characterization of perylenediimide polyisocyanides is reported. In addition to short oligomers, our synthetic approach results in the formation of extremely long, well-defined, and rigid perylenediimide polymers. Ordering and close-packing of the chromophores in these long polymer

  17. Tunable Hydrophobicity in DNA Micelles : Design, Synthesis, and Characterization of a New Family of DNA Amphiphiles

    NARCIS (Netherlands)

    Anaya, Milena; Kwak, Minseok; Musser, Andrew J.; Muellen, Klaus; Herrmann, Andreas; Müllen, Klaus

    2010-01-01

    This work describes the synthesis and characterization of a new family of DNA amphiphiles containing modified nucleobases. The hydrophobicity was imparted by the introduction of a dodec-1-yne chain at the 5-position of the uracil base, which allowed precise and simple tuning of the hydrophobic prope

  18. Synthesis and characterization of conjugated polymer containing azobenzene and oxadiazole units

    Institute of Scientific and Technical Information of China (English)

    Yue Zhang; Shi Jun Yu; Lu Wang; Cong Li

    2009-01-01

    A novel conjugated polymer containing azobenzene and oxadiazole units was synthesized through multi-step synthesis.The structures and properties of monomer and polymer were characterized and evaluated with IR,1H NMR,UV,TGA and GPC,respectively.Polymer with long side chain of alkoxy shows good solubility,thermal stability and photoisomerization property.

  19. Synthesis and characterization of hydroxyapatite crystals: a review study on the analytical methods

    NARCIS (Netherlands)

    Koutsopoulos, S.

    2002-01-01

    For the synthesis of hydroxyapatite crystals from aqueous solutions three preparation methods were employed. From the experimental processes and the characterization of the crystals it was concluded that aging and precipitation kinetics are critical for the purity of the product and its crystallogra

  20. Synthesis and characterization of some N-substituted amides of salicylic acid

    OpenAIRE

    Lupea Xenia Alfa; Padure Mirabela

    2003-01-01

    The synthesis of some N-substituted aromatic amides in the salicylic acid series was achieved, by direct reaction between primary amines and salicylic acid in inert organic solvent, in the presence of PCl3. The compounds that were obtained, partially not described in literature, were characterized by chemical-physical methods.

  1. Synthesis and characterization of some N-substituted amides of salicylic acid

    Directory of Open Access Journals (Sweden)

    Lupea Xenia Alfa

    2003-01-01

    Full Text Available The synthesis of some N-substituted aromatic amides in the salicylic acid series was achieved, by direct reaction between primary amines and salicylic acid in inert organic solvent, in the presence of PCl3. The compounds that were obtained, partially not described in literature, were characterized by chemical-physical methods.

  2. Synthesis and Characterization of the First Organically Templated Layered Cerium Phosphate Fluoride

    National Research Council Canada - National Science Library

    Ranbo Yu; Dan Wang; Shintaro Ishiwata; Takashi Saito; Masaki Azuma; Mikio Takano; Yunfa Chen; Jinghai Li

    2004-01-01

      A novel organically templated layered cerium phosphate fluoride [(CH2)2(NH3)2]0.5[CeIVF3(HPO4)] has been synthesized by hydrothermal synthesis technology, and characterized by means of single-crystal X-ray diffraction...

  3. Design, synthesis, and characterization of nucleosomes containing site-specific DNA damage.

    Science.gov (United States)

    Taylor, John-Stephen

    2015-12-01

    How DNA damaged is formed, recognized, and repaired in chromatin is an area of intense study. To better understand the structure activity relationships of damaged chromatin, mono and dinucleosomes containing site-specific damage have been prepared and studied. This review will focus on the design, synthesis, and characterization of model systems of damaged chromatin for structural, physical, and enzymatic studies.

  4. Synthesis, structure and magnetic properties of 5-(4-Sulfophenylazo) salicylate-bridged 1D coordination polymers containing linear trinuclear metal clusters

    Science.gov (United States)

    Liu, Hong; Song, Li-jun; Ju, Zhan-feng; Li, Wei; Zhang, Jie

    2008-03-01

    Three new trinuclear metal complexes with an azobenzene-containing ligand [M 3(Sasa) 2(Py) 2(H 2O) 8] (Na 2HSasa = 5-(4-Sulfophenylazo) salicylic acid disodium salt; Py = pyridine; M = Cu, Co, Zn), are synthesized through the interface diffusion and structurally characterized by single crystal X-ray diffraction, XRPD analysis and spectral methods. The metal ions in distorted octahedral coordination environments are connected by Sasa ligands to form 1D coordination polymer chain containing the linear trinuclear units with single syn-anti carboxylate bridges. The extensive hydrogen bonding interactions hold these chains together into 3D supramolecular network. Weak antiferromagnetic interactions between adjacent metal ions with J = -1.85 cm -1 and J = -2.81 cm -1 dominate the magnetic properties of Cu(II) and Co(II) complexes, separately.

  5. Synthesis, crystal structure and photo luminescent property of a 3D metal-organic hybrid of Cd(II) constructed by two different bridging carboxylate

    Indian Academy of Sciences (India)

    Biswajit Bhattacharya; Rajdip Dey; Debajyoti Ghoshal

    2013-05-01

    A solvothermal reaction of cadmium (II) nitrate with succinic acid and isonicotinic acid creates a novel 3D metal-organic framework, [Cd3(isonicotinate)2(suc)2] (1). Single crystal X-ray structure determination reveals that complex 1 posses two crystallographically independent Cd(II) centres. The succinate anion acts here as a heptadented ligand and binds five Cd(II) centre simultaneously. The heptacoordinated Cd(II) centres are oxo-bridged by succinate moiety and the hexacoordinated metal centres are terminally connected through four different succinate moiety to make the overall 2D sheet arrangement. In unit cell, the ratio of hexadented Cd(II) and heptadented Cd(II) is 1:2. The new compound was also characterized by luminescence spectra and compared with the luminescence spectra of the pure isonicotinic acid.

  6. Synthesis and Crystal Structure of a Cyano-bridged Bimetallic Complex K3(TMS)2(H2O)2Cr(CN)6 [TMS = Tetramethylene Sulfone

    Institute of Scientific and Technical Information of China (English)

    CHEN Wei; CHE Yun-Xia; ZHENG Ji-Min

    2005-01-01

    The cyano-bridged bimetallic complex K3(TMS)2(H2O)2Cr(CN)6 with three- dimensional microporous structure was synthesized and characterized. The title complex (C14H20CrK3N, Mr = 601.78) crystallizes in monoclinic, space group C2/c with a = 14.357(4), b = 9.331(3), c = 19.180(6)(A), β = 96.754(5)o, V = 2551.6(13) (A)3, Z = 4, Dc = 1.567 g/m3, μ(MoKα) = 1.141 mm-1, F(000) = 1228, the final R = 0.0440 and wR = 0.0990 for 1760 observed reflections (I > 2σ(I)). In the crystal, two [Cr(CN) 6]3- units, four K+ ions and two oxygen atoms of two TMS molecules are linked to form a sixteen-membered ring and an extended three-dimensional structure.

  7. Rare-earth metal hydrides supported by silicon-bridged boratabenzene fluorenyl ligands: synthesis, structure and reactivity.

    Science.gov (United States)

    Wang, Chunhong; Xiang, Li; Leng, Xuebing; Chen, Yaofeng

    2017-01-24

    The reactions of rare-earth metal benzyl complexes supported by silicon-bridged boratabenzene fluorenyl ligands with PhSiH3 in toluene gave the corresponding dinuclear hydrides [{μ-[Me2Si(C13H8)(C5H4BNEt2)]}Ln(μ-H)(THF)]2 (3-Ln; Ln = La, Nd, Gd), wherein the rare-earth metal ions are linked by both silicon-bridged boratabenzene fluorenyl ligands and hydrido ligands. The reactivity of these hydrides toward unsaturated substrates was studied. Among these, alkynides [{μ-[Me2Si(C13H8)(C5H4BNEt2)]}Ln(μ-CCPh)]2 (4-Ln; Ln = La, Nd) were obtained via the σ-bond metathesis reaction, when 3-Ln (Ln = La, Nd) was treated with phenylacetylene. While reacting with 3-hexyne, the mono-addition product [{μ-[Me2Si(C13H8)(C5H4BNEt2)]}Ln]2(μ-H)[μ-C(Et)[double bond, length as m-dash]C(H)Et] (5-Ln; Ln = La, Nd) was formed. Further investigations on the reactivity of 3-La displayed that benzonitrile and tert-butyl isonitrile readily inserted into the La-H bonds, affording an azomethine complex [{μ-[Me2Si(C13H8)(C5H4BNEt2)]}La{μ-N[double bond, length as m-dash]C(H)Ph}]2 (6-La) and an N-tert-butylformimidoyl complex [{μ-[Me2Si(C13H8)(C5H4BNEt2)]}La{μ,η(2)-C(H)[double bond, length as m-dash]N(t)Bu}]2 (7-La), respectively. The reaction with N,N'-diisopropylcarbodiimide at room temperature or at 75 °C gave a dimeric complex [{μ-[Me2Si(C13H8)(C5H4BNEt2)]}La]2(μ-H)[μ-N((i)Pr)CHN((i)Pr)] (8-La) or a monomeric complex [Me2Si(C13H8)(C5H4BNEt2)]La[N((i)Pr)CHN((i)Pr)] (9-La), respectively.

  8. Synthesis and characterization of novel double-cation borohydrides

    Energy Technology Data Exchange (ETDEWEB)

    Frommen, Christoph; Aliouane, Nadir; Deledda, Stefano; Fonneloep, Jon Erling; Grove, Hilde; Llamas-Jansa, Isabel; Lieutenant, Klaus; Sartori, Sabrina; Oestby, Heidi; Soerby, Magnus H.; HaubacK, Bjoern C. [Institute for Energy Technology, Kjeller (Norway). Physics Dept.

    2010-07-01

    A systematic screening for the reaction of transition metal chlorides with alkali borohydrides was performed by mechano-chemical synthesis (ball-milling and cryo-milling). The reaction between LiBH{sub 4} and YCl{sub 3} produced yttrium borohydride Y(BH{sub 4}){sub 3} instead of the targeted LiY(BH{sub 4}){sub 4}. When using NaBH{sub 4}, no indication for the formation of crystalline mixed-metal borohydrides was observed for the chlorides of Ni, Ti, Cu, Rh and Cu. Anion substitution was observed instead which lead to a series of novel Na(BH{sub 4}){sub x}Cl{sub 1-X} type compounds, presumably accompanied by the formation of amorphous transition metal borides. Anion substitution in borohydrides may open up the path to synthesize new compounds with improved thermodynamic properties compared to the pure borohydrides. These findings demonstrate that the successful synthesis of mixed-metal borohydrides remains a challenging task. (orig.)

  9. Synthesis and characterization of hydroxyapatite from fish bone waste

    Energy Technology Data Exchange (ETDEWEB)

    Marliana, Ana, E-mail: na-cwith22@yahoo.co.id; Fitriani, Eka; Ramadhan, Fauzan; Suhandono, Steven; Yuliani, Keti; Windarti, Tri [Chemistry Department, Faculty of Science and Mathematics, Diponegoro University, Indonesia, 50 275 (Indonesia)

    2015-12-29

    Waste fish bones is a problem stemming from activities in the field of fisheries and it has not been used optimally. Fish bones contain calcium as natural source that used to synthesize hydroxyapatite (HA). In this research, HA synthesized from waste fish bones as local wisdom in Semarang. The goal are to produce HA with cheaper production costs and to reduce the environmental problems caused by waste bones. The novelty of this study was using of local fish bone as a source of calcium and simple method of synthesis. Synthesis process of HA can be done through a maceration process with firing temperatures of 1000°C or followed by a sol-gel method with firing at 550°C. The results are analyzed using FTIR (Fourier Transform Infrared), XRD (X-Ray Diffraction) and SEM-EDX (Scanning Electron Microscopy-Energy Dispersive X-Ray). FTIR spectra showed absorption of phosphate and OH group belonging to HA as evidenced by the results of XRD. The average grain size by maceration and synthesized results are not significant different, which is about 69 nm. The ratio of Ca/P of HA by maceration result is 0.89, then increase after continued in the sol-gel process to 1.41. Morphology of HA by maceration results are regular and uniform particle growth, while the morphology of HA after the sol-gel process are irregular and agglomerated.

  10. Synthesis and characterization of polyvinylpyrrolidine assisted tantalum pentoxide films

    Energy Technology Data Exchange (ETDEWEB)

    Subramanian, Vaidyanathan; Ndiege, Nicholas; Seebauer, E.G. [Department of Chemical and Biomolecular Engineering, University of Illinois at Urbana-Champaignm, 600 S. Mathews, Urbana, IL-61801 (United States); Shannon, Mark A. [Department of Mechanical Engineering, University of Illinois at Urbana-Champaignm, 600 S. Mathews, Urbana, IL-61801 (United States); Masel, Richard I. [Department of Chemical and Biomolecular Engineering, University of Illinois at Urbana-Champaignm, 600 S. Mathews, Urbana, IL-61801 (United States)], E-mail: r-masel@uiuc.edu

    2008-06-02

    Micron thick tantalum pentoxide (Ta{sub 2}O{sub 5}) films have been proposed as thermal insulating layers in microchemical systems, but so far it has been difficult to deposit thick enough films over complex substrates. So far sol-gel films cracked upon heating whenever the film thicknesses were above 350 nm. A 350 nm thick film is too thin for effective insulation. Other techniques are not suitable for coating the complex structures associated with microchemical systems. In this paper we report sol-gel synthesis of 1.6 {mu}m thick tantalum pentoxide (Ta{sub 2}O{sub 5}) films. The films are almost crack free, and adhere to silicon surfaces even upon flashing to 900 deg. C. The key to the synthesis is the addition of Polyvinylpyrrolidine (PVP) to the sol. Films grown in the absence of PVP all show cracks upon calcination to 900 deg. C while few cracks are seen with PVP. X-ray diffraction and Fourier transform infra red analysis show that orthorhombic Ta{sub 2}O{sub 5} is formed in all cases. X-ray photoelectron spectroscopy shows the O:Ta ratio to be 2.8:1. This shows that sol-gel is a viable process for making the micron thick films of Ta{sub 2}O{sub 5} needed as insulators for microchemical systems.

  11. MCM-41 ordered mesoporous molecular sieves synthesis and characterization

    Directory of Open Access Journals (Sweden)

    Rogério A.A. Melo

    1999-07-01

    Full Text Available The aim of this work was to study the hydrothermal synthesis of Si and SiAlMCM-41 performed under both autogenic pressure and refluxing conditions. XRD data showed that the MCM-41 phase may be formed by both processes and that the synthesized material in the presence of Al and/or under reflux presents the hexagonally arrangement of less ordered mesopores. However, as verified by XRD and physisorption data, the order was improved with higher synthesis times. 29Si and 1H - 29Si C/P MAS NMR spectra showed that a great part of the Si atoms exists as silanol groups which originate resonance peaks at -110, -100 and -91 ppm. The presence of Al atoms may generate Si(3Si, Al and Si(2Si, 2Al environments which might be contributing to resonance peaks at -100 and -91 ppm. The 27Al MAS NMR spectrum of the as synthesized AlSiMCM-41 showed a resonance peak of tetrahedral framework aluminum close to 53 ppm and two others, one close to 14 ppm attributed to Al(H2O6+3 species and the other a weak signal close to 32 ppm attributed to pentacoordinated Al. 27Al MAS NMR spectra of the calcined sample showed a peak at 0 ppm corresponding to an hexacoordinated extra-framework aluminum formed during calcination.

  12. Silver colloid nanoparticles: synthesis, characterization, and their antibacterial activity.

    Science.gov (United States)

    Panacek, Ales; Kvítek, Libor; Prucek, Robert; Kolar, Milan; Vecerova, Renata; Pizúrova, Nadezda; Sharma, Virender K; Nevecna, Tat'jana; Zboril, Radek

    2006-08-24

    A one-step simple synthesis of silver colloid nanoparticles with controllable sizes is presented. In this synthesis, reduction of [Ag(NH(3))(2)](+) complex cation by four saccharides was performed. Four saccharides were used: two monosaccharides (glucose and galactose) and two disaccharides (maltose and lactose). The syntheses performed at various ammonia concentrations (0.005-0.20 mol L(-1)) and pH conditions (11.5-13.0) produced a wide range of particle sizes (25-450 nm) with narrow size distributions, especially at the lowest ammonia concentrations. The average size, size distribution, morphology, and structure of particles were determined by dynamic light scattering (DLS), transmission electron microscopy (TEM), and UV/Visible absorption spectrophotometry. The influence of the saccharide structure (monosacharides versus disaccharides) on the size of silver particles is briefly discussed. The reduction of [Ag(NH(3))(2)](+) by maltose produced silver particles with a narrow size distribution with an average size of 25 nm, which showed high antimicrobial and bactericidal activity against Gram-positive and Gram-negative bacteria, including highly multiresistant strains such as methicillin-resistant Staphylococcus aureus. Antibacterial activity of silver nanoparticles was found to be dependent on the size of silver particles. A very low concentration of silver (as low as 1.69 mug/mL Ag) gave antibacterial performance.

  13. Synthesis and characterization of monoclinic TiO2 nanosheets

    Institute of Scientific and Technical Information of China (English)

    WU Yu; XU Boqing

    2005-01-01

    A novel two-step method for the synthesis of monoclinic titanium oxide (i.e. TiO2(B)) nanosheets is presented in this report. The method is featured by two steps: 1) synthesis of hydrogen titanate nanosheets, followed by 2) calcination of the titanate nanosheets at elevated temperatures. The hydrogen titanate nanosheets were prepared first by autoclaving anatase TiO2 powders, obtained by air calcining an ethanol-gel of Ti(OH)4 at 500℃, in aqueous NaOH (10 mol/L) at 150―200℃, and then by washing with hydrochloric acid under supersonic irradiation. While sizes of the nanosheets were found to increase with increasing the temperature of the hydrothermal treatment, the calcination at 400―500℃ of the hydrogen titanate nanosheets that were synthesized at higher autoclaving temperatures (180―200℃) produced monoclinic TiO2 nanosheets with a uniform morphology. By contrast, the same calcination of the titanate nanosheets synthesized at the autoclaving temperature 180℃ led to anatase TiO2 nanoparticles.

  14. Solid State Synthesis, Characterization and Antimicrobial Study of 4 ...

    African Journals Online (AJOL)

    MBI

    2014-11-10

    Nov 10, 2014 ... Department of Pure and Industrial Chemistry, Bayero University, P. M. B. ... The complexes obtained were characterized by elemental analysis, ... The processes are believed to be ... This paper is concerned with the design.

  15. Synthesis and characterization of polyamidoamine conjugates of neridronic acid

    CSIR Research Space (South Africa)

    Aderibigbe, BA

    2015-10-01

    Full Text Available of water and it was performed at room temperature thereby making the reaction environmentally friendly and economically viable. These conjugates are potential prodrugs and they were characterized by nuclear magnetic resonance spectroscopy (NMR), Fourier...

  16. synthesis, characterization, electrical and catalytic studies of some ...

    African Journals Online (AJOL)

    B. S. Chandravanshi

    Printed in Ethiopia. © 2015 Chemical Society of ... characterized by elemental analysis, IR and electronic spectra, magnetic susceptibility measurements and thermal analyses. ... Schiff bases offer a versatile and flexible series of ligands due to.

  17. Xanthene-bridged cofacial bisporphyrins.

    Science.gov (United States)

    Chang, C J; Deng, Y; Heyduk, A F; Chang, C K; Nocera, D G

    2000-03-06

    The synthesis and characterization of cofacial bisporphyrins juxtaposed by xanthene-bridged pillars are presented. The one-pot preparation of the xanthene dialdehyde avoids the lengthy bridge synthesis accompanying other cofacial porphyrin systems, thus allowing for the facile preparation of homobimetallic zinc (10), copper (11), and nickel (12) complexes. The cofacial orientation of the two porphyrin macrocycles was confirmed by X-ray crystallography. Structural data are provided for bisporphyrins 10-12: 10 (C79H82N8OZn2), triclinic, space group P1, a = 11.2671(2) A, b = 14.9809(2) A, c = 20.4852(2) A, alpha = 101.6680(10) degrees, beta = 100.8890(10) degrees, gamma = 101.8060(10) degrees, Z = 2; 11 (C79H82N8OCu2), triclinic, space group P1, a = 11.21410(10) A, b = 14.9539(5) A, c = 20.6915(7) A, alpha = 101.810(2) degrees, beta = 101.044(2) degrees, gamma = 101.722(2) degrees, Z = 2; 12 (C79H82N8ONi2), monoclinic, space group C2/c, a = 24.1671(4) A, b = 10.669 A, c = 50.5080(9) A, beta = 99.553(2) degrees, Z = 8. Exciton interactions between the porphyrin rings are apparent in electronic spectra, consistent with the cofacial superstructure. The combination of structural and spectroscopic data provides a basis for the design of additional metal derivatives for the activation of dioxygen and other small molecules.

  18. H-bonding template-directed synthesis of a complete m-PDA-bridged ladder polyhydrosiloxane (OLPHS)

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    A highly ordered m-phenylenediimino-bridged ladder polyhydrosiloxane (abbr. OLPHS) with Mn = 1.24 × 104 was synthesized stoichiometric hydrolysis and dehydrochlorination condensation reaction between Si-Cl and Si-OH bonds. The complete ladder structure of OLPHS has been confirmed by the following three data. Two characteristic Bragg's peaks representing the ladder width (w = 0.94 nm) and ladder thickness (t = 0.42 nm) were observed in XRD analysis, which are consistent with those calculated by molecular simulation. The very sharp absorption with a small half-peak width (w1/2 = 0.5 ppm) for [(-HN)HSiO2/2]n moiety of OLPHS in 29Si NMR spectrum indicated presence of the complete ladder structure. As collateral evidence, a higher glass transition temperature (Tg = 105 ℃) is also recorded in the DSC measurement, implying the high stiffness of ladder chain of OLPHS.(C) 2007 Rong Ben Zhang. Published by Elsevier B.V. on behalf of Chinese Chemical Society. All rights reserved.

  19. Carboxylate-bridged Cu(II) coordination polymeric complex: synthesis, crystal structure, magnetic properties, DNA binding and electrochemical studies

    Indian Academy of Sciences (India)

    SABITHAKALA THATITURI; BHARGAVI GOVINDUGARI; VENKATA RAMANA REDDY CHITTIREDDY

    2017-08-01

    A novel water-soluble carboxylate-bridged copper(II) coordination polymer,Cu-BIG was formed by the reaction of Cu(ClO₄)₂ ·6H₂O and tridentate benzimidazole-glycine conjugate ligand, 2-((1H-benzimidazol- 2-yl)methylamino) acetic acid, BIGH and its structure has been determined by IR, UV, powder XRD, VSM, CV, TGA, DTA, EPR and single crystal X-ray diffraction. Crystallographic studies indicate it to be a coordination polymer with P¯ı Space group. The asymmetric unit of complex contains two Cu(II) ions with elongated square pyramid geometry.The axial positions of theCu(II) atoms are occupied by the carbonyl oxygen of the carboxylate group with the bond distances Cu(1)–O(5)axial , 2.28Å, and Cu(2)–O(2)axial , 2.26Å. The two Cu(II) are connected through the carboxylic group present in BIGH, which provides electron mobilisation in the molecule and hence results in the soft ferromagnetic polymer. An in vitro antibacterial activity study of BIGH and Cu-BIG showed moderate activity against Bacillus subtilis. The DNA binding studies showed the interaction of Cu-BIG with CT-DNA.

  20. High Efficiency Synthesis of Isotactic Polypropylene and Linear Polyethylene Using a New C2-symmetric Carbon-bridged Zirconocene Catalyst

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    Ansa-Cyclohexyl-bis(4,5,6,7-tertrahydro-1-indenyl) zirconium dichloride (5) was used as catalyst for propylene and ethylene polymerization together with methyl aluminoxane (MAO) as the cocatalyst.Isotactic polypropylene (PP) was obtained with the highest activity of 6.37×107g PP (molZr)-1h-1. The mesomeso (mmmmm) pentads sequence content of PP was determined by 13C NMR spectroscopy. The dependence of the microstructure on the reaction temperature and the Al/Zr molar ratio was examined and the catalytic activity of complex 5 was compared with that of the similar ansa-zirconocene 3. The high activity of the new zirconocene 5 for propylene isospectic polymerization at high temperature (60 ℃) is the result of its unique bridged-group structure. Complex 5/MAO displays also high catalytic activity of 0.46×106 to 9.87×106gPE(molZr)-1h-1 in the homo-polymerization of ethylene. The visometric molecular weight of PE ranges from linear polyethylene (LPE).

  1. Synthesis and characterizations of novel magnetic and plasmonic nanoparticles

    Science.gov (United States)

    Dahal, Naween

    This dissertation reports the colloidal synthesis of iron silicide, hafnium oxide core-gold shell and water soluble iron-gold alloy for the first time. As the first part of the experimentation, plasmonic and superparamagnetic nanoparticles of gold and iron are synthesized in the form of core-shell and alloy. The purpose of making these nanoparticles is that the core-shell and alloy nanoparticles exhibit enhanced properties and new functionality due to close proximity of two functionally different components. The synthesis of core-shell and alloy nanoparticles is of special interest for possible application towards magnetic hyperthermia, catalysis and drug delivery. The iron-gold core-shell nanoparticles prepared in the reverse micelles reflux in high boiling point solvent (diphenyl ether) in presence of oleic acid and oleyl amine results in the formation of monodisperse core-shell nanoparticles. The second part of the experimentation includes the preparation of water soluble iron-gold alloy nanoparticles. The alloy nanoparticles are prepared for the first time at relatively low temperature (110 °C). The use of hydrophilic ligand 3-mercapto-1-propane sulphonic acid ensures the aqueous solubility of the alloy nanoparticles. Next, hafnium oxide core-gold shell nanoparticles are prepared for the first time using high temperature reduction method. These nanoparticles are potentially important as a high kappa material in semiconductor industry. Fourth, a new type of material called iron silicide is prepared in solution phase. The material has been prepared before but not in a colloidal solution. The Fe3Si obtained is superparamagnetic. Another phase beta-FeSi 2 is a low band gap (0.85 eV) semiconductor and is sustainable and environmentally friendly. At last, the iron monosilicide (FeSi) and beta-FeSi2 are also prepared by heating iron-gold core-shell and alloy nanoparticles on silicon (111) substrate. The nucleation of gaseous silicon precursor on the melted

  2. Synthesis and characterization of a nanocrystalline diamond aerogel.

    Science.gov (United States)

    Pauzauskie, Peter J; Crowhurst, Jonathan C; Worsley, Marcus A; Laurence, Ted A; Kilcoyne, A L David; Wang, Yinmin; Willey, Trevor M; Visbeck, Kenneth S; Fakra, Sirine C; Evans, William J; Zaug, Joseph M; Satcher, Joe H

    2011-05-24

    Aerogel materials have myriad scientific and technological applications due to their large intrinsic surface areas and ultralow densities. However, creating a nanodiamond aerogel matrix has remained an outstanding and intriguing challenge. Here we report the high-pressure, high-temperature synthesis of a diamond aerogel from an amorphous carbon aerogel precursor using a laser-heated diamond anvil cell. Neon is used as a chemically inert, near-hydrostatic pressure medium that prevents collapse of the aerogel under pressure by conformally filling the aerogel's void volume. Electron and X-ray spectromicroscopy confirm the aerogel morphology and composition of the nanodiamond matrix. Time-resolved photoluminescence measurements of recovered material reveal the formation of both nitrogen- and silicon- vacancy point-defects, suggesting a broad range of applications for this nanocrystalline diamond aerogel.

  3. Synthesis and characterization of vanadiumoxidecatalysts supported on copper orthophosphates

    Science.gov (United States)

    Ouchabi, M.; Baalala, M.; Elaissi, A.; Loulidi, I.; Bensitel, M.

    2017-03-01

    Synthesis of a pure copper orthophosphate (CuP) prepared by Coprecipitation, and CuP modified by impregnation of vanadium (2-12 wt % of V2O5) have been carried out. The solids obtained were investigated as synthesized or after calcination by various physico-chemical techniques such as X-Ray Diffraction (XRD), Infrared Spectroscopy (IR), Thermogravimetric analysis (TGA), and differential thermal analysis (DTA). The results revealed that the solids V/CuP consisted of copper orthophosphate Cu3(PO4)2 as major phases, together with V2O5 as minor phase. The diffraction lines of V2O5 increase by increasing the vanadium content.

  4. Cobalt-based Magnetic Nanoparticles: Design, Synthesis and Characterization

    Science.gov (United States)

    Zamanpour, Mehdi

    The ever-increasing desire for more energy attainable from a smaller volume of matter has driven researchers to explore advanced materials at the molecular or even atomic size scale. Magnetic materials at the nanometer size scale have been the subject of enormous research effort worldwide for more than half a century. Different magnetic nanoparticles have shown different behavior in the absence and presence of an external magnetic field, which has led them to be categorized as soft (easy to demagnetize) or hard (resistive against demagnetization) magnets. Applications range from medical and biomedical devices to magnetic recording media and magnetic sensing have emphasized the importance of this class of materials. Soft magnetic phases have found application in power generation and magnetic targeted drug delivery, while hard magnets have been subject of extensive research for application as energy storage media. Discovery of the exchange-coupling phenomenon between the spins of two adjacent hard and soft magnetic phases which means taking advantage of both high magnetic moment of the soft phase as well as high coercivity of the hard phase has attracted scientists to develop advanced materials for energy storage with no usage of fossil fuels: clean energy. In this Dissertation, synthesis of pure phase, soft FeCo nanoparticles with high magnetic moment and hard phase CoxC nanoparticles possessing high coercivity is reported. The polyol method (chemical co-precipitating at polyhydric alcohol as reducing agent) is used to make FeCo and Co xC nanoparticles and the effects of important reaction kinetics parameters on the structure and magnetic properties of the products are studied. Careful analysis of correlations between these parameters and the properties of the magnetic particles has made synthesis of FeCo and CoxC nanoparticles with desired properties possible. Fabrication of MnAlC-FeCo heterostructures as a rare earth-free alternative for high-performance permanent

  5. Synthesis and characterization of a nanocrystalline diamond aerogel

    Energy Technology Data Exchange (ETDEWEB)

    Pauzauskie, Peter J.; Crowhurst, Jonathan C.; Worsley, Marcus A.; Laurence, Ted A.; Kilcoyne, A. L. David; Wang, Yinmin; Willey, Trevor M.; Visbeck, Kenneth S.; Fakra, Sirine C.; Evans, William J.; Zaug, Joseph M.; Satcher, Jr., Joe H.

    2011-07-06

    Aerogel materials have myriad scientific and technological applications due to their large intrinsic surface areas and ultralow densities. However, creating a nanodiamond aerogel matrix has remained an outstanding and intriguing challenge. Here we report the high-pressure, high-temperature synthesis of a diamond aerogel from an amorphous carbon aerogel precursor using a laser-heated diamond anvil cell. Neon is used as a chemically inert, near-hydrostatic pressure medium that prevents collapse of the aerogel under pressure by conformally filling the aerogel's void volume. Electron and X-ray spectromicroscopy confirm the aerogel morphology and composition of the nanodiamond matrix. Time-resolved photoluminescence measurements of recovered material reveal the formation of both nitrogen- and silicon- vacancy point-defects, suggesting a broad range of applications for this nanocrystalline diamond aerogel.

  6. Green Synthesis, Characterization and Uses of Palladium/Platinum Nanoparticles

    Science.gov (United States)

    Siddiqi, Khwaja Salahuddin; Husen, Azamal

    2016-11-01

    Biogenic synthesis of palladium (Pd) and platinum (Pt) nanoparticles from plants and microbes has captured the attention of many researchers because it is economical, sustainable and eco-friendly. Plant and their parts are known to have various kinds of primary and secondary metabolites which reduce the metal salts to metal nanoparticles. Shape, size and stability of Pd and Pt nanoparticles are influenced by pH, temperature, incubation time and concentrations of plant extract and that of the metal salt. Pd and Pt nanoparticles are broadly used as catalyst, as drug, drug carrier and in cancer treatment. They have shown size- and shape-dependent specific and selective therapeutic properties. In this review, we have discussed the biogenic fabrication of Pd/Pt nanoparticles, their potential application as catalyst, medicine, biosensor, medical diagnostic and pharmaceuticals.

  7. Synthesis and characterization of nano silver ferrite composite

    Science.gov (United States)

    Murthy, Y. L. N.; Kondala Rao, T.; Kasi viswanath, I. V.; Singh, Rajendra

    2010-07-01

    We report the synthesis of nano sized silver ferrite composite having the empirical formula AgFeO 2 by a co-precipitation method. The resulting powders are thin platelets, transparent and a rich ruby red in color in transmission. The X-ray diffraction (XRD) powder data consisted of only nine reflections, and the analysis showed the unit cell to be rhombohedral. The powders showed extensive XRD line broadening and the sizes of the crystals are calculated to be in the range 4-36.5 nm. The morphology of the silver ferrite composite studied using scanning electron microscope showed nano sized particles. The particle size is found to increase with increase in annealing temperature. The magnetic behavior, measured using a vibrating sample magnetometer, indicated a change from paramagnetic to ferromagnetic with increase in particle size.

  8. Synthesis and characterization of silver molybdate nanowires, nanorods and multipods

    Indian Academy of Sciences (India)

    G Nagaraju; G T Chandrappa; Jacques Livage

    2008-06-01

    Silver molybdate nanowires, nanorods and multipods like structures have been prepared by an organic free hydrothermal process using ammonium molybdate and silver nitrate solutions. The powder X-ray diffraction (PXRD) patterns reveal that the silver molybdate belongs to anorthic structure. The thickness, 200–500 nm, for silver molybdate nanorods/wires and 2–5 m for microrods are identified from SEM images. UV-visible spectrum of silver molybdate nanorods/nanowires shows maximum absorbance at 408 nm. Photoluminescence (PL) spectrum exhibits UV emission at 335 nm, violet emission at 408 nm and a weak green emission at 540 nm. The influence of hydrothermal synthesis conditions on silver molybdate nanowires, nanorods and multipods compositions were established.

  9. Synthesis and characterization of mixed melilite-type oxides

    Science.gov (United States)

    Granata, V.; Ubaldini, A.; Fittipaldi, R.; Rocco, L.; Pace, S.; Vecchione, A.

    2017-01-01

    The melilite-type oxides are potential targets for exploring interesting magnetic and electronic properties as well as multiferroicity and magnetoelectric effects. Polycrystalline samples of Ba2Cu1-xMnxGe2O7 have been synthesized by solid state reaction method. The morphology and chemical composition of the samples have been investigated by scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS). By using powder X-ray diffraction, the phase composition of the synthesized compounds and the evolution of their crystallographic axes as a function of the doping have been systematically studied. The synthesis of the polycrystalline compounds reported in this work is a prerequisite for the growth of high quality single crystals of mixed melilite-type oxides essential for the investigations of the complex magnetic phase diagram of these non-centrosymmetric systems.

  10. Chemical Synthesis and Electrochemical Characterization of Nanoporous Gold films

    DEFF Research Database (Denmark)

    Christiansen, Mikkel U-B; Seselj, Nedjeljko; Engelbrekt, Christian

    Nanoporous gold (NPG) is conventionally made via dealloying methods1. We present an alternative method for bottom-up chemical synthesis of nanoporous gold film (cNPGF), with properties resembling those of dealloyed NPG. The developed procedure is simple and only benign chemicals are used....... Chloroauric acid is reduced to nanoparticles (NPs) by 2-(N-morpholino)ethanesulfonate, acting also as a protecting agent for the NPs and as a pH buffer, while potassium chloride is used to control ionic strength. The film formation is controlled by parameters such as temperature, ionic strength...... and protonation of the buffer. Therefore, it is possible to influence the trapping of nanoparticles at the air-liquid interface, yielding porous thin film structures, Figure 1A. The produced cNPGFs have been investigated by atomic force microscopy (AFM), transmission electron microscopy (TEM) and cyclic...

  11. Synthesis, Characterization and properties studies of new magnetic materials

    Science.gov (United States)

    Messai, Amel; Luneau, Dominique

    2015-10-01

    We are interested in molecular polymetallic species having high spin and nuclearities in relation to the field of so call single-molecule magnets (SMMs). The goal is to find a way to synthesis metal clusters which may have application in magnetism and nanosciences. With this purpose, we decided to investigate the coordination chemistry of the Schiff base.Along this way we were able to create cubane-like complexes and elaborate new Single Molecule-Magnets. The idea was to use Schiff base ligands and different metals to generate high nuclear complexes. Complexation of Shiff base with copper has been investigated. Tetranuclear complex with a cubane like core have been synthesised with (Sciff base), with the same base and cobalt we obtains an other single magnetic complex completely different.

  12. Synthesis and Characterization of New Heterocyclic Liquid Crystals

    Directory of Open Access Journals (Sweden)

    D. Srividhya

    2009-01-01

    Full Text Available This investigation enumerates the synthesis and mesomorphic properties of 1,2,3-triazole containing azobenzene liquid crystals. In these liquid crystals the methylene chain length at non polar end was varied from six to ten carbons to investigate the association properties of non polar chain on the melt. The compound was designed to have a polar ether chain at the other side of the molecule adjacent to the triazole ring and synthesized to enhance the dipolar interactions. These alterations in chemical structure produce two series of new liquid crystalline compounds with each series containing five variations in the methylene chain. The structure of the target compounds and the intermediates were confirmed by the 1H NMR, 13C NMR and IR spectral techniques. Polarized microscopic studies revealed that all the compounds in the series exhibited enantiotropic liquid crystalline properties. This was further confirmed using differential scanning calorimetric experiments. The energy minimized structure supports the mesogenic behavior of the structure.

  13. Synthesis and characterization of zeolites prepared from industrial fly ash

    OpenAIRE

    Franus, Wojciech; Wdowin, Magdalena; Franus, Małgorzata

    2014-01-01

    In this paper, we present the possibility of using fly ash to produce synthetic zeolites. The synthesis class F fly ash from the Stalowa Wola SA heat and power plant was subjected to 24 h hydrothermal reaction with sodium hydroxide. Depending on the reaction conditions, three types of synthetic zeolites were formed: Na-X (20 g fly ash, 0.5 dm3 of 3 mol · dm−3 NaOH, 75 °C), Na-P1 (20 g fly ash, 0.5 dm3 of 3 mol · dm−3 NaOH, 95 °C), and sodalite (20 g fly ash, 0.8 dm3 of 5 mol · dm−3 NaOH + 0.4...

  14. Synthesis and characterization of a new high entropy composite matrix

    Science.gov (United States)

    Popescu, G.; Matara, M. A.; Csaki, I.; Popescu, C. A.; Truşcă, R.

    2016-06-01

    Even if high entropy alloys were not reported in a scientific journal till 2003, these new alloys have been investigated since 1995 due to their high temperature properties. In the last years the synthesis of these alloys has been widely investigated. Thus, the present work has been carried out to produce a high entropy composite using an equiatomic AlCrFeMnNi high entropy alloy (HEA) matrix and graphite particles (Gr) as reinforcing material. The high entropy composite was obtained by powder metallurgy route using a planetary ball mill. The mechanically alloyed mixture was investigated by scanning electron microscopy (SEM). Microstructural investigation realized by SEM revealed the homogenous structure of the composite, with multiple phases and decreasing particles size, mostly reaching nanometric scale.

  15. Synthesis and characterization of Gd-doped magnetite nanoparticles

    Science.gov (United States)

    Zhang, Honghu; Malik, Vikash; Mallapragada, Surya; Akinc, Mufit

    2017-02-01

    Synthesis of magnetite nanoparticles has attracted increasing interest due to their importance in biomedical and technological applications. Tunable magnetic properties of magnetite nanoparticles to meet specific requirements will greatly expand the spectrum of applications. Tremendous efforts have been devoted to studying and controlling the size, shape and magnetic properties of magnetite nanoparticles. Here we investigate gadolinium (Gd) doping to influence the growth process as well as magnetic properties of magnetite nanocrystals via a simple co-precipitation method under mild conditions in aqueous media. Gd doping was found to affect the growth process leading to synthesis of controllable particle sizes under the conditions tested (0-10 at% Gd3+). Typically, undoped and 5 at% Gd-doped magnetite nanoparticles were found to have crystal sizes of about 18 and 44 nm, respectively, supported by X-ray diffraction and transmission electron microscopy. Our results showed that Gd-doped nanoparticles retained the magnetite crystal structure, with Gd3+ randomly incorporated in the crystal lattice, probably in the octahedral sites. The composition of 5 at% Gd-doped magnetite was Fe(3-x)GdxO4 (x=0.085±0.002), as determined by inductively coupled plasma mass spectrometry. 5 at% Gd-doped nanoparticles exhibited ferrimagnetic properties with small coercivity ( 65 Oe) and slightly decreased magnetization at 260 K in contrast to the undoped, superparamagnetic magnetite nanoparticles. Templation by the bacterial biomineralization protein Mms6 did not appear to affect the growth of the Gd-doped magnetite particles synthesized by this method.

  16. Synthesis and Characterization of Photosensitive Polyimides for Optical Applications

    Science.gov (United States)

    Kim, Kye-Hyun

    1995-11-01

    The objective of this research was to prepare photosensitive polyimides for optical applications. The work was begun with the synthesis of a series of poly(amic esters) containing cinnamyl groups. However, these systems required high imidization temperatures where they darkened considerably. Two new photosensitive end-capping agents, i.e., 6-(4-aminophenoxy)hexyl methacrylate, and di(2-(methacryloyloxy)ethyl) 5-aminoisophthalate, for polyimides were also prepared. These agents were used along with 2,2^' -bis(3,4-dicarboxyphenyl)hexafluoropropane dianhydride (6FDA) and 2,2^'-bis(trifluoromethyl) -4,4^' -diaminobiphenyl (PFMB) to prepare a series of methacrylate end-capped imide oligomers. However, the oligomers required long exposures to UV-radiation to affect cure. To improve their photosensitivity, multifunctional additives and photoinitiators were used. A difunctional end-capped oligomer that contained trimethylolpropane triacrylate (TMPTA) and trimethylbenzoyldiphenyl phosphine oxide (TMDPO) was highly photosensitive and displayed good photo-patterning properties. The third approach involved the synthesis of a diamine monomer in which methacrylate moieties were attached to the 2- and 2^ '-positions of biphenyl structures. The monomer, i.e., 2,2^'-dimethacryloyloxy -4,4^'-diaminobiphenyl (DMB), was polymerized with commercially available dianhydrides such as 6FDA and 4,4^' -oxydiphthalic anhydride (ODPA). The polyimides obtained were optically transparent and soluble in common organic solvents such as acetone and chloroform. The polymers were highly photosensitive and displayed good photo-patterning properties. The polymers, which afforded high-resolution patterns, did not develop color or shrink during UV-exposure and thermal curing.

  17. Stop Flow Lithography Synthesis and Characterization of Structured Microparticles

    Directory of Open Access Journals (Sweden)

    David Baah

    2014-01-01

    Full Text Available In this study, the synthesis of nonspherical composite particles of poly(ethylene glycol diacrylate (PEG-DA/SiO2 and PEG-DA/Al2O3 with single or multiple vias and the corresponding inorganic particles of SiO2 and Al2O3 synthesized using the Stop Flow Lithography (SFL method is reported. Precursor suspensions of PEG-DA, 2-hydroxy-2-methylpropiophenone, and SiO2 or Al2O3 nanoparticles were prepared. The precursor suspension flows through a microfluidic device mounted on an upright microscope and is polymerized in an automated process. A patterned photomask with transparent geometric features masks UV light to synthesize the particles. Composite particles with vias were synthesized and corresponding inorganic SiO2 and Al2O3 particles were obtained through polymer burn-off and sintering of the composites. The synthesis of porous inorganic particles of SiO2 and Al2O3 with vias and overall dimensions in the range of ~35–90 µm was achieved. BET specific surface area measurements for single via inorganic particles were 56–69 m2/g for SiO2 particles and 73–81 m2/g for Al2O3 particles. Surface areas as high as 114 m2/g were measured for multivia cubic SiO2 particles. The findings suggest that, with optimization, the particles should have applications in areas where high surface area is important such as catalysis and sieving.

  18. Synthesis and structural characterization of manganese olivine lithium phosphate

    Energy Technology Data Exchange (ETDEWEB)

    Herrera Robles, Joel O. [Basic Science Department, IIT, Universidad Autónoma de Ciudad Juárez, Av. del Charro 460 norte Cd. Juárez, Chih. C.P. 32310 (Mexico); Fuentes Cobas, Luis E. [Centro de Investigación en Materiales Avanzados CIMAV, Complejo Industrial, M. Cervantes 120, Chihuahua C.P. 31109 (Mexico); Díaz de la Torre, Sebastián [Instituto Politécnico Nacional, Centro de Investigación e Innovación Tecnológica CIITEC, Azcapotzalco, México, D.F. C.P. 02250 (Mexico); Camacho Montes, Héctor, E-mail: hcamacho@uacj.mx [Basic Science Department, IIT, Universidad Autónoma de Ciudad Juárez, Av. del Charro 460 norte Cd. Juárez, Chih. C.P. 32310 (Mexico); Elizalde Galindo, José T.; García Casillas, Perla E.; Rodríguez González, Claudia A. [Basic Science Department, IIT, Universidad Autónoma de Ciudad Juárez, Av. del Charro 460 norte Cd. Juárez, Chih. C.P. 32310 (Mexico); Álvarez Contreras, Lorena [Centro de Investigación en Materiales Avanzados CIMAV, Complejo Industrial, M. Cervantes 120, Chihuahua C.P. 31109 (Mexico)

    2015-09-15

    Highlights: • LiMnPO{sub 4} was obtained by sol gel method and crystallization in reducing atmosphere. • Magnetic and electric properties are reported for LiMnPO{sub 4}. • Electrochemical properties are also found and enhanced by adding carbon. • SEM and HRTEM show the submicron powder nature. • The multifunctional behavior of LiMnPO{sub 4} is experimentally demonstrated. - Abstract: The manganese olivine lithium phosphate is a multifunctional material. If carbon is added to form a composite LiMnPO{sub 4}–C, electrochemical properties can be enhanced, making this material a good candidate for battery cathode. High magnetic susceptibility is reported for this compound at room temperature. In this work, the magnetic response was measured through a Field Cooling/Zero Field Cooling technique at temperature below 100 K. Weak ferroelectric properties at room temperature were measured. Even though, the promising applications and the interesting properties of this system, the attention received in the literature is relatively low. The synthesis of this material is difficult because of the rapid manganese oxidation and the need of a reducing atmosphere. In fact, only few authors report the synthesis of the pure phase. In the present work, nanostructured LiMnPO{sub 4} is obtained by sol gel chemical method and according to X-ray diffraction patterns, pure LiMnPO{sub 4} is obtained after calcination in a reducing atmosphere (10% H{sub 2} – 90% Ar). Nanostructured LiMnPO{sub 4} is a material with very interesting properties that deserves attentions.

  19. Synthesis, characterization and photochemistry of a new heptamolybdate supported magnesium-aqua coordination complex

    Indian Academy of Sciences (India)

    Savita S Khandolkar; Pallepogu Raghavaiah; Bikshandarkoil R Srinivasan

    2015-09-01

    The synthesis, crystal structure, redox characteristics and photochemistry of a new heptamolyb-date supported magnesium-aqua coordination complex viz. (hmtH)2 [{Mg(H2O)5}2 {Mo7O24}]·3H2O 1 (hmt = hexamethylenetetramine) is reported. The cyclic voltammogram reveals quasireversible redox behaviour while the degradation of rhodamine B (RhB) by 1 under sunlight irradiation indicates its photocatalytic activity. In the crystal structure of 1, two [Mg(H2O)5]2+ units are linked by a 2-bridging bidentate hepta-molybdate ligand resulting in a heptamolybdate supported magnesium-aqua coordinated dianionic complex [{Mg(H2O)5}2 {Mo7O24}]2− charge balanced by two (hmtH)+ cations. The cations, anions and the lattice water molecules are linked by several hydrogen bonding interactions.

  20. Synthesis, Characterization and Magnetic Studies of μ-Oxamido Copper(Ⅱ) -Chromium (Ⅲ) Heterodinuclear Complexes

    Institute of Scientific and Technical Information of China (English)

    李延团; 胡春霞; 焉翠蔚; 廖代正

    2001-01-01

    Three new μ-oxamido-bridged heterodinuclear copper (Ⅱ)-chromium(Ⅲ) complexes formulated[Cu(Me2 oxpn)Cr(L)2](NO3)3, where Me2 oxpn denotes N, N'-bis(3-amino-2,2-dimethylpropyl)oxamido dianion and L represents 5-methy1, 10-phenanthroline(Mephen), 4, 7-diphenl-1, 10-phenanthroline (Ph2phen) or 2,2'-bipyridine(bpy), have ben synthesized and characterized by elemental analyses,IR and electronic spectral studies, magnetic moments of room-temperature and molar conductivity measurements.It is proposed that these complexes have oxamido-bridged structures consisting of planar copper(Ⅱ) and octahedral chromium(Ⅲ) ions. The variable temperature magnetic susceptibilities (4.2-300 K)of complexes [Cu(Me2 oxpn)Cr(Ph2phen)2](NO3)3 (1) and [Cu(Me2 ocpn)Cr(Mephen)2] (NO3)3 (2) were further measured and studied, demonstrating the ferromagnetic interaction between the adjacent chromium(Ⅲ)and copper(Ⅱ)ions through the oxamido-bridge in both camplexes 1 and 2.Based on the spin Hamiltonian, H= -2JS1.S2, the exclange integrals J were evaluated as +21.5 cm-1 for 1 and +22.8 cm-1 for 2.

  1. Synthesis and bioactivity of a side chain bridged paclitaxel: A test of the T-Taxol conformation.

    Science.gov (United States)

    Hodge, Mathis; Chen, Qiao-Hong; Bane, Susan; Sharma, Shubhada; Loew, Maura; Banerjee, Abhijit; Alcaraz, Ana A; Snyder, James P; Kingston, David G I

    2009-05-15

    A knowledge of the bioactive tubulin-binding conformation of paclitaxel (Taxol()) is crucial to a full understanding of the bioactivity of this important anticancer drug, and potentially also to the design of simplified analogs. The bioactive conformation has been shown to be best approximated by the T-Taxol conformation. As a further test of this conclusion, the paclitaxel analog 4 was designed as a compound which has all the chemical functionality necessary for activity, but which cannot adopt the T-Taxol conformation. The synthesis and bioassay of 4 confirmed its lack of activity, and thus provided further support for the T-Taxol conformation as the bioactive tubulin-binding conformation.

  2. Bridging the data gaps in the epidemiology of hepatitis C virus infection in Malaysia using multi-parameter evidence synthesis.

    Science.gov (United States)

    McDonald, Scott A; Mohamed, Rosmawati; Dahlui, Maznah; Naning, Herlianna; Kamarulzaman, Adeeba

    2014-11-07

    Collecting adequate information on key epidemiological indicators is a prerequisite to informing a public health response to reduce the impact of hepatitis C virus (HCV) infection in Malaysia. Our goal was to overcome the acute data shortage typical of low/middle income countries using statistical modelling to estimate the national HCV prevalence and the distribution over transmission pathways as of the end of 2009. Multi-parameter evidence synthesis methods were applied to combine all available relevant data sources - both direct and indirect - that inform the epidemiological parameters of interest. An estimated 454,000 (95% credible interval [CrI]: 392,000 to 535,000) HCV antibody-positive individuals were living in Malaysia in 2009; this represents 2.5% (95% CrI: 2.2-3.0%) of the population aged 15-64 years. Among males of Malay ethnicity, for 77% (95% CrI: 69-85%) the route of probable transmission was active or a previous history of injecting drugs. The corresponding proportions were smaller for male Chinese and Indian/other ethnic groups (40% and 71%, respectively). The estimated prevalence in females of all ethnicities was 1% (95% CrI: 0.6 to 1.4%); 92% (95% CrI: 88 to 95%) of infections were attributable to non-drug injecting routes of transmission. The prevalent number of persons living with HCV infection in Malaysia is estimated to be very high. Low/middle income countries often lack a comprehensive evidence base; however, evidence synthesis methods can assist in filling the data gaps required for the development of effective policy to address the future public health and economic burden due to HCV.

  3. Synthesis, characterization and photophysical properties of ESIPT reactive triazine derivatives

    Energy Technology Data Exchange (ETDEWEB)

    Kuplich, Marcelo D.; Grasel, Fabio S.; Campo, Leandra F.; Rodembusch, Fabiano S.; Stefani, Valter, E-mail: vstefani@iq.ufrgs.br [Laboratorio de Novos Materiais Organicos. Instituto de Quimica. Universidade Federal do Rio Grande do Sul, Porto Alegre, RS (Brazil)

    2012-07-01

    Four new reactive fluorescent triazine derivatives were obtained from nucleophilic aromatic substitution of cyanuric chloride. The compounds were characterized by infrared spectroscopy (IR), nuclear magnetic resonance ({sup 13}C and {sup 1}H NMR) and high resolution mass spectrometry (HRMS MALDI). UV-Vis and steady-state fluorescence (in solution and in solid state) spectroscopies were also applied to characterize the photophysical behavior. The dyes are fluorescent by an intramolecular proton transfer mechanism (ESIPT) in the blue-orange region, with a large Stokes shift between 6365-10290 cm-1. The fluorescent cyanuric derivatives could successfully react with cellulose fibers to give new fluorescent cellulosic materials. (author)

  4. Synthesis and characterization of dihexyldithiocarbamate as a chelating agent in extraction of gold(III)

    Science.gov (United States)

    Fatimah, Soja Siti; Bahti, Husein H.; Hastiawan, Iwan; Permanasari, Anna

    2016-02-01

    The use of dialkyldithiocarbamates as chelating agents of transition metals have been developing for decades. Many chelating agents have been synthesized and used in the extraction of the metals. Studies on particular aspects of extraction of the metals, such as the effect of increasing hydrophobicity of chelating agents on the effectiveness of the extraction, have been done. However, despite the many studies on the synthesis and applications of this type of chelating agents, interests in the aspect of molecular structure of the synthesized ligands and of their complexes, have been limited. This study aimed at synthesizing and characterizing dihexylthiocarbamate, and using the ligand for the extraction of gold III). Characterization of the ligand and of its metal complex were done by using elemental analysis, DTG, and spectroscopic methods to include NMR, (1H, and 13C), FTIR, and MS-ESI. Data on the synthesis, characterization, and the application of the ligand as a chelating agent are presented.

  5. Synthesis and characterization of dihexyldithiocarbamate as a chelating agent in extraction of gold(III)

    Energy Technology Data Exchange (ETDEWEB)

    Fatimah, Soja Siti, E-mail: soja-sf@upi.edu [Departemen Pendidikan Kimia, Universitas Pendidikan Indonesia, Jl. Dr. Setiabudhi No. 229, Bandung 40154 (Indonesia); Department of Chemistry, Faculty of Mathematics and Natural Sciences, Padjadjaran University, Jl. Raya Bandung-Sumedang, Km. 21, Jatinangor (Indonesia); Bahti, Husein H.; Hastiawan, Iwan [Department of Chemistry, Faculty of Mathematics and Natural Sciences, Padjadjaran University, Jl. Raya Bandung-Sumedang, Km. 21, Jatinangor (Indonesia); Permanasari, Anna [Departemen Pendidikan Kimia, Universitas Pendidikan Indonesia, Jl. Dr. Setiabudhi No. 229, Bandung 40154 (Indonesia)

    2016-02-08

    The use of dialkyldithiocarbamates as chelating agents of transition metals have been developing for decades. Many chelating agents have been synthesized and used in the extraction of the metals. Studies on particular aspects of extraction of the metals, such as the effect of increasing hydrophobicity of chelating agents on the effectiveness of the extraction, have been done. However, despite the many studies on the synthesis and applications of this type of chelating agents, interests in the aspect of molecular structure of the synthesized ligands and of their complexes, have been limited. This study aimed at synthesizing and characterizing dihexylthiocarbamate, and using the ligand for the extraction of gold III). Characterization of the ligand and of its metal complex were done by using elemental analysis, DTG, and spectroscopic methods to include NMR, ({sup 1}H, and {sup 13}C), FTIR, and MS-ESI. Data on the synthesis, characterization, and the application of the ligand as a chelating agent are presented.

  6. SYNTHESIS AND CHARACTERIZATION OF A DERIVATIVE CYCLOHEXANONE CHALCONE-TYPE, AS AN INTEGRAL LABORATORY EXPERIENCE

    Directory of Open Access Journals (Sweden)

    Perla E. Hernández-González

    2015-03-01

    Full Text Available At present, chemistry teachers are searching new models that allow integrative laboratory experiences, converging interdisciplinary knowledge of the Chemistry field. With this framework of ideas, this work describes the synthesis and characterization of the (2E,6E-2,6-bis(4-methoxybenzylidenecyclohexanone compound as axis of knowledge in order to encourage the students to develop their cognitive skills, such as critical thinking and problem solving, and also interpretation and analysis of results. The compound was synthesized by a Claisen-Schmidt condensation reaction, involving an aromatic aldehyde and cyclohexanone. The compound was characterized spectroscopically by NMR, IR and UV-Vis. Melting point and solubility tests were also performed. The chemical structure was confirmed by single crystal X-Ray diffraction. In conclusion, this laboratory experience allows students to get involved with the techniques and procedures commonly used in the organic chemistry laboratory to the synthesis and characterization of organic compounds.

  7. Synthesis and characterization of manganese-glycine and copper-glycine adducts

    Directory of Open Access Journals (Sweden)

    Robson Fernandes de Farias

    2002-09-01

    Full Text Available This work reports the synthesis and characterization of adducts of general formula MCl2.ngly, where M= Mn and Cu; n= 2 and 4, and gly= glycine. The manganese adducts were synthesized by dissolution of both, manganese chloride and glycine in water, whereas the copper adducts were obtained by using an alternative solid state synthesis approach. For all adducts, the obtained infrared data shows that the coordination involves the amine nitrogen atom, as well as an oxygen atom of the COO- group. The TG curves for the synthesized adducts exhibit only one mass loss step associated with the release of glycine molecules.

  8. Synthesis and characterization of boehmites obtained from gibbsite in presence of different environments

    Energy Technology Data Exchange (ETDEWEB)

    Denigres Filho, Ricardo Wilson Nastari; Rocha, Gisele de Araujo; Vieira-Coelho, Antonio Carlos, E-mail: acvcoelh@usp.br [Universidade de Sao Paulo (LPSS/EP/USP), SP (Brazil). Departamento de Engenharia Metalurgica e de Materiais. Laboratorio de Materias-Primas Particuladas; Montes, Celia Regina [Centro de Energia Nuclear na Agricultura (NUPEGEL/CENA/USP), Piracicaba, SP (Brazil). Nucleo de Pesquisas Geoquimicas e Geofisicas da Listosfera

    2016-05-15

    In this study, results related to boehmite synthesis by hydrothermal processes starting from a Bayer commercial gibbsite are reported. The processes have been conducted from aqueous suspensions with initial acidic or alkaline pH, without or with acetate ion, at 160 deg C for 72h to 168h. The final materials were characterized by X-ray diffraction (XRD), thermal methods (DTA and TGA) and scanning electron microscopy (SEM). The influence of the synthesis conditions on the morphology of the boehmite crystals obtained from the gibbsite at different hydrothermal processes are discussed. (author)

  9. Synthesis and Characterization of Metal Complexes with Schiff Base Ligands

    Science.gov (United States)

    Wilkinson, Shane M.; Sheedy, Timothy M.; New, Elizabeth J.

    2016-01-01

    In order for undergraduate laboratory experiments to reflect modern research practice, it is essential that they include a range of elements, and that synthetic tasks are accompanied by characterization and analysis. This intermediate general chemistry laboratory exercise runs over 2 weeks, and involves the preparation of a Schiff base ligand and…

  10. Synthesis and characterization of fluorophore attached silver nanoparticles

    Indian Academy of Sciences (India)

    S C G Kiruba Daniel; T Anitha Sironmani; V Tharmaraj; K Pitchumani

    2011-07-01

    Silver nanoparticles stabilized by soluble starch were synthesized and characterized. in vivo studies in rats showed no toxicity and revealed their distribution in various tissues and permeability across BBB. This starch stabilized silver nanoparticles have good biological characteristics to act as a potential promising vector for gene/drug delivery.

  11. Barium titanate inverted opals-synthesis, characterization, and optical properties

    Energy Technology Data Exchange (ETDEWEB)

    Soten, I.; Miguez, H.; Yang, S.M.; Petrov, S.; Coombs, N.; Tetreault, N.; Ozin, G.A. [Toronto Univ., ON (Canada). Dept. of Chemistry; Matsuura, N.; Ruda, H.E. [Toronto Univ., ON (Canada). Dept. of Metallurgy and Materials Science

    2002-01-01

    The engineering of cubic or tetragonal polymorphs of nanocrystalline barium titanate inverted opals has been achieved by thermally induced transformations. Optical characterization demonstrated photonic crystal behavior of the opals. The tuning of the ferroelectric-paraelectric transition around the Curie temperature is shown in this paper. (orig.)

  12. Synthesis and electrical characterization of Graphene Oxide films

    Energy Technology Data Exchange (ETDEWEB)

    Yasin, Muhammad, E-mail: m.yasin@seecs.edu.pk [National University of Sciences and Technology, Islamabad (Pakistan); Polymer Electronics Research Laboratory, Gebze Technical University, Gebze (Turkey); Tauqeer, T.; Zaidi, Syed M.H. [National University of Sciences and Technology, Islamabad (Pakistan); San, Sait E. [Polymer Electronics Research Laboratory, Gebze Technical University, Gebze (Turkey); Department of Physics, Gebze Technical University, 41400 Kocaeli (Turkey); TUBITAK Marmara Research Center, Photonic Technologies Group, TUBITAK Gebze (Turkey); Mahmood, Asad [National Center of Excellence in Physical Chemistry, University of Peshawar, Peshawar (Pakistan); Köse, Muhammet E. [TUBITAK Marmara Research Center, Photonic Technologies Group, TUBITAK Gebze (Turkey); Canimkurbey, Betul [Polymer Electronics Research Laboratory, Gebze Technical University, Gebze (Turkey); Department of Physics, Gebze Technical University, 41400 Kocaeli (Turkey); Department of Physics, Amasya University, 05100 Amasya (Turkey); Okutan, Mustafa [Department of Physics, Yildiz Technical University, Davutpasa, 34210 Istanbul (Turkey)

    2015-09-01

    In this work, we have synthesized Graphene Oxide (GO) using modified Hummers method and investigated its electrical properties using parallel plate impedance spectroscopic technique. Graphene Oxide films were prepared using drop casting method on Indium Tin Oxide (ITO) coated glass substrate. Atomic force microscopy was used to characterize the films' microstructure and surface topography. Electrical characterization was carried out using LCR meter in frequency regime (100 Hz to 10 MHz) at different temperatures. AC conductivity σ{sub ac} of the films was observed to be varied with angular frequency, ω as ω{sup S}, with S < 1. The electrical properties of GO were found to be both frequency and temperature dependent. Analysis showed that GO film contains direct current (DC) and Correlated Barrier Hopping (CBH) conductivity mechanisms at low and high frequency ranges, respectively. Photon absorption and transmittance capability in the visible range and excellent electrical parameters of solution processed Graphene Oxide suggest its suitability for the realization of low cost flexible organic solar cells and organic Thin Film Transistors, respectively. - Highlights: • Synthesize and electrical characterization of Graphene Oxide (GO) Film was undertaken. • Temperature dependent impedance spectroscopy was used for electrical analysis. • AFM was used to characterize films' microstructure and surface topography. • Electrical parameters were found to vary with both temperature and frequency. • GO showed DC and CBH conductivity mechanisms at low and high frequency, respectively.

  13. Rhenium(IV)-copper(II) heterobimetallic complexes with a bridge malonato ligand. Synthesis, crystal structure, and magnetic properties.

    Science.gov (United States)

    Cuevas, Alicia; Chiozzone, Raúl; Kremer, Carlos; Suescun, Leopoldo; Mombrú, Alvaro; Armentano, Donatella; De Munno, Giovanni; Lloret, Francesc; Cano, Juan; Faus, Juan

    2004-11-29

    The Re(IV) complex [ReCl4(mal)]2-, in the form of two slightly different salts, (AsPh4)1.5(HNEt3)0.5[ReCl4(mal)] (1a) and (AsPh4)(HNEt3)[ReCl4(mal)] (1b), and the Re(IV)-Cu(II) bimetallic complexes [ReCl4(mu-mal)Cu(phen)2].CH3CN (2), [ReCl4(mu-mal)Cu(bpy)2] (3), and [ReCl4(mu-mal)Cu(terpy)] (4) (mal=malonate dianion, AsPh4=tetraphenylarsonium cation, HNEt3=triethylammonium cation, phen=1,10-phenanthroline, bpy=2,2'-bipyridine and terpy=2,2':6',2' '-terpyridine) have been synthesized and the structures of 1a, 1b, 2, and 3 determined by single-crystal X-ray diffraction. The structures of 1a and 1b are made up of discrete [ReCl4(mal)]2- anions and AsPh4+ and HNEt3+ cations, held together by electrostatic forces and hydrogen bonds. The Re(IV) atom is surrounded by four chloride anions and a bidentate malonate group, in a distorted octahedral environment. The structure of 2 consist of neutral dinuclear units [ReCl4(mu-mal)Cu(phen)2], with the metal ions united through a bridge carboxilato. The environment of Re(IV) is nearly identical to that in the mononuclear complex, and Cu(II) is five coordinate, being surrounded by four nitrogen atoms of two bidentate phen ligands and one oxygen atom of the malonato ligand. In 3, there are also dinuclear units, [ReCl4(mu-mal)Cu(bpy)2], but the Cu(II) ions complete a distorted octahedral coordination by binding with the free malonato oxygen atom of a neighbor unit, resulting in an infinite chain. The magnetic properties of 1-4 were also investigated in the temperature range 2.0-300 K. The magnetic behavior of 1a and 1b is as expected for a Re(IV) complex with a large value of the zero-field splitting (2D ca. 110 cm(-1)). For the bimetallic complexes, the magnetic coupling between Re(IV) and Cu(II) is antiferromagnetic in 2 (J=-0.39 cm(-1)), ferromagnetic in 4 (J=+1.51 cm(-1)), and nearly negligible in 3 (J=-0.09 cm(-1)).

  14. Synthesis, Structure and Luminescent Properties of Polymeric Copper(Ⅰ) Halide Complexes Bearing Phosphine and N-donor Bridging Ligands

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    Three polymeric copper(Ⅰ) halide complexes bearing phosphine and N-donor bridging ligands, [(PPh3)2Cu2(μ-Br)2(μ-4,4'-bipy)]∞ 1 (bipy=bipyridine), [(PPh3)2Cu2(μ-Br)2(μ-bpe)]∞ 2 (bpe=trans-1,2-bis(4-pyridyl)ethene) and [(PPh3)2Cu2(μ-Cl)2(μ-bpe)]∞ 3, were synthesized by the multilayer diffusion method, and the structures were refined by single-crystal X-ray diffraction. Complex 1 crystallizes in triclinic, space group P-1 with a=9.122(3), b=9.322(3), c=13.201(4) (A),α=106.440(4), β=105.965(5), γ=94.167(5)°, V=1021.3(6) (A), Mr=967.62, Z=1,Dc=1.573 g/cm3, F(000)=486,μ=3.111 mm-1, the final R=0.0383 and wR=0.0960 for 2792observed reflections (I > 2σ(Ⅰ)). Complex 2 crystallizes in triclinic, space group P-1 with a=9.420(3), b=10.209(4), c=12.407(4)(A), α=104.136(6), β=108.132(5), γ=95.338(6)°, V=1081.0(7)(A), Mr=496.83, Z=2, Dc=1.526 g/cm3, F(000)=500,μ=2.941 mm-1, the final R=0.0445 and wR=0.1117 for 3251 observed reflections (I> 2σ(Ⅰ)). Complex 3 crystallizes in triclinic,space group P-1 with a=8.32(1), b=11.53(2), c=13.94(3)(A), α=109.57(3), β=93.85(3), γ=97.28(3)°, V=1242(4)(A)3, Mr=1074.59, Z=1, Dc=1.436 g/cm3, F(000)=548,μ=1.279 mm-1,the final R=0.0786 and wR=0.1586 for 2266 observed reflections (I > 2σ(Ⅰ)). The complexes exhibit intensive solid-state photoluminescence tentatively assigned to an admixture of triplet intraligand (IL) and metal-to-ligand charge-transfer (MLCT) excited state.

  15. Photoactive perylenediimide-bridged silsesquioxane functionalized periodic mesoporous organosilica thin films (PMO-SBA15): synthesis, self-assembly, and photoluminescent and enhanced mechanical properties.

    Science.gov (United States)

    Wahab, M Abdul; Hussain, H; He, Chaobin

    2009-04-21

    Well-organized periodic mesoporous organosilica thin films (designated as PMO-SBA15), having covalently bonded perylene-bridged silesquioxane (PTCDBS) inside their pore channels, are successfully synthesized via sol-gel self-assembly of 1,2-bis(triethoxysilyl)ethane and perylene-bridged silsesquioxane, using micelles of pluronic surfactant (P123) as a template for the first time. The surfactant is successfully removed from the pore channels of PMO-SBA15 by an acidic solvent extraction procedure. The final PMO-SBA15 thin films are characterized by high resolution X-ray diffraction (HRXRD), transmission electron microcopy (TEM), solid-state 29Si and 13C NMR CP/MAS NMR spectroscopy, nitrogen adsorption-desorption measurements, photoluminescence (PL) spectroscopy, and nanoindentation. HRXRD data reveal the formation of well-organized hexagonal channels in the pure PMO-SBA15 films. The intensity of the diffracted X-ray, however, systematically attenuates after incorporation of the perylene functionality inside the hexagonal channels. This is attributed to the low X-ray scattering contrast between the mesostructured organosilica walls and organic moieties (perylene) inside the channels, suggesting the successful incorporation of the photoactive perylene molecules inside the nanochannels. This was further confirmed by photoluminescence spectroscopy and nitrogen adsorption-desorption measurements. Additionally, the mechanical hardness of the functionalized PMO-SBA15 thin films, measured by nanoindentation, is significantly enhanced as compared with that of the pure PMO film. Thermogravimetric analysis (TGA) and elemental analysis suggested the functionalized PMO-SBA15 materials with PTCDBS.

  16. Synthesis, Characterization and Properties of Nanoparticles of Intermetallic Compounds

    Energy Technology Data Exchange (ETDEWEB)

    DiSalvo, Francis J. [Cornell Univ., Ithaca, NY (United States)

    2015-03-12

    The research program from 2010 to the end of the grant focused on understanding the factors important to the synthesis of single phase intermetallic nano-particles (NPs), their size, crystalline order, surface properties and electrochemical activity. The synthetic method developed is a co-reduction of mixtures of single metal precursors by strong, soluble reducing agents in a non-protic solvent, tetrahydrofuran (THF). With some exceptions, the particles obtained by room temperature reduction are random alloys that need to be annealed at modest temperatures (200 to 600 °C) in order to develop an ordered structure. To avoid significant particle size growth and agglomeration, the particles must be protected by surface coatings. We developed a novel method of coating the metal nanoparticles with KCl, a by-product of the reduction reaction if the proper reducing agents are employed. In that case, a composite product containing individual metal nanoparticles in a KCl matrix is obtained. The composite can be heated to at least 600 °C without significant agglomeration or growth in particle size. Washing the annealed product in the presence of catalyst supports in ethylene glycol removes the KCl and deposits the particles on the support. Six publications present the method and its application to producing and studying new catalyst/support combinations for fuel cell applications. Three publications concern the use of related methods to explore new lithium-sulfur battery concepts.

  17. Radiation chemical synthesis and characterization of UO 2 nanoparticles

    Science.gov (United States)

    Roth, Olivia; Hasselberg, Hanna; Jonsson, Mats

    2009-01-01

    In a deep repository for spent nuclear fuel, U(VI)(aq) released upon dissolution of the fuel matrix could, in reducing parts of the system, be converted to U(IV) species which might coalesce and form nanometer-sized UO 2 particles. This type of particles is expected to have different properties compared to bulk UO 2(s). Hence, their properties, in particular the capacity for oxidant consumption, must be investigated in order to assess the effects of formation of such particles in a deep repository. In this work, methods for radiation chemical synthesis of nanometer-sized UO 2 particles, by electron- and γ-irradiation of U(VI) solutions, are presented. Electron-irradiation proved to be the most efficient method, showing high conversions of U(VI) and yielding small particles with a narrow size distribution (22-35 nm). Stable colloidal suspensions were obtained at low pH and ionic strength (pH 3, I = 0.03). Furthermore, the reactivity of the produced UO 2 particles towards H 2O 2 is investigated. The U(IV) fraction in the produced particles was found to be ˜20% of the total uranium content, and the results show that the UO 2 nanoparticles are significantly more reactive than micrometer-sized UO 2 when it comes to H 2O 2 consumption, the major part of the H 2O 2 being catalytically decomposed on the particle surface.

  18. Synthesis and characterization of new polyaniline/nanotube composites

    Energy Technology Data Exchange (ETDEWEB)

    Maser, W.K.; Benito, A.M.; Callejas, M.A.; Seeger, T.; Martinez, M.T.; Schreiber, J.; Muszynski, J.; Chauvet, O.; Osvath, Z.; Koos, A.A.; Biro, L.P

    2003-01-15

    New polyaniline/nanotube (PANI/NT) composites have been synthesized by 'in situ' polymerization processes using both multi-wall carbon nanotubes (MWNTs) and single-wall carbon nanotubes (SWNTs) in concentrations ranging from 2 to 50 wt.%. Although no structural changes are observed using MWNTs above a concentration of 20 wt.%, the in situ synthesis results in electronic interactions between nanotubes and the quinoid ring of PANI leading to enhanced electronic properties and thus to the formation of a genuine PANI/MWNT composite material. On the other hand, using SWNTs favors the formation of inhomogeneous mixtures rather than of a homogeneous composite materials, independent of the SWNT concentration. X-ray diffraction, Raman and transport measurements show the different behavior of both classes of nanotubes in PANI/NT materials. The difficulties in the formation of a true PANI/SWNT composite are related to the far more complex structure of the SWNT material itself, i.e. to the presence of entangled bundles of SWNTs, amorphous carbon and even catalytic metal particles.

  19. PHA-rubber blends: synthesis, characterization and biodegradation.

    Science.gov (United States)

    Bhatt, Rachana; Shah, Dishma; Patel, K C; Trivedi, Ujjval

    2008-07-01

    Medium chain length polyhydroxyalkanoates (mcl-PHA) and different rubbers; namely natural rubber, nitrile rubber and butadiene rubber were blended at room temperature using solution blending technique. Blends constituted 5%, 10% and 15% of mcl-PHA in different rubbers. Thermogravimetric analysis of mcl-PHA showed the melting temperature of the polymer around 50 degrees C. Thermal properties of the synthesized blend were studied by Differential Scanning Calorimetry which confirmed effective blending between the polymers. Blending of mcl-PHA with natural rubber led to the synthesis of a different polymer having the melting point of 90 degrees C. Degradation studies of the blends were carried out using a soil isolate, Pseudomonas sp. 202 for 30 days. Extracellular protein concentration as well as OD660 due to the growth of Pseudomonas sp. 202 was studied. The degradation of blended plastic material, as evidenced by % weight loss after degradation and increase in the growth of organism correlated with the amount of mcl-PHA present in the sample. Growth of Pseudomonas sp. 202 resulted in 14.63%, 16.12% and 3.84% weight loss of PHA:rubber blends (natural, nitrile and butadiene rubber). Scanning electron microscopic studies after 30 days of incubation further confirmed biodegradation of the films.

  20. MOCVD of zirconium oxide thin films: Synthesis and characterization

    Science.gov (United States)

    Torres-Huerta, A. M.; Domínguez-Crespo, M. A.; Ramírez-Meneses, E.; Vargas-García, J. R.

    2009-02-01

    The synthesis of thin films of zirconia often produces tetragonal or cubic phases, which are stable at high temperatures, but that can be transformed into the monoclinic form by cooling. In the present study, we report the deposition of thin zirconium dioxide films by metalorganic chemical vapor deposition using zirconium (IV)-acetylacetonate as precursor. Colorless, porous, homogeneous and well adherent ZrO 2 thin films in the cubic phase were obtained within the temperature range going from 873 to 973 K. The deposits presented a preferential orientation towards the (1 1 1) and (2 2 0) planes as the substrate temperature was increased, and a crystal size ranging between 20 and 25 nm. The kinetics is believed to result from film growth involving the deposition and aggregation of nanosized primary particles produced during the CVD process. A mismatch between the experimental results obtained here and the thermodynamic prediction was found, which can be associated with the intrinsic nature of the nanostructured materials, which present a high density of interfaces.

  1. MOCVD of zirconium oxide thin films: Synthesis and characterization

    Energy Technology Data Exchange (ETDEWEB)

    Torres-Huerta, A.M., E-mail: atohuer@hotmail.com [Centro de Investigacion en Ciencia Aplicada y Tecnologia Avanzada, Unidad Altamira, Instituto Politecnico Nacional, Km. 14.5 Carr. Tampico-Puerto Industrial, C.P. 89600, Altamira, Tamaulipas (Mexico); Dominguez-Crespo, M.A.; Ramirez-Meneses, E. [Centro de Investigacion en Ciencia Aplicada y Tecnologia Avanzada, Unidad Altamira, Instituto Politecnico Nacional, Km. 14.5 Carr. Tampico-Puerto Industrial, C.P. 89600, Altamira, Tamaulipas (Mexico); Vargas-Garcia, J.R. [ESIQIE, Departamento de Metalurgia y Materiales, Instituto Politecnico Nacional. A.P. 75-876, 07300 Mexico, D.F. (Mexico)

    2009-02-15

    The synthesis of thin films of zirconia often produces tetragonal or cubic phases, which are stable at high temperatures, but that can be transformed into the monoclinic form by cooling. In the present study, we report the deposition of thin zirconium dioxide films by metalorganic chemical vapor deposition using zirconium (IV)-acetylacetonate as precursor. Colorless, porous, homogeneous and well adherent ZrO{sub 2} thin films in the cubic phase were obtained within the temperature range going from 873 to 973 K. The deposits presented a preferential orientation towards the (1 1 1) and (2 2 0) planes as the substrate temperature was increased, and a crystal size ranging between 20 and 25 nm. The kinetics is believed to result from film growth involving the deposition and aggregation of nanosized primary particles produced during the CVD process. A mismatch between the experimental results obtained here and the thermodynamic prediction was found, which can be associated with the intrinsic nature of the nanostructured materials, which present a high density of interfaces.

  2. Green synthesis of silver nanoparticles and their characterization by XRD

    Science.gov (United States)

    Mehta, B. K.; Chhajlani, Meenal; Shrivastava, B. D.

    2017-05-01

    A cost effective and environment friendly technique for green synthesis of silver nanoparticles has been reported. Silver nanoparticles have been synthesized using ethanol extract of fruits of Santalum album (Family Santalaceae), commonly known as East Indian sandalwood. Fruits of S.album were collected and crushed. Ethanol was added to the crushed fruits and mixture was exposed to microwave for few minutes. Extract was concentrated by Buchi rotavaporator. To this extract, 1mM aqueous solution of silver nitrate (AgNO3) was added. After about 24 hr incubation Ag+ ions in AgNO3 solution were reduced to Ag atoms by the extract. Silver nanoparticles were obtained in powder form. X-ray diffraction (XRD) pattern of the prepared sample of silver nanoparticles was recorded The diffractogram has been compared with the standard powder diffraction card of JCPDS silver file. Four peaks have been identified corresponding to (hkl) values of silver. The XRD study confirms that the resultant particles are silver nanoparticles having FCC structure. The average crystalline size D, the value of the interplanar spacing between the atoms, d, lattice constant and cell volume have been estimated. Thus, silver nanoparticles with well-defined dimensions could be synthesized by reduction of metal ions due to fruit extract of S.album.

  3. Synthesis and characterization of magnetite nanoparticles from mineral magnetite

    Energy Technology Data Exchange (ETDEWEB)

    Morel, Mauricio, E-mail: mmorel@ing.uchile.cl [Laboratorio de Síntesis y Polímeros, Departamento de ciencias de los Materiales, Facultad de Ciencias Físicas y Matemáticas, Universidad de Chile, Santiago (Chile); Laboratorio de Materiales a Nanoescala, Departamento de ciencias de los Materiales, Facultad de Ciencias Físicas y Matemáticas, Universidad de Chile, Avenue Tupper 2069, Santiago (Chile); Martínez, Francisco, E-mail: polimart@ing.uchile.cl [Laboratorio de Síntesis y Polímeros, Departamento de ciencias de los Materiales, Facultad de Ciencias Físicas y Matemáticas, Universidad de Chile, Santiago (Chile); Mosquera, Edgar [Laboratorio de Materiales a Nanoescala, Departamento de ciencias de los Materiales, Facultad de Ciencias Físicas y Matemáticas, Universidad de Chile, Avenue Tupper 2069, Santiago (Chile)

    2013-10-15

    We have synthesized magnetite nanoparticles with sizes that range from 20 to 30 nm from mineral magnetite roughly 45 μm in size. The procedure consists in the dissolution of the mineral in an acidic medium and subsequent precipitation in a basic medium in the presence of oleic acid. Two experiments were conducted in different gaseous environments. The first was carried out in an environment exposed to air (M1) and the second in an N{sub 2} (M2) environment. The x-ray diffraction results showed a slight difference, which corresponds to the surface oxidation of magnetite. The sizes of the modified nanoparticles were determined through the Scherrer equation and transmission electron microscopy. An organic material mass loss corresponding to 18% was observed through a thermogravimetric analysis. The Fourier transform infrared spectroscopic analysis provides information about the type of bond that is formed on the surface of the nanoparticle, which corresponds to a bidentate chelate. The vibrating sample magnetometer results show a superparamagnetic behavior for sample M1. - Highlights: • A new method for synthesis of nanoparticles from mineral microparticles. • Search agreggate value to the mineral by mean nanoscience. • The stoichiometric ratio of the ions Fe{sup 2+} and Fe{sup 3+} from the mineral magnetite is synergistic.

  4. Synthesis of Mesoporous Titania with Surfactant and its Characterization

    Directory of Open Access Journals (Sweden)

    T. Benkacem

    2008-01-01

    Full Text Available A mesoporous titania was obtained by gelation from Ti-alkoxide in acidic solutions with addition of surfactant cetyltrimetylammonium bromide (CH3(CH215N(CH33Br using a sol-gel process. The effects of surfactant concentration on synthesis of mesoporous titania were studied. The structural characterisation was studied by differential thermal analysis, infrared spectroscopy, X-ray diffraction. Studies by X-ray diffraction showed that crystallisation of TiO2 powder occurs at 200°C, above 200°C we obtained a mixture of two forms-Anatase and rutile. The textural characterisation by nitrogen adsorption-desorption allowed us to observe the variation of the surface area, porous volume and pore diameters according to temperature and [CTAB]/[Ti-alkoxide] molar ratio. The analysis of the results shows that addition of surfactant residue increases considerably its pore diameters. The deposit thin layers has been realized with a sol prepared with the destabilization of colloidal solutions process. Scanning electron-spectroscopy observation for thermally treated (at 400 and 600°C samples, showed homogeneous layers without cracking.

  5. Synthesis, Characterization and Thermal Diffusivity of Holmium and Praseodymium Zirconates

    Directory of Open Access Journals (Sweden)

    Stopyra M.

    2016-06-01

    Full Text Available A2B2O7 oxides with pyrochlore or defected fluorite structure are among the most promising candidates for insulation layer material in thermal barrier coatings. The present paper presents the procedure of synthesis of holmium zirconate Ho2Zr2O7 and praseodymium zirconate Pr2Zr2O7 via Polymerized-Complex Method (PCM. Thermal analysis of precursor revealed that after calcination at relatively low temperature (700°C fine-crystalline, single-phase material is obtained. Thermal diffusivity was measured in temperature range 25-200°C, Ho2Zr2O7 exhibits lower thermal diffusivity than Pr2Zr2O7. Additionally, PrHoZr2O7 was synthesized. The powder in as-calcined condition is single-phase, but during the sintering decomposition of solid solution took place and Ho-rich phase precipitated. This material exhibited the best insulating properties among the tested ones.

  6. Metallic iron nanoparticles: Flame synthesis, characterization and magnetic properties

    Institute of Scientific and Technical Information of China (English)

    Yunfeng Li; Yanjie Hu; Guangjian Huang; Chunzhong Li

    2013-01-01

    Metallic iron (Fe) nanoparticles (NPs) with a typical core-shell structure have been prepared by a simple and continuous flame spray pyrolysis (FSP) method,which are stabilized by the corresponding Fe3O4 shell with a thickness of 4-6 nm.The size of metallic Fe cores is about 30-80 nm.The core-shell structured iron NPs show an air stability as long as one month as a result of the protection of oxide shell.Through the control of the residence time of materials in flame and flame atmosphere,metallic Fe and iron oxides are obtained,showing a better external magnetic field responsibility.It is concluded that the evolution of morphology and composition of flame-made magnetic NPs could be attributed to the competition mechanism between reduction and oxidation reactions of in situ flame combustion,which offers more choices and better effective design strategy for the synthesis of advanced functional materials via FSP techniques.

  7. Synthesis and Characterization of Gold Nanoparticles by Tryptophane

    Directory of Open Access Journals (Sweden)

    Azim Akbarzadeh

    2009-01-01

    Full Text Available Problem statement: Preparation and synthesis of gold nanoparticles with small size and suitable stability is very important and applicable particularly in medicine. In this study, we have prepared gold nanoparticles by chemical reduction method employing L-Tryptophane as a reducing agent for ionic gold. Approach: The gold nanoparticles are the most employed amongst the different metallic nanoparticles in the fields of nanomedicine and nanobiotechnology. Therefore, the employed method should provide suitable particle size, shape and particle distribution in order to obtain nanoparticles of high activity and efficiency indicating the importance of the technique. In this study, HAuCl4 .3H2O, L-Tryptophane and polyethyleneglycol (PEG were used to produce AuCl-4 ions. They were acted as pre-material, reducing and stabilizing agents respectively. Results: The size, distribution and formation of gold nanoparticles were confirmed by Transmission Electron Microscopy (TEM indicating the diameter of gold nanoparticles at the range of 10-25 nm and UV spectroscopy. The formed nanoparticles showed the highest absorption at 518 nm. Conclusion: The gold nanoparticles were stable in PEG1000. Since these nanoparticles have suitable size distribution they can be considered as a suitable candidate to be employed in nanomedicine and nanobiotechnology.

  8. Synthesis, characterization, and metabolism studies of fluspidine enantiomers.

    Science.gov (United States)

    Holl, Katharina; Falck, Evamaria; Köhler, Jens; Schepmann, Dirk; Humpf, Hans-Ulrich; Brust, Peter; Wünsch, Bernhard

    2013-12-01

    The enantiomers of the potent σ1 ligand fluspidine (1) were prepared by using chiral preparative HPLC. Synthesis of racemic tosylate 2 and subsequent separation of enantiomers yielded (R)-2 and (S)-2 in excellent enantiomeric purities. The fluspidine enantiomers (R)-1 and (S)-1 were synthesized from (R)-2 and (S)-2 by nucleophilic substitution with tetra-n-butylammonium fluoride, affording (R)-1 with 99.6 % ee and (S)-1 with 96.4 % ee. Tosylates (R)-2 and (S)-2 can also serve as precursors for the radiosynthesis of enantiomerically pure radiotracers [(18) F](R)-1 and [(18) F](S)-1. The absolute configuration of the pure enantiomers was elucidated by comparison of their CD spectra with a calculated CD spectrum of a simplified model compound. In receptor binding studies, both enantiomers displayed very high σ1 receptor affinity and selectivity against the σ2 receptor. (R)-Fluspidine ((R)-1) is the eutomer, with a Ki value of 0.57 nM and a eudysmic ratio of 4. Incubation of (R)-1 and (S)-1 with rat liver microsomes led to the identification of seven and eight metabolites, respectively. Although the S-configured enantiomer formed additional metabolite (S)-1-3, it is metabolically more stable than (R)-1. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Synthesis, characterization and optical properties of nanocrystalline lead molybdate

    Energy Technology Data Exchange (ETDEWEB)

    Anandakumar, V.M. [Department of Physics University of Kerala, Thiruvananthapuram (India); Department of Physics, Mahatma Gandhi College, Thiruvananthapuram (India); Khadar, M.A. [Department of Physics University of Kerala, Thiruvananthapuram (India); Centre for Nanosciences and Nanotechnology, University of Kerala, Thiruvananthapuram (India)

    2008-11-15

    Lead molybdate (PbMoO{sub 4}) finds wide practical application due to its acousto-optic and luminescent properties. In the present study, nanoparticles of PbMoO{sub 4} of different grain sizes were synthesized through chemical precipitation technique. Precipitation reactions carried out in non-aqueous media below room temperature were used for the synthesis of samples of two lower grain sizes. The crystal structure and grain size of the samples were determined using X-ray diffraction and transmission electron microscopy. UV-Visible absorption spectra showed a broad absorption peak for the sample with average grain size of 52 nm which is blue shifted considerably as the average grain size was reduced to 14 nm. The fundamental absorption follows an exponential edge indicating Urbach-like behaviour. The temperature dependence of Urbach parameter is also determined. The micro-Raman spectra and FT Raman spectra of the samples were recorded and the features in the Raman spectra are discussed. (copyright 2008 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  10. Synthesis and characterization of robust magnetic carriers for bioprocess applications

    Energy Technology Data Exchange (ETDEWEB)

    Kopp, Willian, E-mail: willkopp@gmail.com [Federal University of São Carlos-UFSCar, Graduate Program in Chemical Engineering, Rodovia Washington Luiz, km 235, São Carlos, São Paulo 13565-905 (Brazil); Silva, Felipe A., E-mail: eq.felipe.silva@gmail.com [Federal University of São Carlos-UFSCar, Graduate Program in Chemical Engineering, Rodovia Washington Luiz, km 235, São Carlos, São Paulo 13565-905 (Brazil); Lima, Lionete N., E-mail: lionetenunes@yahoo.com.br [Federal University of São Carlos-UFSCar, Graduate Program in Chemical Engineering, Rodovia Washington Luiz, km 235, São Carlos, São Paulo 13565-905 (Brazil); Masunaga, Sueli H., E-mail: sueli.masunaga@gmail.com [Department of Physics, Montana State University-MSU, 173840, Bozeman, MT 59717-3840 (United States); Tardioli, Paulo W., E-mail: pwtardioli@ufscar.br [Department of Chemical Engineering, Federal University of São Carlos-UFSCar, Rodovia Washington Luiz, km 235, São Carlos, São Paulo 13565-905 (Brazil); Giordano, Roberto C., E-mail: roberto@ufscar.br [Department of Chemical Engineering, Federal University of São Carlos-UFSCar, Rodovia Washington Luiz, km 235, São Carlos, São Paulo 13565-905 (Brazil); Araújo-Moreira, Fernando M., E-mail: faraujo@df.ufscar.br [Department of Physics, Federal University of São Carlos-UFSCar, Rodovia Washington Luiz, km 235, São Carlos, São Paulo 13565-905 (Brazil); and others

    2015-03-15

    Highlights: • Silica magnetic microparticles were synthesized for applications in bioprocesses. • The process to produce magnetic microparticles is inexpensive and easily scalable. • Microparticles with very high saturation magnetization were obtained. • The structure of the silica magnetic microparticles could be controlled. - Abstract: Magnetic carriers are an effective option to withdraw selected target molecules from complex mixtures or to immobilize enzymes. This paper describes the synthesis of robust silica magnetic microparticles (SMMps), particularly designed for applications in bioprocesses. SMMps were synthesized in a micro-emulsion, using sodium silicate as the silica source and superparamagnetic iron oxide nanoparticles as the magnetic core. Thermally resistant particles, with high and accessible surface area, narrow particle size distribution, high saturation magnetization, and with superparamagnetic properties were obtained. Several reaction conditions were tested, yielding materials with saturation magnetization between 45 and 63 emu g{sup −1}, particle size between 2 and 200 μm and average diameter between 11.2 and 15.9 μm, surface area between 49 and 103 m{sup 2} g{sup −1} and pore diameter between 2 and 60 nm. The performance of SMMps in a bioprocess was evaluated by the immobilization of Pseudomonas fluorescens lipase on to octyl modified SMMp, the biocatalyst obtained was used in the production of butyl butyrate with good results.

  11. Synthesis and characterization of several molybdenum chloride cluster compounds

    Energy Technology Data Exchange (ETDEWEB)

    Beers, W.W.

    1983-06-01

    Investigation into the direct synthesis of Mo/sub 4/Cl/sub 8/(P(C/sub 2/H/sub 5/)/sub 3/)/sub 4/ from Mo/sub 2/(OAc)/sub 4/ led to a synthetic procedure that produces yields greater than 80%. The single-crystal structure disclosed a planar rectangular cluster of molybdenum atoms. Metal-metal bond distances suggest that the long edges of the rectangular cluster should be considered to be single bonds and the short metal-metal bonds to be triple bonds. This view is reinforced by an extended Hueckel calculation. Attempts to add a metal atom to Mo/sub 4/Cl/sub 8/(PR/sub 3/)/sub 4/ to form Mo/sub 5/Cl/sub 10/(PR/sub 3/)/sub 3/ led instead to a compound with the composition Mo/sub 8/Cl/sub 16/(PR/sub 3/)/sub 4/. Solution and reflectance uv-visible spectra and x-ray photoelectron spectra suggest that tetranuclear molybdenum units are present. The facile reaction between Mo/sub 8/Cl/sub 16/(PR/sub 3/)/sub 4/ and PR/sub 3/ imply that the linkage between tetrameric units is weak.

  12. Synthesis and characterization of NiMnIn nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Aksoy, Seda, E-mail: eaksoy@itu.edu.tr

    2015-01-01

    The off-stoichiometric Ni{sub 50}Mn{sub 34}In{sub 16} intermetalic Heusler nanoparticles have been prepared by laser ablation in distilled water from the target alloy using femtosecond laser system. The properties of the particles were characterized by electron microscopy and magnetometer techniques. The particle mean size of 28 nm was estimated by using the scanning electron microscopy images. However, the transmission electron microscopy results revealed that spherical cluster-like particles have been also produced. The magnetic field-induced structural transition was found in the particles with a starting temperature of around 250 K. - Highlights: • Ni–Mn–In Heusler nanoparticles are prepared by laser ablation method. • Structural properties are characterized by SEM and TEM. • Magnetic properties are discussed by the temperature-dependent magnetization and the magnetic field-dependent magnetization measurements.

  13. Synthesis and characterization of polyaniline as emeraldine salt

    Energy Technology Data Exchange (ETDEWEB)

    Gawri, Isha; Khatta, Swati; Singh, K. P.; Tripathi, S. K., E-mail: surya@pu.ac.in, E-mail: surya-tr@yahoo.com [Department of Physics, Center of Advanced Study in Physics, Panjab University, Chandigarh-160 014 (India)

    2016-05-06

    Polyaniline in emeraldine salt (PANI-ES) form was successfully synthesized by oxidative polymerization of aniline using ammonium peroxidisulphate as oxidant in the presence of hydrochloric acid as catalyst under ice bath condition. The as prepared powdered sample was characterized using X-Ray Diffraction (XRD) and Fourier Transform Infrared (FTIR) spectroscopy. Using XRD, the average crystalline size was found to be 5.63 nm and d-spacing corresponding to crystalline peak 2θ = 25.08° had come out to be 4.2 Å. Also FTIR absorption spectra showed all the characteristics bands of PANI –ES. The ohmic contact between the PANI-ES film and the substrate was confirmed by Current-Voltage (I-V) characterization.

  14. Synthesis and characterization of optically transparent epoxy matrix nanocomposites

    Energy Technology Data Exchange (ETDEWEB)

    Esposito Corcione, C., E-mail: carola.corcione@unile.it [Dipartimento di Ingegneria dell' Innovazione Via Monteroni 73100, Lecce (Italy); Manera, M.G. [IMM-CNR Istituto per la microelettronica e microsistemi - sezione di Lecce, c/o campus universitario, via per Monteroni, 73100 Lecce (Italy); Maffezzoli, A. [Dipartimento di Ingegneria dell' Innovazione Via Monteroni 73100, Lecce (Italy); Rella, R. [IMM-CNR Istituto per la microelettronica e microsistemi - sezione di Lecce, c/o campus universitario, via per Monteroni, 73100 Lecce (Italy)

    2009-08-01

    In this work optically transparent nanocomposites were prepared and characterized from an optical and morphological point of view. An organically modified boehmite was added at different concentrations in a diglycidyl ether of bisphenol A (DGEBA) epoxy matrix, hardened with a polyether diamine. Nanocomposites were characterized structurally by X-ray diffraction (XRD), optically by UV-Vis-NIR spectrophotometry and their morphology was investigated by Atomic Force Microscopy (AFM). Morphological investigation reveals the presence of boehmite particles dispersed in the epoxy matrix in different dimensions ranging from ten to hundreds of nanometers; some aggregation in the particles is the tendency noticed in the AFM images. The acquisition of multiple AFM images in different areas of the sample was used for a statistical analysis of the volumetric distribution of boehmite aggregates. The obtained result, (3.6 {+-} 0.3)%vol, is well comparable to thermogravimetric analysis.

  15. Synthesis and characterization of europium doped LiF phosphor

    Energy Technology Data Exchange (ETDEWEB)

    Villalobos, M. L.; Vallejo, M. A.; Sosa A, M. [Universidad de Guanajuato, Division de Ciencias e Ingenierias, Loma del Bosque No. 103, Lomas del Campestre, 37150 Leon, Guanajuato (Mexico); Diaz T, L. A., E-mail: villaloboscm2010@licifug.ugto.mx [Centro de Investigaciones en Optica, A. C., Loma del Bosque No. 115, Lomas del Campestre, 37150 Leon, Guanajuato (Mexico)

    2015-10-15

    LiF with different dopants has been one of the most investigated materials to use as thermoluminescent dosimeter. In this paper, we present the preparation method, the characterization and the thermoluminescent response of Eu doped LiF irradiated with X-rays. Pure and Eu doped LiF samples with different dopant concentration (0, 0.25, 0.5, 0.75 and 1 % mol) were synthesized using the precipitation method. The samples were structurally characterized by X-ray diffraction (XRD), the diffraction patterns showed a main cubic crystalline structure and a secondary hexagonal structure. The photoluminescence spectrum exhibited four well defined peaks characteristic of the Eu{sup 3+} ion. Thermoluminescent (Tl) glow curves of x-ray irradiated samples showed a well-defined single peak around 200 degrees C, except for the pure and 0.25% Eu doped samples. (Author)

  16. Synthesis and characterization of hydrogel bonded with rare earth

    Institute of Scientific and Technical Information of China (English)

    YAN Changhao; JIAO Lianlian; GUO Chunfang; ZHANG Ming; QIU Guanming

    2008-01-01

    Chitosan-poly(acrylic acid) hydrogel bonded with Eu3+ was prepared by radical solution polymerization. Biodegradable chitosan,N,N'-methylen-diacrylamide, and potassium persulphate were used as the basic material, cross-linking agent, and initiator, respectively. The structure and thermal property of hydrogel were characterized by infrared spectrometry, X-ray diffraction, scanning electron microscopy, and differential scanning calorimetry. The swollen property and fluorescent performance were also characterized. The results showed that the rare earth presented unique distribution in the hydrogel due to the formation of chemical bonds after polymerization. The glass transition tem-perature of the hydrogel decreased remarkably, which might broaden the range of its elastic application considerably. Moreover, the charac-teristic fluorescent emission of Eu3+ was observed in the hydrogel, which was indicative of the excellent luminescent performance.

  17. Synthesis and Characterization of Novel Epoxy Geopolymer Hybrid Composites

    Directory of Open Access Journals (Sweden)

    Oreste Tarallo

    2013-09-01

    Full Text Available The preparation and the characterization of novel geopolymer-based hybrid composites are reported. These materials have been prepared through an innovative synthetic approach, based on a co-reticulation in mild conditions of commercial epoxy based organic resins and a metakaolin-based geopolymer inorganic matrix. This synthetic strategy allows the obtainment of a homogeneous dispersion of the organic particles in the inorganic matrix, up to 25% in weight of the resin. The materials obtained present significantly enhanced compressive strengths and toughness with respect to the neat geopolymer, suggesting their wide utilization for structural applications. A preliminary characterization of the porous materials obtained by removing the organic phase from the hybrid composites by means of heat treatments is also reported. Possible applications of these materials in the field of water purification, filtration, or as lightweight insulating materials are envisaged.

  18. Synthesis, characterization, and antiplasmodial activity of polymer-incorporated aminoquinolines.

    Science.gov (United States)

    Aderibigbe, B A; Neuse, E W; Sadiku, E R; Ray, S Shina; Smith, P J

    2014-06-01

    In this research, aminoquinoline compounds were synthesized, characterized, and incorporated into water-soluble polymers to form conjugates. The conjugates were characterized by X-ray diffraction, thermal gravimetric analysis, scanning electron microscope, Fourier transform infrared spectroscopy, and nuclear magnetic resonance spectroscopy to confirm the successful incorporation of the aminoquinoline compound on to the polymer. The synthesized conjugates were screened for in vitro antiplasmodial activity in triplet test against chloroquine-sensitive strain of Plasmodium falciparum and chloroquine drug was used as a reference drug in all the experiments. A full dose-response was performed to determine the concentration inhibiting 50% of parasite growth (IC50 value). Polymeric conjugates containing 3-diethylamino-1-propylamine solubilizing units were found to be most active against the chloroquine-sensitive strain of P. falciparum.

  19. Template synthesis, characterization and transformations of iron nanowires while aging

    Energy Technology Data Exchange (ETDEWEB)

    Jagminas, Arunas [Institute of Chemistry, A. Gostauto 9, LT-01108 Vilnius (Lithuania)], E-mail: jagmin@ktl.mii.lt; Mazeika, Kestutis; Reklaitis, Jonas [Institute of Physics, Savanoriu 231, LT-02300 Vilnius (Lithuania); Kurtinaitiene, Marija [Institute of Chemistry, A. Gostauto 9, LT-01108 Vilnius (Lithuania); Baltrunas, Dalis [Institute of Physics, Savanoriu 231, LT-02300 Vilnius (Lithuania)

    2008-05-15

    Densely packed arrays of various materials demonstrating enhanced magnetic properties remain of great interest nowadays. In this study, transmission electron microscopy (TEM), Moessbauer spectroscopy (MS) and powder X-ray diffraction (XRD) were used to characterize the morphology, composition and phase of iron nanowires (nws) deposited from the developed solution within alumina template pores of the average diameter of ca.15 nm by the alternating current (ac) electrolysis protocol. The same investigations were performed after Fe nws storage in the air for several months. Characterization of the as-grown product shows the formation of the crystalline {alpha}-Fe nws array with a preferred [1 1 0] nw growth direction. The aging of samples leads to the corrosion of Fe nws mainly from the template top side while aging of Fe nws liberated from the template and kept for several months under ambient conditions results in the corrosion of nws along their full length producing catkin-twig shapes.

  20. Electrochemical synthesis and characterization of Cu2Se nanowires

    Science.gov (United States)

    Kaur, Harmanmeet; Kaur, Jaskiran; Singh, Lakhwant; Singh, Surinder

    2013-12-01

    Copper Selenide (Cu2Se) nanowires were successfully fabricated via potentiostatic electrodeposition using polycarbonate membranes (Whatmann, USA) with nominal pore diameter of 100 nm. The morphology of the so fabricated nanowires was examined by field emission scanning electron microscopy (FE-SEM). Later the samples were characterized for their structural, optical and electrical properties by XRD, UV-visible spectroscopy and I-V respectively.

  1. Synthesis and characterization of novel dipeptide ester prodrugs of acyclovir

    Science.gov (United States)

    Nashed, Yasser E.; Mitra, Ashim K.

    2003-07-01

    Four dipeptide (Gly-Gly, Gly-Val, Val-Val, Val-Gly) ester prodrugs of 9-[(2-hydroxyethoxy)methyl]guanine (acyclovir, ACV) were synthesized. LC/MS was used to characterize the new prodrugs. Both 1H NMR and 13C NMR spectra of the four prodrugs of ACV were measured and assigned based on spectral comparison with compounds of similar structures.

  2. Synthesis, characterization and thermal properties of thiosalicylate ionic liquids

    Indian Academy of Sciences (India)

    Cecilia Devi Wilfred; Fadwa Babiker Mustafa

    2013-11-01

    In an attempt to produce new functionalized ionic liquids, a series of thiosalicylate ionic liquids based on imidazolium, ammonium, phosphonium, choline and pyrrolidinium cations were synthesized. The compounds were characterized by Infra Red (IR), Nuclear Magnetic Resonance (NMR) and mass spectra (ESI-MS). Their glass-transition temperatures, melting points and decomposition temperatures have been measured. Physicochemical properties of ionic liquids are influenced by alkyl chain length and nature of the cation of ionic liquids.

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

    Energy Technology Data Exchange (ETDEWEB)

    Asha, E-mail: arana5752@gmail.com [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)

    2016-05-23

    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.

  4. Synthesis and Characterization of Thermosetting Polyimide Oligomers for Microelectronics Packaging

    OpenAIRE

    2000-01-01

    A series of reactive phenylethynyl endcapped imide oligomers has been prepared in either fully cyclized or amic acid precursor form. Soluble oligomers have been synthesized with controlled molecular weights ranging from 2- to 12 Kg/mol. Molecular weight characterization was performed using SEC (size exclusion chromatography) and 13C-NMR, revealing good agreement between the theoretical and experimental (Mn) values. Crosslinked polyimides were obtained by solution or melt processing the oli...

  5. Synthesis and Characterization of Nitrogen-Doped Graphene

    OpenAIRE

    Palaniuk, D. Ryan

    2012-01-01

    Approved for public release; distribution is unlimited Self standing nitrogen doped graphene sheets were produced by reduction-expansion method, which utilizes graphite oxide (GO) and urea as precursor materials. For comparison, an Atmospheric Microwave Plasma Torch system (ATP) was used to produce graphene samples under argon and nitrogen atmospheres from GO. Graphene samples were characterized by XRD, TEM, SEM, BET and Raman Spectroscopy. The GO and urea mixtures decomposition-reduction ...

  6. Synthesis and characterization of gelatin based polyester urethane scaffold

    Indian Academy of Sciences (India)

    S Sarkar; A Chourasia; S Maji; S Sadhukhan; S Kumar; B Adhikari

    2006-10-01

    For tissue engineering purpose two gelatin based polyester urethane scaffolds of different compositions were prepared from lactic acid, polyethylene glycol 400 (PEG 400) and characterized by FTIR, XRD for their mechanical and morphological properties using SEM and optical microscopic analyses. Degradation and swelling studies of gelatin based polyester urethane scaffolds in phosphate buffer saline (PBS) were performed. Human keratinocyte cells were cultured within these scaffolds, which showed good cell adherence and proliferation.

  7. Synthesis and characterization of new azo containing Schiff base macrocycle

    Institute of Scientific and Technical Information of China (English)

    Saeed Malek-Ahmadi; Amir Abdolmaleki

    2011-01-01

    Fully conjugated Schiff base macrocycle has been prepared through a simple and mild condition, a one-pot cyclization procedure of four-component without using a template. The condensation reaction of related bis (hydroxybenzaldehyde) with phenylenediamines to prepare a conjugated [2 + 2] Schiff base macrocycle has been investigated and fluorescent [2 + 2] Schiff base macrocycles with N2O2 binding pockets has been prepared and characterized by elemental analysis,' H NMR, IR, fluorescent, UV-visible and MALDI mass spectroscopies.

  8. Synthesis and spectral characterization of a decavanadate/chitosan complex

    OpenAIRE

    ZHETCHEVA, Violeta Dimitrova KASSABOVA; PAVLOVA, Lilyana Parvanova

    2014-01-01

    A decavanadate/chitosan complex was synthesized by crosslinking chitosan with decavanadate anions at a pH of 3. The materials were characterized by Fourier transformed infrared spectroscopy (FT-IR), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), absorption spectroscopy (UV-Vis), and transmission electron microscopy (TEM). The spectroscopic results indicated that the decavanadate/chitosan complex was successfully obtained as result of an ionic crosslinking of the chi...

  9. Synthesis,Characterization and Biological Activities of Novel Acrylamide Compounds

    Institute of Scientific and Technical Information of China (English)

    XU Liang-zhong; XU Zhong-jie; ZHANG Gong-sheng; ZHOU Kai; ZHAI Zhi-wei

    2008-01-01

    With dimethomorph and flumorph as the leading compounds,four novel acrylamide compounds with two types of structure were designed and synthesized by means of the method of"me too chemistry".The target compounds were characterized by 1H NMR,IR,MS,and elemental analysis.The influences of solvent and raw material on the yield were investigated and optimum processing conditions were determined.The results of preliminary biological tests show that all those compounds exhibit certain antifungal activities.

  10. Synthesis and characterization of novel multifunctional epoxy resin

    Institute of Scientific and Technical Information of China (English)

    Jue Cheng; Jing Chen; Wan Tai Yang

    2007-01-01

    A novel multifunctional epoxy resin was synthesized by polyphenol and epichlorohydrin. The structure and molecular weight of the multifunctional epoxy were characterized by FTIR and ESI-MS. DSC and DMTA were used to investigate the thermal property of multifunctional epoxy cured by DDS. The thermal resistance of the synthesized multifunctional epoxy was much better than a standard diglycidyl ether of bisphenol-A epoxy.

  11. Synthesis and characterization of heterocyclic substituted fluoran compounds

    Directory of Open Access Journals (Sweden)

    SACHIN V. PATEL

    2007-11-01

    Full Text Available New quinazolinone-substituted fluoran compounds were synthesized by reaction of keto acid, 2’-carboxy-2-hydroxy-4-N-pyrrolidinylbenzophenone with different quinazolinone derivatives in the presence of conc. sulphuric acid. All the synthesized fluoran compounds were characterized by spectroscopic methods (IR, 1H-NMR and UV–visible spectroscopy and elemental analysis. The fluoran compounds are colourless or nearly colourless and develop colour on contact with electron-accepting compounds.

  12. SYNTHESIS AND CHARACTERIZATION OF AN ORDERED LADDER POLYESTER

    Institute of Scientific and Technical Information of China (English)

    Ping-ping Zhang; Tao-yi Zhang; Chuan-feng Zhu; Yu-xia Diao; You-zhi Wan; Ping Xie; Rong-ben Zhang

    2006-01-01

    An ordered ladder polyester (LPE) was first synthesized through the ladder superstructure (LS) constructed by concerted interactions of hydroxyl- and aramide-based H-bonding and p-terphenyl (TP)-based π-stacking by dehydrochlorination condensation using phosgene (COCl2) as coupling agent. LPE was characterized by GPC, FTIR, NMR,XRD, DSC and AFM. Among them, a distinct image of regularly linear alignment corresponding to the ladder main chain of LPE was first revealed by high-resolution AFM.

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

    Science.gov (United States)

    Asha, Goyal, Sneh Lata; Kishore, Nawal

    2016-05-01

    Polyaniline (PANI) and PANI /cobalt chloride composites were synthesized by in situ chemical oxidative polymerization of aniline with CoCl2.6H2O 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.

  14. Synthesis and structural characterization of CsNiP crystal

    Indian Academy of Sciences (India)

    G S Gopalakrishna; B H Doreswamy; M J Mahesh; M Mahendra; M A Sridhar; J Shashidhara Prasad; K G Ashamanjari

    2004-02-01

    CsNiP crystals were synthesized by hydrothermal technique and characterized by the X-ray diffraction method. This alkaline transition metal phosphide crystallizes in the hexagonal system with space group P6$_3/mmc$ and cell parameters, = 7.173(2) Å, = 5.944(9) Å, = 264.87(7) Å3 and = 2. The final residual factor is 1 = 0.0362 for 206 reflections with > 2().

  15. Synthesis and characterization of HPMA copolymer-5-FU conjugates

    Institute of Scientific and Technical Information of China (English)

    Fang Yuan; Fu Chen; Qing Yu Xiang; Xuan Qin; Zhi Rong Zhang; Yuan Huang

    2008-01-01

    N-(2-Hydroxypropyl)methacrylamide copolymer-5-fluorouracil (PHPMA-FU)conjugates were synthesized by a novel and simplified synthetic mute,and characterized by UV,FTIR and HPLC analyses.The conjugated content of 5-fluorouracil (5-FU)was 3.41 ± 0.07 wt%.The stabilities of PHPMA-FU conjugates under different conditions were studied.The results showed that HPMA copolymer was a potential carrier for tumor-targeting delivery of 5-FU.

  16. Bridge Management Systems

    DEFF Research Database (Denmark)

    Thoft-Christensen, Palle

    In this paper bridge management systems are discussed with special emphasis on management systems for reinforced concrete bridges. Management systems for prestressed concrete bridges, steel bridges, or composite bridges can be developed in a similar way....

  17. 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: chriswittee@gmail.com [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)

    2016-11-15

    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)

  18. A novel vanadium n-propylamino phosphate catalyst: synthesis, characterization and applications

    Directory of Open Access Journals (Sweden)

    Rajini Anumula

    2013-02-01

    Full Text Available A novel, lamellar type Vanadium n-propylamino phosphate catalyst is synthesized and characterized by using various physicochemical techniques such as Powder X-ray diffraction, Scanning electron microscopy/Energy dispersive X-ray analysis, Thermogravimetry/Differential thermal analysis, Fourier transform Infrared analysis, Electron spin resonance spectroscopy, Ultraviolet - Visible Diffuse reflectance spectroscopy, X-ray Photoelectron spectroscopy, 31P Magic angle spinning Nuclear Magnetic Resonance spectroscopy and Catalytic applications toward Octahydroquinazolinone synthesis. It is found that the n-propylamine is present as sandwich between Vanadyl phosphate layers. Most of the Vanadium is present as V4+ ions in tetrahedral co-ordination. Vanadium n-propylamino phosphate catalyses Octahydroquinazolinone synthesis more effeciently and the optimum conditions required for Octahydroquinazolinone synthesis are, Benzaldehyde (2 mmol, Dimedone (2 mmol, Urea (4 mmol, Methanol + Water (1:1, 5 mL and Catalyst (0.05 g. A plausible mechanism is also proposed.

  19. New Dilated LMI Characterization for the Multiobjective Full-Order Dynamic Output Feedback Synthesis Problem

    Directory of Open Access Journals (Sweden)

    Zrida Jalel

    2010-01-01

    Full Text Available This paper introduces new dilated LMI conditions for continuous-time linear systems which not only characterize stability and performance specifications, but also, performance specifications. These new conditions offer, in addition to new analysis tools, synthesis procedures that have the advantages of keeping the controller parameters independent of the Lyapunov matrix and offering supplementary degrees of freedom. The impact of such advantages is great on the multiobjective full-order dynamic output feedback control problem as the obtained dilated LMI conditions always encompass the standard ones. It follows that much less conservatism is possible in comparison to the currently used standard LMI based synthesis procedures. A numerical simulation, based on an empirically abridged search procedure, is presented and shows the advantage of the proposed synthesis methods.

  20. Refined Synthesis and Characterization of Controlled Diameter, Narrow Size Distribution Microparticles for Aerospace Research Applications

    Science.gov (United States)

    Tiemsin, Pacita I.; Wohl, Christopher J.

    2012-01-01

    Flow visualization using polystyrene microspheres (PSL)s has enabled researchers to learn a tremendous amount of information via particle based diagnostic techniques. To better accommodate wind tunnel researchers needs, PSL synthesis via dispersion polymerization has been carried out at NASA Langley Research Center since the late 1980s. When utilizing seed material for flow visualization, size and size distribution are of paramount importance. Therefore, the work described here focused on further refinement of PSL synthesis and characterization. Through controlled variation of synthetic conditions (chemical concentrations, solution stirring speed, temperature, etc.) a robust, controllable procedure was developed. The relationship between particle size and salt concentration, MgSO4, was identified enabling the determination of PSL diameters a priori. Suggestions of future topics related to PSL synthesis, stability, and size variation are also described.