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Sample records for metal complex preparation

  1. Preparation and Characterization of Double Metal Cyanide Complex Catalysts

    Weilin Guo

    2003-01-01

    Full Text Available A series of double metal cyanide (DMC complex catalysts were prepared in two different methods by using ß-cyclodextrin, PEG-1000 and Tween-60 as an additional complex ligands respectively. It was showed that a mixture of crystalline and amorphous DMC was synthesized by using traditional method in which the additional complex ligand was added after the precipitation of DMC. Amorphous and dispersed DMC with higher activity could be obtained when the additional complex ligand was added in the reactant solution before reaction. The effect of additional complex ligand and preparation method on the crystalline state and catalytic property of DMC were also investigated.

  2. Metal-isonitrile adducts for preparing radionuclide complexes

    Carpenter, A.P.; Linder, K.E.; Maheu, L.J.; Patz, M.A.; Thompson, J.S.; Tulip, T.H.; Subramanyam, V.

    1988-01-01

    An method for preparing a coordination complex of isonitrile ligand and a radioisotope of Te, Ru, Co, Pt, Re, Os, Ir, W, Re, Cr, Mo, Mn, Ni, Rh, Nb and Ta from a non-radioactive metal adduct of the isonitrile

  3. Preparation of Palladium-Impregnated Ceria by Metal Complex Decomposition for Methane Steam Reforming Catalysis

    Worawat Wattanathana

    2017-01-01

    Full Text Available Palladium-impregnated ceria materials were successfully prepared via an integrated procedure between a metal complex decomposition method and a microwave-assisted wetness impregnation. Firstly, ceria (CeO2 powders were synthesized by thermal decomposition of cerium(III complexes prepared by using cerium(III nitrate or cerium(III chloride as a metal source to form a metal complex precursor with triethanolamine or benzoxazine dimer as an organic ligand. Palladium(II nitrate was consequently introduced to the preformed ceria materials using wetness impregnation while applying microwave irradiation to assist dispersion of the dopant. The palladium-impregnated ceria materials were obtained by calcination under reduced atmosphere of 10% H2 in He stream at 700°C for 2 h. Characterization of the palladium-impregnated ceria materials reveals the influences of the metal complex precursors on the properties of the obtained materials. Interestingly, the palladium-impregnated ceria prepared from the cerium(III-benzoxazine dimer complex revealed significantly higher BET specific surface area and higher content of the more active Pdδ+ (δ > 2 species than the materials prepared from cerium(III-triethanolamine complexes. Consequently, it exhibited the most efficient catalytic activity in the methane steam reforming reaction. By optimization of the metal complex precursors, characteristics of the obtained palladium-impregnated ceria catalysts can be modified and hence influence the catalytic activity.

  4. Preparation and characterisation of some transition metal complexes of niacinamide (vitamin b3)

    Hasan, M.M.; Hossain, M.E.; Halim, M.E.

    2015-01-01

    Niacinamide forms metal complexes of general formula (M(C/sub 6/H/sub 6/N/sub 2/O)2)Cl/sub 2/; where M = Mn(II), Co(II), Ni(II), Cu(II) and Zn(II) in the aqueous medium. The complexes were formulated by comparing the experimental and calculated data for C, H, N and metal. The prepared complexes were characterized by different physicochemical methods. The UV-vis, FTIR spectral analysis and thermo gravimetric analysis (TGA). TGA of these complexes have been discussed. Magnetic susceptibility values indicate that all complexes except Zn complex are paramagnetic in nature. The redox properties of the metal ions in the Mn, Cu and Zn complexes have been discussed from the cyclic voltammetric studies. In all cases the systems are quasi reversible. (author)

  5. Preparation and Characterization of Styrene Bearing Diethanolamine Side Group, Styrene Copolymer Systems, and Their Metal Complexes

    Aslışah Açıkses

    2018-01-01

    Full Text Available The two copolymer systems of styrene bearing diethanol amine side group and styrene were prepared by free radical polymerization method at 60°C in presence of 1,4-dioxane as solvent and AIBN as initiator. Their metal complexes were prepared by reaction of the copolymer used as ligand P(DEAMSt-co-StL′′ and Ni(II and Co(II metal ions, which was carried out in presence of ethanol and NaOH at 65°C for 48 h in pH = 7.5. The structures of the copolymers used as ligand and metal complexes were identified by FT-IR, 1H-NMR spectra, and elemental analysis. The properties of the copolymers used as ligand and metal complexes were characterized by SEM-EDX, AAS, DSC, TGA, and DTA techniques. Then, the electrical properties of the copolymers and metal complexes were examined as a function of the temperature and frequency, and the activation energies (Ea were estimated with conductivity measurements.

  6. Ultrafine yttria-stabilized zirconia powders prepared by pyrolysis of a metal-oxalate-cellulose complex

    Solov`eva, L.V.; Bashmakov, I.A.; Kaputskii, F.N. [Research Institute of Physicochemical Problems, Minsk (Belarus)] [and others

    1995-12-01

    Preparation of high-purity submicron powders with uniform particles is a key stage in the fabrication of high-quality ceramics. For this purpose, chemical methods are commonly used. Recently, pyrolysis of salt-cellulose compositions has gained acceptance for the preparation of mixed oxide powders. This method ensures control of the morphology and particle size of the resultant powders. In this work, the authors present an environmentally safe method for preparing ZrO{sub 2}-based powders from metal-oxalate-cellulose complexes (MOCC) used as precursors instead of soluble metal salts physisorbed on the cellulose surface. The powders obtained by this method feature higher dispersity than their commercially available analogs.

  7. Preparation and properties of chitosan-metal complex: Some factors influencing the adsorption capacity for dyes in aqueous solution.

    Rashid, Sadia; Shen, Chensi; Yang, Jing; Liu, Jianshe; Li, Jing

    2018-04-01

    Chitosan-metal complexes have been widely studied in wastewater treatment, but there are still various factors in complex preparation which are collectively responsible for improving the adsorption capacity need to be further studied. Thus, this study investigates the factors affecting the adsorption ability of chitosan-metal complex adsorbents, including various kinds of metal centers, different metal salts and crosslinking degree. The results show that the chitosan-Fe(III) complex prepared by sulfate salts exhibited the best adsorption efficiency (100%) for various dyes in very short time duration (10min), and its maximum adsorption capacity achieved 349.22mg/g. The anion of the metal salt which was used in preparation played an important role to enhance the adsorption ability of chitosan-metal complex. SO 4 2- ions not only had the effect of crosslinking through electrostatic interaction with amine group of chitosan polymer, but also could facilitate the chelation of metal ions with chitosan polymer during the synthesis process. Additionally, the pH sensitivity and the sensitivity of ionic environment for chitosan-metal complex were analyzed. We hope that these factors affecting the adsorption of the chitosan-metal complex can help not only in optimizing its use but also in designing new chitosan-metal based complexes. Copyright © 2017. Published by Elsevier B.V.

  8. The preparation and use of metal salen complexes derived from cyclobutane diamine

    Patil, Smita

    The helix is an important chiral motif in nature, there is increasing development in field of helical transition metal complexes and related supramolecular structures. Hence, the goals of this work are to apply the principles of helicity in order to produce metal complexes with predictable molecular shapes and to study their properties as asymmetric catalysts. Computational studies suggest that the (1R,2 R)-cyclobutyldiamine unit can produce highly twisted salen complexes with a large energy barrier between the M and P helical forms. To test this prediction, the tartrate salt of (1R,2R)-cyclobutyldiamine was synthesized and condensed with a series of saliclaldehydes to produce novel salen ligands. The salicylaldehydes chosen have extended phenanthryl or benz[a]anthryl sidearms to encourage formation of helical coordination complexes. These ligands were metallated with zinc, iron and manganese salts to produce salen metal complexes which were characterized by NMR analysis, high-resolution mass spectrometry, and IR spectroscopy. A second ligand type, neutral bis(pyridine-imine) has also been synthesized from (1R,2R)-cyclobutyldiamine and quinolylaldehydes. The synthesis of bis(pyridine-imine) ligands was conducted using greener method, solvent assisted grinding. These ligands, in-situ with nickel metal salts, showed good catalytic activity for asymmetric Diels-Alder reactions. The third ligand type studied was chiral acid-functionalized Schiff-base ligands. These were synthesized by the condensation of 3-formyl-5-methyl salicylic acid and (1R,2R)-cyclobutyldiamine. With this type of ligand, there is possibility of producing both mono and dinuclear metal complexes. In our studies, we were only able to synthesize mononuclear complexs. These were tested as catalysts for asymmetric direct Mannich-type reaction, but were found to be ineffective.

  9. Preparation, structure and microbial evaluation of metal complexes of the second generation quinolone antibacterial drug lomefloxacin

    Sadeek, Sadeek A.; El-Shwiniy, Walaa H.

    2010-09-01

    Lomefloxacinate of Y(III), Zr(IV) and U(VI) were isolated as solids with the general formula; [Y(LFX) 2Cl 2]Cl·12H 2O, [ZrO(LFX) 2Cl]Cl·15H 2O and [UO 2(LFX) 3](NO 3) 2·4H 2O. The new synthesized complexes were characterized with physicochemical and diverse spectroscopic techniques (IR, UV-Vis. and 1H NMR spectroscopies) as well as thermal analyses. In these complexes lomefloxacin act as bidentate ligand bound to the metal ions through the pyridone oxygen and one carboxylate oxygen. The kinetic parameters of thermogravimetric (TGA) and its differential (DTG), such as entropy of activation, activation energy, enthalpy of activation and Gibbs free energy evaluated by using Coats- Redfern and Horowitz- Metzger equations for free lomefloxacin and three complexes were carried out. The bond stretching force constant and length of the U dbnd O bond for the [UO 2(LFX) 3](NO 3) 2·4H 2O complex were calculated. The antimicrobial activity of lomefloxacin and its metal complexes was tested against different bacterial species, such as Staphylococcus aureus ( S. aureus), Escherichia coli ( E. coli) and Pseudomonas aeruginosa ( P. aeruginosa) as Gram-positive and Gram-negative bacterial species and also against two species of antifungal, penicillium ( P. rotatum) and trichoderma ( T. sp.). The three complexes are of a good action against three bacterial species but the Y(III) complex exhibit excellent activity against Pseudomonas aeruginosa ( P. aeruginosa), when compared to the free lomefloxacin.

  10. Complexation-Induced Phase Separation: Preparation of Metal-Rich Polymeric Membranes

    Villalobos Vazquez de la Parra, Luis Francisco

    2017-08-01

    The majority of state-of-the-art polymeric membranes for industrial or medical applications are fabricated by phase inversion. Complexation induced phase separation (CIPS)—a surprising variation of this well-known process—allows direct fabrication of hybrid membranes in existing facilities. In the CIPS process, a first step forms the thin metal-rich selective layer of the membrane, and a succeeding step the porous support. Precipitation of the selective layer takes place in the same solvent used to dissolve the polymer and is induced by a small concentration of metal ions. These ions form metal-coordination-based crosslinks leading to the formation of a solid skin floating on top of the liquid polymer film. A subsequent precipitation in a nonsolvent bath leads to the formation of the porous support structure. Forming the dense layer and porous support by different mechanisms while maintaining the simplicity of a phase inversion process, results in unprecedented control over the final structure of the membrane. The thickness and morphology of the dense layer as well as the porosity of the support can be controlled over a wide range by manipulating simple process parameters. CIPS facilitates control over (i) the thickness of the dense layer throughout several orders of magnitude—from less than 15 nm to more than 6 μm, (ii) the type and amount of metal ions loaded in the dense layer, (iii) the morphology of the membrane surface, and (iv) the porosity and structure of the support. The nature of the CIPS process facilitates a precise loading of a high concentration of metal ions that are located in only the top layer of the membrane. Moreover, these metal ions can be converted—during the membrane fabrication process—to nanoparticles or crystals. This simple method opens up fascinating possibilities for the fabrication of metal-rich polymeric membranes with a new set of properties. This dissertation describes the process in depth and explores promising

  11. Complexation-Induced Phase Separation: Preparation of Metal-Rich Polymeric Membranes

    Villalobos, Luis Francisco

    2017-01-01

    The majority of state-of-the-art polymeric membranes for industrial or medical applications are fabricated by phase inversion. Complexation induced phase separation (CIPS)—a surprising variation of this well-known process—allows direct fabrication

  12. Conducting metal dithiolate complexes

    Underhill, A. E.; Ahmad, M. M.; Turner, D. J.

    1985-01-01

    Further work on the chemical composition of the one-dimensional metallic metal dithiolene complex Li-Pt(mnt) is reported. The electrical conduction and thermopower properties of the nickel and palladium complexes are reported and compared with those of the platinum compound......Further work on the chemical composition of the one-dimensional metallic metal dithiolene complex Li-Pt(mnt) is reported. The electrical conduction and thermopower properties of the nickel and palladium complexes are reported and compared with those of the platinum compound...

  13. Oligocyclopentadienyl transition metal complexes

    de Azevedo, Cristina G.; Vollhardt, K. Peter C.

    2002-01-18

    Synthesis, characterization, and reactivity studies of oligocyclopentadienyl transition metal complexes, namely those of fulvalene, tercyclopentadienyl, quatercyclopentadienyl, and pentacyclopentadienyl(cyclopentadienyl) are the subject of this account. Thermal-, photo-, and redox chemistries of homo- and heteropolynuclear complexes are described.

  14. Preparation of titanium oxide and metal titanates as powders, thin films, and microspheres by complex sol-gel process

    Deptula, A.; Olczak, T.; Lada, W.; Chmielewski, A.G.; Jakubaszek, U.; Sartowska, B.; Goretta, K.C.; Alvani, C.; Casadio, S.; Contini, V.

    2006-01-01

    Titanium oxide, for many years an important pigment, has recently been applied widely as a photocatalyst or as supports for metallic catalysts, gas sensors, photovoltaic solar cells, and water and air purification devices. Titanium oxide (TiO 2 ) and titanates based on Ba, Sr and Ca were prepared from commercial solutions of TiCl 4 and HNO 3 . The main preparation steps for the sols consisted of elimination of Cl - by distillation with HNO 3 and addition of metal hydroxides for the titanates. Resulting sols were gelled and used to: (a) prepare irregularly shaped powders by evaporation; (b) produce by a dipping technique thin films on glass, Ag or Ti supports; (c) produce spherical powders (diameters <100 μm) by solvent extraction. Results of thermal and X-ray-diffraction analyses indicated that the temperatures required to form the various compounds were lower than those necessary to form the compounds by conventional solid-state reactions and comparable to those required with use of organometallic based sol-gel methods. Temperatures of formation could be further reduced by addition of ascorbic acid (ASC) to the sols

  15. Complexation induced phase separation: preparation of composite membranes with a nanometer thin dense skin loaded with metal ions

    Villalobos Vazquez de la Parra, Luis Francisco

    2015-04-21

    We present the development of a facile phase-inversion method for forming asymmetric membranes with a precise high metal ion loading capacity in only the dense layer. The approach combines the use of macromolecule-metal intermolecular complexes to form the dense layer of asymmetric membranes with nonsolvent-induced phase separation to form the porous support. This allows the independent optimization of both the dense layer and porous support while maintaining the simplicity of a phase-inversion process. Moreover, it facilitates control over (i) the thickness of the dense layer throughout several orders of magnitude—from less than 15 nm to more than 6 μm, (ii) the type and amount of metal ions loaded in the dense layer, (iii) the morphology of the membrane surface, and (iv) the porosity and structure of the support. This simple and scalable process provides a new platform for building multifunctional membranes with a high loading of well-dispersed metal ions in the dense layer.

  16. Complexation induced phase separation: preparation of composite membranes with a nanometer thin dense skin loaded with metal ions

    Villalobos Vazquez de la Parra, Luis Francisco; Karunakaran, Madhavan; Peinemann, Klaus-Viktor

    2015-01-01

    We present the development of a facile phase-inversion method for forming asymmetric membranes with a precise high metal ion loading capacity in only the dense layer. The approach combines the use of macromolecule-metal intermolecular complexes to form the dense layer of asymmetric membranes with nonsolvent-induced phase separation to form the porous support. This allows the independent optimization of both the dense layer and porous support while maintaining the simplicity of a phase-inversion process. Moreover, it facilitates control over (i) the thickness of the dense layer throughout several orders of magnitude—from less than 15 nm to more than 6 μm, (ii) the type and amount of metal ions loaded in the dense layer, (iii) the morphology of the membrane surface, and (iv) the porosity and structure of the support. This simple and scalable process provides a new platform for building multifunctional membranes with a high loading of well-dispersed metal ions in the dense layer.

  17. New polymer-supported ion-complexing agents: Design, preparation and metal ion affinities of immobilized ligands

    Alexandratos, Spiro D.

    2007-01-01

    Polymer-supported reagents are comprised of crosslinked polymer networks that have been modified with ligands capable of selective metal ion complexation. Applications of these polymers are in environmental remediation, ion chromatography, sensor technology, and hydrometallurgy. Bifunctional polymers with diphosphonate/sulfonate ligands have a high selectivity for actinide ions. The distribution coefficient for the uranyl ion from 1 M nitric acid is 70,000, compared to 900 for the monophosphonate/sulfonate polymer and 200 for the sulfonic acid ion-exchange resin. A bifunctional trihexyl/triethylammonium polymer has a high affinity and selectivity for pertechnetate and perchlorate anions from groundwater. In one example, its distribution coefficient for perchlorate ions in the presence of competing anions is 3,300,000, compared to 203,180 for a commercially available anion-exchange resin. Polystyrene modified with N-methyl-D-glucamine ligands is capable of selectively complexing arsenate from groundwater. It complexes 99% of the arsenate present in a solution of 100 mg/L arsenate with 560 mg/L sulfate ions. Its selectivity is retained even in the presence of 400 mg/L phosphate. There is no affinity for arsenate above pH 9, allowing for the polymer to be regenerated with moderate alkali solution. In studies aimed at developing a Hg(II)-selective resin, simple amine resins were found to have a high Hg(II) affinity and that affinity is dependent upon the solution pH and the counterion

  18. Magnesium oxide prepared via metal-chitosan complexation method: Application as catalyst for transesterification of soybean oil and catalyst deactivation studies

    Almerindo, Gizelle I.; Probst, Luiz F. D.; Campos, Carlos E. M.; de Almeida, Rusiene M.; Meneghetti, Simoni M. P.; Meneghetti, Mario R.; Clacens, Jean-Marc; Fajardo, Humberto V.

    2011-10-01

    A simple method to prepare magnesium oxide catalysts for biodiesel production by transesterification reaction of soybean oil with ethanol is proposed. The method was developed using a metal-chitosan complex. Compared to the commercial oxide, the proposed catalysts displayed higher surface area and basicity values, leading to higher yield in terms of fatty acid ethyl esters (biodiesel). The deactivation of the catalyst due to contact with CO2 and H2O present in the ambient air was verified. It was confirmed that the active catalytic site is a hydrogenocarbonate adsorption site.

  19. Selenophene transition metal complexes

    White, Carter James [Iowa State Univ., Ames, IA (United States)

    1994-07-27

    This research shows that selenophene transition metal complexes have a chemistry that is similar to their thiophene analogs. Selenophene coordination has been demonstrated and confirmed by molecular structure in both the η5- and the η1(Se)-coordination modes. The reaction chemistry of selenophene complexes closely resembles that of the analogous thiophene complexes. One major difference, however, is that selenophene is a better donor ligand than thiophene making the selenophene complexes more stable than the corresponding thiophene complexes. The 77Se NMR chemical shift values for selenophene complexes fall within distinct regions primarily depending on the coordination mode of the selenophene ligand. In the final paper, the C-H bond activation of η1(S)-bound thiophenes, η1(S)-benzothiophene and η1(Se)-bound selenophenes has been demonstrated. The deprotonation and rearrangement of the η1(E)-bound ligand to the carbon bound L-yl complex readily occurs in the presence of base. Reprotonation with a strong acid gives a carbene complex that is unreactive towards nucleophilic attack at the carbene carbon and is stable towards exposure to air. The molecular structure of [Cp(NO)(PPh3)Re(2-benzothioenylcarbene)]O3SCF3 was determined and contains a Re-C bond with substantial double bond character. Methyl substitution for the thienylcarbene or selenylcarbene gives a carbene that rearranges thermally to give back the η1(E)-bound complex. Based on these model reactions, a new mechanism for the H/D exchange of thiophene over the hydrodesulfurization catalyst has been proposed.

  20. Preparative Radiation Chemistry of Transition Metal Complexes; Radiosynthese de complexes de metaux de transition; Radiatsionno-khimicheskij sintez kompleksnykh soedinenij perekhodnykh metallov; Radiosintesis de complejos de los metales de transicion

    Gustorf, E. Koerner Von; Jun, M. -J.; Koller, H.; Schenck, G. O. [Max-Planck-Institut fuer Kohlenforschung, Abteilung Strahlenchemie, Muelheim-Ruhr, Federal Republic of Germany (Germany)

    1963-11-15

    {pi}-complexes and carbonyl compounds of transition metals have a technical importance because of their special reactivity and catalytic activity. The following investigations have been made by us: 1. Radiation chemical synthesis of transition metal {pi}- complexes Examples are the preparation of maleic-acid-anhydride-iron-tetracarbonyl, fumaric-acid-dimethylesteriron- tetracarbonyl, methacrylic-acid-methylester-iron-tetracarbonyl, vinylacetate-iron-tetiacarbonyl, etc. by Co{sup 60} {gamma}-irradiation of Fe(CO){sub 5} and the corresponding unsaturated compounds. 2. Chemical reactions with radiation-chemically formed {pi}-complexes Examples are the polymerization of vinyl compounds at room temperature by the action of organic halogen compounds on complexes such as methacryl-acid-methylester-iron-tetracarbonyl, vinylacetate-iron- tetracarbonyl, etc. 3. Synthesis of {pi}-complexes and carbonyl compounds of transition metals by irradiation Examples are the Co{sup 60} {gamma}-irradiation of [(C{sub 5}H{sub 5}){sub 2}Fe], [(C{sub 5}H{sub 5}){sub 2N}i], CH{sub 3}C{sub 5}H{sub 4}Mn(CO){sub 3}, (C{sub 5}H{sub 5})TiCl{sub 2},Fe(CO){sub 5}, Ni(CO){sub 4} , in halogen hydrocarbons. (author) [French] Les complexes {pi} et les composes carbonyles des metaux de transition ont une importance du point de vue technique en raison de leur reactivite speciale et de leur activite catalytique. L'auteur a fait des experiences sur les questions suivantes: 1. Radiosynthese de complexes {pi} de metaux de transition. Exemple: preparation d'anhydride maleique-fer tetracarbonyle, de fumarate de dimethyle-fer tetracarbonyle, de methacrylate de methyle-fer tetracarbonyl, d'acetate de vinyle-fer tetracarbonyle, etc., par exposition de Fe(CO){sub 5} et des composes non satures correspondant aux rayons gamma du cobalt-60. 2. Reactions chimiques avec des complexes n formes par voie radiochimique. Exemple: polymerisation de composes vinyliques a temperature ambiante en presence de composes organiques

  1. METAL COMPLEXES OF SALICYLHYDROXAMIC ACID AND 1,10 ...

    Preferred Customer

    Metal complexes which are formed in biological systems between a ligand and a metal ion are in dynamic ... In a continuation of our research work oriented towards studying the .... Antimicrobial activity techniques. Preparation of test samples.

  2. Complex metal hydrides

    Ley, Morten Brix

    2014-01-01

    og batterier de to mest lovende energibærere til mobile applikationer. Komplekse metalhydrider er blevet undersøgt i vid udstrækning over de sidste tyve år, siden de gravimetrisk og volumetrisk kan indeholde store mængder brint. Derfor er metal borhydrider velegnet til faststofopbevaring af brint...

  3. Cell complexes of transition metals in biochemistry and medicine

    Voloshin, Ya.Z.; Varzatskij, O.A.; Bubnov, Yu.N.

    2007-01-01

    Basic directions and prospects of use of cell complexes of transition metals in medicine and biochemistry are considered: incapsulation of radioactive metal ions for radiotherapy and diagnostics; preparation of contrast compounds for magnetic resonance tomography, antidotes and pharmaceutical preparation of prolonged effect, preparations for boron-neutron-capture therapy of neoplasms, antioxidants; membrane transport of metal ions; study of interaction of cell metal complexes with nucleic acids; possibility of use of self-assembly of cell complexes for imitation of ligases and use of clathrochelates as linkers; design of inhibitors of viruses for AIDS therapy [ru

  4. benzimidazole metal complexes

    aUnité de Recherche de Chimie de l'Environnement et Moléculaire Structurale, Université des Frères. Mentouri .... determine the quantum chemical parameters for the title ..... retical study of benzazole thioether and its zinc complex.

  5. Application of preparations on the basis of a metal complex for the production of a contrast medium for utilization in tomo-densitometry

    Dietlin, F.; Heitz, F.

    1994-01-01

    The present invention relates to measurements by tomo-densitometry. It relates in particular to compositions usable in tomo-densitometry which are comprised of a solution consisting at least of a salt or a complex of metal of which the atomic weight is comprised between 24 and 66 associated with an appropriate solvent or vehicle

  6. Carbonic anhydrase inhibitors. A general approach for the preparation of water-soluble sulfonamides incorporating polyamino-polycarboxylate tails and of their metal complexes possessing long-lasting, topical intraocular pressure-lowering properties.

    Scozzafava, Andrea; Menabuoni, Luca; Mincione, Francesco; Supuran, Claudiu T

    2002-03-28

    Reaction of polyamino-polycarboxylic acids or their dianhydrides with aromatic/heterocyclic sulfonamides possessing a free amino/imino/hydrazino/hydroxy group afforded mono- and bis-sulfonamides containing polyamino-polycarboxylic acid moieties in their molecule. The acids/anhydrides used in synthesis included IDA, NTA, EDDA, EDTA and EDTA dianhydride, DTPA and DTPA dianhydride, EGTA and EGTA dianhydride, and EDDHA, among others. All the newly prepared derivatives showed strong affinity toward isozymes I, II, and IV of carbonic anhydrase (CA). Metal complexes of the new compounds have also been prepared. Metal ions used in such preparations included di- and trivalent main-group and transition cations, such as Zn(II), Cu(II), Al(III), etc. Some of the new sulfonamides/disulfonamides obtained in this way, as well as their metal complexes, behaved as nanomolar CA inhibitors against isozymes II and IV, being slightly less effective in inhibiting isozyme I. Some of these sulfonamides as well as their metal complexes strongly lowered intraocular pressure (IOP) when applied topically, directly into the normotensive/glaucomatous rabbit eye, as 1-2% water solutions/suspensions. The good water solubility of these sulfonamide CA inhibitors, correlated with the neutral pH of their water solutions used in the ophthalmologic applications and the long duration of action of the IOP-lowering effect, makes them interesting candidates for developing novel types of antiglaucoma drugs devoid of serious topical side effects.

  7. Metal complex derivatives of hydrogen uranyl phosphate

    Grohol, D.; Blinn, E.L.

    1994-01-01

    Derivatives of hydrogen uranyl phosphate were prepared by incorporating transition metal complexes into the uranyl phosphate matrix. The transition metal complexes employed include bis(ethylenediamine)copper(II), bis(1,3-propanediamine)copper(II) chloride, (triethylenetetramine)copper(II), (1,4,8,11-tetraazacyclotetradecane)copper(II), (1,4,8,12-tetraazacyclopentadecane)copper(II), (1,4,8,11-tetraazacyclotetradecane)nickel(II) chloride, (triethylenetetramine)nickel(II) and others. The chemical analyses of these derivatives indicated that the incorporation of the transition metal complexes into the uranyl phosphate matrix via ion exchange was not stoichiometric. The extent of ion exchange is dependent on the size and structure of the transition metal complex. All complexes were characterized by X-ray powder diffractometry, electronic and infrared spectra, thermal analyses and chemical analysis. An attempt was made to correlate the degree of quenching of the luminescence of the uranyl ion to the spacing between the uranyl phosphate layers in the derivatives

  8. Transition Metal Complexes and Catalysis

    approaches towards the study of bonding in transition metal complexes. Despite .... industrial scale reactions for the production of organic compounds using transition ..... It has found several applications as an engineering thermoplastic. .... and processes of interest to the company, that is, applied research. It is this very ...

  9. Metal complexes with 5-aminotetrazole

    Lavrenova, L.G.; Larionov, S.V.; Grankina, Z.A.; Ikorskij, V.N.

    1983-01-01

    Nitrate and chloride complexes of Co(2), Ni(2), Cu(2), Cd(2), Hg(2), Pb(2) with 5 aminotetrazole (ATE) and compoUnds Zn(ATE') 2 and Cd(ATEE') 2 , where ATE' is a 5 aminotetrazole ano /nion. On the base of spectroscopic data (spectrophotometry, IR- spectra, EPR and magnetic measurements assumptions on M(2) coordination in complexes are made. Most probably ATE is a bridge ligand which is joined by two nitrogen atoms to various M(2) ions. In Co(2), Ni(2) and Cu(ATE) 3 -Cl 2 compounds the metal has a distorted actahedral coordination and forms MN 6 unit, which suggests the interaction of metal ions with ATE nitrogen atoms along the Z-axis. In the Cu(ATE) 2 (NO 3 ) 2 octahedral complex the CuN 4 O 2 coordination unit is realized at the expense of participation of nitratogroups in coordination

  10. PROCESS FOR PREPARING URANIUM METAL

    Prescott, C.H. Jr.; Reynolds, F.L.

    1959-01-13

    A process is presented for producing oxygen-free uranium metal comprising contacting iodine vapor with crude uranium in a reaction zone maintained at 400 to 800 C to produce a vaporous mixture of UI/sub 4/ and iodine. Also disposed within the maction zone is a tungsten filament which is heated to about 1600 C. The UI/sub 4/, upon contacting the hot filament, is decomposed to molten uranium substantially free of oxygen.

  11. PREPARATION OF OXOPORPHINATOMANGANESE (IV) COMPLEX

    Willner, I.; Otvos, J.; Calvin, M.

    1980-07-01

    Oxo-manganese-tetraphenylporphyrin (O=Mn{sup IV}-TPP) has been prepared by an oxygen-transfer reaction from iodosylbenzene to MnIITPP and characterized by its i.r. and field desorption mass spectra, which are identical to those of the product obtained by direct oxidation of Mn{sup III}(TPP) in an aqueous medium; it transfers oxygen to triphenylphosphine to produce triphenylphosphine oxide, and it is suggested that similar intermediates are important in oxygen activation by cytochrome P-450 as well as in the photosynthetic evolution of oxygen.

  12. Sample preparation and characterization of technetium metal

    Minato, Kazuo; Serizawa, Hiroyuki; Fukuda, Kousaku; Itoh, Mitsuo

    1997-10-01

    Technetium-99 is a long-lived fission product with a half-life of about 2.1 x 10 5 years, which decays by β-emission. For the transmutation of 99 Tc, research on solid technetium was started. Technetium metal powder purchased was analyzed by X-ray diffraction, γ-ray spectrometry, and inductively coupled plasma-atomic emission spectrometry and -mass spectrometry. The lattice parameters obtained were agreed with the reported values. The metallic impurity was about 15 ppm, where aluminum and iron contributed mainly. No impurity nuclide with γ-emission was found. Using the technetium metal powder, button-, rod-, and disk-shaped samples of technetium metal were prepared by arc-melting technique. Thermal diffusivity of technetium metal was measured on a disk sample from room temperature to 1173 K by laser flash method. The thermal diffusivity decreased with increasing temperature though it was almost constant above 600 K. (author)

  13. TDPAC studies on metal-complex ferrimagnets

    Ohkubo, Yoshitaka [Kyoto Univ., Kumatori, Osaka (Japan). Research Reactor Inst.; Abe, Shizuko; Okada, Takuya [and others

    1997-03-01

    TDPAC spectra of {sup 117}In (left-arrow {sup 117}Cd) and {sup 111}Cd (left-arrow {sup 111m}Cd) in the mixed metal complex N(C{sub 4}H{sub 9}){sub 4}(M(II)Fe(III)(C{sub 2}O{sub 4}){sub 3})(M=Fe,Ni), the related substraces and LiNbO{sub 3} have been studied. In this paper, pure potassium iron (III) oxalate was prepared and mixed metal complexes were synthesized by changing amount of reagents and the order added, then observed by TDPAC. 2 mol%Cd was dispersed throughout potassium iron oxalate and potassium nickel oxalate, formulating M(II){sub 0.98}Cd(II){sub 0.02}C{sub 2}O{sub 4}{center_dot}2H{sub 2}O (M=Fe, Ni) with the same crystal structure. The formation reaction of mixed metal complex-Fe(II) was faster than that of iron oxalate. Its mixed metal complex-Ni(II) was slower than that of iron oxalate. The rate of quadrupole oscillation was obtained by {omega}{sub Q}({sup 117}In)=67.3 Mrad/s and {omega}{sub Q}({sup 111}Cd)=29.7 Mrad/s of which values were determined by TDPAC spectra of {sup 117}In and {sup 111}Cd in LiNbO{sub 3} at 4K. The value showed pure ion bond of oxygen coordinated with {sup 117}In and {sup 111}Cd. 0.08 {eta} was determined by TDPAC spectrum of {sup 111}Cd(left-arrow {sup 111m}Cd). The rate of {omega}{sub Q} of mixed metal oxalate complex was larger than 2.3, indicating 5s and 5p orbital electron took part in bond of oxygen of oxalic acid or approaching oxygen ion to In nucleus depend on the structual relaxation in decaying of {sup 117}In(left-arrow {sup 117}Cd). (S.Y.)

  14. Synthesis, characterization and biological profile of metal and azo-metal complexes of embelin

    R. Aravindhan

    2014-12-01

    Full Text Available The present study emphasizes synthesis and bioprofiling of embelin, embelin-metal (EM and embelin-azo-metal (EAM complexes in detail. EM complexes were prepared using pure embelin and d-block transition elements, namely Mn, Fe, Co, Ni, Cu, and Zn. Similarly, EAM complexes were synthesized using phenyl azo-embelin with the said transition metals. Embelin, EM, and EAM complexes were subjected to ultra violet visible spectroscopy, Fourier transform infrared spectroscopy, nuclear magnetic resonance, electrospray ionization mass spectrometry, thermogravimetric analysis, carbon hydrogen nitrogen sulfur analysis. With regard to bioprofiling, the test complexes were studied for the antioxidant and antimicrobial activities. Results revealed that the prepared EM and EAM complexes form octahedral complexes with embelin with the yield in the range of 45–75%. All the instrumental analyses authenticate the interaction of metals with bidentate embelin through its enolic and quinonic oxygen atoms as [M(Emb2(H2O2]H2O and [M(Emb-Azo2(H2O2]. The antioxidant profile studies suggested that upon complexation with metals, the free radical scavenging activity of embelin reduced significantly. But, with regard to antimicrobial activity, cobalt and nickel embelin complexes displayed>80% growth inhibition in comparison with embelin alone. The hemolytic activity studies suggested that both embelin and the metal complexes are non-hemolytic. The reason for the reduction in antioxidant and an increase in antimicrobial activities were discussed in detail.

  15. A procedure for preparing alkali metal hydrides

    Lemieux, R.U.; Sanford, C.E.; Prescott, J.F.

    1976-01-01

    A plain low cost, procedure for the continuous, low temperature preparation of sodium or potassium hydrides using cheap reagents is presented. Said invention is especially concerned with a process of purifying of a catalytic exchange liquid used for deuterium enrichment, in which an alkali metal hydride is produced as intermediate product. The procedure for producing the sodium and potassium hydrides consists in causing high pressure hydrogen to be absorbed by a mixture of at least a lower monoalkylamine and an alkylamide of an alkali metal from at least one of said amines [fr

  16. Synthesis and photoluminescent properties of Sr{sub (1−x)}Si{sub 2}O{sub 2}N{sub 2}: xEu{sup 2+} phosphor prepared by polymer metal complex method for WLEDs applications

    Hassan, Dhia A., E-mail: dhia_hassan@yahoo.com [Department of Materials Science and Engineering, College of Materials, Xiamen University, Xiamen 361005 (China); Department of Chemistry, College of Education for Pure Science, University of Basrah, Basrah 61004 (Iraq); Xu, Jian; Chen, Yibin; Li, Langkai [Department of Materials Science and Engineering, College of Materials, Xiamen University, Xiamen 361005 (China); Zeng, Renjie, E-mail: rjzeng@xmu.edu.cn [Department of Materials Science and Engineering, College of Materials, Xiamen University, Xiamen 361005 (China); Fujian Key Lab of Advanced Special Materials, Xiamen University, Xiamen 361005 (China)

    2016-07-15

    Highlights: • SrSi{sub 2}O{sub 2}N{sub 2}: Eu{sup 2+} phosphor was prepared by polymer metal complex (pechini method). • The annealing time was decreased from 6 h in solid state method to 3 h. • The particles are crystalline and dispersed well with average size 6.5 μm. - Abstract: Green emitting Sr{sub (1−x)}Si{sub 2}O{sub 2}N{sub 2}: xEu{sup 2+} (x = 0, 0.02, 0.04, 0.06, 0.08 and 0.1) phosphors were synthesized by polymer metal complex or pechini method. The XRD results confirm the formation of a pure phase at 1400 °C for 3 h. The SEM and particles size results indicate that the prepared phosphor consists of a polyhedral crystalline shape with well dispersed and the average particle size around 6.5 μm. The maximum PL intensity was found at 0.04% Eu{sup 2+} with a wide emission band between 460 and 640 nm and a green emission peak at 531.4 nm. The external quantum efficiency of 0.04% Eu{sup 2+} sample was 43.13%. The results indicate that pechini method is an alternative way and close in efficiency to the solid state method to prepare SrSi{sub 2}O{sub 2}N{sub 2} phosphor with higher homogeneity and more uniform size distribution for near UV and blue region applications for white light emitting diodes WLEDs.

  17. Metallic complexes with glyphosate: a review

    Coutinho, Cláudia F. B.; Mazo, Luiz Henrique

    2005-01-01

    We present studies involving metallic ions and the herbicide glyphosate. The metallic complexes of Cu(II), Zn(II), Mn(II), Ni(II), Cd(II), Pb(II), Cr(III), Fe(III), Co(III), ammonium, sodium, Ag(I), alkaline earth metals and of some lanthanides ions are described. The complexes are discussed in terms of their synthesis, identification, stability and structural properties, based on data from the current literature.

  18. Metallic complexes with glyphosate: a review

    Coutinho, Claudia F.B.; Mazo, Luiz Henrique

    2005-01-01

    We present studies involving metallic ions and the herbicide glyphosate. The metallic complexes of Cu(II), Zn(II), Mn(II), Ni(II), Cd(II), Pb(II), Cr(III), Fe(III), Co(III), ammonium, sodium, Ag(I), alkaline earth metals and of some lanthanides ions are described. The complexes are discussed in terms of their synthesis, identification, stability and structural properties, based on data from the current literature. (author)

  19. Preparation of the pur uranium-metal

    Goldschmidt, B.; Vertes, P.

    1955-01-01

    A detailed description of the chemical processes used to prepare in the factory of Bouchet of the CEA (Seine-Et-Oise) pur metal uranium with either relatively rich ores, or extracts coming of physical or chemical treatment of poor ores. The nitric treatment of ores succeeds to the production of uranate of impure sodium carbonate. This last last product is dissolved in nitric acid and the uranyl nitrate is extracted by tributyl-phosphate diluted in an inert solvent. The uranyl nitrate pure is re-extracted and successively transformed in uranium peroxide, in orange oxide then in brown oxide which is transformed in fluoride by the anhydrous hydrofluoric acid. Uranate fluoride is then reduced in metal by the pure calcium with an yield superior to 99%. (authors) [fr

  20. Complexes of natural carbohydrates with metal cations

    Alekseev, Yurii E; Garnovskii, Alexander D; Zhdanov, Yu A

    1998-01-01

    Data on the interaction of natural carbohydrates (mono-, oligo-, and poly-saccharides, amino sugars, and natural organic acids of carbohydrate origin) with metal cations are surveyed and described systematically. The structural diversity of carbohydrate metal complexes, caused by some specific features of carbohydrates as ligands, is demonstrated. The influence of complex formation on the chemical properties of carbohydrates is discussed. It is shown that the formation of metal complexes plays an important role in the configurational and conformational analysis of carbohydrates. The practical significance of the coordination interaction in the series of carbohydrate ligands is demonstrated. The bibliography includes 571 references.

  1. Preparation and nucleation of spherical metallic droplet

    Bing-ge Zhao

    2015-03-01

    Full Text Available The preparation and solidification of metallic droplets attract more and more attention for their significance in both engineering and scientific fields. In this paper, the preparation and characterization of Sn-based alloy droplets using different methods such as atomization and consumable electrode direct current arc (CDCA technique are reviewed. The morphology and structure of these droplets were determined by optical microscopy, X-ray diffraction (XRD and scanning electron microscopy (SEM. The solidification behavior of single droplet was systematically studied by means of scanning calorimetry (DSC, and the nucleation kinetics was also calculated. In particular, the development of fast scanning calorimetry (FSC made it possible to investigate the evolution of undercooling under ultrafast but controllable heating and cooling conditions. The combination of CDCA technique and FSC measurements opens up a new door for quantitative studies on droplet solidification, which is accessible to demonstrate some theories by experiments.

  2. Preparation of oxide materials from metal alkoxides

    Turevskaya, E.P.; Turova, N.Ya.; Yanovskaya, M.I.

    2000-01-01

    The results of studies on the sol-gel technologies on the basis of alkoxides are presented. The synthesis and properties of titanates zirconates, niobates, tantalates, vanadates and solid solutions on the basis of Mo, W and Bi oxides, iron oxides and high-temperature superconductors are presented. The most important aspects, determining the choice of optimal conditions for preparation of oxides of concrete compositions with required properties are pointed out. Accomplishment of the whole chain of studies made it possible to synthesize a broad range of metal alkoxides and study their properties and also carry out large-scale studies on preparation of various oxides and materials on the basis thereof, using the source base of the sol-gel method [ru

  3. Preparation and electrochemical properties of core-shell carbon coated Mn-Sn complex metal oxide as anode materials for lithium-ion batteries

    Zhang, Ruixue; Fang, Guoqing; Liu, Weiwei; Xia, Bingbo; Sun, Hongdan; Zheng, Junwei; Li, Decheng

    2014-02-01

    In this study, we synthesized a carbon coated Mn-Sn metal oxide composite with core-shell structure (MTO@C) via a simple glucose hydrothermal reaction and subsequent carbonization approach. When the MTO@C composite was applied as an anode material for lithium-ion batteries, it maintained a reversible capacity of 409 mA h g-1 after 200 cycles at a current density of 100 mA g-1. The uniformed and continuous carbon layer formed on the MTO nanoparticles, effectively buffered the volumetric change of the active material and increased electronic conductivity, which thus prolonged the cycling performance of the MTO@C electrode.

  4. Pharmacologically significant tetraaza macrocyclic metal complexes ...

    MOHAMMAD SHAKIR

    2017-11-22

    Nov 22, 2017 ... structural biological models.6 Hence, biological prop- erties of ... poor water solubility, exhibits intrinsic resistance and ..... pdb). The metal complex files were drawn using. ChemDraw (MM2) and their energies were minimized.

  5. Preparation of significant complexes of selected transition elements with appropriate ligands

    Abbas, Hala Hassan

    2000-06-01

    New complexes of copper (II), nickel (II) and cobalt (II) have been prepared using triphenylphosphine and benzofurazan-1-oxide as ligands. Benzofurazan-1-oxide was prepared from the reaction between o-nitrophenyl azide and toluene as a catalyst. These complexes have been identified by means of infrared spectra and also melting points determination. The coordination bonding was found to be through phosphorus-metal and nitrogen metal. The melting points and colour confirmed are used as initial confirmation or identification procedure. Stability constants were studied to the new complexes prepared which is in good agreement with reported value for similar complexes. (Author)

  6. Preparation of significant complexes of selected transition elements with appropriate ligands

    Abbas, Hala Hassan

    2000-06-01

    New complexes of copper (II), nickel (II) and cobalt (II) have been prepared using triphenylphosphine and benzofurazan-1-oxide as ligands. Benzofurazan-1-oxide was prepared from the reaction between o-nitrophenyl azide and toluene as a catalyst. These complexes have been identified by means of infra-red spectra and also melting points determination. The coordination bonding was found to be through phosphorus-metal and nitrogen-metal. The melting points and colour confirmed are used as initial confirmation or identification procedure. Stability constants were studied to the new complexes prepared which is in good agreement with reported value for similar complexes. (Author)

  7. Physicochemical and biological properties of new steroid metal complexes

    Huber, R.

    1980-04-01

    The aim of this investigation was to prepare stable steroid metal chelates by chemical conversion of the natural steroid hormones testerone, 5α-dihydrotestosterone (5α-DHT) and estradiol and to characterize these by means of their spectroscopic and other physico-chemical properties. In addition, various measuring techniques for the qualitative and quantitative study of complex stabilities and hydrolytic properties were employed. The distribution of some tritiated steroid metal complexes in the tissues of rats was tested using whole animal autoradiography, mainly with a view to identifying whether selective concentration occurs in certain organs. (orig.) [de

  8. Preparation and electrochemical properties of core-shell carbon coated Mn–Sn complex metal oxide as anode materials for lithium-ion batteries

    Zhang, Ruixue [Key Laboratory of Lithium Battery Materials of Jiangsu Province, Institute of chemical power sources, Soochow University, Suzhou 215006 (China); Fang, Guoqing; Liu, Weiwei [Key Laboratory of Lithium Battery Materials of Jiangsu Province, Institute of chemical power sources, Soochow University, Suzhou 215006 (China); Changzhou Institute of Energy Storage Materials and Devices, Changzhou 213000 (China); Xia, Bingbo; Sun, Hongdan; Zheng, Junwei [Key Laboratory of Lithium Battery Materials of Jiangsu Province, Institute of chemical power sources, Soochow University, Suzhou 215006 (China); Li, Decheng, E-mail: lidecheng@suda.edu.cn [Key Laboratory of Lithium Battery Materials of Jiangsu Province, Institute of chemical power sources, Soochow University, Suzhou 215006 (China)

    2014-02-15

    In this study, we synthesized a carbon coated Mn–Sn metal oxide composite with core-shell structure (MTO@C) via a simple glucose hydrothermal reaction and subsequent carbonization approach. When the MTO@C composite was applied as an anode material for lithium-ion batteries, it maintained a reversible capacity of 409 mA h g{sup −1} after 200 cycles at a current density of 100 mA g{sup −1}. The uniformed and continuous carbon layer formed on the MTO nanoparticles, effectively buffered the volumetric change of the active material and increased electronic conductivity, which thus prolonged the cycling performance of the MTO@C electrode.

  9. Preparation and electrochemical properties of core-shell carbon coated Mn–Sn complex metal oxide as anode materials for lithium-ion batteries

    Zhang, Ruixue; Fang, Guoqing; Liu, Weiwei; Xia, Bingbo; Sun, Hongdan; Zheng, Junwei; Li, Decheng

    2014-01-01

    In this study, we synthesized a carbon coated Mn–Sn metal oxide composite with core-shell structure (MTO@C) via a simple glucose hydrothermal reaction and subsequent carbonization approach. When the MTO@C composite was applied as an anode material for lithium-ion batteries, it maintained a reversible capacity of 409 mA h g −1 after 200 cycles at a current density of 100 mA g −1 . The uniformed and continuous carbon layer formed on the MTO nanoparticles, effectively buffered the volumetric change of the active material and increased electronic conductivity, which thus prolonged the cycling performance of the MTO@C electrode.

  10. High fluorescence emission of carboxylic acid functionalized polystyrene/BaTiO{sub 3} nanocomposites and rare earth metal complexes: Preparation and characterization

    Cao, X. T.; Showkat, A. M.; Wang, Z.; Lim, K. T., E-mail: ktlim@pknu.ac.kr [Department of Imaging System Engineering, Pukyong National University, Busan 608-737 (Korea, Republic of)

    2015-03-30

    Noble fluorescence nanocomposite compound based on barium titanate nanoparticles (BTO), polystyrene (PSt), and terbium ion (Tb{sup 3+}) was synthesized by a combination of surface-initiated reversible addition-fragmentation chain transfer (RAFT) polymerization, Friedel-Crafts alkylation reaction and coordinate chemistry. Initially, a modification of surface of BTO was conducted by an exchange process with S-benzyl S’-trimethoxysilylpropyltrithiocarbonate to create macro-initiator for polymerization of styrene. Subsequently, aryl carboxylic acid functionalized polystyrene grafted barium titanate (BTO-g-PSt-COOH) was generated by substitution reaction between 4-(Chloromethyl) benzoic acid and PSt chains. The coordination of the nanohybrids with Tb{sup 3+} ions afforded fluorescent Tb{sup 3+} tagged aryl carboxylic acid functionalized polystyrene grafted barium titanate (BTO-g-PSt-Tb{sup 3+}) complexes. Structure, morphology, and fluorescence properties of nanohybrid complexes were investigated by respective physical and spectral studies. FT-IR and SEM analyses confirmed the formation of BTO-g-PSt-Tb{sup 3+}nanohybrids. Furthermore, TGA profiles demonstrated the grafting of aryl carboxylic acid functionalized polystyrene on BTO surface. Optical properties of BTO-g-PSt-Tb{sup 3+} complexes were investigated by fluorescence spectroscopy.

  11. Quinonoid metal complexes: toward molecular switches.

    Dei, Andrea; Gatteschi, Dante; Sangregorio, Claudio; Sorace, Lorenzo

    2004-11-01

    The peculiar redox-active character of quinonoid metal complexes makes them extremely appealing to design materials of potential technological interest. We show here how the tuning of the properties of these systems can be pursued by using appropriate molecular synthetic techniques. In particular, we focus our attention on metal polyoxolene complexes exhibiting intramolecular electron transfer processes involving either the ligand and the metal ion or the two dioxolene moieties of a properly designed ligand thus inducing electronic bistability. The transition between the two metastable electronic states can be induced by different external stimuli such as temperature, pressure, light, or pH suggesting the use of these systems for molecular switches.

  12. Cationic rare-earth metal SALEN complexes.

    Liu, Qiancai; Meermann, Christian; Görlitzer, Hans W; Runte, Oliver; Herdtweck, Eberhardt; Sirsch, Peter; Törnroos, Karl W; Anwander, Reiner

    2008-11-28

    Complexes (Salpren(tBu,tBu))Y[N(SiHMe2)2](thf) and (SALEN(tBu,tBu))La[N(SiHMe2)2](thf) (SALEN(tBu,tBu) = Salcyc(tBu,tBu) and Salpren(tBu,tBu)) were prepared from Ln[N(SiHMe2)2]3(thf)2 and H2SALEN(tBu,tBu). The yttrium complex was characterized by X-ray crystallography revealing intrinsic solid-state structural features: the metal centre is displaced by 1.05 angstroms from the [N2O2] least squares plane of a highly bent Salpren(tBu,tBu) ligand (angle(Ph,Ph) dihedral angle of 80.4(1) degrees ) and is coordinated asymmetrically by the silylamide ligand exhibiting one significant Y---(HSi) beta-agostic interaction (Y-N1-Si1, 106.90(9) degrees; Y---Si1, 3.2317(6) angstroms). Complexes (SALEN(tBu,tBu))Ln[N(SiHMe2)2](thf)n (n = 1, Sc; n = 2, Y, La) react with ammonium tetraphenylborate to form the ion pairs [(SALEN(tBu,tBu))Ln(thf)n][BPh4]. The cationisation was proven by X-ray crystal structure analyses of [(Salpren(tBu,tBu))Sc(thf)2][B(C6H5)4].2(thf) and [(Salpren(tBu,tBu))Ln(thf)3][B(C6H5)4].4(thf) (Ln = Y, La), showing an octahedral and pentagonal-bipyramidal coordination geometry, respectively.

  13. Preparation of Indium Pentetate Complex (111 In-DTPA)

    Shahhosseini, S.; Farshidfar, G.R.; Najafi, R.

    2000-01-01

    There is no organometallic compound of Indium know to exist naturally in the human body. However, a number of compounds prepared with 111 In have been evaluated for localization studies. The useful radioactive decay characteristics and the suitable chemical properties of the metal ion have drawn attention of many investigators resulting in the preparation of numerous 111 In labeled compounds for potential medical applications. One of them is 111 In-DTPA complex that is used for cerebral spinal fluid studies. In the present study, DTPA has been chelated with 111 In by employing various methods and then tested for its stability in vitro during storage and in human plasma. Three methods for the preparation of 11 1In-DTPA were used. In every method, labeling efficiency and radiochemical purity were determined by chromatography systems

  14. Mesoporous metal oxides and processes for preparation thereof

    Suib, Steven L.; Poyraz, Altug Suleyman

    2018-03-06

    A process for preparing a mesoporous metal oxide, i.e., transition metal oxide. Lanthanide metal oxide, a post-transition metal oxide and metalloid oxide. The process comprises providing an acidic mixture comprising a metal precursor, an interface modifier, a hydrotropic ion precursor, and a surfactant; and heating the acidic mixture at a temperature and for a period of time sufficient to form the mesoporous metal oxide. A mesoporous metal oxide prepared by the above process. A method of controlling nano-sized wall crystallinity and mesoporosity in mesoporous metal oxides. The method comprises providing an acidic mixture comprising a metal precursor, an interface modifier, a hydrotropic ion precursor, and a surfactant; and heating the acidic mixture at a temperature and for a period of time sufficient to control nano-sized wall crystallinity and mesoporosity in the mesoporous metal oxides. Mesoporous metal oxides and a method of tuning structural properties of mesoporous metal oxides.

  15. Preparation of Radiopharmaceuticals Labeled with Metal Radionuclides

    Welch, M.J.

    2012-02-16

    The overall goal of this project was to develop methods for the production of metal-based radionuclides, to develop metal-based radiopharmaceuticals and in a limited number of cases, to translate these agents to the clinical situation. Initial work concentrated on the application of the radionuclides of Cu, Cu-60, Cu-61 and Cu-64, as well as application of Ga-68 radiopharmaceuticals. Initially Cu-64 was produced at the Missouri University Research Reactor and experiments carried out at Washington University. A limited number of studies were carried out utilizing Cu-62, a generator produced radionuclide produced by Mallinckrodt Inc. (now Covidien). In these studies, copper-62-labeled pyruvaldehyde Bis(N{sup 4}-methylthiosemicarbazonato)-copper(II) was studied as an agent for cerebral myocardial perfusion. A remote system for the production of this radiopharmaceutical was developed and a limited number of patient studies carried out with this agent. Various other copper radiopharmaceuticals were investigated, these included copper labeled blood imaging agents as well as Cu-64 labeled antibodies. Cu-64 labeled antibodies targeting colon cancer were translated to the human situation. Cu-64 was also used to label peptides (Cu-64 octriatide) and this is one of the first applications of a peptide radiolabeled with a positron emitting metal radionuclide. Investigations were then pursued on the preparation of the copper radionuclides on a small biomedical cyclotron. A system for the production of high specific activity Cu-64 was developed and initially the Cu-64 was utilized to study the hypoxic imaging agent Cu-64 ATSM. Utilizing the same target system, other positron emitting metal radionuclides were produced, these were Y-86 and Ga-66. Radiopharmaceuticals were labeled utilizing both of these radionuclides. Many studies were carried out in animal models on the uptake of Cu-ATSM in hypoxic tissue. The hypothesis is that Cu-ATSM retention in vivo is dependent upon the

  16. Alkane Soluble Transition Metal Complexes.

    1983-10-01

    lCam ludoalNm’s W S. has aA F. . Hadley. uppokli *mvahs Capm amAe Hall. 1~i. 6. 08 o.. ILDuataA ulpmr. Cai. 1d. CAM 4. 111aII. lop C Themm. - hftupvtm of...phoahines.3 descrbed previously.’ In this analyuis a series of assumption . isre onadc Our reasons for doing this were twofold. in order to enable a lhoea...nalytical method to be used. It sii be w-me First, pfmospftane complexes have been widely used as be. apparent that the assumptions that must be made

  17. Preparation, properties, and some recent studies of the actinide metals

    Haire, R.G.

    1985-01-01

    The actinide elements form a unique series of metals. The variation in their physial properties combined with the varying availability of the different elements offers a challenge to the preparative scientist. This article provides a brief review of selected methods used for preparing μg to kg amounts of the actinide metals and the properties of these metals. In addition, some recent studies on selected actinide metals are discussed. 62 refs

  18. Self-organization in metal complexes

    Radecka-Paryzek, W.

    1999-01-01

    Inorganic self-organization involves the spontaneous generation of well-defined supramolecular architectures from metal ions and organic ligands. The basic concept of supramolecular chemistry is a molecular recognition. When the substrate are metal ions, recognition is expressed in the stability and selectivity of metal ion complexation by organic ligands and depends on the geometry of the ligand and on their binding sites that it contains. The combination of the geometric features of the ligand units and the coordination geometries of the metal ions provides very efficient tool for the synthesis of novel, intriguing and highly sophisticated species such as catenanes, box structures, double and triple helicates with a variety of interesting properties. The article will focus on the examples of inorganic self-organization involving the templating as a first step for the assembly of supramolecular structures of high complexity. (author)

  19. On monosubstituted cyanurate complexes of transition metals

    Sejfer, G.B.; Tarasova, Z.A.

    1995-01-01

    Complex monosubstituted cyanurates of transition metals K 2 [Eh(H 2 C 3 N 3 O 3 ) 4 ]x4H 2 ) where Eh = Mn, Co, Ni, Cu, Zn, Cd are synthesized and investigated by means of IR - spectroscopy and thermal analysis methods. It is shown that only thermal decomposition of a manganese complex leads to the production of this metal oxide. All other derivatives decompose with the production of a free metal, because decomposition of these substances in argon atmosphere occurs through an intermediate production of their nitrides. An assumption is made that nitroduction of yttrium or rare earth element salts (instead of transition or alkali metal derivatives) as accelerating additions will facilitate increase of polyisocyanurate resin thermal stability. 25 refs.; 2 figs.; 3 tabs

  20. Reaction mechanisms of metal complexes

    Hay, R W

    2000-01-01

    This text provides a general background as a course module in the area of inorganic reaction mechanisms, suitable for advanced undergraduate and postgraduate study and/or research. The topic has important research applications in the metallurgical industry and is of interest in the science of biochemistry, biology, organic, inorganic and bioinorganic chemistry. In addition to coverage of substitution reactions in four-, five- and six-coordinate complexes, the book contains further chapters devoted to isomerization and racemization reactions, to the general field of redox reactions, and to the reactions of coordinated ligands. It is relevant in other fields such as organic, bioinorganic and biological chemistry, providing a bridge to organic reaction mechanisms. The book also contains a chapter on the kinetic background to the subject with many illustrative examples which should prove useful to those beginning research. Provides a general background as a course module in the area of inorganic reaction mechanis...

  1. Preparation of fine Ni powders from nickel hydrazine complex

    Park, Jung Woo; Chae, Eun H.; Kim, Sang H.; Lee, Jong Ho; Kim, Jeong Wook; Yoon, Seon Mi; Choi, Jae-Young

    2006-01-01

    Fine nickel powders with narrow size distribution have been prepared from the reduction of nickel hydrazine complexes in aqueous solution. The pure nickel hydrazine complexes, [Ni(N 2 H 4 ) 3 ]Cl 2 were prepared with the molar ratio of N 2 H 4 /Ni 2+ = 4.5, while a mixture of complexes, such as Ni(N 2 H 4 ) 2 Cl 2 , [Ni(N 2 H 4 ) 3 ]Cl 2 , and [Ni(NH 3 ) 6 ]Cl 2 were formed with N 2 H 4 /Ni 2+ 2+ to metallic Ni powder proceeded via the formation of nickel hydroxide which was reduced by hydrazine liberated from the ligand exchange reaction between the nickel hydrazine complex and NaOH. The standard deviation of the particle size decreased with the decreasing molar concentration of nickel hydrazine complex while the mean particle size increased. As the amount of hydrazine increased, the surface roughness of the particles was improved significantly due to the catalytic decomposition of the excess hydrazine at the surface of the nickel particle. It was found that average particle size could be controlled from 150 to 380 nm by adjusting the reaction molar ratio and temperature

  2. Facile Preparation of Hybrid Zinc Porphyrin Dendrimer Using Coordination Complex

    Choi, Go-Eun; Shin, Eun Ju [Sunchon National University, Suncheon (Korea, Republic of)

    2016-03-15

    Porphyrins and metalloporphyrins have been investigated extensively due to their important role in natural photosynthesis, strong absorption in visible region, good light-harvesting properties, unique photophysical and electrochemical properties, and the development of simple synthetic routes for various derivatives. Dendrimers have globular structure with branches of repeating units and wide diversity of the architecture because their size, shape, and functionalities can be tailored. Numerous dendrimers have been designed and synthesized for various applications ranging from catalyst to drug delivery. Both pyridine dendrons Py-PD and Py-AD were successfully coordinated at axial position on central zinc metal cation in zinc porphyrin dendrimers ZnP-AD, ZnP-AD2, or ZnP-AD4. Therefore, it was proven that the formation of axial coordination complex between metal-centered dendrimer and ligand-containing dendron provides another facile method for the preparation of new hybrid dendrimer.

  3. Colour interceptions, thermal stability and surface morphology of polyester metal complexes

    Zohdy, M.H.

    2005-01-01

    Chelating copolymers via grafting of acrylic acid (AAc) and acrylamide (AAm/AAc) comonomer mixture onto polyester micro fiber fabrics (PETMF) using gamma-radiation technique were prepared. The prepared graft chains (PETMF-g-AAc) and (PETMF-g-PAAc/PAAm) acted as chelating sites for some selected transition metal ions. The prepared graft copolymers and their metal complexes were characterized using thermogravimetric analysis (TGA), colour parameters and surface morphology measurements. The colour interception and strength measurements showed that the metal complexation is homogeneously distributed. The results showed that the thermal stability of PETMF was improved after graft copolymerization and metal complexes. Moreover, the degree of grafting enhanced the thermal stability values of the grafted and complexed copolymers up to 25% of magnitude, on the other hand the activation energy of the grafted-copolymer with acrylic acid increased up to 80%. The SEM observation gives further supports to the homogenous distribution of grafting and metal complexation

  4. Preparation and characterization of several transition metal oxides

    Wold, A.; Dwight, K.

    1989-01-01

    The structure-property relationships of several conducting transition metal oxides, as well as their preparative methods, are presented in this paper. The importance of preparing homogeneous phases with precisely known stoichiometry is emphasized. A comparison is also made of the various techniques used to prepare both polycrystalline and single crystal samples. For transition metal oxides, the metallic properties are discussed either in terms of metal-metal distances which are short enough to result in metallic behavior, or in terms of the formation of a π* conduction band resulting from covalent metal-oxygen interactions. Metallic behavior is observed when the conduction bands are populated with either electrons or holes. The concentration of these carriers can be affected by either cation or anion substitutions. The discussion in this presentation will be limited to the elements Re, Ti, V, Cr, Mo, and Cu

  5. Preparation and characteristics of CNT-metal composites

    Pityana, SL

    2006-01-01

    Full Text Available The success in keeping carbon nanotubes (CNT) bonded to stainless steel provides a possible method for the preparation of CNT-metal composites. Alternative methods for the preparation of CNT-metal composites include hot pressing, sintering, etc...

  6. Environmentally friendly preparation of metal nanoparticles

    The book chapter summarizes the “state of the art” in the exploitation of various environmentally-friendly synthesis approaches, reaction precursors and conditions to manufacture metal and metal oxide nanoparticles for a vast variety of purposes.

  7. Process for the preparation of fine grain metal carbide powders

    Gortsema, F.P.

    1976-01-01

    Fine grain metal carbide powders are conveniently prepared from the corresponding metal oxide by heating in an atmosphere of methane in hydrogen. Sintered articles having a density approaching the theoretical density of the metal carbide itself can be fabricated from the powders by cold pressing, hot pressing or other techniques. 8 claims, no drawings

  8. Development of the Method for Preparation of Actinide Metals

    Shiokawa, Y.; Hasegawa, K.; Takahashi, M.; Suzuki, K.

    1997-01-01

    The uranium amalgam was quantitatively prepared by electrolysis from the aqueous solution containing acetic acid and sodium acetate using mercury cathode. A bright button or brown porous one of uranium metal was obtained by thermal decomposition of the amalgam. The purity was found to be much higher than commercial grade metal of ca.99.95%. As a result of this work, the simple and easy procedure for preparation of uranium metal with high purity level on the laboratory scale has been developed.

  9. Anharmonic Vibrational Spectroscopy on Metal Transition Complexes

    Latouche, Camille; Bloino, Julien; Barone, Vincenzo

    2014-06-01

    Advances in hardware performance and the availability of efficient and reliable computational models have made possible the application of computational spectroscopy to ever larger molecular systems. The systematic interpretation of experimental data and the full characterization of complex molecules can then be facilitated. Focusing on vibrational spectroscopy, several approaches have been proposed to simulate spectra beyond the double harmonic approximation, so that more details become available. However, a routine use of such tools requires the preliminary definition of a valid protocol with the most appropriate combination of electronic structure and nuclear calculation models. Several benchmark of anharmonic calculations frequency have been realized on organic molecules. Nevertheless, benchmarks of organometallics or inorganic metal complexes at this level are strongly lacking despite the interest of these systems due to their strong emission and vibrational properties. Herein we report the benchmark study realized with anharmonic calculations on simple metal complexes, along with some pilot applications on systems of direct technological or biological interest.

  10. PREPARATIONS AND APPLICATION OF METAL NANOPARTICLES

    Adlim, Adlim

    2010-01-01

    Terminology of metal nanoparticles, the uniqueness properties in terms of the surface atom, the quantum dot, and the magnetism are described. The further elaboration was on the synthesis of nanoparticles. Applications of metal nanoparticles in electronic, ceramic medical and catalysis were overviewed. The bibliography includes 81 references with 99% are journal articles.   Keywords: metal nanoparticles

  11. PREPARATIONS AND APPLICATION OF METAL NANOPARTICLES

    Adlim Adlim

    2010-06-01

    Full Text Available Terminology of metal nanoparticles, the uniqueness properties in terms of the surface atom, the quantum dot, and the magnetism are described. The further elaboration was on the synthesis of nanoparticles. Applications of metal nanoparticles in electronic, ceramic medical and catalysis were overviewed. The bibliography includes 81 references with 99% are journal articles.   Keywords: metal nanoparticles

  12. Review on preparation techniques of particle reinforced metal matrix composites

    HAO Bin

    2006-02-01

    Full Text Available This paper reviews the investigation status of the techniques for preparation of metal matrix composites and the research outcomes achieved recently. The mechanisms, characteristics, application ranges and levels of development of these preparation techniques are analyzed. The advantages and the disadvantages of each technique are synthetically evaluated. Lastly, the future directions of research and the prospects for the preparation techniques of metal matrix composites are forecasted.

  13. Preparation of the pur uranium-metal; La preparation de l'uranium-metal pur

    Goldschmidt, B; Vertes, P [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

    1955-07-01

    A detailed description of the chemical processes used to prepare in the factory of Bouchet of the CEA (Seine-Et-Oise) pur metal uranium with either relatively rich ores, or extracts coming of physical or chemical treatment of poor ores. The nitric treatment of ores succeeds to the production of uranate of impure sodium carbonate. This last last product is dissolved in nitric acid and the uranyl nitrate is extracted by tributyl-phosphate diluted in an inert solvent. The uranyl nitrate pure is re-extracted and successively transformed in uranium peroxide, in orange oxide then in brown oxide which is transformed in fluoride by the anhydrous hydrofluoric acid. Uranate fluoride is then reduced in metal by the pure calcium with an yield superior to 99%. (authors) [French] Description detaillee des procedes chimiques mis en jeu pour preparer a l'Usine du Bouchet du Commissariat a l'Energie Atomique (Seine-et-Oise) l'uranium metal pur a partir soit de minerais relativement riches, soit de concentres provenant de traitement physique ou chimique de minerais pauvres. Le traitement nitrique des minerais aboutit a la production d'uranate de soude impur. Ce dernier est a son tour dissous dans l'acide nitrique et le nitrate d'uranyle est extrait par du tributyl-phosphate dilue par un solvant inerte. Le nitrate d'uranyle pur reextrait est transforme successivement en peroxyde d'uranium, en oxyde orange puis en oxyde brun qui est transforme en fluorure par l'acide fluorhydrique anhydre. Le fluorure uraneux est reduit en metal par le calcium pur avec un rendement superieur a 99 %. (auteurs)

  14. Preparation of the pur uranium-metal; La preparation de l'uranium-metal pur

    Goldschmidt, B.; Vertes, P. [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

    1955-07-01

    A detailed description of the chemical processes used to prepare in the factory of Bouchet of the CEA (Seine-Et-Oise) pur metal uranium with either relatively rich ores, or extracts coming of physical or chemical treatment of poor ores. The nitric treatment of ores succeeds to the production of uranate of impure sodium carbonate. This last last product is dissolved in nitric acid and the uranyl nitrate is extracted by tributyl-phosphate diluted in an inert solvent. The uranyl nitrate pure is re-extracted and successively transformed in uranium peroxide, in orange oxide then in brown oxide which is transformed in fluoride by the anhydrous hydrofluoric acid. Uranate fluoride is then reduced in metal by the pure calcium with an yield superior to 99%. (authors) [French] Description detaillee des procedes chimiques mis en jeu pour preparer a l'Usine du Bouchet du Commissariat a l'Energie Atomique (Seine-et-Oise) l'uranium metal pur a partir soit de minerais relativement riches, soit de concentres provenant de traitement physique ou chimique de minerais pauvres. Le traitement nitrique des minerais aboutit a la production d'uranate de soude impur. Ce dernier est a son tour dissous dans l'acide nitrique et le nitrate d'uranyle est extrait par du tributyl-phosphate dilue par un solvant inerte. Le nitrate d'uranyle pur reextrait est transforme successivement en peroxyde d'uranium, en oxyde orange puis en oxyde brun qui est transforme en fluorure par l'acide fluorhydrique anhydre. Le fluorure uraneux est reduit en metal par le calcium pur avec un rendement superieur a 99 %. (auteurs)

  15. Salts of alkali metal anions and process of preparing same

    Dye, James L.; Ceraso, Joseph M.; Tehan, Frederick J.; Lok, Mei Tak

    1978-01-01

    Compounds of alkali metal anion salts of alkali metal cations in bicyclic polyoxadiamines are disclosed. The salts are prepared by contacting an excess of alkali metal with an alkali metal dissolving solution consisting of a bicyclic polyoxadiamine in a suitable solvent, and recovered by precipitation. The salts have a gold-color crystalline appearance and are stable in a vacuum at -10.degree. C. and below.

  16. Preparation of reactive and refractory metal powders (Paper No. 25)

    Sundaram, C.V.; Sharma, B.P.; Krishnan, T.S.

    1979-01-01

    In devising processes for the preparation of refractory and reactive metal powders, one has to reckon with many relevant factors. The choice of specific flowsheets is governed by the characteristics of the metal compounds and the reducing agents, the purity required and achievable in the as-reduced powder, the need for further refining of the metal, the possibilities of chemical/physical/mechanical comminution of the purified metal without contamination, and the end application of the powder metal. Micron size zirconium powder used as trigger material in photo-flash bulbs and detonator compositions, tantalum powder of controlled particle size and high purity for the production of electrolytic capacitors, and beryllium metal powder for the preparation of hot pressed powder metallurgy components are illustrative of the variety of reactive metal powders for industrial applications. The work carried out at the Bhabha Atomic Research Centre, Bombay, on the preparation of special metal powders, with particular emphasis on Group IV and V metals and also beryllium is presented. Reduction of metal oxides with alkaline earth metals/hydrides, reduction of metal halides with sodium/magnesium, vacuum arc and electron beam melt purification followed by comminution by hydrogen embrittlement/mechanical comminution are among the processes discussed. (auth.)

  17. Studies on Oligomer Metal Complexes Derived from Bisamic Acid of Pyromellitic Dianhydride and 4-Bromoaniline

    Patel, Yogesh S.

    2014-01-01

    Novel oligomer metal complexes (2a–f) of the ligand 2,5-bis((4-bromophenyl)carbamoyl) terephthalic acid (1) were prepared using transition metal salts and characterized by various spectroscopic techniques. The geometry of oligomer metal complexes was carried out by electronic spectral analysis and magnetic measurement studies. Polymeric properties have also been carried out. Ligand was synthesized using pyromellitic dianhydride and 4-bromoaniline. It was duly characterized. All novel synthesi...

  18. Process for electrolytically preparing uranium metal

    Haas, Paul A.

    1989-01-01

    A process for making uranium metal from uranium oxide by first fluorinating uranium oxide to form uranium tetrafluoride and next electrolytically reducing the uranium tetrafluoride with a carbon anode to form uranium metal and CF.sub.4. The CF.sub.4 is reused in the fluorination reaction rather than being disposed of as a hazardous waste.

  19. PREPARATION OF METAL OXIDE POWDERS FROM METAL LOADED VERSATIC ACID

    KAKIHATA, Takayuki; USAMI, Kensuke; YAMAMOTO, Hideki; SHIBATA, Junji

    1998-01-01

    A production process for metal oxide powders was developed using a solvent extraction method. Versatic Acid 10 and D2EHPA solutions containing copper, zinc and nickel were used for a precipitation-stripping process, where oxalic acid was added to the solution as a precipitation reagent.Copper, zinc and nickel oxalates were easily formed in an aqueous phase, and 99.9% of precipitation was obtained for each metal during this process. These metal oxalates were easily converted to metal oxides by...

  20. Tritium in metals: Techniques of preparation

    Laesser, R.; Klatt, K.H.; Mecking, P.; Wenzl, H.

    1982-08-01

    In order to study the behavior of tritium in metals, an all metal apparatus has been built for the safe handling of 100 mg of tritium. Samples of palladium, vanadium, niobium, and tantalum were loaded with tritium, deuterium or hydrogen. Some details of the phase diagrams could be established by DTA and by measurement of the lattice parameters. The diffusion of tritium in V, Nb, and Ta was studied with the Gorsky-effect. (TWO)

  1. Biological activities of some Fluoroquinolones-metal complexes

    McRoy

    DNA cleavage studies of some synthesized metal complexes of fluoroquinolone ... Although the FQs are generally characterized by a broad antimicrobial spectrum ..... six Coordinate 3rd metal complexes with N- (5 –Phenyl-3,4- thiadiazol-2-yl).

  2. Studies on Oligomer Metal Complexes Derived from Bisamic Acid of Pyromellitic Dianhydride and 4-Bromoaniline.

    Patel, Yogesh S

    2014-01-01

    Novel oligomer metal complexes (2a-f) of the ligand 2,5-bis((4-bromophenyl)carbamoyl) terephthalic acid (1) were prepared using transition metal salts and characterized by various spectroscopic techniques. The geometry of oligomer metal complexes was carried out by electronic spectral analysis and magnetic measurement studies. Polymeric properties have also been carried out. Ligand was synthesized using pyromellitic dianhydride and 4-bromoaniline. It was duly characterized. All novel synthesized compounds 1 and 2a-f were evaluated for their antibacterial and antifungal activity. The results showed significantly higher antibacterial and antifungal activity of oligomer metal complexes compared to the ligand.

  3. An improved method of preparation of nanoparticular metal oxide catalysts

    2014-01-01

    The present invention concerns an improved method of preparation of nanoparticular vanadium oxide/anatase titania catalysts having a narrow particle size distribution. In particular, the invention concerns preparation of nanoparticular vanadium oxide/anatase titania catalyst precursors comprising...... combustible crystallization seeds upon which the catalyst metal oxide is coprecipitated with the carrier metal oxide, which crystallization seeds are removed by combustion in a final calcining step....

  4. Preparation and Purification of natural uranium metal by Iodine method

    Taies, J.A.

    2008-01-01

    In this work ,glass-metal apparatus was designed and manufactured which used for preparing a high purity uranium.The reaction is simply take place between iodine vapour and uranium metal at 500C in closed system to form uranium tetra iodide which is decomposed on hot wire at high temperature around 1100C.Also another apparatus was made from Glass and used for preparing a high purity of UI 4 more than 99.9%purity

  5. Chemical bonding of hydrogen molecules to transition metal complexes

    Kubas, G.J.

    1990-01-01

    The complex W(CO) 3 (PR 3 ) 2 (H 2 ) (CO = carbonyl; PR 3 = organophosphine) was prepared and was found to be a stable crystalline solid under ambient conditions from which the hydrogen can be reversibly removed in vacuum or under an inert atmosphere. The weakly bonded H 2 exchanges easily with D 2 . This complex represents the first stable compound containing intermolecular interaction of a sigma-bond (H-H) with a metal. The primary interaction is reported to be donation of electron density from the H 2 bonding electron pair to a vacant metal d-orbital. A series of complexes of molybdenum of the type Mo(CO)(H 2 )(R 2 PCH 2 CH 2 PR 2 ) 2 were prepared by varying the organophosphine substitutent to demonstrate that it is possible to bond either dihydrogen or dihydride by adjusting the electron-donating properties of the co-ligands. Results of infrared and NMR spectroscopic studies are reported. 20 refs., 5 fig

  6. Preparation of self-supporting thin metal target films

    Wang Xiuying; Ge Suxian; Yin Jianhua; Yin Xu; Jin Genming

    1989-01-01

    The preparation method and equipment for thin metal self-supporting target without oil contamination are described. The influence of target films contaminated by oil vapor on accuracy of nuclear-physics experimental data are also discussed. The analytical results on carbon content in the prepared films of three elements show that the equipment is very effective for eliminating contamination

  7. Metal ammine complexes for hydrogen storage

    Christensen, Claus H.; Sørensen, Rasmus Zink; Johannessen, Tue

    2005-01-01

    The hopes of using hydrogen as an energy carrier are severely dampened by the fact that there is still no safe, high-density method available for storing hydrogen. We investigate the possibility of using metal ammine complexes as a solid form of hydrogen storage. Using Mg(NH3)(6)Cl-2 as the example......, we show that it can store 9.1% hydrogen by weight in the form of ammonia. The storage is completely reversible, and by combining it with an ammonia decomposition catalyst, hydrogen can be delivered at temperatures below 620 K....

  8. Evaluation of heavy metal complex phytotoxicity

    Vita Vasilyevna Datsenko

    2016-07-01

    Full Text Available The experimental data dealing with the effect of heavy metals contained in the technogenic contaminated soils on plant objects under controlled conditions was discussed. The aim of this work is to define the quantitative indicators of copper and zinc potential phytotoxicity, namely germination energy, simultaneous germination and duration of the test plants. It was found that the activity of the test plant growth is linked with copper and zinc complex action. Joint effect of copper and zinc is manifested both in inhibition of lettuce growth and determined, above all, by the nature contamination, soil properties and biological specificity of the test plants.

  9. Development of the method for preparation of actinide metals

    Shiokawa, Y.; Hasegawa, K.; Takahashi, M.; Suzuki, K.

    1997-01-01

    The uranium amalgam was quantitatively prepared by electrolysis from the aqueous solution containing acetic acid and sodium acetate using mercury cathode. A bright button or brown porous one of uranium metal was obtained by thermal decomposition of the amalgam. The purity was found to be much higher than commercial grade metal of ca.99.95%. As a result of this work, the simple and easy procedure for preparation of uranium metal with high purity level on the laboratory scale has been developed. (author)

  10. Some transition metal complexes derived from mono- and di-ethynyl perfluorobenzenes

    Armitt, D.J.; Bruce, M.I.; Gaudio, M.; Zaitseva, N.N.; Skelton, B.W.; White, A.H.; Le Guennic, B.; Halet, J.-F.; Fox, M.A.; Roberts, R.L.; Hartl, F.; Low, P.J.

    2008-01-01

    Transition metal alkynyl complexes containing perfluoroaryl groups have been prepared directly from trimethylsilyl-protected mono- and di-ethynyl perfluoroarenes by simple desilylation/metallation reaction sequences. Reactions between Me3SiC CC6F5 and RuCl(dppe)Cp'[Cp' = Cp, Cp*] in the presence of

  11. Preparation of magnesium metal matrix composites by powder metallurgy process

    Satish, J.; Satish, K. G., Dr.

    2018-02-01

    Magnesium is the lightest metal used as the source for constructional alloys. Today Magnesium based metal matrix composites are widely used in aerospace, structural, oceanic and automobile applications for its light weight, low density(two thirds that of aluminium), good high temperature mechanical properties and good to excellent corrosion resistance. The reason of designing metal matrix composite is to put in the attractive attributes of metals and ceramics to the base metal. In this study magnesium metal matrix hybrid composite are developed by reinforcing pure magnesium with silicon carbide (SiC) and aluminium oxide by method of powder metallurgy. This method is less expensive and very efficient. The Hardness test was performed on the specimens prepared by powder metallurgy method. The results revealed that the micro hardness of composites was increased with the addition of silicon carbide and alumina particles in magnesium metal matrix composites.

  12. Complexes in polyvalent metal - Alkali halide melts

    Akdeniz, Z.; Tosi, M.P.

    1991-03-01

    Experimental evidence is available in the literature on the local coordination of divalent and trivalent metal ions by halogens in some 140 liquid mixtures of their halides with alkali halides. After brief reference to classification criteria for main types of local coordination, we focus on statistical mechanical models that we are developing for Al-alkali halide mixtures. Specifically, we discuss theoretically the equilibrium between (AlF 6 ) 3- and (AlF 4 ) - complexes in mixtures of AlF 3 and NaF as a function of composition in the NaF-rich region, the effect of the alkali counterion on this equilibrium, the possible role of (AlF 5 ) 2- as an intermediate species in molten cryolite, and the origin of the different complexing behaviours of Al-alkali fluorides and chlorides. We also present a theoretical scenario for processes of structure breaking and electron localization in molten cryolite under addition of sodium metal. (author). 26 refs, 2 tabs

  13. Preparation of Metal Nanoparticles via Sonochemical Reduction

    Saura Puig, Oriol

    2011-01-01

    Pure nickel, copper and zinc nanoparticles were prepared from chlorides of these elements using ultrasound with three different reducing agents (zinc, aluminum and magnesium). In the second part, syntheses of nickel-copper alloy and nickel-zinc using ultrasound were investigated. The products were characterized by powder X-ray diffraction. The reaction parameters, such as sonification time, the amount of reagents and reaction conditions were modified to observe variations in...

  14. Composite nanoparticles containing rare earth metal and methods of preparation thereof

    Kandapallil, Binil Itty Ipe; Krishnan, Lakshmi; Johnson, Francis

    2018-04-10

    The present invention is directed to composite nanoparticles comprising a metal, a rare earth element, and, optionally, a complexing ligand. The invention is also directed to composite nanoparticles having a core-shell structure and to processes for preparation of composite nanoparticles of the invention.

  15. Preparing English Language Learners for Complex Reading

    Silva, Janice; Delleman, Paul; Phesia, Andria

    2013-01-01

    Although the Common Core state standards' goal of ensuring that every student leaves high school prepared to meet the demands of college and career is laudable, it's daunting for teachers who serve English language learners. The authors, educators at a private bilingual school in Mexico, describe how they used short excerpts of longer works giving…

  16. Metallized xerographic plates and their preparation

    1976-01-01

    Xerographic plates, particularly xeroradiographic plates, suitable for soft or hard x-ray exposure require margins or edges suitable for handling and mounting. In order to fabricate such plates, it is convenient to apply a peripheral mask over the substrate during application of at least the photoconductive layer. Use of masks, however, tend to promote peripheral plate irregularities usually because of scratches or other uneveness at or under the margin of the applied mask. Such imperfections spawn corresponding electrical field irregularities which can now be minimized or avoided altogether by grounding the margins with metal overcoats

  17. Infrared Spectroscopy of Metal Ion Complexes: Models for Metal Ligand Interactions and Solvation

    Duncan, Michael

    2006-03-01

    Weakly bound complexes of the form M^+-Lx (M=Fe, Ni, Co, etc.; L=CO2, C2H2, H2O, benzene, N2) are prepared in supersonic molecular beams by laser vaporization in a pulsed-nozzle cluster source. These species are mass analyzed and size-selected in a reflectron time-of-flight mass spectrometer. Clusters are photodissociated at infrared wavelengths with a Nd:YAG pumped infrared optical parametric oscillator/amplifier (OPO/OPA) laser or with a tunable infrared free-electron laser. M^+-(CO2)x complexes absorb near the free CO2 asymmetric stretch near 2349 cm-1 but with an interesting size dependent variation in the resonances. Small clusters have blue-shifted resonances, while larger complexes have additional bands due to surface CO2 molecules not attached to the metal. M^+(C2H2)n complexes absorb near the C-H stretches in acetylene, but resonances in metal complexes are red-shifted with repect to the isolated molecule. Ni^+ and Co^+ complexes with acetylene undergo intracluster cyclization reactions to form cyclobutadiene. Transition metal water complexes are studied in the O-H stretch region, and partial rotational structure can be measured. M^+(benzene) and M^+(benzene)2 ions (M=V, Ti, Al) represent half-sandwich and sandwich species, whose spectra are measured near the free benzene modes. These new IR spectra and their assignments will be discussed as well as other new IR spectra for similar complexes.

  18. Novel Metals and Metal Complexes as Platforms for Cancer Therapy

    Frezza, Michael; Hindo, Sarmad; Chen, Di; Davenport, Andrew; Schmitt, Sara; Tomco, Dajena; Dou, Q. Ping

    2010-01-01

    Metals are essential cellular components selected by nature to function in several indispensable biochemical processes for living organisms. Metals are endowed with unique characteristics that include redox activity, variable coordination modes, and reactivity towards organic substrates. Due to their reactivity, metals are tightly regulated under normal conditions and aberrant metal ion concentrations are associated with various pathological disorders, including cancer. For these reasons, coo...

  19. Synthesis, characterization, anti-microbial, DNA binding and cleavage studies of Schiff base metal complexes

    Poomalai Jayaseelan

    2016-09-01

    Full Text Available A novel Schiff base ligand has been prepared by the condensation between butanedione monoxime with 3,3′-diaminobenzidine. The ligand and metal complexes have been characterized by elemental analysis, UV, IR, 1H NMR, conductivity measurements, EPR and magnetic studies. The molar conductance studies of Cu(II, Ni(II, Co(II and Mn(II complexes showed non-electrolyte in nature. The ligand acts as dibasic with two N4-tetradentate sites and can coordinate with two metal ions to form binuclear complexes. The spectroscopic data of metal complexes indicated that the metal ions are complexed with azomethine nitrogen and oxyimino nitrogen atoms. The binuclear metal complexes exhibit octahedral arrangements. DNA binding properties of copper(II metal complex have been investigated by electronic absorption spectroscopy. Results suggest that the copper(II complex bind to DNA via an intercalation binding mode. The nucleolytic cleavage activities of the ligand and their complexes were assayed on CT-DNA using gel electrophoresis in the presence and absence of H2O2. The ligand showed increased nuclease activity when administered as copper complex and copper(II complex behave as efficient chemical nucleases with hydrogen peroxide activation. The anti-microbial activities and thermal studies have also been studied. In anti-microbial activity all complexes showed good anti-microbial activity higher than ligand against gram positive, gram negative bacteria and fungi.

  20. BIOASSAY STUDIES OF METAL(II) COMPLEXES OF 2,2'-(ETHANE ...

    Preferred Customer

    diyldiimino)diacetic acid (EDDA) were prepared and characterized. Coordination complexes of the EDDA ... corresponding amines with alkyl halide to bear diammines of the same class with different substituents. ... Bioassay studies of metal(II) complexes of 2,2'-(ethane-1,2-diyldiimino)diacetic acid. Bull. Chem. Soc. Ethiop.

  1. Extraction of fluoride metal complexes by octanols

    Baklanova, I.V.; Nikolaev, A.I.; Il'in, E.G.; Majorov, V.G.

    2005-01-01

    The extraction of niobium(V) and tantalum(V) by octanols, including 1-octanol, 2-octanol, and iso-octanol (2-ethylhexanol), was studied. The composition of the octanols and their solubility in various aqueous solutions were evaluated. The capacity of the octanols for tantalum(V) and niobium(V), the extraction properties of the octanols, the viscosity of extracts under conditions of metal fluoride extraction, and the temperature dependence of the viscosity of the octanols were studied. The composition of the extracted complexes was studied by IR and NMR spectroscopy and chemical analysis, and the hydration-solvation mechanism of the extraction of tantalum(V) and niobium(V) was supported [ru

  2. PREPARATION OF A POLYMER ARTICLE FOR SELECTIVE METALLIZATION

    2008-01-01

    The present invention relates to the field of selective metallization, and in particular to preparing a polymer article for selective metallization by submerging the article in a first liquid, and while submergedirradiate the article by a laser beam the area of the article on which the metal...... is to be deposited. An activation step, prior to the selective metallization, comprises submerging the article in an activation liquid for depositing seedparticles in the selected area. The irradiation of the selected area is proportionate so as to cause a temporary meltingof the polymer in the surface...... of the selected area of the polymer article. The invention is advantageous in that the preparation may be performed with a relatively high scan rate across the polymer article, and in that a quite limited use of toxic chemicals....

  3. Preparation and characterization of artemether inclusion complexes ...

    curve soluble complex system (referred to as the AL system), and a stability constant (KC) value of 143. M-1. ... Index Medicus, JournalSeek, Journal Citation Reports/Science Edition, Directory of Open Access Journals .... The differences between the data sets were .... Characterization, thermodynamic parameters, molecular.

  4. Theoretical studies of transition metal complexes with nitriles and isocyanides

    Kuznetsov, Maksim L

    2002-01-01

    Theoretical studies of transition metal complexes with nitriles and isocyanides are reviewed. The electronic structures and the nature of coordination bonds in these complexes are discussed. The correlation between the electronic structures of transition metal complexes with nitriles and isocyanides and their structural properties, spectroscopic characteristics, and reactivities are considered. The bibliography includes 121 references.

  5. Metal complexation capacity of Antarctic lacustrine sediments.

    Alberti, Giancarla; Mussi, Matteo; Quattrini, Federico; Pesavento, Maria; Biesuz, Raffaela

    2018-04-01

    The purpose of this study is to implement a work that is a part of a project funded by the Italian National Antarctic Research Program (PNRA, Piano Nazionale di Ricerche in Antartide) within the main thematic focus "Chemical Contamination-Global Change". This research was devoted to detect and characterize micro and nano components with strong complexing capability towards metal ions at trace level in sea water, lakes and lacustrine sediments, sampled during the XXII expedition of PNRA. In particular, in the present work, the sorption complexation capacity of an Antarctic lacustrine sediments toward Cu(II) and Pb(II) is described. The characterization of the sorption was undertaken, studying kinetics and isotherm profiles. The lake here considered is Tarn Flat in the area of Terra Nova Bay. The sorption equilibria of Cu(II) and Pb(II) on the lacustrine sediments were reached in about 10 h, and they were best modelled by the Langmuir equation. Preliminary, to establish if the data here obtained were consistent with those reported for the same area in other expeditions, a common multivariate techniques, namely the principal component analysis (PCA), was applied and finally the consistency of the data has been confirmed. Copyright © 2018 Elsevier Ltd. All rights reserved.

  6. Complex metal hydrides for hydrogen, thermal and electrochemical energy storage

    Møller, Kasper T.; Sheppard, Drew; Ravnsbæk, Dorthe B.

    2017-01-01

    field. This review illustrates that complex metal hydrides may store hydrogen in the solid state, act as novel battery materials, both as electrolytes and electrode materials, or store solar heat in a more efficient manner as compared to traditional heat storage materials. Furthermore, it is highlighted...... how complex metal hydrides may act in an integrated setup with a fuel cell. This review focuses on the unique properties of light element complex metal hydrides mainly based on boron, nitrogen and aluminum, e.g., metal borohydrides and metal alanates. Our hope is that this review can provide new...

  7. A made in Brazil metallic sample preparation facility

    Holt, B.J.; Diaz, J.V.; Huber, J.G.; Luengo, C.A.

    A facility, built locally, for the preparation of metallic compounds and alloys of common use in solid state physics in described. This facility includes a multipurpose furnace (FORARCO I) and accessories which are capable of melting, quenching, casting and annealing. (author) [pt

  8. Preparation of carbon-free TEM microgrids by metal sputtering

    Janbroers, S.; Kruijff, T.R. de; Xu, Q.; Kooyman, P.J.; Zandbergen, H.W.

    2009-01-01

    A new method for preparing carbon-free, temperature-stable Transmission Electron Microscope (TEM) grids is presented. An 80% Au/20% Pd metal film is deposited onto a 'holey' microgrid carbon supported on standard mixed-mesh Au TEM grids. Subsequently, the carbon film is selectively removed using plasma cleaning. In this way, an all-metal TEM film is made containing the 'same' microgrid as the original carbon film. Although electron transparency of the foil is reduced significantly, the open areas for TEM inspection of material over these areas are maintained. The metal foil can be prepared with various thicknesses and ensures good electrical conductivity. The new Au/Pd grids are stable to at least 775 K under vacuum conditions.

  9. Preparation of carbon-free TEM microgrids by metal sputtering

    Janbroers, S., E-mail: stephan.janbroers@albemarle.com [Albemarle Catalysts B.V., Nieuwendammerkade 1-3, 1030 BE, Amsterdam (Netherlands); Kavli Institute of Nanoscience, Delft University of Technology, Lorentzweg 1, 2628 CJ Delft (Netherlands); Kruijff, T.R. de; Xu, Q. [Kavli Institute of Nanoscience, Delft University of Technology, Lorentzweg 1, 2628 CJ Delft (Netherlands); Kooyman, P.J. [DelftChemTech, Delft University of Technology, Julianalaan 136, 2628 BL, Delft (Netherlands); Kavli Institute of Nanoscience, Delft University of Technology, Lorentzweg 1, 2628 CJ Delft (Netherlands); Zandbergen, H.W. [Kavli Institute of Nanoscience, Delft University of Technology, Lorentzweg 1, 2628 CJ Delft (Netherlands)

    2009-08-15

    A new method for preparing carbon-free, temperature-stable Transmission Electron Microscope (TEM) grids is presented. An 80% Au/20% Pd metal film is deposited onto a 'holey' microgrid carbon supported on standard mixed-mesh Au TEM grids. Subsequently, the carbon film is selectively removed using plasma cleaning. In this way, an all-metal TEM film is made containing the 'same' microgrid as the original carbon film. Although electron transparency of the foil is reduced significantly, the open areas for TEM inspection of material over these areas are maintained. The metal foil can be prepared with various thicknesses and ensures good electrical conductivity. The new Au/Pd grids are stable to at least 775 K under vacuum conditions.

  10. Preparation of carbon-free TEM microgrids by metal sputtering.

    Janbroers, S; de Kruijff, T R; Xu, Q; Kooyman, P J; Zandbergen, H W

    2009-08-01

    A new method for preparing carbon-free, temperature-stable Transmission Electron Microscope (TEM) grids is presented. An 80% Au/20% Pd metal film is deposited onto a 'holey' microgrid carbon supported on standard mixed-mesh Au TEM grids. Subsequently, the carbon film is selectively removed using plasma cleaning. In this way, an all-metal TEM film is made containing the 'same' microgrid as the original carbon film. Although electron transparency of the foil is reduced significantly, the open areas for TEM inspection of material over these areas are maintained. The metal foil can be prepared with various thicknesses and ensures good electrical conductivity. The new Au/Pd grids are stable to at least 775K under vacuum conditions.

  11. Plutonium metal preparation and purification at Los Alamos, 1984

    Christensen, D.C.; Williams, J.D.; McNeese, J.A.; Fife, K.W.

    1984-01-01

    Plutonium metal preparation and purification are well established at Los Alamos. Metal is prepared by calcothermic reduction of both PuF 4 and PuO 2 . Metal is purified by halide slagging, casting, and electrorefining. The product from the production sequence is ultrapure plutonium metal. All of the processes involve high temperature operation and all but casting involve molten salt media. Development efforts are fourfold: (1) recover plutonium values from residues; (2) reduce residue generation through process improvements and changes; (3) recycle of reagents, and (4) optimize and integrate all processes into a close-loop system. Plutonium residues are comprised of oxides, chlorides, colloidal metal suspensions, and impure metal heels. Pyrochemical recovery techniques are under development to address each residue. In addition, we are looking back at each residue generation step and are making process changes to reduce plutonium content in each residue. Reagent salt is the principle media used in pyrochemical processing. The regeneration and recycle of these reagents will both reduce our waste handling and operating expense. The fourth area, process optimization, involves both existing processes and new process developments. A status of efforts in all four of these areas will be summarized

  12. Preparation and utilization of metal oxide fine powder

    Kim, Joon Soo; Jang, Hee Dong; Lim, Young Woong; Kim, Sung Don; Lee, Hi Sun; Lee, Hoo In; Kim, Chul Joo; Shim, Gun Joo; Jang, Dae Kyu [Korea Inst. of Geology Mining and Materials, Taejon (Korea, Republic of)

    1995-12-01

    Metal oxide fine powders finds many applications in industry as new materials. It is very much necessary for the development of such powders to improve the domestic industry. The purpose of present research is to develop a process for the preparation and utilization of metal oxide fine powder. This project is consisted of two main subjects. (1) Production of ultrafine metal oxide powder: Ultrafine metal oxide powder is defined as a metal oxide powder of less than 100 nanometer in particle size. Experiments for the control of particle size and distributions in the various reaction system and compared with results of (2 nd year research). Various reaction systems were adopted for the development of feasible process. Ultrafine particles could be prepared even higher concentration of TiCl{sub 4} and lower gas flowrate compared to TiCl{sub 4}-O{sub 2} system in the TiCl{sub 4}-Air-H{sub 2}O system. Ultrafine Al{sub 2}O{sub 3} powders also prepared with the change of concentration and gas flowrate. Experiments on the treatment of surface characteristics of ultrafine TiO{sub 2} powders were investigated using esterification and surface treating agents. A mathematical model that can predict the particle size and distribution was also developed. (2) Preparation of cerium oxide for high-grade polishing powder: Used cerium polishing powder was recycled for preparation of high grade cerium oxide polishing powder. Also, cerium hydroxide which was generated as by-product in processing of monazite ore was used as another material. These two materials were leached respectively by using acid, and the precipitate was gained in each leached solution by adjusting pH of the solution, and by selective crystallization. These precipitates were calcined to make high grade cerium oxide polishing powder. The effect of several experimental variables were investigated, and the optimum conditions were obtained through the experiments. (author). 81 refs., 49 figs., 27 tabs.

  13. Microreactor and method for preparing a radiolabeled complex or a biomolecule conjugate

    Reichert, David E; Kenis, Paul J. A.; Wheeler, Tobias D; Desai, Amit V; Zeng, Dexing; Onal, Birce C

    2015-03-17

    A microreactor for preparing a radiolabeled complex or a biomolecule conjugate comprises a microchannel for fluid flow, where the microchannel comprises a mixing portion comprising one or more passive mixing elements, and a reservoir for incubating a mixed fluid. The reservoir is in fluid communication with the microchannel and is disposed downstream of the mixing portion. A method of preparing a radiolabeled complex includes flowing a radiometal solution comprising a metallic radionuclide through a downstream mixing portion of a microchannel, where the downstream mixing portion includes one or more passive mixing elements, and flowing a ligand solution comprising a bifunctional chelator through the downstream mixing portion. The ligand solution and the radiometal solution are passively mixed while in the downstream mixing portion to initiate a chelation reaction between the metallic radionuclide and the bifunctional chelator. The chelation reaction is completed to form a radiolabeled complex.

  14. Metal oxalate complexes as novel inorganic dopants: Studies on ...

    Unknown

    UV-visible and IR spectral features not only confirmed the polyaniline doping by complex anions but also substantiated ... MoS3 dopant. Although inorganic metal complexes bear- ... distilled water and then with methanol and acetone until.

  15. Preparation of L-asparagine complex with technetium

    Persano, S.C.M.

    1981-01-01

    The preparation of technetium chelated to L-asparagine is aimed at for obtention of potentially useful radiopharmaceutical in nuclear medicine. The reduction of pertechnetate anion ( 99 TcO - 4 and sup(99m) TcO - 4 ) using hydrazine as a reducing agent is studied with use of polarographic spectrophotometric and chromatographic methods. Spectrophotometric determination shows that the aqueous solution of amonium sup(-99m) Tc pertechnetate absorbs at 244, 248 and 290 nm. After reduction the species absorbs at 330 and near 495-530 nm. Polarographic measurements with 0,1 N NaOH electrolyte show a half-wave potential E sub(1/2 = -0,82 V for technetium +VII. After the addition of increasing amounts of hydrazine into a solution containing Tc+VII, the half wave potential shifts to more positives values, indicating the reduction of Tc+VII. Chromatographic determinations are in good agreement with polarographic analysis, emphatizing reduction of Tc+IV by hydrazine. The reduced 99 Tc shows ability of being incorporated into L-asparagine forming a cristalline compound with melting point 118.6 0 C. Infrared absorption spectrometry shows that amino and carboxyl groups are bound to the metal in this complex. The yield of sup(99m) Tc incorporation into L-asparagine at 60 0 C in 30 minutes is up to 95%. The labeled complex can be presented as a radiopharmaceutical product. Tissue distribution performed in groups of normal and bearing lymphoma Walker 256 Wistar rats (50-60) shows that the radiopharmaceutical concentrates seletively in the tumor and is fastly excreted by the kidney and it doesn't have significant affinity for any organ, being so adequate for the formation of tumoral images. (Authors) [pt

  16. Lability of Nanoparticulate Metal Complexes at a Macroscopic Metal Responsive (Bio)interface

    Duval, Jérôme F.L.; Town, Raewyn M.; Leeuwen, Van Herman P.

    2018-01-01

    The lability of metal complexes expresses the extent of the dissociative contribution of the complex species to the flux of metal ions toward a macroscopic metal-responsive (bio)interface, for example, an electrodic sensor or an organism. While the case of molecular ligands is well-established, it

  17. Preparation of Dithizone Functionalized Polystyrene for Detecting Heavy Metal Ion

    Shin, Hyeon Ho; Kim, Younghun [Kwangwoon University, Seoul (Korea, Republic of)

    2015-04-15

    Colorimetric sensors were usually used to detect specific metal ions using selective color change of solutions. While almost organic dye in colorimetric sensors detected single molecule, dithizone (DTZ) solution could be separately detected above 5 kinds of heavy metal ions by the change of clear color. Namely, DTZ could be used as multicolorimetric sensors. However, DTZ was generally used as aqueous type and paper/pellet-type DTZ was not reported yet. Therefore, in this work, polystyrene (PS) was prepared to composite with DTZ and then DTZ/PS pellet was obtained, which was used to selectively detect 10 kinds of heavy metal ions. When 10 ppm of Hg and Co ions was exposed in DTZ/PS pellets, clear color change was revealed. It is noted that DTZ/PS pellet could be used in detecting of heavy metal ion as dry type.

  18. Chemistry and Properties of Complex Intermetallics from Metallic Fluxes

    Kanatzidis, Mercouri G. [Northwestern Univ., Evanston, IL (United States)

    2015-03-28

    This project investigated the reaction chemistry and synthesis of new intermetallic materials with complex compositions and structures using metallic fluxes as solvents. It was found that the metallic fluxes offer several key advantages in facilitating the formation and crystal growth of new materials. The fluxes mostly explored were liquid aluminum, gallium and indium. The main purpose of this project was to exploit the potential of metallic fluxes as high temperature solvent for materials discovery in the broad class of intermetallics. This work opened new paths to compound formation. We discovered many new Si (or Ge)-based compounds with novel structures, bonding and physicochemical properties. We created new insights about the reaction chemistry that is responsible for stabilizing the new materials. We also studied the structural and compositional relationships to understand their properties. We investigated the use of Group-13 metals Al, Ga and In as solvents and have generated a wide variety of new results including several new ternary and quaternary materials with fascinating structures and properties as well as new insights as to how these systems are stabilized in the fluxes. The project focused on reactions of metals from the rare earth element family in combination with transition metals with Si and Ge. For example molten gallium has serves both as a reactive and non-reactive solvent in the preparation and crystallization of intermetallics in the system RE/M/Ga/Ge(Si). Molten indium behaves similarly in that it too is an excellent reaction medium, but it gives compounds that are different from those obtained from gallium. Some of the new phase identified in the aluminide class are complex phases and may be present in many advanced Al-matrix alloys. Such phases play a key role in determining (either beneficially or detrimentally) the mechanical properties of advanced Al-matrix alloys. This project enhanced our basic knowledge of the solid state chemistry

  19. Derivatized Pentadentate Macrocyclic Ligands and Their Transition Metal Complexes

    Muhammad S. Khan

    2002-06-01

    Full Text Available The reaction of the pendant hydroxyethyl group in the planar pentadentate macrocyclic ligand,1,11-bis(2’-hydroxyethyl-4,8;12,16;17,21-trinitrilo-1,2,10,11-tetraazacyclohenicosa- 2,4,6,9,12,14,18,20-octaene (L2, derived from the condensation of 2,6-pyridinedialdehyde with 6,6’-bis(2’ hydroxyethylhydrazino -2,2’-bipyridine (L1, has been investigated. Esterification reactions are facile, and the reaction of the hydroxyethyl-substituted macrocycle with thionyl chloride yields a chloroethyl derivative. Metal complexes of the new derivatized macrocyclic ligands L3-6having general formula ML3-6X2.nH2O (M = Mn, Fe, Co, Ni, Cu, Zn are readily prepared.

  20. Complexes of 3.6 kDa Maltodextrin with Some Metals

    Christopher H. Schilling

    2004-06-01

    Full Text Available Preparation of magnesium, lanthanum, and bismuth(III complexes of 3.6 kDa maltodextrin and some properties of the resulting materials are presented. The metal derivatives contain metals bound to the oxygen atoms of the hydroxyl groups of maltodextrin. Additionally, the metal atoms are coordinated to the hydroxyl groups of the D-glucose units of the macroligand. Such coordination stabilized the metal – oxygen bond against hydrolysis, even in boiling water. The presence of magnesium and lanthanum atoms increased the thermal stability of maltodextrin, whereas bismuth atoms decreased it.

  1. Plasmon hybridization in complex metallic nanostructures

    Hao, Feng

    With Plasmon Hybridization (PH) and Finite-Difference Time-Domain (FDTD) method, we theoretically investigated the optical properties of some complex metallic nanostructures (coupled nanoparticle/wire, nanostars, nanorings and combined ring/disk nanocavity systems). We applied the analytical formulism of PH studying the plasmonic coupling of a spherical metallic nanoparticle and an infinite long cylindrical nanowire. The plasmon resonance of the coupled system is shown shifted in frequency, which highly depends on the polarization of incident light relative to the geometry of the structure. We also showed the nanoparticle serves as an efficient antenna coupling the electromagnetic radiation into the low-energy propagating wire plasmons. We performed an experimental and theoretical analysis of the optical properties of gold nanorings with different sizes and cross sections. For light polarized parallel to the ring, the optical spectrum sensitively depends on the incident angle. When light incidence is normal to the ring, two dipolar resonance is observed. As the incident light is titled, some previously dark mulipolar plasmon resonances will be excited as a consequence of the retardation. The concept of plasmon hybridization is combined with the power of brute-force numerical methods to understand the plasmonic properties of some very complicated nanostructures. We showed the plasmons of a gold nanostar are a result of hybridization of the plasmons of the core and the tips of the particle. The core serves as a nanoantenna, dramatically enhanced the optical spectrum and the field enhancement of the nanostar. We also applied this method analyzing the plasmonic modes of a nanocavity structure composed of a nanodisk with a surrounding minoring. For the concentric combination, we showed the nature of the plasmon modes can be understood as the plasmon hybrization of an individual ring and disk. The interation results in a blueshifted and broadened superradiant antibonding

  2. Superconductivity of ternary metal compounds prepared at high pressures

    Shirotani, I

    2003-01-01

    Various ternary metal phosphides, arsenides, antimonides, silicides and germanides have been prepared at high temperatures and high pressures. These ternary metal compounds can be classified into four groups: [1] metal-rich compounds MM' sub 4 X sub 2 and [2] MM'X, [3] non-metal-rich compounds MXX' and [4] MM' sub 4 X sub 1 sub 2 (M and M' = metal element; X and X' = non-metal element). We have studied the electrical and magnetic properties of these materials at low temperatures, and found many new superconductors with the superconducting transition temperature (T sub c) of above 10 K. The metal-rich compound ZrRu sub 4 P sub 2 with a tetragonal structure showed the superconducting transition at around 11 K, and had an upper critical field (H sub c sub 2) of 12.2 tesla (T) at 0 K. Ternary equiatomic compounds ZrRuP and ZrRuSi crystallize in two modifications, a hexagonal Fe sub 2 P-type structure [h-ZrRuP(Si)] and an orthorhombic Co sub 2 P-type structure [o-ZrRuP(Si)]. Both h-ZrRuP and h-ZrRuSi have rather h...

  3. 40 CFR 721.4596 - Diazo substituted carbomonocyclic metal complex.

    2010-07-01

    ... 40 Protection of Environment 30 2010-07-01 2010-07-01 false Diazo substituted carbomonocyclic... Specific Chemical Substances § 721.4596 Diazo substituted carbomonocyclic metal complex. (a) Chemical... as a diazo substituted carbomonocyclic metal complex (PMN P-94-1039) is subject to reporting under...

  4. Tris-diamine-derived transition metal complexes of flurbiprofen as ...

    admin

    butyrylcholinesterase (BChE) inhibitory activities. Method: Tris-diamine-derived transition metal complexes of Co(II), Ni(II), and Mn(II) were synthesized and characterized ... Conductance measurements indicated that diamine-derived metal complexes of ..... contributes to enhanced biological activity, and provides novel ...

  5. Mixed Metal Complexes of Isoniazid and Ascorbic Acid: Chelation ...

    HP

    these ligands and their metal complexes have revealed the bi-dentate coordination of isoniazid ligand to ... of the drugs on coordination with a metal is enhanced ..... James, O.O., Nwinyi, C.O. and. Allensela, M.A. (2008). Cobalt(II) complexes of mixed antibiotics: Synthesis,. Characterization, antimicrobial potential and their.

  6. Metallacyclopentadienes: structural features and coordination in transition metal complexes

    Dolgushin, Fedor M; Yanovsky, Aleksandr I; Antipin, Mikhail Yu

    2004-01-01

    Results of structural studies of polynuclear transition metal complexes containing the metallacyclopentadiene fragment are overviewed. The structural features of the complexes in relation to the nature of the substituents in the organic moiety of the metallacycles, the nature of the transition metals and their ligand environment are analysed. The main structural characteristics corresponding to different modes of coordination of metallacyclopentadienes to one or two additional metal centres are revealed.

  7. Characterization of La2MoO6 prepared by the cation complexation technique

    Rocha, R.A.; Muccillo, E.N.S.

    2005-01-01

    The La 2 MoO 6 mixed oxide was prepared by the cation complexation technique using citric acid as complexant agent. The main purpose of this work was to obtain a mesoporous powder with relatively high specific surface area. The thermal decomposition behavior of the metal complex was studied by thermal analysis and Fourier transform infrared spectroscopy. A specific surface area value of ∼15 m 2 g -1 was obtained by nitrogen adsorption/desorption measurements. X-ray diffraction patterns of calcined mesoporous materials reveal that even though a low degree of crystallinity is attained, this phase may be obtained at low temperatures

  8. Radiation chemical route for preparation of metal nanoparticles

    Kapoor, S.; Mukherjee, T.

    2006-01-01

    Nanoparticles show properties that are neither seen in the bulk or at atomic level. The unusual properties are governed by quantum size effect. Due to this various methodologies have been endeavored to control the size of the particles. In the present work we show the use of two complimentary techniques (radiation and photo) to synthesize and control the size of the metal particles. In-situ synthesis of fine silver, thallium and cadmium particles has been carried out by gamma-irradiation and electron pulse irradiation at room temperature in the pre-organized gel of polyacrylamide or cyclodextrin cavity. The role of generation of nuclei in high concentrations in stabilization of metal nanoparticles in hydrophobic cavity is shown. Similarly the importance of entrapment of metal ions in the polymer matrix during its formation is highlighted. The work is further extended to exploit the microemulsion droplets for stabilization of Cd nanoparticles. Utility of pulse radiolysis in probing the mechanism of the formation of metal nanoparticles is also shown. Ultrafast laser pulses were employed to control the morphology of the pre-prepared Pt nanoparticles. The changes in reduction of shape and size are considered to occur through melting and vaporization of the nanoparticles. Pt nanoparticles were coated on the inner walls of the tubular pyrex reactor and tested for their catalytic activity for oxidation of CO. It was observed that Pt nanoparticles prepared in the presence of a stabilizer (gelatin) showed a higher tendency to adhere to the inner walls of the pyrex reactor as compared to that prepared in the presence of silica nanoparticles. The catalyst was found to be active at ≥150 degree C giving CO 2 . Chemically reduced Pt nanoparticles stabilized on silica nanoparticles gave ∼7% CO conversion per hr. However, radiolytically prepared Pt nanoaprticles stabilized by gelatin gave ∼10% conversion per hr. The data indicates that catalytic oxidation of CO takes place

  9. Synthesis and characterization of transition metal complexes derived from some biologically active furoic acid hydrazones

    P. Venkateswar Rao

    2007-04-01

    Full Text Available Two new physiologically active ligands, N’-2-[(E-1-hydroxy-4-methyl-2-oxo-2H-8-chromenyl ethylidene-2-furan carbohydrazide (HMCFCH and N’-2-[(Z-1-(4-hydroxy-6-methyl-2-oxo-2H-pyranyl ethylidene]-furan carbohydrazide (HMPFCH and their VO(II, Mn(II, Fe(II, Co(II, Ni(II and Cu(II complexes have been prepared. The ligands and the metal complexes have been characterized by elemental analyses, electrical conductance, magnetic susceptibility measurements, UV-Vis, IR, and ESR spectroscopic data. Basing on the above data, Fe(II and Co(II complexes of HMCFCH and HMPFCH have been assigned a dimeric octahedral geometry. VO(II complexes of HMCFCH and HMPFCH have been assigned sulfate bridged dimeric square pyramidal geometry. Mn(II complex of HMCFCH has been assigned a dimeric octahedral geometry, where as Mn(II complex of HMPFCH has been ascribed to monomeric octahedral geometry. Cu(II and Ni(II complexes of HMCFCH have been ascribed to a polymeric structure. Ni(II complex of HMPFCH has been assigned a dimeric square planar geometry. Cu(II complex of HMPFCH has been proposed an octahedral geometry. The ligands and their metal chelates were screened against S. aureus and P. aeruginosa. The ligands and the metal complexes have been found to be active against these microorganisms. The ligands show more activity than the metal complexes.

  10. N-heterocyclic carbene metal complexes as bio-organometallic antimicrobial and anticancer drugs.

    Patil, Siddappa A; Patil, Shivaputra A; Patil, Renukadevi; Keri, Rangappa S; Budagumpi, Srinivasa; Balakrishna, Geetha R; Tacke, Matthias

    2015-01-01

    Late transition metal complexes that bear N-heterocyclic carbene (NHC) ligands have seen a speedy growth in their use as both, metal-based drug candidates and potentially active homogeneous catalysts in a plethora of C-C and C-N bond forming reactions. This review article focuses on the recent developments and advances in preparation and characterization of NHC-metal complexes (metal: silver, gold, copper, palladium, nickel and ruthenium) and their biomedical applications. Their design, syntheses and characterization have been reviewed and correlated to their antimicrobial and anticancer efficacies. All these initial discoveries help validate the great potential of NHC-metal derivatives as a class of effective antimicrobial and anticancer agents.

  11. Photochemical activation and reactivity of polynuclear transition-metal-complex molecules. Progress report, June 1981-May 31, 1982

    Endicott, J.F.; Lintvedt, R.L.

    1982-01-01

    Significant results obtained during the year are summarized for the following programs: (1) reversible, two electron transfer at a single potential in binuclear complexes; (2) photophysics of polyketonate complexes; (3) synthetic strategies and characterization of heavy metal heterobinuclear complexes; (4) high yield synthesis of ligands capable of binding 3 and 4 metal ions per molecule. Electrochemical studies have uncovered a number of new binuclear metal complexes that undergo reversible two-electron reduction at single potential including Cu(II) complexes with two different coordination environments, mixed Ni(II), Cu(II) complexes and binuclear Ni(II) complexes. In each case the species that exhibit these electron transfer properties have been shown to be Na + ion-paired complexes. Several new trinuclear molecular complexes have been prepared and characterized that contain two UO 2 2+ ions and one transition metal ion. The electrochemistry, absorption spectra, and luminescence have been investigated

  12. Preparation of microcellular foam in cylindrical metal targets

    Apen, P.G.; Armstrong, S.V.; Moore, J.E.; Espinoza, B.F.; Gurule, V.; Gobby, P.L.; Williams, J.M.

    1992-01-01

    The preparation of microcellular foam in cylindrical gold targets is described. The goal cylinders were fabricated by electroplating gold onto a silicon bronze mandrel and leaching the mandrel with concentrated nitric acid. After several rinsing and cleaning steps, the cylinders were filled with a solution containing trimethylolpropanetriacrylate (TMPTA). Low density, microcellular polymeric foam was prepared by in situ photopolymerization of the TMPTA solution. Foam preparation was extremely sensitive to metal ion contaminants. In particular, copper ions left behind from the leaching process inhibit polymerization and must be removed in order to obtain uniform, non-shrinking foams. A study on the effects of potential contaminants and polymerization inhibitors on TMPTA photopolymerization is presented. In addition, a procedure for the effective leaching and cleaning of gold cylinders is described

  13. Preparation and characterization of uranium alkoxides through oxidation of uranium metal

    Gordon, P.L.; Sauer, N.N.; Burns, C.J.; Watkin, J.G.; Van Der Sluys, W.G.

    1993-01-01

    Currently the authors are investigating the preparation of halide-containing uranium alkoxides by simultaneous halogen and alcohol oxidation of uranium metal. They recently reported the formation of U 2 I 4 (O-i-Pr) 4 (HO-i-Pr) 2 which upon addition of excess isopropanol forms UI 2 (O-i-Pr) 2 (HO-i-Pr) 2 . They report further characterization and reactivity for this monomeric species. Attempts to prepare similar complexes are being made using chlorine gas in the presence of other alcohols. They describe this ongoing research

  14. Bridging-ligand-substitution strategy for the preparation of metal-organic polyhedra

    Li, Jian-Rong; Zhou, Hong-Cai

    2010-10-01

    Metal-organic polyhedra-discrete molecular architectures constructed through the coordination of metal ions and organic linkers-have recently attracted considerable attention due to their intriguing structures, their potential for a variety of applications and their relevance to biological self-assembly. Several synthetic routes have been investigated to prepare these complexes. However, to date, these preparative methods have typically been based on the direct assembly of metal ions and organic linkers. Although these routes are convenient, it remains difficult to find suitable reaction conditions or to control the outcome of the assembly process. Here, we demonstrate a synthetic strategy based on the substitution of bridging ligands in soluble metal-organic polyhedra. The introduction of linkers with different properties from those of the initial metal-organic polyhedra can thus lead to new metal-organic polyhedra with distinct properties (including size and shape). Furthermore, partial substitution can also occur and form mixed-ligand species that may be difficult to access by means of other approaches.

  15. Reactivity of monoolefin ligand in transition metal complexes

    Rybinskaya, M.I.

    1978-01-01

    The main tendencies in the coordinated olefin ligand property changes are discussed in the transition metal complexes in comparison with free olefins. The review includes the papers published from 1951 up to 1976. It has been shown that in complexes with transition metal cations olefin π-base acquires the ability to react with nucleophylic reagents. Olefin π-acids in complexes with zero valent metals are easily subjected to electrophylic reagent action. At coordination with transition metal cations the olefin properties are generally preserved, while in the zero-valent metal complexes the nonsaturated ligand acquires the properties of a saturated compounds. The ability of transition metal cations in complexes to intensify reactions of nucleophylic bimolecular substitution of vinyl halogen is clearly detected in contrast to the zero valent metal complexes. It has been shown that investigations of the coordinated olefin ligand reactivity give large possibilities in the further development of the organic synthesis. Some reactions are taken as the basis of important industrial processes

  16. Preparation and Characterization of a Complex of Paeonol and ...

    Methods: The complex of paeonol and HP-β-CD was prepared by freeze-drying method. Its physicochemical properties were studied by phase-solubility method, ultraviolet-visible spectrometry (UV), infrared spectrometry (IR), scanning electron microscopy (SEM), x-ray diffractometry (XRD) and thermogravimetric/differential ...

  17. N-acyl thioureas - selective ligands for complexing of heavy metals and noble metals

    Schuster, M.

    1992-01-01

    Acyl thioureas are complexing agents for heavy metals that are easily produced and very stable. Their favourable toxicological data make them particularly suitable for industrial applications, e.g. detoxification of metallic process solutions or solvent extraction of metals. (orig.) [de

  18. Alkylation and arylation of alkenes by transition metal complexes

    Volkova, L.G.; Levitin, I.Ya.; Vol'pin, M.E.

    1975-01-01

    In this paper are reviewed methods of alkylation and irylation of unsaturated compounds with complexes of transition metals (Rh, Pd). Analysis of alkylation and arylation of olefines with organic derivatives of transition metals, obtained as a result of exchange reactions between organic compounds of transition metals and salts of metals of the 8th group of the periodic system, allows a conclusion as to the wide possibilities of these reactions in the synthesis of various derivatives of unsaturated compounds. In all the reactions under consideration, intermediate formation of sigma-complexes is assumed. Also considered are alkylation and arylation of olefines with organic derivatives of halogens in the presence of compounds of metals of the 8th group of the periodic system, as well as arylation of olefines with aromatic compounds in the presence of salts of transition metals

  19. Kinetics of the reactions of hydrated electrons with metal complexes

    Korsse, J.

    1983-01-01

    The reactivity of the hydrated electron towards metal complexes is considered. Experiments are described involving metal EDTA and similar complexes. The metal ions studied are mainly Ni 2+ , Co 2+ and Cu 2+ . Rates of the reactions of the complexes with e - (aq) were measured using the pulse radiolysis technique. It is shown that the reactions of e - (aq) with the copper complexes display unusually small kinetic salt effects. The results suggest long-range electron transfer by tunneling. A tunneling model is presented and the experimental results are discussed in terms of this model. Results of approximate molecular orbital calculations of some redox potentials are given, for EDTA chelates as well as for series of hexacyano and hexaquo complexes. Finally, equilibrium constants for the formation of ternary complexes are reported. (Auth./G.J.P.)

  20. Thiosemicarbazone complexes of the platinum metals. A story of ...

    Unknown

    Thiosemicarbazone complexes; platinum metals; variable coordination; ... carbonylic carbon via one or two intervening atoms, D,N,S tricoordination usually takes .... modelling studies show that in this coordination mode, the phenyl ring of the.

  1. 3d-METAL COMPLEXES WITH BARBITURIC ACID DERIVATIVES

    T. V. Koksharova

    2015-04-01

    Full Text Available The various aspects of the 3d-metal complexes with barbiturates and uric acid chemistry such as composition, structure, physicochemical properties, possible fields of application – have been illustrated in this review

  2. Structural systematics of some metal complexes with 4,5 ...

    study reveals that each metal(II) centre in the four complexes adopts distorted octahedral geometry with MN6 ... potassium permanganate (E Merck, India), potassium. 717 ... The final reaction solu- ..... ble in water, methanol, acetonitrile, etc.

  3. Sub-chronic toxicological studies of transition metal complexes of ...

    Md. Sharif Hasan

    2017-01-18

    Jan 18, 2017 ... naproxen showed more side effects than metal complexes which ..... Fosslein E. Adverse effects of nonsteroidal anti-inflammatory drugs on the ... association increases the anti-inflammatory and analgesic activity of ibuprofen.

  4. Synthesis and characterization of some metal complexes of a Schiff ...

    KEY WORDS: Metal complexes, Schiff base, Ninhydrin, α,L-Alanine, .... Buck Scientific Infrared Spectrophotometer Model 500 in the range of 4000 .... Assignments based on Nakamoto [35], ν - stretching vibration, δ - bending or deformation.

  5. Bovine Serum Albumin Metal Complexes for Mimic of SOD

    Key Lab. Eco-Environment-Related Polymer Materials of Ministry of Education, Key Lab. ... scaffold and the metal complex functioned as the catalytic active center. ... small molecule.22 It is found that the antioxidative ... and absence, respectively, of the measured compound. ... monitor the interaction of metal ions with BSA.

  6. Inkjet Printing of 3D Metallic Silver Complex Microstructures

    Wits, Wessel Willems; Sridhar, Ashok; Dimitrov, D.

    2010-01-01

    To broaden the scope of inkjet printing, this paper focuses on printing of an organic silver complex ink on glass substrates towards the fabrication of metallic 3D microstructures. The droplet formation sequence of the inkjet printer is optimised to print continuous layers of metal. A brief

  7. Revisited: the conception of lability of metal complexes

    Leeuwen, van H.P.

    2001-01-01

    Starting from the original reaction layer concept, the voltammetric properties of electroinactive metal complexes are critically reviewed in terms of their finite rates of dissociation into electroactive free metal ions. The limiting conditions for the reaction layer-based flux expressions are made

  8. Studies concerning the preparation of the 153Sm complex with EDTMP (ethylenediaminetetra methylenephosphonic acid) and other 153Sm complexes with other phosphonates, at room temperature

    Gasiglia, Haroldo Taurian

    2000-01-01

    This work presents a study on the preparation of the complexes 1 53S m - EDTMP, 153 Sm - HEDP, 153 Sm - NTMP, 153 Sm - DTPMP and 153 Sm - HDTMP at room temperature. The preparation of the complex 153 Sm - HDTMP, under heating (70 - 72 deg C), was also studied. Several factors affecting the 153 Sm - EDTMP complexing yields were studied, due to its importance for use in Nuclear Medicine. These factors were: the molar ratio [ligand] / [metal], the ligand concentration and the incubation time of the mixture ligand-metal. The preparation of this complex, in low molar ratios, was also investigated. A study of the 153 Sm - EDTMP concerning the 'in vitro' stability, when this complex was prepared in low radioactive concentrations was performed. A study on the temperature influence on its degradation, when this complex was obtained in higher radioactive concentrations, was also performed. The preparation of the complexes 153 Sm - HEDP, 153 Sm - NTMP, 153 Sm - DTPMP and 153 Sm - HDTMP was investigated by preparing the complexes in two situations: high molar ratio and ligand concentration and low molar ratio and ligand concentration. The 'in vitro' stability of each complex, obtained in low radioactive concentration was studied. In the specific case of the complex 153 Sm - HDTMP, its biological distribution in mice was performed. All the complexes were investigated by high performance liquid chromatography (HPLC) and its complexing yields were determined by other three chromatographic processes: ionic exchange, thin layer chromatography (TLC - SG) and paper chromatography. The chromatographic processes were performed by association with specific radiochemical techniques. This work also presents a comparative study on the chromatograms obtained by thin layer chromatography (TLC - SG) and paper chromatography, when evaluated by the technique of cutting the strips into pieces and the chromatograms performed directly on a radiochromatography. The shape of the chromatograms and R

  9. Compartmentation and complexation of metals in hyperaccumulator plants

    Barbara eLeitenmaier

    2013-09-01

    Full Text Available Hyperaccumulators are being intensely investigated. They are not only interesting in scientific context due to their strange behaviour in terms of dealing with high concentrations of metals, but also because of their use in phytoremediation and phytomining, for which understanding the mechanisms of hyperaccumulation is crucial. Hyperaccumulators naturally use metal accumulation as a defence against herbivores and pathogens, and therefore deal with accumulated metals in very specific ways of complexation and compartmentation, different from non-hyperaccumulator plants and also non-hyperaccumulated metals. For example, in contrast to non-hyperaccumulators, in hyperaccumulators even the classical phytochelatin-inducing metal, cadmium, is predominantly not bound by such sulfur ligands, but only by weak oxygen ligands. This applies to all hyperaccumulated metals investigated so far, as well as hyperaccumulation of the metalloid arsenic. Stronger ligands, as they have been shown to complex metals in non-hyperaccumulators, are in hyperaccumulators used for transient binding during transport to the storage sites. This confirmed that enhanced active metal transport, and not metal complexation, is the key mechanism of hyperaccumulation. Hyperaccumulators tolerate the high amount of accumulated heavy metals by sequestering them into vacuoles, usually in large storage cells of the epidermis. This is mediated by strongly elevated expression of specific transport proteins in various tissues from metal uptake in the shoots up to the storage sites in the leaf epidermis. However, this mechanism seems to be very metal specific. Non-hyperaccumulated metals in hyperaccumulators seem to be dealt with like in non-hyperaccumulator plants, i.e. detoxified by binding to strong ligands such as metallothioneins.

  10. Preparation of lead titanate zirconate from metal citrates

    Bastos, C.M.R.

    1994-01-01

    Lead titanate zirconate (PZT) preparation from its metal constituent citrates have been investigated. Metal citrates were obtained by forced precipitation using a dehydration alcohol mixture. Salt solutions of lead nitrate and octahydrated zirconyl chloride, and titanium tetrachloride were treated separately with citric acid and ammonium hydroxide. Zirconium, titanium and lead oxides resulted from thermal decomposition of corresponding citrates at 500 0 C, 450 0 C and 250 0 C, respectively. Lead titanate (PT) and lead zirconate (P Z) were obtained by calcining at 450 0 C and 500 0 C, respectively, after adequate heating of citrates mechanically mixed in ethyl ether. PZT samples were obtained with different starting stoichiometry. Rhombohedral PZT-1 53/47 sample was prepared from co precipitating zirconyl ammonium and ammonium lead citrates in presence of ethanolic titanium oxide dispersion, and calcinating at 800 0 C. Rhombohedral PZT-q 52/48 sample was obtained from heating at 500 0 C for 2 hours a mixture of metal citrates coprecipitated by dehydration mixture of acetone-ethanol-formic acid (2:1:0,06). Tetragonal PZT-m stoichiometry 53/47 sample were obtained by calcining at after 600 0 C for 2 hours after heating a mechanically mixed metal citrates. PT phase arose at 400 0 C. PZT-m powders obtained in a range of 400 0 C-800 0 C were isostatically pressed, and sintered at 1100 0 C and 1200 0 C in saturated Pb O atmosphere. Rhombohedral sintered PZT was obtained with 7,78 g.cm -3 at 1200 0 C. (author). 123 refs, 53 figs, 32 tabs

  11. Preparation of self-supporting metallic foils of nickel isotopes

    Sugai, Isao.

    1975-01-01

    This is the fourth report on the practical methods of target preparation for use in low energy nuclear experiments following the previous one (INS-J-150). An electroplating method has been developed as a dependable and reproducible technique for making self-supporting metallic foils of nickel in the thickness range of 0.5 to 10 mg/cm 2 . The procedures minimized the necessary amount of material so that nickel isotopes could be processed economically. Impurity contamination of the nickel foils during the electroplating process was less than 500 ppm, and the thickness variation in each foil was less than 3% of the central thickness. (auth.)

  12. Lability of nanoparticulate metal complexes in electrochemical speciation analysis

    van Leeuwen, Herman P.; Town, Raewyn M.

    2016-01-01

    Lability concepts are elaborated for metal complexes with soft (3D) and hard (2D) aqueous nanoparticles. In the presence of a non-equilibrium sensor, e.g. a voltammetric electrode, the notion of lability for nanoparticulate metal complexes, M-NP, reflects the ability of the M-NP to maintain...... equilibrium with the reduced concentration of the electroactive free M2+ in its diffusion layer. Since the metal ion binding sites are confined to the NP body, the conventional reaction layer in the form of a layer adjacent to the electrode surface is immaterial. Instead an intraparticulate reaction zone may...... of the electrochemical technique is crucial in the lability towards the electrode surface. In contrast, for nanoparticulate complexes it is the dynamics of the exchange of the electroactive metal ion with the surrounding medium that governs the effective lability towards the electrode surface....

  13. Metal plasmon enhanced europium complex luminescence

    Liu Feng; Aldea, Gabriela; Nunzi, Jean-Michel

    2010-01-01

    The plasmon enhanced luminescence of a rare-earth complex Tris(6, 6, 7, 7, 8, 8, 8-heptafluoro-2, 2-dimethyl-3, 5-octanedionato) europium (Eu(fod) 3 ) was investigated. A polyvinyl alcohol (PVA) thin film was successfully adopted as a spacer to separate the Eu complex from the silver island film (SIF), and five-fold enhancement of the radiative decay rate of the Eu complex on SIF was demonstrated based on the luminescence intensity and lifetime measurement. Investigation of the distance dependent luminescence indicates that 7 nm is an optimal distance for SIF enhanced Eu luminescence. Plasmon enhanced rare-earth luminescence based on an organic film spacer would find potential applications in plasmon enhanced organic light emitting diode (OLED) devices.

  14. Photochemical activation and reactivity of polynuclear transition metal complex molecules. Final report

    Endicott, J.F.; Lintvedt, R.L.

    1982-06-01

    Several bi- and trinuclear metal complexes containing ligands from β-polyketonates have been synthesized and characterized including homo- and hetero-polynuclear complexes. New synthetic approaches to the preparation of heterobi- and trinuclear complexes have been developed that allow the preparation of a large number of molecules containing heavy-metal ions such as Pd 2+ or UO 2 2+ and a first-row transition-metal ion. The electrochemical properties of these complexes have been investigated and many exhibit the ability to transfer two electrons at very nearly the same potential. Photochemical studies on binuclear Cu(II) and Ni(II) showed that these compounds yielded reduced metal species and decomposition upon irradiation. Luminescence of hetero-complexes of uranyl polyketonates is observed at 77 0 K with the UO 2 2+ moiety functioning as an isolated chromophore in which emission is observed only on direct excitation of UO 2 2+ and energy transfer to lower states in the molecule is not observed

  15. Mixed metal complexes of isoniazid and ascorbic acid: chelation ...

    Novel mixed complexes of isoniazid and ascorbic acid have been synthesized and characterized using infrared, electronic absorption data, elemental analysis, molar conductivity, melting point, thin layer chromatography and solubility. The metal ions involved in the complex formation are Cu2+, Zn2+ and Cd2+. The melting ...

  16. Metal complex catalysis in the synthesis of organoaluminium compounds

    Dzhemilev, Usein M; Ibragimov, Askhat G

    2000-01-01

    The published data on the synthesis of organoaluminium compounds involving metal complex catalysts are generalised and systematised. Hydro-, carbo- and cycloalumination reactions of alkenes, conjugated dienes and alkynes catalysed by Ti and Zr complexes are considered in detail. The use of organoaluminium reagents in organic synthesis and novel reactions involving these compounds are discussed. The bibliography includes 240 references.

  17. An Experiment on Isomerism in Metal-Amino Acid Complexes.

    Harrison, R. Graeme; Nolan, Kevin B.

    1982-01-01

    Background information, laboratory procedures, and discussion of results are provided for syntheses of cobalt (III) complexes, I-III, illustrating three possible bonding modes of glycine to a metal ion (the complex cations II and III being linkage/geometric isomers). Includes spectrophotometric and potentiometric methods to distinguish among the…

  18. Preparation and properties of amylose complexes prepared from hexadecylamine and its hydrochloride salt

    Amylose inclusion complexes were prepared from jet-cooked aqueous mixtures of high amylose corn starch and 1-hexadecylamine (HDA). Slow-cooling produced torus/disc-shaped spherulites, whereas aggregates of smaller spherulites were obtained by rapid-cooling in ice. The morphologies and 6(1)V x-ray ...

  19. DFT study on metal-mediated uracil base pair complexes

    Ayhan Üngördü

    2017-11-01

    Full Text Available The most stable of metal-mediated uracil base pair complexes were determined. Method was used density functional theory, B3LYP. The calculations of systems containing C, H, N, O were described by 6-311++G(d,p and cc-PVTZ basis sets and LANL2DZ and SDD basis sets was used for transition metals. Then Egap values of complexes were calculated and the electrical conductivity of the complexes for single nanowires was studied by band theory. Metal-mediated uracil base pair complexes which will be used as conductive wires in nanotechnology were predicted. In nanoworld, this study is expected to show a way for practical applications.

  20. Facile preparation of superhydrophobic surfaces based on metal oxide nanoparticles

    Bao, Xue-Mei; Cui, Jin-Feng; Sun, Han-Xue; Liang, Wei-Dong; Zhu, Zhao-Qi; An, Jin; Yang, Bao-Ping; La, Pei-Qing; Li, An

    2014-06-01

    A novel method for fabrication of superhydrophobic surfaces was developed by facile coating various metal oxide nanoparticles, including ZnO, Al2O3 and Fe3O4, on various substrates followed by treatment with polydimethylsiloxane (PDMS) via chemical vapor deposition (CVD) method. Using ZnO nanoparticles as a model, the changes in the surface chemical composition and crystalline structures of the metal oxide nanoparticles by PDMS treatment were investigated by X-ray photoelectron spectroscopy (XPS), X-ray powder diffraction (XRD) and Fourier transform infrared (FTIR) analysis. The results show that the combination of the improved surface roughness generated from of the nanoparticles aggregation with the low surface-energy of silicon-coating originated from the thermal pyrolysis of PDMS would be responsible for the surface superhydrophobicity. By a simple dip-coating method, we show that the metal oxide nanoparticles can be easily coated onto the surfaces of various textural and dimensional substrates, including glass slide, paper, fabric or sponge, for preparation of superhydrophobic surfaces for different purpose. The present strategy may provide an inexpensive and new route to surperhydrophobic surfaces, which would be of technological significance for various practical applications especially for separation of oils or organic contaminates from water.

  1. Facile preparation of superhydrophobic surfaces based on metal oxide nanoparticles

    Bao, Xue-Mei; Cui, Jin-Feng; Sun, Han-Xue; Liang, Wei-Dong; Zhu, Zhao-Qi; An, Jin; Yang, Bao-Ping; La, Pei-Qing; Li, An

    2014-01-01

    A novel method for fabrication of superhydrophobic surfaces was developed by facile coating various metal oxide nanoparticles, including ZnO, Al 2 O 3 and Fe 3 O 4 , on various substrates followed by treatment with polydimethylsiloxane (PDMS) via chemical vapor deposition (CVD) method. Using ZnO nanoparticles as a model, the changes in the surface chemical composition and crystalline structures of the metal oxide nanoparticles by PDMS treatment were investigated by X-ray photoelectron spectroscopy (XPS), X-ray powder diffraction (XRD) and Fourier transform infrared (FTIR) analysis. The results show that the combination of the improved surface roughness generated from of the nanoparticles aggregation with the low surface-energy of silicon-coating originated from the thermal pyrolysis of PDMS would be responsible for the surface superhydrophobicity. By a simple dip-coating method, we show that the metal oxide nanoparticles can be easily coated onto the surfaces of various textural and dimensional substrates, including glass slide, paper, fabric or sponge, for preparation of superhydrophobic surfaces for different purpose. The present strategy may provide an inexpensive and new route to surperhydrophobic surfaces, which would be of technological significance for various practical applications especially for separation of oils or organic contaminates from water.

  2. Facile preparation of superhydrophobic surfaces based on metal oxide nanoparticles

    Bao, Xue-Mei; Cui, Jin-Feng; Sun, Han-Xue; Liang, Wei-Dong; Zhu, Zhao-Qi; An, Jin; Yang, Bao-Ping; La, Pei-Qing; Li, An, E-mail: lian2010@lut.cn

    2014-06-01

    A novel method for fabrication of superhydrophobic surfaces was developed by facile coating various metal oxide nanoparticles, including ZnO, Al{sub 2}O{sub 3} and Fe{sub 3}O{sub 4}, on various substrates followed by treatment with polydimethylsiloxane (PDMS) via chemical vapor deposition (CVD) method. Using ZnO nanoparticles as a model, the changes in the surface chemical composition and crystalline structures of the metal oxide nanoparticles by PDMS treatment were investigated by X-ray photoelectron spectroscopy (XPS), X-ray powder diffraction (XRD) and Fourier transform infrared (FTIR) analysis. The results show that the combination of the improved surface roughness generated from of the nanoparticles aggregation with the low surface-energy of silicon-coating originated from the thermal pyrolysis of PDMS would be responsible for the surface superhydrophobicity. By a simple dip-coating method, we show that the metal oxide nanoparticles can be easily coated onto the surfaces of various textural and dimensional substrates, including glass slide, paper, fabric or sponge, for preparation of superhydrophobic surfaces for different purpose. The present strategy may provide an inexpensive and new route to surperhydrophobic surfaces, which would be of technological significance for various practical applications especially for separation of oils or organic contaminates from water.

  3. Group 4 Metalloporphyrin diolato Complexes and Catalytic Application of Metalloporphyrins and Related Transition Metal Complexes

    Du, Guodong [Iowa State Univ., Ames, IA (United States)

    2003-01-01

    In this work, the first examples of group 4 metalloporphyrin 1,2-diolato complexes were synthesized through a number of strategies. In general, treatment of imido metalloporphyrin complexes, (TTP)M=NR, (M = Ti, Zr, Hf), with vicinal diols led to the formation of a series of diolato complexes. Alternatively, the chelating pinacolate complexes could be prepared by metathesis of (TTP)MCl2 (M = Ti, Hf) with disodium pinacolate. These complexes were found to undergo C-C cleavage reactions to produce organic carbonyl compounds. For titanium porphyrins, treatment of a titanium(II) alkyne adduct, (TTP)Ti(η2-PhC≡CPh), with aromatic aldehydes or aryl ketones resulted in reductive coupling of the carbonyl groups to produce the corresponding diolato complexes. Aliphatic aldehydes or ketones were not reactive towards (TTP)Ti(η2-PhC≡CPh). However, these carbonyl compounds could be incorporated into a diolato complex on reaction with a reactive precursor, (TTP)Ti[O(Ph)2C(Ph)2O] to provide unsymmetrical diolato complexes via cross coupling reactions. In addition, an enediolato complex (TTP)Ti(OCPhCPhO) was obtained from the reaction of (TTP)Ti(η2-PhC≡CPh) with benzoin. Titanium porphyrin diolato complexes were found to be intermediates in the (TTP)Ti=O-catalyzed cleavage reactions of vicinal diols, in which atmospheric oxygen was the oxidant. Furthermore, (TTP)Ti=O was capable of catalyzing the oxidation of benzyl alcohol and α-hydroxy ketones to benzaldehyde and α-diketones, respectively. Other high valent metalloporphyrin complexes also can catalyze the oxidative diol cleavage and the benzyl alcohol oxidation reactions with dioxygen. A comparison of Ti(IV) and Sn(IV) porphyrin chemistry was undertaken. While chelated diolato complexes were invariably obtained for titanium porphyrins on treatment with 1,2-diols, the reaction of vicinal diols with tin porphyrins gave a number of products, including mono

  4. Preparation and characterizations of new U(IV) and U(VI) complexes with carboxylate ligands

    Sbrignadello, G; Tomat, G; Battiston, G; Vigato, P A [Consiglio Nazionale delle Ricerche, Padua (Italy). Lab. di Chimica e Tecnologia dei Radioelementi

    1978-01-01

    The synthesis and characterization of some uranyl(VI) complexes containing glycolate (gly = CH/sub 2/OHCOO/sup -/) and methoxyacetate (MeOAc = CH/sub 3/OCH/sub 2/COO/sup -/) ligands with metal:ligand ratios of 1:1 and 1:2 are reported. In addition, new stable uranium(IV) complexes containing the same ligands, or the oxydiacetate (oda = /sup -/OOCCH/sub 2/OCH/sub 2/COO/sup -/) anion, have been prepared by photolysing aqueous solutions of uranyl(VI) nitrate in the presence of an excess of ligand. The possible structures of these complexes are discussed on the basis of IR results. The photoproduction mechanism of U(IV) complexes is proposed from electronic and spectrofluorimetric spectra and quantum yield data.

  5. Spectroscopic characterization of metal complexes of novel Schiff base. Synthesis, thermal and biological activity studies

    Omar, M. M.; Mohamed, Gehad G.; Ibrahim, Amr A.

    2009-07-01

    Novel Schiff base (HL) ligand is prepared via condensation of 4-aminoantipyrine and 2-aminobenzoic acid. The ligand is characterized based on elemental analysis, mass, IR and 1H NMR spectra. Metal complexes are reported and characterized based on elemental analyses, IR, 1H NMR, solid reflectance, magnetic moment, molar conductance and thermal analyses (TGA, DrTGA and DTA). The molar conductance data reveal that all the metal chelates are non-electrolytes. IR spectra show that HL is coordinated to the metal ions in a uninegatively tridentate manner with NNO donor sites of the azomethine N, amino N and deprotonated caroxylic-O. From the magnetic and solid reflectance spectra, it is found that the geometrical structures of these complexes are octahedral. The thermal behaviour of these chelates shows that the hydrated complexes losses water molecules of hydration in the first step followed immediately by decomposition of the anions and ligand molecules in the subsequent steps. The activation thermodynamic parameters, such as, E*, ΔH*, ΔS* and ΔG* are calculated from the DrTG curves using Coats-Redfern method. The synthesized ligands, in comparison to their metal complexes also were screened for their antibacterial activity against bacterial species, Escherichia Coli, Pseudomonas aeruginosa, Staphylococcus Pyogones and Fungi (Candida). The activity data show that the metal complexes to be more potent/antibacterial than the parent Shciff base ligand against one or more bacterial species.

  6. Multiheteromacrocycles that Complex Metal Ions. Second Progress Report, 1 May 1975 -- 30 April 1976

    Cram, D. J.

    1976-01-15

    Objective is to develop cyclic and polycyclic host organic compounds to complex and lipophilize metal ions. Macrorings were synthesized: (OCH{sub 2} CH{sub 2} O CH{sub 2}COCH{sub 2} COCH{sub 2}){sub 2} and (OCH{sub 2} CH{sub 2} O CH{sub 2} COCH{sub 2} COCH{sub 2}){sub 3}. The smaller ring complexes divalent metals 10{sup 1+9} times better than the open-chain model CH{sub 3} O CH{sub 2} CO CH{sub 2} COCH{sub 2} O CH{sub 3}, and the order in which metal ions are complexed is Cu{sup 2+}, UO{sub 2}{sup 2+} greater than Ni{sup 2+} greater than Fe{sup 2+}, Co{sup 2+}, Zn{sup 2+}, Cd{sup 2+} greater than Mn{sup 2+}. The UO{sub 2}{sup 2+} and Cu{sup 2+} complexes were isolated and characterized. The larger ring complexes trivalent metals 10{sup 0.9-1.7} times better than the open- chain model compound, and the order is La{sup 3+}, Ce{sup 3+} greater than Cr{sup 3+}. Five other macrocycles were also synthesized, and their binding constants with Na, K, NH{sub 4}, and Cs picrates were measured. Six compounds containing one macroring and two inward-pointing ArOH or ArOCH{sub 3} groups were also prepared and tested for binding of Li, Na, K, Rb, and NH{sub 4} picrates. Racemic compounds containing two binaphthyls and its sulfur analog were prepared. Cage-shaped multiheteromacrocycles containing ten O ligand sites or four S and six O ligand sites were prepared and the binding capability of the first compound for picrates studied. Two ring systems with phosphonate ester groups were also prepared. (DLC)

  7. Metal Complexes for Organic Optoelectronic Applications

    Huang, Liang

    Organic optoelectronic devices have drawn extensive attention by over the past two decades. Two major applications for Organic optoelectronic devices are efficient organic photovoltaic devices(OPV) and organic light emitting diodes (OLED). Organic Solar cell has been proven to be compatible with the low cost, large area bulk processing technology and processed high absorption efficiencies compared to inorganic solar cells. Organic light emitting diodes are a promising approach for display and solid state lighting applications. To improve the efficiency, stability, and materials variety for organic optoelectronic devices, several emissive materials, absorber-type materials, and charge transporting materials were developed and employed in various device settings. Optical, electrical, and photophysical studies of the organic materials and their corresponding devices were thoroughly carried out. In this thesis, Chapter 1 provides an introduction to the background knowledge of OPV and OLED research fields presented. Chapter 2 discusses new porphyrin derivatives- azatetrabenzylporphyrins for OPV and near infrared OLED applications. A modified synthetic method is utilized to increase the reaction yield of the azatetrabenzylporphyrin materials and their photophysical properties, electrochemical properties are studied. OPV devices are also fabricated using Zinc azatetrabenzylporphyrin as donor materials. Pt(II) azatetrabenzylporphyrin were also synthesized and used in near infra-red OLED to achieve an emission over 800 nm with reasonable external quantum efficiencies. Chapter 3, discusses the synthesis, characterization, and device evaluation of a series of tetradentate platinum and palladium complexesfor single doped white OLED applications and RGB white OLED applications. Devices employing some of the developed emitters demonstrated impressively high external quantum efficiencies within the range of 22%-27% for various emitter concentrations. And the palladium complex, i

  8. The first example of intensive luminescence of LMCT state based on metal complexes in solution

    Lukova, G.V.; Vasil'ev, V.P.; Smirnov, V.A.; Huhn, W.

    2007-01-01

    A bridge complex rac-C 6 H 10 (IndH 4 ) 2 ZrC 2 , featuring a unique long-living luminescence in liquid solutions at 20 deg C, has been prepared for the first time by catalytic hydrogenation of bis-indinyl complex C 6 H 10 (Ind) 2 Zr 2 Cl 2 . It has been identified that quantum yields of luminescence of the complex solutions at room temperature are the greatest ones for the known compounds possessing emission states of charge transfer from ligand to metal. Linear correlations of quantum yield of metal complex luminescence in a solution with steric features of the solvent molecules have been detected for the first time [ru

  9. Homogeneous Catalysis with Metal Complexes Fundamentals and Applications

    Duca, Gheorghe

    2012-01-01

    The book about homogeneous catalysis with metal complexes deals with the description of the reductive-oxidative, metal complexes  in a liquid phase (in polar solvents, mainly in water, and less in nonpolar solvents). The exceptional importance of the redox processes in chemical systems, in the reactions occuring in living organisms, the environmental processes, atmosphere, water, soil, and in industrial technologies (especially in food-processing industries) is discussed. The detailed practical aspects of the established regularities are explained for solving the specific practical tasks in various fields of industrial chemistry, biochemistry, medicine, analytical chemistry and ecological chemistry. The main scope of the book is the survey and systematization of the latest advances in homogeneous catalysis with metal complexes. It gives an overview of the research results and practical experience accumulated by the author during the last decade.

  10. Wastewater treatment from heavy metal ions using nanoactivated complexes of natural zeolite and diatomite

    Malkin Polad

    2018-04-01

    Full Text Available Despite the wide practical use of sorption methods and complexones in treatment of industrial wastewater, some problems are still to be solved in this field. These are the most significant: insufficient sorption capacity of materials, lack of reliable methods for regenerating sorbents and resource-saving ecology friendly treatment technologies with the use of sorbents as well as methods of utilization of heavy metals from waste by complex formation. An important factor affecting the behavior of heavy metals in the soil is the medium acidity. With a neutral and slightly alkaline reaction of the medium, hardly soluble compounds are formed: hydroxides, sulphides, phosphates, carbonates, and oxalates of heavy metals. When acidity increases the reverse process runs in the soil: hardly soluble compounds become more mobile, while mobility of many heavy metals increases. However, the effect of soil acidity on mobility of heavy metals is ambiguous. Although mobility of many heavy metals decreases with increasing pH of the medium (for example, Fe, Mn, Zn, Co, etc., there are a number of metals whose mobility increases with soil neutralization. These include molybdenum and chromium, which are able to form soluble salts in a weak ly acidic and alkaline medium. In addition, heavy metals such as mercury and cadmium are able to maintain mobility in an alkaline medium through formation of complex compounds with organic matter in soils. Heavy metals interact with a solid phase of the soil by mechanisms of specific and nonspecific adsorption. In this article, a technique of wastewater treatment from heavy metal ions using nanoactivated complexes of natural zeolite and diatomite is proposed. This technique can reduce significant costs in preparation of raw materials and subsequent chemical modification of them. Technological solutions aimed at disposal and recycling of industrial wastewater have been proposed. These solutions make it possible to obtain the water

  11. Flame spray synthesis under a non-oxidizing atmosphere: Preparation of metallic bismuth nanoparticles and nanocrystalline bulk bismuth metal

    Grass, Robert N.; Stark, Wendelin J. [Institute for Chemical and Bioengineering, ETH Zuerich (Switzerland)], E-mail: wendelin.stark@chem.ethz.ch

    2006-10-15

    Metallic bismuth nanoparticles of over 98% purity were prepared by a modified flame spray synthesis method in an inert atmosphere by oxygen-deficient combustion of a bismuth-carboxylate based precursor. The samples were characterized by X-ray diffraction, thermal analysis and scanning electron microscopy confirming the formation of pure, crystalline metallic bismuth nanoparticles. Compression of the as-prepared powder resulted in highly dense, nanocrystalline pills with strong electrical conductivity and bright metallic gloss.

  12. Preparation of Radiopharmaceuticals Labeled with Metal Radionuclides. Final Report

    Welch, M.J.

    2012-01-01

    The overall goal of this project was to develop methods for the production of metal-based radionuclides, to develop metal-based radiopharmaceuticals and in a limited number of cases, to translate these agents to the clinical situation. Initial work concentrated on the application of the radionuclides of Cu, Cu-60, Cu-61 and Cu-64, as well as application of Ga-68 radiopharmaceuticals. Initially Cu-64 was produced at the Missouri University Research Reactor and experiments carried out at Washington University. A limited number of studies were carried out utilizing Cu-62, a generator produced radionuclide produced by Mallinckrodt Inc. (now Covidien). In these studies, copper-62-labeled pyruvaldehyde Bis(N 4 -methylthiosemicarbazonato)-copper(II) was studied as an agent for cerebral myocardial perfusion. A remote system for the production of this radiopharmaceutical was developed and a limited number of patient studies carried out with this agent. Various other copper radiopharmaceuticals were investigated, these included copper labeled blood imaging agents as well as Cu-64 labeled antibodies. Cu-64 labeled antibodies targeting colon cancer were translated to the human situation. Cu-64 was also used to label peptides (Cu-64 octriatide) and this is one of the first applications of a peptide radiolabeled with a positron emitting metal radionuclide. Investigations were then pursued on the preparation of the copper radionuclides on a small biomedical cyclotron. A system for the production of high specific activity Cu-64 was developed and initially the Cu-64 was utilized to study the hypoxic imaging agent Cu-64 ATSM. Utilizing the same target system, other positron emitting metal radionuclides were produced, these were Y-86 and Ga-66. Radiopharmaceuticals were labeled utilizing both of these radionuclides. Many studies were carried out in animal models on the uptake of Cu-ATSM in hypoxic tissue. The hypothesis is that Cu-ATSM retention in vivo is dependent upon the oxygen

  13. Preparation of trialkylindium by alkylation of metallic indium

    Eremeev, I.V.; Danov, S.M.; Sakhipov, V.R.

    1995-01-01

    The investigation results on production of trialkyl indium by alkylation of metallic indium are presented. In contradistinction to the known techniques for the production of trialkyls on indium by alkylation it is suggested to separate the synthesis into two steps. At the first step indium is alkylated by alkylhalide to alkyl indium halide, and at the second alkylation is carried out using. Grignard reagent. The techniques for preparation of trimethyl- and triethylindium, developed on the bases of this scheme, are noted for good reproducibility, allow to preclude, agglomeration of indium during the synthesis, as well as to reduce the consumption coefficients, and amounts, of the introduced starting reagents, i.e. magnesium and alkylhalide. Refs. 16

  14. Complexation-induced supramolecular assembly drives metal-ion extraction.

    Ellis, Ross J; Meridiano, Yannick; Muller, Julie; Berthon, Laurence; Guilbaud, Philippe; Zorz, Nicole; Antonio, Mark R; Demars, Thomas; Zemb, Thomas

    2014-09-26

    Combining experiment with theory reveals the role of self-assembly and complexation in metal-ion transfer through the water-oil interface. The coordinating metal salt Eu(NO3)3 was extracted from water into oil by a lipophilic neutral amphiphile. Molecular dynamics simulations were coupled to experimental spectroscopic and X-ray scattering techniques to investigate how local coordination interactions between the metal ion and ligands in the organic phase combine with long-range interactions to produce spontaneous changes in the solvent microstructure. Extraction of the Eu(3+)-3(NO3(-)) ion pairs involves incorporation of the "hard" metal complex into the core of "soft" aggregates. This seeds the formation of reverse micelles that draw the water and "free" amphiphile into nanoscale hydrophilic domains. The reverse micelles interact through attractive van der Waals interactions and coalesce into rod-shaped polynuclear Eu(III) -containing aggregates with metal centers bridged by nitrate. These preorganized hydrophilic domains, containing high densities of O-donor ligands and anions, provide improved Eu(III) solvation environments that help drive interfacial transfer, as is reflected by the increasing Eu(III) partitioning ratios (oil/aqueous) despite the organic phase approaching saturation. For the first time, this multiscale approach links metal-ion coordination with nanoscale structure to reveal the free-energy balance that drives the phase transfer of neutral metal salts. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Heterobimetallic coordination polymers involving 3d metal complexes and heavier transition metals cyanometallates

    Peresypkina, Eugenia V. [Nikolaev Institute of Inorganic Chemistry, SB RAS, Novosibirsk 630090 (Russian Federation); Samsonenko, Denis G. [Nikolaev Institute of Inorganic Chemistry, SB RAS, Novosibirsk 630090 (Russian Federation); Novosibirsk State University, Novosibirsk 630090 (Russian Federation); Vostrikova, Kira E., E-mail: vosk@niic.nsc.ru [Nikolaev Institute of Inorganic Chemistry, SB RAS, Novosibirsk 630090 (Russian Federation); LMI, Université Claude Bernard Lyon 1, 69622 Villeurbanne Cedex (France)

    2015-04-15

    The results of the first steps in the design of coordination polymers based on penta- and heptacyanometallates of heavier d transitions metals are presented. The 2D structure of the coordination polymers: [(Mn(acacen)){sub 2}Ru(NO)(CN){sub 5}]{sub n} and two complexes composed of different cyanorhenates, [Ni(cyclam)]{sub 2}[ReO(OH)(CN){sub 4}](ClO{sub 4}){sub 2}(H{sub 2}O){sub 1.25} and [Cu(cyclam)]{sub 2}[Re(CN){sub 7}](H{sub 2}O){sub 12}, was confirmed by single crystal XRD study, the rhenium oxidation state having been proved by the magnetic measurements. An amorphism of [M(cyclam)]{sub 3}[Re(CN){sub 7}]{sub 2} (M=Ni, Cu) polymers does not allow to define strictly their dimensionality and to model anisotropic magnetic behavior of the compounds. However, with high probability a honey-comb like layer structure could be expected for [M(cyclam)]{sub 3}[Re(CN){sub 7}]{sub 2} complexes, studied in this work, because such an arrangement is the most common among the bimetallic assemblies of hexa- and octacyanometallates with a ratio [M(cyclam)]/[M(CN){sub n}]=3/2. For the first time was prepared and fully characterized a precursor (n-Bu{sub 4}N){sub 2}[Ru(NO)(CN){sub 5}], soluble in organic media. - Graphical abstract: The very first results in the design of 2D coordination polymers based on penta- and heptacyanometallates of 4d and5d transitions metals are presented. - Highlights: • Design of coordination polymers based on penta- and heptacyanometallates. • New Ru and Re cyanide based heterobimetallic coordination complexes. • Hydrolysis and ox/red processes involving [Re(CN){sub 7}]{sup 3+} during crystallization. • High magnetic anisotropy of [M(cyclam)]{sub 3}[Re(CN){sub 7}]{sub 2}(H{sub 2}O){sub n}, M=Cu, Ni, complexes.

  16. Complex Metal Hydrides for Hydrogen, Thermal and Electrochemical Energy Storage

    Moller, Kasper T.; Sheppard, Drew; Ravnsbaek, Dorthe B.

    2017-01-01

    Hydrogen has a very diverse chemistry and reacts with most other elements to form compounds, which have fascinating structures, compositions and properties. Complex metal hydrides are a rapidly expanding class of materials, approaching multi-functionality, in particular within the energy storage...... inspiration to solve the great challenge of our time: efficient conversion and large-scale storage of renewable energy....... field. This review illustrates that complex metal hydrides may store hydrogen in the solid state, act as novel battery materials, both as electrolytes and electrode materials, or store solar heat in a more efficient manner as compared to traditional heat storage materials. Furthermore, it is highlighted...

  17. Green methods for preparing highly co2 selective and h2s tolerant metal organic frameworks

    Eddaoudi, Mohamed

    2015-12-23

    A green route for preparing a metal organic framework include mixing metal precursor with a ligand precursor to form a solvent-free mixture; adding droplets of water to the mixture; heating the mixture at a first temperature after adding the water; and isolating the metal organic framework material including the metal and the ligand.

  18. Synthesis and optical properties of enantiomeric cinchonidine/cinchonine-terpyridine derivatives and their metal complexes

    Wang, Hui-Ting; Wu, Wen-Jie; Liu, Jiang; Chen, Meng; Qian, Dong-Jin; Zhang, Li; Liu, Minghua

    2016-01-01

    We report here the synthesis and spectroscopic properties of two enantiomeric chiral tridentate ligands (TPyCCD and TPyCCN) composed of terpyridine (TPy) and cinchonidine (CCD) or cinchonine (CCN) substituent, as well as their metal complexes with Zn 2+ , Fe 2+ , Eu 3+ , and Tb 3+ ions. For the pure ligands, the fluorescent emission intensity increased as their concentrations increased in the dilute solutions, but they decreased when the concentrations were greater than 6.9×10 −6 mol/l due to concentration quenching. No significant influence on ligand luminescence was observed for the Zn 2+ /Fe 2+ –TPyCCD and –TPyCCN metal complexes. Their lanthanide (Eu 3+ and Tb 3+ ) complexes displayed both ligand and lanthanide ion emissions, suggesting that the excited energy of both ligands could be transferred to the central Eu 3+ and Tb 3+ ions. Mirror-image circular dichroism spectra were recorded, with several signals centered at about 230, 250–270, 296, and 320 nm; the first ones corresponded to the chiral CCD and CCN substituents, while the latter ones corresponded to the TPy substituent and the metal–TPy (M-TPy) coordination units. It is suggested that the chirality of TPy and the metal complexes was induced by the coexisting chiral CCD and CCN substituents. In addition, due to formation of the metal complexes, the relative intensity of the chiral signals of M–TPy coordination units was enhanced at about 320 nm. - Highlights: • Cinchona alkaloid-terpyridine derivatives and metal complexes were prepared. • Cinchona alkaloid-terpyridine derivatives gave off luminescence at 362 nm. • Ligand excited energy could efficiently transferred to lanthanide ions. • Chirality of terpyridine and metal complexes was induced.

  19. THE THEORY OF DEVELOPMENT OF SUPPORTED METAL-COMPLEX CATALYSTS

    T. L. Rakitskaya

    2015-06-01

    Full Text Available Some results of the investigations for the purpose of development of supported metal-complex catalysts for phosphine and carbon monoxide oxidation as well as for ozone decomposition are summarized. The activity of such catalysts has been found to depend not only on a nature of a central atom and ligands but also on a nature of supports. The theoretical model explaining mechanisms of surface complex formation taking into account the influence of physicochemical and structural-adsorption properties of the supports (SiO2, Al2O3, carbon materials, zeolites, dispersed silicas, lamellar aluminosilicates, etc. has been proposed. For quantitative description of the support effect, such a thermodynamic parameter as the adsorbed water activity assignable with the help of water vapor adsorption isotherms has been introduced. Successive stability constants of the surface metal complexes have been calculated by the kinetic method and, hence, compositions and partial catalytic activity of the latter have been determined. Taking into account the competitive adsorption of metal ions on the supports, some schemes of formation of surface bimetallic complexes have been suggested. The compositions of the supported metal-complex catalysts have been optimized to meet requirements of their use in respirators and plants for air purification from foregoing gaseous toxicants.

  20. Properties- and applications of quasicrystals and complex metallic alloys.

    Dubois, Jean-Marie

    2012-10-21

    This article aims at an account of what is known about the potential for applications of quasicrystals and related compounds, the so-called family of Complex Metallic Alloys (CMAs‡). Attention is focused at aluminium-based CMAs, which comprise a large number of crystalline compounds and quasicrystals made of aluminium alloyed with transition metals (like Fe or Cu) or normal metals like Mg. Depending on composition, the structural complexity varies from a few atoms per unit cell up to thousands of atoms. Quasicrystals appear then as CMAs of ultimate complexity and exhibit a lattice that shows no periodicity anymore in the usual 3-dimensional space. Properties change dramatically with lattice complexity and turn the metal-type behaviour of simple Al-based crystals into a far more complex behaviour, with a fingerprint of semi-conductors that may be exploited in various applications, potential or realised. An account of the ones known to the author is given in the light of the relevant properties, namely light absorption, reduced adhesion and friction, heat insulation, reinforcement of composites for mechanical devices, and few more exotic ones. The role played by the search for applications of quasicrystals in the development of the field is briefly addressed in the concluding section.

  1. Preparation and analysis of multilayer composites based on polyelectrolyte complexes

    Petrova, V. A. [Russian Academy of Sciences, Institute of Macromolecular Compounds (Russian Federation); Orekhov, A. S. [Russian Academy of Sciences, Shubnikov Institute of Crystallography, Federal Scientific Research Centre “Crystallography and Photonics” (Russian Federation); Chernyakov, D. D. [St. Petersburg State Chemical Pharmaceutical Academy (Russian Federation); Baklagina, Yu. G. [Russian Academy of Sciences, Institute of Macromolecular Compounds (Russian Federation); Romanov, D. P. [Russian Academy of Sciences, Grebenshchikov Institute of Silicate Chemistry (Russian Federation); Kononova, S. V. [Russian Academy of Sciences, Institute of Macromolecular Compounds (Russian Federation); Volod’ko, A. V.; Ermak, I. M. [Russian Academy of Sciences, Elyakov Pacific Institute of Bioorganic Chemistry, Far-Eastern Branch (Russian Federation); Klechkovskaya, V. V., E-mail: klechvv@ns.crys.ras.ru [Russian Academy of Sciences, Shubnikov Institute of Crystallography, Federal Scientific Research Centre “Crystallography and Photonics” (Russian Federation); Skorik, Yu. A., E-mail: yury-skorik@mail.ru [Russian Academy of Sciences, Institute of Macromolecular Compounds (Russian Federation)

    2016-11-15

    A method for preparing multilayer film composites based on chitosan has been developed by the example of polymer pairs: chitosan–hyaluronic acid, chitosan–alginic acid, and chitosan–carrageenan. The structure of the composite films is characterized by X-ray diffractometry and scanning electron microscopy. It is shown that the deposition of a solution of hyaluronic acid, alginic acid, or carrageenan on a chitosan gel film leads to the formation of a polyelectrolyte complex layer at the interface, which is accompanied by the ordering of chitosan chains in the surface region; the microstructure of this layer depends on the nature of contacting polymer pairs.

  2. Triheterometallic Lanthanide Complexes Prepared from Kinetically Inert Lanthanide Building Blocks

    Sørensen, Thomas Just; Tropiano, Manuel; Kenwright, Alan M.

    2017-01-01

    Three molecular structures, each containing three different lanthanide(III) centres, have been prepared by coupling three kinetically inert lanthanide(III) complexes in an Ugi reaction. These 2 kDa molecules were purified by dialysis and characterised by NMR and luminescence techniques. The photo...... and lanthanide(III) centres in these molecules inhibits the efficient sensitisation of europium. We conclude that the intramolecular collisions required for efficient Dexter energy transfer from the sensitiser to the lanthanide(III) centre can be prevented by steric congestion....

  3. Nano-Ag complexes prepared by γ-radiolysis and their structures and physical properties

    Kim, Hwa-Jung; Choi, Seong-Ho; Park, Hae-Jun

    2012-01-01

    In this study, nano-silver (nano-Ag) complexes showing different properties have been synthesized as follows. Polypyrrolidone (PVP)-stabilized silver colloids (NAg), nano-Ag bound to silica (SiO 2 ) (NSS), and nano-Ag bound to a complex of SiO 2 and polyaniline (PANI) (NSSPAI) were prepared via γ-irradiation at room temperature. NAg and NSS used PVP as a colloidal stabilizer, while NSSPAI did not use PVP as a colloidal stabilizer. Interesting bonding properties occurred in the nano-Ag complex and anticipated structural changes were clearly shown through a surface analysis of x-ray photoelectron spectroscopy (XPS). The morphologies by field emission-scanning electron microscopy (FE-SEM) analysis showed that nano-Ag complexes have various particle sizes ranging from 10 to 30 nm. NSS (average, 10 nm) and NSSPAI (average, 30 nm) showed a uniformly spherical shape and size, while NAg did not. From the reflection peaks in the x-ray diffraction (XRD) patterns, surface crystallinity of the nano-Ag complexes was indicated to be in the same degree as that of NSSPAI>NSS>NAg. Also, in the contact angle (CA) determination, surface hydrophobicity of NSSPAI was stronger than those of NSS and NAg, relatively. The different nano-Ag complexes prepared by γ-irradiation can be applicable in various industry fields due to the increase in specific property. - Highlights: ► Nano-Ag complexes showing different properties have been synthesized via γ-irradiation. ► Nano-Ag colloid (NAg), nano-Ag bound to SiO 2 (NSS), nano-Ag bound to SiO 2 and PANI complex (NSSPAI). ► Nano-Ag complexes were the same based on Ag metal. ► Results clearly showed fascinating/different physical properties. ► Different nano-Ag complexes can be applicable in various industry fields.

  4. Preparation and characterization of aluminium-silica metal matrix composite

    Mallikarjuna, G. B.; Basavaraj, E.

    2018-04-01

    Aluminum alloys are widely used in aerospace and automobile industries due to their low density and good mechanical properties, better corrosion resistance and wear, low thermal coefficient of expansion as compared to conventional metals and alloys. The excellent properties of these materials and relatively low production cost make them a very attractive for a variety of applications. In this present work, Al alloy LM13-SiO2 composites were produced by stir casting method. The reinforcement SiO2 particle size used for preparation of composites are 106 µm, 150 µm, 250 µm and 355 µm with varying amount of 3 to 12 wt% in steps of 3. The prepared composite specimens were machined as per test standards. Effects of weight percentage of SiO2 particles on wear, tensile strength of Al alloy LM13-SiO2 composites have been investigated. The microstructures of the composites were studied to know the dispersion of the SiO2 particles in matrix. Experimental results shows that there is enhanced mechanical properties, when silica weighing 9% was added to the base aluminium alloy and also similar trend exists in all four different micron size of silica and also it has been observed that addition of SiO2 particles significantly improves wear resistance properties as compared with that of unreinforced matrix.

  5. Zeolites as supports for transition-metal complexes

    Le Van Mao, R

    1979-01-01

    The unique structural characteristics of the zeolites, including the presence of molecular-size cages and channels and of an internal electrostatic field, make them promising as supports for converting homogeneous to heterogeneous catalysts. The acidic sites on the zeolites may also contribute to catalysis of reactions, such as hydrocracking; may stabilize metal complexes in a highly disperse state; and may improve activity or selectivity. Recent studies on the synthesis of new types of zeolite-supported complexes of transition metals (TM), such as Co, Cu, Ag, Fe, Mo, Ru, Rh, Re, and Os, suggest the feasibility of the direct introduction of some TM complexes into the zeolitic cages during zeolite synthesis, especially during the crystallization phase. This method may considerably reduce the structural limitations associated with the incorporation of TM complexes into zeolites by conventional methods.

  6. New Transition metal assisted complex borohydrides for hydrogen storage

    Sesha Srinivasan; Elias Lee Stefanakos; Yogi Goswami

    2006-01-01

    High capacity hydrogen storage systems are indeed essential for the on-board vehicular application that leads to the pollution free environment. Apart from the various hydrogen storage systems explored in the past, complex hydrides involving light weight alkali/alkaline metals exhibits promising hydrogenation/ dehydrogenation characteristics. New transition metal assisted complex borohydrides [Zn(BH 4 ) 2 ] have been successfully synthesized by an inexpensive mechano-chemical process. These complex hydrides possesses gravimetric hydrogen storage capacity of ∼8.4 wt.% at around 120 C. We have determined the volumetric hydrogen absorption and desorption of these materials for a number of cycles. Another complex borohydride mixture LiBH 4 /MgH 2 catalyzed with ZnCl 2 has been synthesized and characterized using various analytical techniques. (authors)

  7. Preparation and chemical studies on Tc(III) complexes containing polyaminocarboxylic acids

    Gonzalez, R.; Kremer, C.; Chiozzone, R.; Torres, J.; Rivero, M.; Kremer, E.; Leon, A.

    1998-01-01

    Tc(III)-edta (edta = ethylenediaminetetraacetate), Tc(III)-dtpa (dtpa = diethylenetriaminepentaacetate) and Tc(III)-mebrofenin (mebrofenin = 3-bromo-2,4,6-trimethylacetanilideiminodiacetate) complexes were prepared by ligand substitution reactions on hexakis(thiourea)technetium(III) cation with the polycarboxylates. By a combination of different techniques (UV-Vis, IR and 1 H-NMR spectroscopy, Tc elemental analyses and cerimetric titrations) it was concluded that 1:1 complexes are formed with edta and dtpa while mebrofening adopts a 2:1 (ligand to metal) stoichiometry. Complementary, molecular mechanics calculations were performed to analyze the spatial arrangement of the molecules. The stability of the Tc(III) complexes was studied in aqueous solution by paper chromatography, paper electrophoresis and cyclic voltammetry. The chelates are rather stable, in particular when compared with the precursor. (orig.)

  8. The metallic ratios as limits of complex valued transformations

    Falcon, Sergio; Plaza, Angel

    2009-01-01

    We study the presence of the metallic ratios as limits of two complex valued transformations. These complex variable functions are introduced and related with the two geometric antecedents for each triangle in a particular triangle partition, the four-triangle longest-edge (4TLE) partition. In this way, the fractality of a geometric diagram for the classes of dissimilar generated triangles is also explained.

  9. Anticancer Activity of Metal Complexes: Involvement of Redox Processes

    Jungwirth, Ute; Kowol, Christian R.; Keppler, Bernhard K.; Hartinger, Christian G.; Berger, Walter; Heffeter, Petra

    2012-01-01

    Cells require tight regulation of the intracellular redox balance and consequently of reactive oxygen species for proper redox signaling and maintenance of metal (e.g., of iron and copper) homeostasis. In several diseases, including cancer, this balance is disturbed. Therefore, anticancer drugs targeting the redox systems, for example, glutathione and thioredoxin, have entered focus of interest. Anticancer metal complexes (platinum, gold, arsenic, ruthenium, rhodium, copper, vanadium, cobalt, manganese, gadolinium, and molybdenum) have been shown to strongly interact with or even disturb cellular redox homeostasis. In this context, especially the hypothesis of “activation by reduction” as well as the “hard and soft acids and bases” theory with respect to coordination of metal ions to cellular ligands represent important concepts to understand the molecular modes of action of anticancer metal drugs. The aim of this review is to highlight specific interactions of metal-based anticancer drugs with the cellular redox homeostasis and to explain this behavior by considering chemical properties of the respective anticancer metal complexes currently either in (pre)clinical development or in daily clinical routine in oncology. PMID:21275772

  10. The role of metal complexes in nuclear reactor decontamination

    Prince, A.A.M.; Raghavan, P.S.; Gopalan, R. [Madras Christian College, Tambaram, Chennai (India); Velmurugan, S.; Narasimhan, S.V. [Bhabha Atomic Research Center (BARC) (IN). Water and Steam Chemistry Lab. (WSCL)

    2006-07-15

    Chemical decontamination is the process of removal of radioactivity from corrosion products formed on structural materials in the nuclear reactors. These corrosion products cause problems for the operation and maintenance of the plants. Removal of the radioactive contaminants can be achieved by dissolving the oxide from the system surface using organic complexing agents in low concentrations known as dilute chemical decontamination (DCD) formulations. These organic complexing agents attack the oxide surface and form metal complexes, which further accelerate the dissolution process. The stability of the complexes plays an important role in dissolving the radioactive contaminated oxides. In addition, the DCD process is operated through ion exchange resins for the removal of the dissolved metal ions and radioactive nuclides. In the present study, the kinetics of dissolution of various model corrosion products such as magnetite (Fe{sub 3}O{sub 4}), hematite ({alpha}-Fe{sub 2}O{sub 3}) and maghemite ({gamma}-Fe{sub 2}O{sub 3}) have been studied in the presence of complexing agents such as ethylenediaminetetraacetic acid (EDTA), nitrilotriacetic acid (NTA), hydroxyethylethylenediaminepentaacetic acid (HEEDTA), and 2,6 pyridinedicarboxylic acid (PDCA). The reductive roles of metal complexes and organic reducing agents are discussed. (orig.)

  11. Transition metal M(II complexes with isonicotinoylhydrazone-9-anthraldehyde

    Dianu M.L.

    2010-01-01

    Full Text Available New complexes of isonicotinoylhydrazone-9-anthraldehyde with Cu(II, Co(II and Ni(II have been prepared and characterized by analytical and physico-chemical techniques, such as elemental and thermal analyses, magnetic susceptibility and conductivity measurements, and electronic, EPR and IR spectral studies. The infrared spectral studies revealed the bidentate or monodentate nature of the Schiff base in the complexes; the pyridine nitrogen does not participate in the coordination. A tetrahedral geometry is suggested for the nitrate-complexes and an octahedral geometry for the others. Thermal studies support the chemical formulation of these complexes.

  12. Biodegradation of metal citrate complexes and implications for toxic-metal mobility

    Francis, A.J.; Dodge, C.J.; Gillow, J.B.

    1992-01-01

    The presence of synthetic and naturally occurring chelating agents in nuclear and toxic-metal wastes is a major concern because of their potential to enhance mobilization of metal ions away from the disposal sites. Of particular interest is citric acid, which is present in low-level and transuranic radioactive wastes and in domestic and industrial wastes (as washing fluids, for instance), as well as being found naturally. Citrate ions form multidentate, stable complexes with a variety of toxic metals and radionuclides; but biodegradation of these complexes, precipitating the metal ions as insoluble hydroxides, oxides or other salts, may retard migration. Here we report a study of the biodegradation of citrate complexes of Ca, Fe(II), Fe(III), Cd, Cu, Ni, Pb and U. Several of these complexes were not readily degraded by bacteria, and the biodegradability depended on the chemical nature of the complex, not on the toxicity of the metal to the bacteria. This resistance to biodegradation implies that citrate complexation may play an important part in migration of these hazardous wastes. (author)

  13. Method for synthesizing metal bis(borano) hypophosphite complexes

    Cordaro, Joseph G.

    2013-06-18

    The present invention describes the synthesis of a family of metal bis(borano) hypophosphite complexes. One procedure described in detail is the syntheses of complexes beginning from phosphorus trichloride and sodium borohydride. Temperature, solvent, concentration, and atmosphere are all critical to ensure product formation. In the case of sodium bis(borano) hypophosphite, hydrogen gas was evolved upon heating at temperatures above 150.degree. C. Included in this family of materials are the salts of the alkali metals Li, Na and K, and those of the alkaline earth metals Mg and Ca. Hydrogen storage materials are possible. In particular the lithium salt, Li[PH.sub.2(BH.sub.3).sub.2], theoretically would contain nearly 12 wt % hydrogen. Analytical data for product characterization and thermal properties are given.

  14. Metathesis synthesis and characterization of complex metal fluoride ...

    Administrator

    V MANIVANNAN*, P PARHI and JONATHAN W KRAMER. Department of Mechanical Engineering, Campus Delivery 1374, Colorado State University, Fort Collins,. CO 80523, USA. MS received 30 April 2008. Abstract. Metathesis synthesis of complex metal fluorides using mechanochemical activation has been reported.

  15. DNA interactions and biocidal activity of metal complexes of ...

    Narendrula Vamsikrishna

    The Schiff bases and metal complexes were characterized by analytical and spectral methods like elemental analysis, ... cleavages.8–10 Cisplatin and its second generation com- ..... in DMSO. The test microorganisms were grown on nutrient agar medium in ...... effects on polymer characteristics Appl. Organomet. Chem.

  16. Dimeric Complexes of Tryptophan with M2+ Metal Ions

    Dunbar, R. C.; Steill, J. D.; Polfer, N. C.; Oomens, J.

    2009-01-01

    IRMPD spectroscopy using the FELIX free electron laser and a Fourier transform ICR mass spectrometer was used to characterize the structures of electrosprayed dimer complexes M(2+)Trp(2) of tryptophan with a series of eight doubly charged metal ions, including alkaline earths Ca, Sr, and Ba, and

  17. Sub-chronic toxicological studies of transition metal complexes of ...

    However, Naproxen metal complexes showed comparatively lower side effects than naproxen. Hematological report suggested that naproxen was in process of initiating inflammation which was justified by decreasing the mean value hemoglobin and hematocrit level and increasing the white blood cells level. There were ...

  18. Lability criteria for metal complexes in micro-electrode voltammetry

    Leeuwen, van H.P.; Pinheiro, J.P.

    1999-01-01

    Theoretical expressions are derived for the voltammetric lability criteria of metal complexes in the micro-electrode regime. The treatment includes three limiting situations: (i) the macro-electrode limit, where both the diffusion layer and the dissociation reaction layer are linear; (ii) an

  19. Schiff base transition metal complexes for Suzuki–Miyaura cross

    Schiff base ligand and its complex with iron (Fe), cobalt (Co), nickel (Ni) and copper (Cu) ions were synthesized using 4-aminoacetophenone and salicylaldehyde and characterized. FTIR spectrum shows that bidentate coordination of metal ions with ligand where O, N are electron donating sites of azomethine group.

  20. Group 4 Metal Complexes of Chelating Cyclopentadienyl-ketimide Ligands

    Večeřa, M.; Varga, Vojtěch; Císařová, I.; Pinkas, Jiří; Kucharczyk, P.; Sedlařík, V.; Lamač, Martin

    2016-01-01

    Roč. 35, č. 5 (2016), s. 785-798 ISSN 0276-7333 R&D Projects: GA ČR(CZ) GA14-08531S; GA MŠk(CZ) LO1504 Institutional support: RVO:61388955 Keywords : group 4 metal complexes * cyclopentadienyl-ketimide ligands * metallocenes Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 3.862, year: 2016

  1. Selective transport and incorporation of highly charged metal and metal complex ions in self-assembled polyelectrolyte multilayer membranes

    Toutianoush, Ali; Tieke, Bernd

    2002-01-01

    The transport of aqueous salts containing mono-, di- and trivalent metal and tetravalent metal complex ions across ultrathin polyvinylammonium/polyvinylsulphate (PVA/PVS) membranes is described. The membranes were prepared by electrostatic layer-by-layer (LBL) assembly of the two polyelectrolytes. Using spectroscopic measurements and permeability studies, it is demonstrated that the transport of copper(II) chloride, lanthanum(III) chloride, barium chloride and potassium hexacyanoferrate(II) is accompanied by the permanent incorporation of the metal and metal complex ions in the membrane. Upon the uptake of copper, lanthanum and hexacyanoferrate ions, the membranes become cross-linked so that the permeation rates of other salts not taken up by the membrane, e.g. sodium chloride, potassium chloride and magnesium chloride, are decreased. The uptake of barium ions leads to a decrease of the cross-linking density of the membrane so that the permeation rate of NaCl is increased. Possible mechanisms for the ion uptake are discussed

  2. Metal complexes of the fourth generation quinolone antimicrobial drug gatifloxacin: Synthesis, structure and biological evaluation

    Sadeek, Sadeek A.; El-Shwiniy, Walaa H.

    2010-08-01

    Three metal complexes of the fourth generation quinolone antimicrobial agent gatifloxacin (GFLX) with Y(ΙΙΙ), Zr(ΙV) and U(VΙ) have been prepared and characterized with physicochemical and spectroscopic techniques. In these complexes, gatifloxacin acts as a bidentate deprotonated ligand bound to the metal through the ketone oxygen and a carboxylato oxygen. The complexes are six-coordinated with distorted octahedral geometry. The kinetic parameters for gatifloxacin and the three prepared complexes have been evaluated from TGA curves by using Coats-Redfern (CR) and Horowitz-Metzeger (HM) methods. The calculated bond length and force constant, F(U dbnd O), for the UO 2 bond in uranyl complex are 1.7522 Å and 639.46 N m -1. The antimicrobial activity of the complexes has been tested against microorganisms, three bacterial species, such as Staphylococcus aureus ( S. aureus), Escherichia coli ( E. coli) and Pseudomonas aeruginosa ( P. aeruginosa) and two fungi species, penicillium ( P. rotatum) and trichoderma ( T. sp.), showing that they exhibit higher activity than free ligand.

  3. Biotransformation of uranium and transition metal citrate complexes by clostridia

    Francis, A.J.; Joshi-Tope, G.A.; Dodge, C.J.; Gillow, J.B.

    2002-01-01

    Clostridium sphenoides, which uses citric acid as its sole carbon source, metabolized equimolar Fe(III)-citrate with the degradation of citric acid and the reduction of Fe(III) to Fe(II), but not the U(VI)-citrate complex. However, in the presence of excess citric acid or added glucose it was reduced to U(IV)-citrate. In contrast, Clostridium sp., which ferments glucose but not citrate, reduced Fe(III)-citrate to Fe(II)-citrate and U(VI)-citrate to U(IV)-citrate only when supplied with glucose. These results show that complexed uranium is readily accessible as an electron acceptor despite the bacterium's inability to metabolize the organic ligand complexed to the actinide. These results also show that the metabolism of the metal-citrate complex depends upon the type of complex formed between the metal and citric acid. Fe(III) forms a bidentate complex with citric acid and was metabolized, whereas U forms a binuclear complex with citric acid and was recalcitrant. (author)

  4. Preparation of metal-resistant immobilized sulfate reducing bacteria beads for acid mine drainage treatment.

    Zhang, Mingliang; Wang, Haixia; Han, Xuemei

    2016-07-01

    Novel immobilized sulfate-reducing bacteria (SRB) beads were prepared for the treatment of synthetic acid mine drainage (AMD) containing high concentrations of Fe, Cu, Cd and Zn using up-flow anaerobic packed-bed bioreactor. The tolerance of immobilized SRB beads to heavy metals was significantly enhanced compared with that of suspended SRB. High removal efficiencies of sulfate (61-88%) and heavy metals (>99.9%) as well as slightly alkaline effluent pH (7.3-7.8) were achieved when the bioreactor was fed with acidic influent (pH 2.7) containing high concentrations of multiple metals (Fe 469 mg/L, Cu 88 mg/L, Cd 92 mg/L and Zn 128 mg/L), which showed that the bioreactor filled with immobilized SRB beads had tolerance to AMD containing high concentrations of heavy metals. Partially decomposed maize straw was a carbon source and stabilizing agent in the initial phase of bioreactor operation but later had to be supplemented by a soluble carbon source such as sodium lactate. The microbial community in the bioreactor was characterized by denaturing gradient gel electrophoresis (DGGE) and sequencing of partial 16S rDNA genes. Synergistic interaction between SRB (Desulfovibrio desulfuricans) and co-existing fermentative bacteria could be the key factor for the utilization of complex organic substrate (maize straw) as carbon and nutrients source for sulfate reduction. Copyright © 2016 Elsevier Ltd. All rights reserved.

  5. Intraparticulate Metal Speciation Analysis of Soft Complexing Nanoparticles. The Intrinsic Chemical Heterogeneity of Metal-Humic Acid Complexes

    Town, R. M.; van Leeuwen, Herman P.

    2016-01-01

    ion condensation potential for higher valency counterions within the intraparticulate double layer zone of the soft NP. The approach offers new insights into the intrinsic heterogeneity of the HA. complexes, as revealed by the intraparticulate speciation as a function of the true degree of inner......-sphere complexation, theta(M). The ensuing intrinsic heterogeneity parameters, Gamma, for CdHA and CuHA complexes are in very good agreement with those obtained from dynamic electrochemical stripping chronopotentiometric measurements. The overall intraparticulate metal ion speciation is found to depend on theta...

  6. Enzyme-Free Electrochemical Glucose Sensors Prepared by Dealloying Pd-Ni-P Metallic Glasses

    Yuqiao Zeng

    2014-01-01

    Full Text Available We report the formation of enzyme-free electrochemical glucose sensors by electrochemical dealloying palladium-containing Pd-Ni-P metallic glasses. When metallic glasses with different Pd contents are used as the dealloying precursor alloys, palladium-based nanoporous metals with different ligament and pore sizes can be obtained. The chemical compositions of the nanoporous metals also vary according to the different precursor compositions. All the as-obtained nanoporous metals exhibit electrochemical catalytic activity towards the oxidation of d-glucose, indicating that the nanoporous metals prepared by dealloying the Pd-Ni-P metallic glasses are promising materials for enzyme-free electrochemical glucose sensor.

  7. Novel strategy for the preparation of graphene-encapsulated mesoporous metal oxides with enhanced lithium storage

    Lin, Rong; Yue, Wenbo; Niu, Fangzhou; Ma, Jie

    2016-01-01

    As potential anode materials for lithium-ion batteries, mesoporous metal oxides show high reversible capacities but relatively poor cycle stability due to the structural collapse during cycles. Graphene-encapsulated mesoporous metal oxides may increase the electronic conductivity of the composite as well as stabilize the mesostructure of metal oxides, thereby enhancing the electrochemical performance of mesoporous metal oxides. Herein we describe a novel strategy for the preparation of graphene-encapsulated mesoporous metal oxides (SnO_2, Mn_3O_4), which exhibit superior electrochemical performance compared to pure mesoporous metal oxides. Moreover, some mesoporous metal oxides may be further reduced to low-valence metal oxides when calcined in presence of graphene. Mesoporous metal oxides with high isoelectric points are not essential for this synthesis method since metal oxides are connected with graphene through mesoporous silica template, thus expanding the types of graphene-encapsulated mesoporous metal oxides.

  8. Ibandronate metal complexes: solution behavior and antiparasitic activity.

    Demoro, Bruno; Rostán, Santiago; Moncada, Mauricio; Li, Zhu-Hong; Docampo, Roberto; Olea Azar, Claudio; Maya, Juan Diego; Torres, Julia; Gambino, Dinorah; Otero, Lucía

    2018-03-01

    To face the high costs of developing new drugs, researchers in both industry and academy are looking for ways to repurpose old drugs for new uses. In this sense, bisphosphonates that are clinically used for bone diseases have been studied as agents against Trypanosoma cruzi, causative parasite of Chagas disease. In this work, the development of first row transition metal complexes (M = Co 2+ , Mn 2+ , Ni 2+ ) with the bisphosphonate ibandronate (iba, H 4 iba representing the neutral form) is presented. The in-solution behavior of the systems containing iba and the selected 3d metal ions was studied by potentiometry. Mononuclear complexes [M(H x iba)] (2-x)- (x = 0-3) and [M(Hiba) 2 ] 4- together with the formation of the neutral polynuclear species [M 2 iba] and [M 3 (Hiba) 2 ] were detected for all studied systems. In the solid state, complexes of the formula [M 3 (Hiba) 2 (H 2 O) 4 ]·6H 2 O were obtained and characterized. All obtained complexes, forming [M(Hiba)] - species under the conditions of the biological studies, were more active against the amastigote form of T. cruzi than the free iba, showing no toxicity in mammalian Vero cells. In addition, the same complexes were selective inhibitors of the parasitic farnesyl diphosphate synthase (FPPS) enzyme showing poor inhibition of the human one. However, the increase of the anti-T. cruzi activity upon coordination could not be explained neither through the inhibition of TcFPPS nor through the inhibition of TcSPPS (T. cruzi solanesyl-diphosphate synthase). The ability of the obtained metal complexes of catalyzing the generation of free radical species in the parasite could explain the observed anti-T. cruzi activity.

  9. Bibliographies on radiation chemistry. 9. Metal ions and complexes. Part A: Cobalt, rhodium, iridium

    Hoffman, M Z; Ross, A B

    1986-01-01

    The one-electron oxidation and reduction of metal ions and complexes can yield species in unusual oxidation states, and ligand-radicals coordinated to the central metal. These often unstable species can be mechanistically important intermediates in thermal, photochemical, and electrochemical reactions involving metal-containing substances. Their generation via radiolysis provides an alternate means of characterizing them using kinetic and spectroscopic techniques. We hope these bibliographies on the radiation chemistry of metal ions and complexes, presented according to periodic groups, will prove useful to researchers in metallo-redox chemistry. These bibliographies contain only primary literature sources; reviews are not included. However, a list of general review articles on the radiation chemistry of metal ions and complexes is presented here in the first section which covers cobalt, rhodium and iridium, Group 9 in the new IUPAC notation. Additional parts of the bibliography are planned, covering other periodic groups. Part A of the bibliography was prepared by a search of the Radiation Chemistry Data Center Bibliographic Data Base (RCDCbib) through January 1986 for papers on rhodium, iridium and cobalt compounds, and radiolysis (both continuous and pulsed). Papers in which the use of metal compounds was incidental to the primary objective of the study were excluded. Excluded also were publications in unrefereed and obscure sources such as meeting proceedings, internal reports, dissertations, and patents. The majority of the studies in the resultant compilation deal with experiments performed on solutions, mainly aqueous, although a substantial fraction is devoted to solid-state esr measurements. The references are listed in separate sections for each of the metals, and are presented in approximate chronological order.

  10. Preparation of 186Re complexes of dimercaptosuccinic acid hydroxy ethylidine diphosphonate

    Kothari, K.; Pillai, M.R.A.; Unni, P.R.; Mathakar, A.R.; Shimpi, H.H.; Noronha, O.P.D.; Samuel, A.M.

    1998-01-01

    99m Tc(V)-DMSA and 99m Tc-HEDP are widely used for imaging medullary carcinoma and bone, respectively. 186 Re-HEDP is now well established as a therapeutic radiopharmaceutical for palliation of pain due to bone metastases. It is expected that 186/188 Re(V)-DMSA could find application for treating medullary carcinoma. In the present paper we report the work carried out for the preparation of 186 Re complexes of DMSA and HEDP and their bio-distribution studies in Wistar rats. 186 Re was prepared by irradiation of natural Re metal at a flux of 3x10 13 neutrons/cm 2 /s for seven days and processed after a cooling period of four days. The specific activity of 186 Re formed was ∼35 mCi/mg. Complexes with RC purity >98% could be prepared in both the cases by carefully optimizing the reaction conditions. Bio-distribution studies carried out in rats revealed that pharmacological behaviour of 186 Re(V)-DMSA was similar to that of 99m Tc(V)-DMSA. 186 Re-HEDP showed a bone uptake of ∼ 30% at 3 h post injection which remained almost constant for 48 h. (author)

  11. Controlling Magnetism of a Complex Metallic System Using Atomic Individualism

    Mudryk, Y.; Paudyal, D.; Pecharsky, V. K.; Gschneidner, K. A., Jr.; Misra, S.; Miller, G. J.

    2010-08-01

    When the complexity of a metallic compound reaches a certain level, a specific location in the structure may be critically responsible for a given fundamental property of a material while other locations may not play as much of a role in determining such a property. The first-principles theory has pinpointed a critical location in the framework of a complex intermetallic compound—Gd5Ge4—that resulted in a controlled alteration of the magnetism of this compound using precise chemical tools.

  12. Charge transfers in complex transition metal alloys (Ti2Fe)

    Abramovici, G.

    1998-01-01

    We introduce a new non-orthogonal tight-binding model, for complex alloys, in which electronic structure is characterized by charge transfers. We give the analytic calculation of a charge transfer, in which overlapping two-center terms are rigorously taken into account. Then, we apply numerically this result to an approximant phase of a quasicrystal of Ti 2 Fe alloy. This model is more particularly adapted to transition metals, and gives realistic densities of states. (orig.)

  13. The dynamic behavior of the exohedral transition metal complexes ...

    Home; Journals; Journal of Chemical Sciences; Volume 129; Issue 7. The dynamic behavior of the exohedral transition metal complexes of B₄₀ : η⁶- and η⁷-B₄₀Cr(CO) ₃ and Cr(CO) ₃η⁷-B₄η₀-Cr(CO) ₃. NAIWRIT KARMODAK ELUVATHINGAL D JEMMIS. REGULAR ARTICLE Volume 129 Issue 7 July 2017 pp ...

  14. Novel metal oxides prepared by ingenious synthetic routes

    Rao, C.N.R.; Gopalakrishnan, J.; Vidyasagar, K.; Ganguli, A.K.; Ramanan, A.; Ganapathi, L.

    1986-01-01

    Several novel oxides have been prepared by the decomposition of carbonate precursors of calcite structure of the general formulas Mn/sub 1-x/M/sub x/CO 3 (M = Mg,Co,Cd), Ca/sub 1-x/M/sup prime//sub x/CO 3 , and Ca/sub 1-x/-yM/sup //sub x/M/sup double-prime//sub y/CO 3 (M',M'' = Mn,Fe,Co). Typical of the oxides synthesized are a variety of monoxides, Mn/sub 1-x/M/sub x/O, of rocksalt structure and perovskite-related oxides such as Ca 2 FeCoO 5 , Ca 2 Co 2 O 5 , and Ca 3 Fe 2 MnO 8 , many of them exhibiting novel anion-vacancy-ordered superstructures. An interesting series of oxides prepared by the topotactic reduction of Ca 2 Fe/sub 2-x/Mn/sub x/O/sub 6-y/ (synthesized by the decomposition of the corresponding carbonate precursors) is Ca 2 Fe/sub 2-x/Mn/sub x/O 5 where three different coordination polyhedra (octahedra, tetrahedra, and square pyramids) of the transition metals coexist. Topotactic reduction of LaCoO 3 and LaNiO 3 yields new oxides, La 2 Co 2 O 5 and La 2 Ni 2 O 5 , possessing anion-vacancy-ordered superstructures. While La 2 Co 2 O 5 adopts the brownmillerite structure, La 2 Ni 2 O 5 exhibits a new type of vacancy ordering with octahedral and square-planar coordination of Ni 2+ . Slightly reduced LaNiO 3 seem to exhibit crystallographic shear (CS) planes similar to WO/sub 3-x/. Topotactic dehydration of isostructural Mo/sub 1-x/W/sub x/O 3 x H 2 O provides a convenient route for the synthesis of Mo/sub 1-x/W/sub x/O 3 (0 3 -related structure

  15. High index of refraction films for dielectric mirrors prepared by metal-organic chemical vapor deposition

    Brusasco, R.M.

    1989-01-01

    A wide variety of metal oxides with high index of refraction can be prepared by Metal-Organic Chemical Vapor Deposition. We present some recent optical and laser damage results on oxide films prepared by MOCVD which could be used in a multilayer structure for highly reflecting (HR) dielectric mirror applications. The method of preparation affects both optical properties and laser damage threshold. 10 refs., 8 figs., 4 tabs

  16. Spectro Analytical, Computational and In Vitro Biological Studies of Novel Substituted Quinolone Hydrazone and it's Metal Complexes.

    Nagula, Narsimha; Kunche, Sudeepa; Jaheer, Mohmed; Mudavath, Ravi; Sivan, Sreekanth; Ch, Sarala Devi

    2018-01-01

    Some novel transition metal [Cu (II), Ni (II) and Co (II)] complexes of nalidixic acid hydrazone have been prepared and characterized by employing spectro-analytical techniques viz: elemental analysis, 1 H-NMR, Mass, UV-Vis, IR, TGA-DTA, SEM-EDX, ESR and Spectrophotometry studies. The HyperChem 7.5 software was used for geometry optimization of title compound in its molecular and ionic forms. Quantum mechanical parameters, contour maps of highest occupied molecular orbitals (HOMO) and lowest unoccupied molecular orbitals (LUMO) and corresponding binding energy values were computed using semi empirical single point PM3 method. The stoichiometric equilibrium studies of metal complexes carried out spectrophotometrically using Job's continuous variation and mole ratio methods inferred formation of 1:2 (ML 2 ) metal complexes in respective systems. The title compound and its metal complexes screened for antibacterial and antifungal properties, exemplified improved activity in metal complexes. The studies of nuclease activity for the cleavage of CT- DNA and MTT assay for in vitro cytotoxic properties involving metal complexes exhibited high activity. In addition, the DNA binding properties of Cu (II), Ni (II) and Co (II) complexes investigated by electronic absorption and fluorescence measurements revealed their good binding ability and commended agreement of K b values obtained from both the techniques. Molecular docking studies were also performed to find the binding affinity of synthesized compounds with DNA (PDB ID: 1N37) and "Thymidine phosphorylase from E.coli" (PDB ID: 4EAF) protein targets.

  17. Synthesis, characterization, antibacterial and antifungal studies of some transition and rare earth metal complexes of N-benzylidene-2-hydroxybenzohydrazide

    T.K. Chondhekar

    2011-12-01

    Full Text Available The solid complexes of Cu(II, Co(II, Mn(II, La(III and Ce(III were prepared from bidentate Schiff base, N-benzylidene-2-hydroxybenzohydrazide. The Schiff base ligand was synthesized from 2-hyhdroxybenzohydrazide and benzaldehyde. These metal complexes were characterized by molar conductivity, magnetic susceptibility, thermal analysis, X-ray diffraction, FTIR, 1H-NMR, UV-Vis and mass spectroscopy. The analytical data of these metal complexes showed metal:ligand ratio of 1:2. The physico-chemical study supports the presence of square planar geometry around Cu(II and octahedral geometry around Mn(II, Co(II, La(III and Ce(III ions. The IR spectral data reveal that the ligand behaves as bidentate with ON donor atom sequence towards central metal ion. The molar conductance values of metal complexes suggest their non-electrolyte nature. The X-ray diffraction data suggest monoclinic crystal system for these complexes. Thermal behavior (TG/DTA and kinetic parameters calculated by Coats-Redfern method are suggestive of more ordered activated state in complex formation. The ligand and their metal complexes were screened for antibacterial activity against Staphylococcus aureus and Escherichia coli and fungicidal activity against Aspergillus niger and Trichoderma.

  18. The impact of metal transport processes on bioavailability of free and complex metal ions in methanogenic granular sludge

    Bartacek, J.; Fermoso, F.G.; Vergeldt, F.; Gerkema, E.; Maca, J.; As, van H.; Lens, P.N.L.

    2012-01-01

    Bioavailability of metals in anaerobic granular sludge has been extensively studied, because it can have a major effect on metal limitation and metal toxicity to microorganisms present in the sludge. Bioavailability of metals can be manipulated by bonding to complexing molecules such as

  19. Mechanics of metal-catecholate complexes: The roles of coordination state and metal types

    Xu, Zhiping

    2013-01-01

    There have been growing evidences for the critical roles of metal-coordination complexes in defining structural and mechanical properties of unmineralized biological materials, including hardness, toughness, and abrasion resistance. Their dynamic (e.g. pH-responsive, self-healable, reversible) properties inspire promising applications of synthetic materials following this concept. However, mechanics of these coordination crosslinks, which lays the ground for predictive and rational material design, has not yet been well addressed. Here we present a first-principles study of representative coordination complexes between metals and catechols. The results show that these crosslinks offer stiffness and strength near a covalent bond, which strongly depend on the coordination state and type of metals. This dependence is discussed by analyzing the nature of bonding between metals and catechols. The responsive mechanics of metal-coordination is further mapped from the single-molecule level to a networked material. The results presented here provide fundamental understanding and principles for material selection in metal-coordination-based applications. PMID:24107799

  20. Protection of metal artefacts with the formation of metal-oxalates complexes by Beauveria bassiana.

    Edith eJoseph

    2012-01-01

    Full Text Available Several fungi present high tolerance to toxic metals and some are able to transform metals into metal-oxalate complexes. In this study, the ability of Beauveria bassiana to produce copper oxalates was evaluated in vitro. Growth performance was tested on various copper-containing media. B. bassiana proved highly resistant to copper, tolerating concentrations of up to 20 g.L-1, and precipitating copper oxalates on all media tested. Chromatographic analyses showed that this species produced oxalic acid as sole metal chelator. The production of metal-oxalates can be used in the restoration and conservation of archaeological and modern metal artefacts. The production of copper-oxalates was confirmed directly using metallic pieces (both archaeological and modern. The conversion of corrosion products into copper oxalates was demonstrated as well. In order to assess whether the capability of B. bassiana to produce metal-oxalates could be applied to other metals, iron and silver were tested as well. Iron appears to be directly sequestered in the wall of the fungal hyphae forming oxalates and probably goethite. However, the formation of a homogeneous layer on the object is not yet optimal. Silver nitrate was extracellularly reduced into nanoparticles of elemental silver by an unknown mechanism. The production of copper oxalates is immediately applicable for the conservation of copper-based artefacts. For iron and silver this is not yet the case. However, the vast ability of B. bassiana to transform toxic metals using different immobilization mechanisms seems to offer considerable possibilities for industrial applications, such as the bioremediation of contaminated soils or the green synthesis of chemicals.

  1. 40 CFR Appendix B to Part 414 - Complexed Metal-Bearing Waste Streams

    2010-07-01

    ... 414—Complexed Metal-Bearing Waste Streams Chromium Azo dye intermediates/Substituted diazonium salts + coupling compounds Vat dyes Acid dyes Azo dyes, metallized/Azo dye + metal acetate Acid dyes, Azo...

  2. Cermet materials prepared by combustion synthesis and metal infiltration

    Holt, Joseph B.; Dunmead, Stephen D.; Halverson, Danny C.; Landingham, Richard L.

    1991-01-01

    Ceramic-metal composites (cermets) are made by a combination of self-propagating high temperature combustion synthesis and molten metal infiltration. Solid-gas, solid-solid and solid-liquid reactions of a powder compact produce a porous ceramic body which is infiltrated by molten metal to produce a composite body of higher density. AlN-Al and many other materials can be produced.

  3. THE ROLE OF METAL ION ON PHYSIOCHEMICAL PROPERTIES OF METAL ALUMINATES PREPARED BY IMPREGNATION METHOD

    S. Komeili

    2017-03-01

    Full Text Available A series of MAl2O4 (M=Ni, Zn, and Cu aluminates were prepared by using impregnation method; the metal content of the products was ranged between 5wt% to 25wt%. The samples were characterized by x-ray diffraction (XRD, Brunauer Emmett Teller (BET surface area, NH3 temperature-programmed desorption (NH3-TPD, and inductively coupled argon plasma (ICP. The specific surface areas of zinc, nickel and copper aluminates were in the ranges of 47-77m2/g, 63-87m2/g and 1.6-3m2/g, respectively. The surface acidity decreased in the order of CuAl2O4<< NiAl2O4< ZnAl2O4<< Al2O3. By increasing the amount of metals in the samples, the number of acidic sites decreased, but their strength did not significantly change. Ni-aluminates have fewer acidic sites than Zn-aluminates, particularly in strong acid sites

  4. On complexing of trivalent iron alcoholates. On transition metal alkoxyaluminates

    Rogova, T.V.; Turova, N.Ya.; Kozlova, N.I.

    1986-01-01

    When studying solubility in system Y(OR) 3 -Fe(OR) 3 -ROH (where R=i-Pr), the existence in solution of two complexes YF 2 (OR) 9 and YFe 3 (OR) 12 is ascertained, the range of X-ray amorphous glass formation being located between the two compositions. Preparative, IR- and mass-spectrometric studies of the glasses testify to the absence of bimetal alcoholates of Fe and Y of a definite composition in solid and gaseous phases

  5. Late transition metal m-or chemistry and D6 metal complex photoeliminations

    Sharp, Paul [Univ. of Missouri, Columbia, MO (United States)

    2015-07-31

    With the goal of understanding and controlling photoreductive elimination reactions from d6 transition metal complexes as part of a solar energy storage cycle we have investigated the photochemistry of Pt(IV) bromo, chloro, hydroxo, and hydroperoxo complexes. Photoreductive elimination reactions occur for all of these complexes and appear to involve initial Pt-Br, Pt-Cl, or Pt-O bond fission. In the case of Pt-OH bond fission, the subsequent chemistry can be controlled through hydrogen bonding to the hydroxo group.

  6. Preparation and examination of properties of samarium-153-EDTMP complex

    Nowak, M.; Garnuszek, P.; Lukasiewicz, A.; Wozniak, I.; Zulczyk, W.; Licinska, I.

    1995-01-01

    Preparation and properties of ethylenediaminetetramethylenephosphonic acid (EDTMP) as well as some properties of 153 Sm-EDTMP chelate have been examined. The chelate formed by samarium-153 (46.3 h, β - -decay) with EDTMP exhibits high bone uptake and can be used for treatment of disseminated, painful skeletal metastases. The purity and stability of solutions of 153 Sm-EDTMP chelate were examined in a broad range of samarium concentration and 153 Sm specific activity. The complex under study was examined by radio-TLC, -electrophoresis and radio-HPLC. The results obtained suggest the small size of molecules of 153 Sm-EDTMP chelate as compared with molecules of ''free''EDTMP. The results of biodistribution of 153 Sm-EDTMP determined in rats indicate the quick blood clearance, high deposition of radioactivity in bone and quick excretion of radioactivity into urine. No specific uptake of 153 Sm-EDTMP in extra-skeletal organs was found. (author). 42 refs, 13 figs, 22 tabs

  7. Metal Complexation with Chitosan and its Grafted Copolymer

    Abo-Hussen, A.A.; Elkholy, S.S.; Elsabee, M.Z.

    2005-01-01

    The adsorption of M (II); Co (II), Ni (If), Cu (II), Zn (II) and Cd (II) from aqueous solutions by chitosan flakes and beads have been studied. The maximum up-take of M (II) ions on chitosan beads was greater than on flakes. Batch adsorption experiments were carried out as a function of ph, agitation period and initial concentration of the metal ions. A ph of 6.0 was found to be optimum for M (II) adsorption on chitosan flakes and beads. The uptake of the ions was determined from the changes in its concentration, as measured by ultraviolet and visible spectroscopy. The metal ions uptake of chitosan grafted with vinyl pyridine (VP) is higher than that of the chitosan. The experimental data of the adsorption equilibrium from M (II)-solutions correlated well with the Langmuir and Freundlich equations. Several spectroscopic methods have been used to study the formation of the polymer/metal cation complex. The cation coordination is accompanied by proton displacement off the polymer or by fixation of a hydroxide ion in aqueous solutions. The largest ionic displacement is observed with Cu (II) and Zn (II) demonstrating the largest affinity of chitosan for these ions. The FT-IR spectral of the complexes show that both the amino and hydroxyl groups of chitosan participated in the chelation process. The ESR spectra of Cu-complex show an absorption at gi 2.06, g// = 2.23, A// x 10-4 (cm-1) = 160 and G = 3.8 indicating the formation of square planar structure. The adsorption of M (II) ions followed the sequence Cu (II) > Zn (II) > Cd (II) > Ni (II) > Co (II), this order seems to be independent on the size and the physical form of chitosan. SEM shows small membranous structure on the surface of chitosan flakes as compared to Cu (Il)- chitosan complex. EDTA was used for the desorption studies

  8. Preparation, spectral, X-ray powder diffraction and computational studies and genotoxic properties of new azo-azomethine metal chelates

    Bitmez, Şirin; Sayin, Koray; Avar, Bariş; Köse, Muhammet; Kayraldız, Ahmet; Kurtoğlu, Mükerrem

    2014-11-01

    A new tridentate azo-azomethine ligand, N‧-[{2-hydroxy-5-[(4-nitrophenyl)diazenyl]phenyl}methylidene]benzohydrazidemonohydrate, (sbH·H2O) (1), is prepared by condensation of benzohydrazide and 2-hydroxy-5-[(4-nitrophenyl)diazenyl]benzaldehyde (a) with treatment of a solution of diazonium salt of p-nitroaniline and 2-hydroxybenzaldehyde in EtOH. The five coordination compounds, [Co(sb)2]·4H2O (2), [Ni(sb)2]·H2O (3), [Cu(sb)2]·4H2O (4), [Zn(sb)2]·H2O (5) and [Cd(sb)2]·H2O (6) are prepared by reacting the Co(II), Ni(II), Cu(II), Zn(II) and Cd(II) ions with the ligand. The structures of the compounds are elucidated from the elemental analyses data and spectroscopic studies. It is found the ligand acts as a tridentate bending through phenolic and carbonyl oxygens and nitrogen atom of the Cdbnd Nsbnd group similar to the most of salicylaldimines. Comparison of the infrared spectra of the ligand and its metal complexes confirm that azo-Schiff base behaves as a monobasic tridentate ligand towards the central metal ion with an ONO donor sequence. Upon complexation with the ligand, the Cd(II), and Zn(II) ions form monoclinic structures, while Co(II), Cu(II) and Ni(II) ions form orthorhombic structures. Quantum chemical calculations are performed on tautomers and its metal chelates by using DFT/B3LYP method. Most stable tautomer is determined as tautomer (1a). The geometrical parameters of its metal chelates are obtained as theoretically. The NLO properties of tautomer (1a) and its metal complexes are investigated. Finally, the ligand and its metal complexes are assessed for their genotoxicity.

  9. A simple method for the preparation of difficult 99mTc complexes using surface adsorbed stannous ions

    Maddalena, D.J.; Snowdon, G.M.; Pojer, P.M.

    1987-01-01

    A simple new technique where stannous tin is adsorbed on the inner surface of plastic tubing and used to reduce ( 99m Tc) pertechnetate prior to labelling radiopharmaceuticals, has been evaluated, using some lipophillic and metal containing ligands. Complexes formed using the technique had good labelling efficiency and behaved the same in rat biodistribution studies as those prepared using conventional labelling methods. The labelling efficiency of the ligands was not related to their lipophillicity suggesting that this technique may be useful for labelling lipophillic and other difficult ligands such as those containing metals, which are incompatible with free stannous ions in solution. (M.E.L.) [es

  10. Organodioxygen complexes of some group 4B metal ions

    Tarafder, M.T.H.; Akhter Hossain; Gino Mariotto

    2003-09-01

    Organodioxygen complexes of some group 4B metal ions, viz., zirconium(IV), tin(IV) and lead(II) containing monodentate, bidentate and tridentate ligands were synthesized and characterized. The complexes have the compositions of [Zr(O)(O 2 )2C 5 H 5 N.H 2 O], [Zr(O)(O 2 - ) 2 .2OPPh 3 ], [Sn(O 2 )(C 9 H 6 NO) 2 ], [Sn(0 2 ) 2 .(CH 2 ) 2 (NH 2 ) 2 ], [Pb(O 2 - )(C 5 H 5 N) 2 NO 3 ], [Pb(O 2 )(C 8 H 6 NOH)], [Pb(O 2 - )(det)NO 3 ] and [PbO 2 - ) (C 5 H 4 NCOOH)NO 3 .H 2 O]. Because of apparent linearity of M- O 2 grouping, the V 1 (O-O) stretching modes were only Raman active, giving bands at 810- 841 cm 1 for the peroxo complexes (1, 3, ,4 and 6), while the bands in the superoxo complexes (2, 5, 7 and 8) appeared at 1020- 1100 cm -1 . The peroxo complex of Zr(IV) containing monodentate ligands were found to oxidize trans-stilbene to trans-stilbene oxide under stoichiometric conditions. The organoperoxo complexes of tin and lead were insensitive to oxidative processes. (author)

  11. Preparation and Characterization of Metal Soaps of Cocos nucifera ...

    This study investigated the extraction of Cocos nucifera seed oil (CSO) from Cocos nucifera seed using aqueous processing and the production of metal soaps from the oil and their characterization in terms of colour, pH, free caustic alkalinity, foaming power, foam stability, and corrosion inhibition test. The metal soaps of the ...

  12. A series of 2D metal-quinolone complexes: Syntheses, structures, and physical properties

    He, Jiang-Hong [College of Chemistry and Chemical Engineering, Southwest University, Chongqing 400715 (China); Xiao, Dong-Rong, E-mail: xiaodr98@yahoo.com.cn [College of Chemistry and Chemical Engineering, Southwest University, Chongqing 400715 (China); Chen, Hai-Yan; Sun, Dian-Zhen; Yan, Shi-Wei; Wang, Xin; Ye, Zhong-Li [College of Chemistry and Chemical Engineering, Southwest University, Chongqing 400715 (China); Luo, Qun-Li, E-mail: qlluo@swu.edu.cn [College of Chemistry and Chemical Engineering, Southwest University, Chongqing 400715 (China); Wang, En-Bo, E-mail: wangeb889@nenu.edu.cn [Key Laboratory of Polyoxometalate Science of Ministry of Education, Department of Chemistry, Northeast Normal University, Changchun 130024 (China)

    2013-02-15

    Six novel 2D metal-quinolone complexes, namely [Cd(cfH)(bpdc)]{center_dot}H{sub 2}O (1), [M(norfH)(bpdc)]{center_dot}H{sub 2}O (M=Cd (2) and Mn (3)), [Mn{sub 2}(cfH)(odpa)(H{sub 2}O){sub 3}]{center_dot}0.5H{sub 2}O (4), [Co{sub 2}(norfH)(bpta)({mu}{sub 2}-H{sub 2}O)(H{sub 2}O){sub 2}]{center_dot}H{sub 2}O (5) and [Co{sub 3}(saraH){sub 2}(Hbpta){sub 2}(H{sub 2}O){sub 4}]{center_dot}9H{sub 2}O (6) (cfH=ciprofloxacin, norfH=norfloxacin, saraH=sarafloxacin, bpdc=4,4 Prime -biphenyldicarboxylate, odpa=4,4 Prime -oxydiphthalate, bpta=3,3 Prime ,4,4 Prime -biphenyltetracarboxylate) have been synthesized and characterized. Compounds 1-3 consist of 2D arm-shaped layers based on the 1D {l_brace}M(COO){r_brace}{sub n}{sup n+} chains. Compounds 4 and 5 display 2D structures based on tetranuclear manganese or cobalt clusters with (3,6)-connected kgd topology. Compound 6 exhibits a 2D bilayer structure, which represents the first example of metal-quinolone complexes with 2D bilayer structure. By inspection of the structures of 1-6, it is believed that the long aromatic polycarboxylate ligands are important for the formation of 2D metal-quinolone complexes. The magnetic properties of compounds 3-6 was studied, indicating the existence of antiferromagnetic interactions. Furthermore, the luminescent properties of compounds 1-2 are discussed. - Graphical abstract: Six novel 2D metal-quinolone complexes have been prepared by self-assemblies of the quinolones and metal salts in the presence of long aromatic polycarboxylates. Highlights: Black-Right-Pointing-Pointer Compounds 1-3 consist of novel 2D arm-shaped layers based on the 1D {l_brace}M(COO){r_brace}{sub n}{sup n+} chains. Black-Right-Pointing-Pointer Compounds 4 and 5 are two novel 2D layers based on tetranuclear Mn or Co clusters with kgd topology. Black-Right-Pointing-Pointer Compound 6 is the first example of metal-quinolone complexes with 2D bilayer structure. Black-Right-Pointing-Pointer Compounds 1-6 represent six unusual

  13. Metal doped fluorocarbon polymer films prepared by plasma polymerization using an RF planar magnetron target

    Biederman, H.; Holland, L.

    1983-01-01

    Fluorocarbon films have been prepared by plasma polymerization of CF 4 using an RF planar magnetron with an aluminium target. More than one order of magnitude higher deposition rate has been achieved in comparison with an r.f. diode system operated under similar conditions of monomer pressure and flow rate and power input. A glow discharge in a CF 4 [25%]-argon[75%] mixture was used to incorporate aluminium from a target electrode into the polymer films. The foregoing mixture and another based on CF 4 [87%]-argon[13%] were used in the RF discharge with a copper target. Some experiments with a gold target and pure CF 4 as the inlet gas were also made. The film structure was examined by SEM and TEM and characteristic micrographs are presented here. The composition of the films was estimated from an EAS study. The sheet resistivity of the metal/polymer film complexes was determined. (orig.)

  14. Infrared transmission study of lanthanide fullerides SmxC60 prepared by metal vapor synthesis

    Zhao, W.; Simmons, W.B. Jr.; Sweany, R.L.

    1997-01-01

    Lanthanide fulleride Sm x C 60 films were prepared by metal vapor synthesis and the valence state of the C 60 cage in the films was investigated by infrared transmission spectroscopy. Three films with different doping contents of Sm showed red-shift frequencies of F 1u (4) at 1347, 1362 and 1392 (1411) cm -1 , respectively, indicating that the major phase with corresponding valence state n∼-5, -3 and -1 might exist in the films. The other major additional feature of activated pentagonal pinch mode A g (2) was observed at 1445 or 1448 cm -1 in the films, which suggested that the Sm atoms might bond to the five-membered ring of the C 60 cage and ferrocene-like Sm x C 60 complexes might be formed. (orig.)

  15. 40 CFR 721.2097 - Azo chromium complex dyestuff preparation (generic name).

    2010-07-01

    ... 40 Protection of Environment 30 2010-07-01 2010-07-01 false Azo chromium complex dyestuff... New Uses for Specific Chemical Substances § 721.2097 Azo chromium complex dyestuff preparation... substance identified generically as an azo chromium complex dyestuff preparation (PMN P-95-240) is subject...

  16. Catalytic hydrogenation using complexes of base metals with tridentate ligands

    Hanson, Susan K.; Zhang, Guoqi; Vasudevan, Kalyan V.

    2017-02-14

    Complexes of cobalt and nickel with tridentate ligand PNHP.sup.R are effective for hydrogenation of unsaturated compounds. Cobalt complex [(PNHP.sup.Cy)Co(CH.sub.2SiMe.sub.3)]BAr.sup.F.sub.4 (PNHP.sup.Cy=bis[2-(dicyclohexylphosphino)ethyl]amine, BAr.sup.F.sub.4=B(3,5-(CF.sub.3).sub.2C.sub.6H.sub.3).sub.4)) was prepared and used with hydrogen for hydrogenation of alkenes, aldehydes, ketones, and imines under mild conditions (25-60.degree. C., 1-4 atm H.sub.2). Nickel complex [(PNHP.sup.Cy)Ni(H)]BPh.sub.4 was used for hydrogenation of styrene and 1-octene under mild conditions. (PNP.sup.Cy)Ni(H) was used for hydrogenating alkenes.

  17. Catalytic hydrogenation using complexes of base metals with tridentate ligands

    Vasudevan, Kalyan V.; Zhang, Guoqi; Hanson, Susan K.

    2016-09-06

    Complexes of cobalt and nickel with tridentate ligand PNHP.sup.R are effective for hydrogenation of unsaturated compounds. Cobalt complex [(PNHP.sup.Cy)Co(CH.sub.2SiMe.sub.3)]BAr.sup.F.sub.4 (PNHP.sup.Cy=bis[2-(dicyclohexylphosphino)ethyl]amine, BAr.sup.F.sub.4=B(3,5-(CF.sub.3).sub.2C.sub.6H.sub.3).sub.4)) was prepared and used with hydrogen for hydrogenation of alkenes, aldehydes, ketones, and imines under mild conditions (25-60.degree. C., 1-4 atm H.sub.2). Nickel complex [(PNHP.sup.Cy)Ni(H)]BPh.sub.4 was used for hydrogenation of styrene and 1-octene under mild conditions. (PNP.sup.Cy)Ni(H) was used for hydrogenating alkenes.

  18. Neutral glycoconjugated amide-based calix[4]arenes: complexation of alkali metal cations in water.

    Cindro, Nikola; Požar, Josip; Barišić, Dajana; Bregović, Nikola; Pičuljan, Katarina; Tomaš, Renato; Frkanec, Leo; Tomišić, Vladislav

    2018-02-07

    Cation complexation in water presents a unique challenge in calixarene chemistry, mostly due to the fact that a vast majority of calixarene-based cation receptors is not soluble in water or their solubility has been achieved by introducing functionalities capable of (de)protonation. Such an approach inevitably involves the presence of counterions which compete with target cations for the calixarene binding site, and also rather often requires the use of ion-containing buffer solutions in order to control the pH. Herein we devised a new strategy towards the solution of this problem, based on introducing carbohydrate units at the lower or upper rim of calix[4]arenes which comprise efficient cation binding sites. In this context, we prepared neutral, water-soluble receptors with secondary or tertiary amide coordinating groups, and studied their complexation with alkali metal cations in aqueous and methanol (for the comparison purpose) solutions. Complexation thermodynamics was quantitatively characterized by UV spectrometry and isothermal titration calorimetry, revealing that one of the prepared tertiary amide derivatives is capable of remarkably efficient (log K ≈ 5) and selective binding of sodium cations among alkali metal cations in water. Given the ease of the synthetic procedure used, and thus the variety of accessible analogues, this study can serve as a platform for the development of reagents for diverse purposes in aqueous media.

  19. Preparation of solid-state samples of a transition metal coordination compound for synchrotron radiation photoemission studies

    Crotti, C; Celestino, T; Fontana, S

    2003-01-01

    The aim of this research was to identify a sample preparation method suitable for the study of transition metal complexes by photoemission spectroscopy with synchrotron radiation as the X-ray source, even in the case where the compound is not evaporable. Solid-phase samples of W(CO) sub 4 (dppe) [dppe=1,2-bis(diphenylphosphino)ethane] were prepared according to different methods and their synchrotron radiation XPS spectra measured. The spectra acquired from samples prepared by spin coating show core level peaks only slightly broader than the spectrum recorded from UHV evaporated samples. Moreover, for these samples the reproducibility of the binding energy values is excellent. The dependence of the spin coating technique on parameters such as solvent and solution concentration, spinning speed and support material was studied. The same preparation method also allowed the acquisition of valence band spectra, the main peaks of which were clearly resolved. The results suggest that use of the spin coating techniqu...

  20. Photochemical preparation of aluminium oxide layers via vacuum ultraviolet irradiation of a polymeric hexanoato aluminium complex

    Wennrich, L.; Khalil, H.; Bundesmann, C.; Decker, U.; Gerlach, J.W.; Helmstedt, U.; Manova, D.; Naumov, S.; Prager, L.

    2013-01-01

    By means of photochemical conversion of thin layers of a polymeric hexanoato aluminium complex as the precursor, thin aluminium oxide layers were prepared onto silicon wafers. The precursor compound was synthesized and characterized by several analytical techniques like NMR, FTIR, XPS, ICP, and found to be a polymeric aluminium-containing coordination compound which has been proposed to be a hydroxo-bridged aluminium chain with pendant hexanoyl side-chains ascertained as catena-poly[{di(κ-O,O-hexanoato)aluminium}(μ-hydroxo)] (PHAH). Thin layers deposited from a solution of PHAH in toluene onto silicon wafers were irradiated using VUV radiation from a xenon excimer lamp. The layers were characterized by XPS, XRD, XRR, and spectroscopic ellipsometry. VUV radiation with a radiant exposure of E = 36 J cm −2 led to almost carbon-free amorphous layers with a composition close to that of alumina having a density of about 2.1 g cm −3 . Thus, using the example of a polymeric aluminium complex, the potential of the photochemical conversion of metal complexes into oxides could be shown as an alternative method, in addition to sol–gel techniques, for the generation of thin plane metal-oxide layers at normal temperature and pressure. Highlights: ► A polymeric aluminium complex was synthesized and characterized by NMR, FTIR, XPS and ICP. ► Thin layers of the compound were irradiated using vacuum-UV radiation and converted to AlO x . ► Quantum-chemical calculations explain the conversion mechanism.

  1. Fixation of metallic sulfosalicylate complexes on an anionic exchange resin

    Cahuzac, S.

    1969-06-01

    Since sulfosalicylate ions have acid-base properties, sulfosalicylate complexes have an apparent stability which varies with the ph. As a result, the fixation of sulfo-salicylates on an anionic exchange resin depends on the ph of the solution in equilibrium with the resin. This research has been aimed at studying the influence of the ph on the fixation on an anionic exchange resin (Dowex 1 x 4) of sulfosalicylate anions on the one hand, and of metallic sulfosalicylate complexes on the other hand. In the first part of this work, a determination has been made, by frontal analysis of the distribution of sulfosalicylate ions in the resin according to the total sulfosalicylate I concentration in the aqueous solution in equilibrium with the resin. The exchange constants of these ions between the resin and the solution have been calculated. In the second part, a study has been made of the fixation of anionic sulfosalicylate complexes of Fe(III), Al(III), Cr(III), Cu(II), Ni(II), Co(II), Zn(II), Mn(II), Cd(II), Fe(II) and UO 2 2+ . By measuring the partition coefficients of these different elements between the resin and the solution it has been possible to give interpretation for the modes of fixation of the metallic ions, and to calculate their exchange constant between the resin and the solution. The relationship has been established for each metallic element studied, between its partition coefficient, the ph and the total concentration of the complexing agent in solution. Such a relationship makes it possible to predict, for given conditions, the nature of the species in solution and in the resin, as well as the partition coefficient of a metallic, element. Finally, in the third part of the work, use has been made of results obtained previously, to carry out some separations (Ni 2+ - Co 2+ ; Ni 2+ - Co 2+ - Cu 2+ ; UO 2 2+ - Fe 3+ ; UO 2 2+ - Cr 3+ ; UO 2 2+ - Cu 2+ ; UO 2 2+ - Ni 2+ ; UO 2 2+ - Co 2+ ; UO 2 2+ - Mn 2+ and UO 2 2+ - Cd 2+ ), as well as the purification

  2. Preparation of oxide glasses from metal alkoxides by sol-gel method

    Kamiya, K.; Yoko, T.; Sakka, S.

    1987-01-01

    An investigation is carried out on the types of siloxane polymers produced in the course of the hydrolysis of silicon tetraethoxide, as well as the preparation of oxide glasses from metal alkoxides by the sol-gel method.

  3. Development of luminescent sensors based on transition metal complexes for the detection of nitroexplosives.

    Sathish, Veerasamy; Ramdass, Arumugam; Velayudham, Murugesan; Lu, Kuang-Lieh; Thanasekaran, Pounraj; Rajagopal, Seenivasan

    2017-12-12

    The detection of chemical explosives is a major area of research interest and is essential for the military as well as homeland security to counter the catastrophic effects of global terrorism. In recent years, tremendous effort has been devoted to the development of luminescent materials for the detection of explosives in the vapor, solution, and solid states with a high degree of selectivity and sensitivity and a rapid response time. Apart from the wide range of organic fluorescent chemosensors, transition metal complexes play a prominent role in the sensing of nitroaromatic explosives owing to their rich photophysical characteristics. This review briefly summarizes the salient features of the design and preparation of transition metal (Zn(ii), Ir(iii), Pd(ii), Pt(ii), Re(i) and Ru(ii)) complexes/metallacycles/metallosupramolecules with emphasis on their photophysical properties, sensing behavior, mechanism of action, and the driving forces for detecting explosives and future prospects and challenges. Most of the probes that have been reported to date act as "turn-off" luminescent sensors because their emission (intensity, lifetime, and quantum yield) is eventually quenched upon sensing with nitroaromatic compounds (NACs) through photo-induced electron or energy transfer. These unique properties of transition metal complexes in response to explosives open up new vistas for the development of real world applications such as on-site detection, in-field security, forensic research, etc.

  4. Solvent properties of hydrazine in the preparation of metal chalcogenide bulk materials and films.

    Yuan, Min; Mitzi, David B

    2009-08-21

    A combination of unique solvent properties of hydrazine enables the direct dissolution of a range of metal chalcogenides at ambient temperature, rendering this an extraordinarily simple and soft synthetic approach to prepare new metal chalcogenide-based materials. The extended metal chalcogenide parent framework is broken up during this process, and the resulting metal chalcogenide building units are re-organized into network structures (from 0D to 3D) based upon their interactions with the hydrazine/hydrazinium moieties. This Perspective will review recent crystal and materials chemistry developments within this family of compounds and will briefly discuss the utility of this approach in metal chalcogenide thin-film deposition.

  5. Complexation of metal ions with humic acid: charge neutralization model

    Kim, J.I.; Czerwinski, K.R.

    1995-01-01

    A number of different approaches are being used for describing the complexation equilibrium of actinide ions with humic or fulvic acid. The approach chosen and verified experimentally by Tu Muenchen will be discussed with notable examples from experiment. This approach is based on the conception that a given actinide ion is neutralized upon complexation with functional groups of humic or fulvic acid, e.g. carboxylic and phenolic groups, which are known as heterogeneously cross-linked polyelectrolytes. The photon energy transfer experiment with laser light excitation has shown that the actinide ion binding with the functional groups is certainly a chelation process accompanied by metal ion charge neutralization. This fact is in accordance with the experimental evidence of the postulated thermodynamic equilibrium reaction. The experimental results are found to be independent of origin of humic or fulvic acid and applicable for a broad range of pH. (authors). 23 refs., 7 figs., 1 tab

  6. Complexing agent and heavy metal removals from metal plating effluent by electrocoagulation with stainless steel electrodes.

    Kabdaşli, Işik; Arslan, Tülin; Olmez-Hanci, Tuğba; Arslan-Alaton, Idil; Tünay, Olcay

    2009-06-15

    In the present study, the treatability of a metal plating wastewater containing complexed metals originating from the nickel and zinc plating process by electrocoagulation using stainless steel electrodes was experimentally investigated. The study focused on the effect of important operation parameters on electrocoagulation process performance in terms of organic complex former, nickel and zinc removals as well as sludge production and specific energy consumption. The results indicated that increasing the applied current density from 2.25 to 9.0 mA/cm(2) appreciably enhanced TOC removal efficiency from 20% to 66%, but a further increase in the applied current density to 56.25 mA/cm(2) did not accelerate TOC removal rates. Electrolyte concentration did not affect the process performance significantly and the highest TOC reduction (66%) accompanied with complete heavy metal removals were achieved at the original chloride content ( approximately 1500 mg Cl/L) of the wastewater sample. Nickel removal performance was adversely affected by the decrease of initial pH from its original value of 6. Optimum working conditions for electrocoagulation of metal plating effluent were established as follows: an applied current density of 9 mA/cm(2), the effluent's original electrolyte concentration and pH of the composite sample. TOC removal rates obtained for all electrocoagulation runs fitted pseudo-first-order kinetics very well (R(2)>92-99).

  7. Alkali-crown ether complexes at metal surfaces

    Thontasen, Nicha; Deng, Zhitao; Rauschenbach, Stephan [Max Planck Institute for Solid State Research, Stuttgart (Germany); Levita, Giacomo [University of Trieste, Trieste (Italy); Malinowski, Nikola [Max Planck Institute for Solid State Research, Stuttgart (Germany); Bulgarian Academy of Sciences, Sofia (Bulgaria); Kern, Klaus [Max Planck Institute for Solid State Research, Stuttgart (Germany); EPFL, Lausanne (Switzerland)

    2010-07-01

    Crown ethers are polycyclic ethers which, in solution, selectively bind cations depending on the size of the ring cavity. The study of a single host-guest complex is highly desirable in order to reveal the characteristics of these specific interactions at the atomic scale. Such detailed investigation is possible at the surface where high resolution imaging tools like scanning tunneling microscopy (STM) can be applied. Here, electrospray ion beam deposition (ES-IBD) is employed for the deposition of Dibenzo-24-crown-8 (DB24C8)-H{sup +}, -Na{sup +} and -Cs{sup +} complexes on a solid surface in ultrahigh vacuum (UHV). Where other deposition techniques have not been successful, this deposition technique combines the advantages of solution based preparation of the complex ions with a highly clean and controlled deposition in UHV. Single molecular structures and the cation-binding of DB24C8 at the surface are studied in situ by STM and MALDI-MS (matrix assisted laser desorption ionization mass spectrometry). The internal structure of the complex, i.e. ring and cavity, is observable only when alkali cations are incorporated. The BD24C8-H{sup +} complex in contrast appears as a compact feature. This result is in good agreement with theoretical models based on density functional theory calculations.

  8. Observation of metallic sphere–complex plasma interactions in microgravity

    Schwabe, M; Zhdanov, S; Hagl, T; Huber, P; Rubin-Zuzic, M; Zaehringer, E; Thomas, H M; Lipaev, A M; Molotkov, V I; Naumkin, V N; Fortov, V E; Vinogradov, P V

    2017-01-01

    The PK-3 Plus laboratory on board the International Space Station is used to study the interaction between metallic spheres and a complex plasma. We show that the metallic spheres significantly affect both the local plasma environment and the microparticle dynamics. The spheres charge under the influence of the plasma and repel the microparticles, forming cavities surrounding the spheres. The size of the cavity around a sphere is used to study the force balance acting on microparticles at the cavity edge. We show that the ion drag force and pressure force from other microparticles balances with the electric force acting from the sphere to within 20%. At intermediate distances from the sphere surface, the interaction between the microparticles and the metallic spheres is attractive due to the drag force stemming from the ions which are moving towards the highly charged spheres. The spheres thus strongly affect the plasma fluxes. This modification of the plasma flux can lead to an effective surface tension acting on the microparticles, and to the excitation of dust-density waves near the spheres, as the local electric field crosses a threshold. (paper)

  9. Green methods for preparing highly co2 selective and h2s tolerant metal organic frameworks

    Eddaoudi, Mohamed; Shekhah, Osama; Belmabkhout, Youssef

    2015-01-01

    A green route for preparing a metal organic framework include mixing metal precursor with a ligand precursor to form a solvent-free mixture; adding droplets of water to the mixture; heating the mixture at a first temperature after adding the water

  10. Preparation and use of crystalline bis-monoorganic phosphonate and phosphate salts of tetravalent metals

    Maya, L.

    1980-06-26

    A method of preparing and using the crystalline organic derivatives of the tetravalent metal phosphates and phosphonates provides for the contacting of an aqueous solution of a metal nitrate, with a solution of an organophosphorus acid for a period of time at room temperature that is sufficient for the formation of a metal phosphate product, and thereafter recovering said product. According to the invention, the product of the disclosed process is used in effecting analytical separations, such as ion exchange and chromatography.

  11. Removal of Heavy Metals from Drinking Water by Magnetic Carbon Nanostructures Prepared from Biomass

    Muneeb Ur Rahman Khattak, Muhammad; Zahoor, Muhammad; Muhammad, Bakhtiar; Khan, Farhat Ali; Ullah, Riaz; AbdEI-Salam, Naser M.

    2017-01-01

    Heavy metals contamination of drinking water has significant adverse effects on human health due to their toxic nature. In this study a new adsorbent, magnetic graphitic nanostructures were prepared from watermelon waste. The adsorbent was characterized by different instrumental techniques (surface area analyzer, FTIR, XRD, EDX, SEM, and TG/DTA) and was used for the removal of heavy metals (As, Cr, Cu, Pb, and Zn) from water. The adsorption parameters were determined for heavy metals adsorpti...

  12. IRMPD Action Spectroscopy of Alkali Metal Cation-Cytosine Complexes: Effects of Alkali Metal Cation Size on Gas Phase Conformation

    Yang, B.; Wu, R.R.; Polfer, N.C.; Berden, G.; Oomens, J.; Rodgers, M.T.

    2013-01-01

    The gas-phase structures of alkali metal cation-cytosine complexes generated by electrospray ionization are probed via infrared multiple photon dissociation (IRMPD) action spectroscopy and theoretical calculations. IRMPD action spectra of five alkali metal cation-cytosine complexes exhibit both

  13. Photoinitiated Electron Collection in Mixed-Metal Supramolecular Complexes: Development of Photocatalysts for Hydrogen Production. Final Report of Progress August 2017

    Tanko, James M. [Virginia Polytechnic Inst. and State Univ. (Virginia Tech), Blacksburg, VA (United States). Dept. of Chemistry

    2017-08-01

    Mixed-metal supramolecular complexes containing one or two RuII light absorbing subunits coupled through polyazine bridging ligands to a RhIII reactive metal center were prepared for use as photocatalysts for the production of solar H2 fuel from H2O. The electrochemical, photophysical, and photochemical properties upon variation of the monodentate, labile ligands coordinated to the Rh reactive metal center were investigated.

  14. Effect of preparation method of metal hydride electrode on efficiency of hydrogen electrosorption process

    Giza, Krystyna [Czestochowa University of Technology (Poland). Faculty of Production Engineering and Materials Technology; Drulis, Henryk [Trzebiatowski Institute of Low Temperatures and Structure Research PAS, Wroclaw (Poland)

    2016-02-15

    The preparation of negative electrodes for nickel-metal hydride batteries using LaNi{sub 4.3}Co{sub 0.4}Al{sub 0.3} alloy is presented. The constant current discharge technique is employed to determine the discharge capacity, the exchange current density and the hydrogen diffusion coefficient of the studied electrodes. The electrochemical performance of metal hydride electrode is strongly affected by preparation conditions. The results are compared and the advantages and disadvantages of preparation methods of the electrodes are also discussed.

  15. Hydrogen storage and evolution catalysed by metal hydride complexes.

    Fukuzumi, Shunichi; Suenobu, Tomoyoshi

    2013-01-07

    The storage and evolution of hydrogen are catalysed by appropriate metal hydride complexes. Hydrogenation of carbon dioxide by hydrogen is catalysed by a [C,N] cyclometalated organoiridium complex, [Ir(III)(Cp*)(4-(1H-pyrazol-1-yl-κN(2))benzoic acid-κC(3))(OH(2))](2)SO(4) [Ir-OH(2)](2)SO(4), under atmospheric pressure of H(2) and CO(2) in weakly basic water (pH 7.5) at room temperature. The reverse reaction, i.e., hydrogen evolution from formate, is also catalysed by [Ir-OH(2)](+) in acidic water (pH 2.8) at room temperature. Thus, interconversion between hydrogen and formic acid in water at ambient temperature and pressure has been achieved by using [Ir-OH(2)](+) as an efficient catalyst in both directions depending on pH. The Ir complex [Ir-OH(2)](+) also catalyses regioselective hydrogenation of the oxidised form of β-nicotinamide adenine dinucleotide (NAD(+)) to produce the 1,4-reduced form (NADH) under atmospheric pressure of H(2) at room temperature in weakly basic water. In weakly acidic water, the complex [Ir-OH(2)](+) also catalyses the reverse reaction, i.e., hydrogen evolution from NADH to produce NAD(+) at room temperature. Thus, interconversion between NADH (and H(+)) and NAD(+) (and H(2)) has also been achieved by using [Ir-OH(2)](+) as an efficient catalyst and by changing pH. The iridium hydride complex formed by the reduction of [Ir-OH(2)](+) by H(2) and NADH is responsible for the hydrogen evolution. Photoirradiation (λ > 330 nm) of an aqueous solution of the Ir-hydride complex produced by the reduction of [Ir-OH(2)](+) with alcohols resulted in the quantitative conversion to a unique [C,C] cyclometalated Ir-hydride complex, which can catalyse hydrogen evolution from alcohols in a basic aqueous solution (pH 11.9). The catalytic mechanisms of the hydrogen storage and evolution are discussed by focusing on the reactivity of Ir-hydride complexes.

  16. Arc plasma assisted rotating electrode process for preparation of metal pebbles

    Mohanty, T.; Tripathi, B.M.; Mahata, T.; Sinha, P.K.

    2014-01-01

    Spherical beryllium pebbles of size ranging from 0.2-2 mm are required as neutron multiplying material in solid Test Blanket Module (TBM) of International Thermonuclear Experimental Reactor (ITER). Rotating electrode process (REP) has been identified as a suitable technique for preparation of beryllium pebbles. In REP, arc plasma generated between non-consumable electrode (cathode) and rotating metal electrode (anode) plays a major role for continuous consumption of metal electrode and preparation of spherical metal pebbles. This paper focuses on description of the process, selection of sub-systems for development of REP experimental set up and optimization of arc parameters, such as, cathode geometry, arc current, arc voltage, arc gap and carrier gas flow rate for preparation of required size spherical metal pebbles. Other parameters which affect the pebbles sizes are rotational speed, metal electrode diameter and physical properties of the metal. As beryllium is toxic in nature its surrogate metals such as stainless steel (SS) and Titanium (Ti) were selected to evaluate the performance of the REP equipment. Several experiments were carried out using SS and Ti electrode and process parameters have been optimized for preparation of pebbles of different sizes. (author)

  17. Frustration across the periodic table: heterolytic cleavage of dihydrogen by metal complexes.

    Bullock, R Morris; Chambers, Geoffrey M

    2017-08-28

    This perspective examines frustrated Lewis pairs (FLPs) in the context of heterolytic cleavage of H 2 by transition metal complexes, with an emphasis on molecular complexes bearing an intramolecular Lewis base. FLPs have traditionally been associated with main group compounds, yet many reactions of transition metal complexes support a broader classification of FLPs that includes certain types of transition metal complexes with reactivity resembling main group-based FLPs. This article surveys transition metal complexes that heterolytically cleave H 2 , which vary in the degree that the Lewis pairs within these systems interact. Many of the examples include complexes bearing a pendant amine functioning as the base with the metal functioning as the hydride acceptor. Consideration of transition metal compounds in the context of FLPs can inspire new innovations and improvements in transition metal catalysis.This article is part of the themed issue 'Frustrated Lewis pair chemistry'. © 2017 The Author(s).

  18. Oligomeric rare-earth metal cluster complexes with endohedral transition metal atoms

    Steinberg, Simon; Zimmermann, Sina; Brühmann, Matthias; Meyer, Eva; Rustige, Christian; Wolberg, Marike; Daub, Kathrin; Bell, Thomas; Meyer, Gerd, E-mail: gerd.meyer@uni-koeln.de

    2014-11-15

    Comproportionation reactions of rare-earth metal trihalides (RX{sub 3}) with the respective rare-earth metals (R) and transition metals (T) led to the formation of 22 oligomeric R cluster halides encapsulating T, in 19 cases for the first time. The structures of these compounds were determined by single-crystal X-ray diffraction and are composed of trimers ((T{sub 3}R{sub 11})X{sub 15}-type, P6{sub 3}/m), tetramers ((T{sub 4}R{sub 16})X{sub 28}(R{sub 4}) (P-43m), (T{sub 4}R{sub 16})X{sub 20} (P4{sub 2}/nnm), (T{sub 4}R{sub 16})X{sub 24}(RX{sub 3}){sub 4} (I4{sub 1}/a) and (T{sub 4}R{sub 16})X{sub 23} (C2/m) types of structure) and pentamers ((Ru{sub 5}La{sub 14}){sub 2}Br{sub 39}, Cc) of (TR{sub r}){sub n} (n=2–5) clusters. These oligomers are further enveloped by inner (X{sup i}) as well as outer (X{sup a}) halido ligands, which possess diverse functionalities and interconnect like oligomers through i–i, i–a and/or a–i bridges. The general features of the crystal structures for these new compounds are discussed and compared to literature entries as well as different structure types with oligomeric T centered R clusters. Dimers and tetramers originating from the aggregation of (TR{sub 6}) octahedra via common edges are more frequent than trimers and pentamers, in which the (TR{sub r}) clusters share common faces. - Graphical abstract: Rare earth-metal cluster complexes with endohedral transition metal atoms (TR{sub 6}) may connect via common edges or faces to form dimers, trimers, tetramers and pentamers of which the tetramers are the most prolific. Packing effects and electron counts play an important role. - Highlights: • Rare-earth metal cluster complexes encapsulate transition metal atoms. • Oligomers are built via connection of octahedral clusters via common edges or faces. • Dimers through pentamers with closed structures are known. • Tetramers including a tetrahedron of endohedral atoms are the most prolific.

  19. Redistribution of mineral elements in wheat grain when applying the complex enzyme preparations based on phytase

    Elena Kuznetsova

    2016-01-01

    Full Text Available Biogenic minerals play an important role in the whole human nutrition, but they are included in the grain of the phytates that reduces their bioavailability. Whole wheat bread is generally considered a healthy food, but the presence of mineral elements in it is insignificant, because of weak phytate degradation. From all sources of exogenous phytase the most productive are microscopic fungi. To accelerate the process of transition hard mineral elements are mobilized to implement integrated cellulolytic enzyme preparation based on the actions of phytase (producer is Penicillium canescens. Phytase activity was assessed indirectly by the rate of release of phosphate from the substrate. It has been established that the release rate of the phosphoric acid substrate is dependent on the composition of the drug and the enzyme complex is determined by the presence of xylanase. The presented experimental data shows that a cellulase treatment of the grain in conjunction with the β-glucanase or xylanase leading to an increase in phytase activity could be 1.4 - 2.3 times as compared with the individual enzymes. As a result of concerted action of enzymes complex preparation varies topography grain, increase the pore sizes in seed and fruit shells that facilitate the penetration of the enzyme phytase in the aleurone layer to the site of phytin hydrolysis and leads to an increase in phytase activity. In terms of rational parameters of enzymatic hydrolysis, the distribution of mineral elements in the anatomical parts of the grain after processing complex enzyme preparation with the help of X-ray detector EMF miniCup system in a scanning electron microscope JEOL JSM 6390 were investigated. When processing enzyme preparation wheat trend in the distribution of mineral elements, characteristic of grain - the proportion of these elements in the aleurone layer decreases, and in the endosperm increases. Because dietary fiber and phytate found together in the

  20. Synthesis of metal complexes involving Schiff base ligand with methylenedioxy moiety: spectral, thermal, XRD and antimicrobial studies.

    Sundararajan, M L; Jeyakumar, T; Anandakumaran, J; Karpanai Selvan, B

    2014-10-15

    Metal complexes of Zn(II), Cd(II), Ni(II), Cu(II), Fe(III), Co(II), Mn(II) Hg(II), and Ag(I) have been synthesized from Schiff base ligand, prepared by the condensation of 3,4-(methylenedioxy)aniline and 5-bromo salicylaldehyde. All the compounds have been characterized by using elemental analysis, molar conductance, FT-IR, UV-Vis, (1)H NMR, (13)C NMR, mass spectra, powder XRD and thermal analysis (TG/DTA) technique. The elemental analysis suggests the stoichiometry to be 1:1 (metal:ligand). The FT-IR, (1)H NMR, (13)C NMR and UV-Vis spectral data suggest that the ligand coordinate to the metal atom by imino nitrogen and phenolic oxygen as bidentate manner. Mass spectral data further support the molecular mass of the compounds and their structure. Powder XRD indicates the crystalline state and morphology of the ligand and its metal complexes. The thermal behaviors of the complexes prove the presence of lattice as well as coordinated water molecules in the complexes. Melting point supports the thermal stability of all the compounds. The in vitro antimicrobial effects of the synthesized compounds were tested against five bacterial and three fungal species by well diffusion method. Antioxidant activities have also been performed for all the compounds. Metal complexes show more biological activity than the Schiff base. Copyright © 2014 Elsevier B.V. All rights reserved.

  1. TEM specimen preparation of semiconductor-PMMA-metal interfaces

    Thangadurai, P.; Lumelsky, Yulia; Silverstein, Michael S.; Kaplan, Wayne D.

    2008-01-01

    Transmission electron microscopy (TEM) cross-section specimens of PMMA in contact with gold and Si were prepared by focused ion beam (FIB) and compared with plan-view PMMA specimens prepared by a dip-coating technique. The specimens were characterized by TEM and electron energy loss spectroscopy (EELS). In the cross-section specimens, the thin films of PMMA were located in a Si-PMMA-Au multilayer. Different thicknesses of PMMA films were spin-coated on the Si substrates. The thickness of the TEM specimens prepared by FIB was estimated using EELS to be 0.65 of the plasmon mean-free-path. Along the PMMA-Au interface, Au particle diffusion into the PMMA was observed, and the size of the Au particles was in the range of 2-4 nm. Dip-coating of PMMA directly on Cu TEM grids resulted in thin specimens with a granular morphology, with a thickness of 0.58 of the plasmon mean-free-path. The dip-coated specimens were free from ion milling induced artifacts, and thus serve as control specimens for comparison with the cross-sectioned specimens prepared by FIB

  2. Preparation and Characterization of a Complex of Paeonol and ...

    thermogravimetric/differential scanning calorimetry (TG/DSC). Results: The phase-solubility results showed that paeonol formed a 1:1 stoichiometric complex with. HP-β-CD while UV and IR spectra suggested that HP-β-CD and paeonol in the complex interacted by a non-covalent bond. SEM and XRD indicate that the heat ...

  3. Structural and thermal characterization of ternary complexes of piroxicam and alanine with transition metals: Uranyl binary and ternary complexes of piroxicam. Spectroscopic characterization and properties of metal complexes

    Mohamed, Gehad G.

    2005-12-01

    Ternary Fe(III), Co(II), Ni(II), Cu(II), Zn(II) and UO 2(II) complexes with piroxicam (Pir) drug (H 2L 1) and dl-alanine (Ala) (HL 2) and also the binary UO 2(II) complex with Pir were studied. The structures of the complexes were elucidated using elemental, IR, molar conductance, magnetic moment, diffused reflectance and thermal analyses. The UO 2(II) binary complex was isolated in 1:2 ratio with the formula [UO 2(H 2L) 2](NO 3) 2. The ternary complexes were isolated in 1:1:1 (M:H 2L 1:L 2) ratios. The solid complexes were isolated in the general formulae [M(H 2L)(L 2)(Cl) n(H 2O) m]· yH 2O (M = Fe(III) ( n = 2, m = 0, y = 1), Co(II) ( n = 1, m = 1, y = 2) and Ni(II) ( n = 1, m = 1, y = 0)); [M(H 2L)(L 2)](X) z· yH 2O (M = Cu(II) (X = AcO, z = 1, y = 0), Zn(II) (X = AcO, z = 1, y = 3) and UO 2(II) (X = NO 3, z = 1, y = 2)). Pir behaves as a neutral bidentate ligand coordinated to the metal ions via the pyridine-N and carbonyl-O groups, while Ala behaves as a uninegatively bidentate ligand coordinated to the metal ions via the deprotonated carboxylate-O and amino-N. The magnetic and reflectance spectral data show that the complexes have octahedral geometry except Cu(II) and Zn(II) complexes have tetrahedral structures. The thermal decomposition of the complexes was discussed in relation to structure, and the thermodynamic parameters of the decomposition stages were evaluated.

  4. Preparation of 147Pm metal and the determination of the melting point and phase transformation temperatures

    Angelini, P.; Adair, H.L.

    1976-07-01

    The promethium metal used in the determination of the melting point and phase transformation temperatures was prepared by reduction of promethium oxide with thorium metal at 1600 0 C and distilling the promethium metal into a quartz dome. The melting point and phase transformation temperatures of promethium metal were found to be 1042 +- 5 0 C and 890 +- 5 0 C, respectively. The ratio for the heat of the high-temperature transformation to the heat of fusion was determined to be 0.415

  5. Neutron diffraction studies of transition metal hydride complexes

    Koetzle, T.F.; Bau, R.

    1976-01-01

    Investigations of H 3 Ta(C 5 H 5 ) 2 (III), HW 2 (CO) 9 (NO) (IV), and HW 2 (CO) 8 (NO) (P(OCH 3 ) 3 ) (V) have been completed. Preliminary results are available for HFeCo 3 (CO) 9 [P(OCH 3 ) 3 ] 3 (VII). This work, together with studies of HMo 2 (C 5 H 5 ) 2 (CO) 4 (P(CH 3 ) 2 ) (VI) and [(C 2 H 5 ) 4 N] + [HCr 2 (CO) 10 ] - carried out at Argonne has led to some general observations on the geometry and the nature of bonding in these compounds. For example, in the structures of IV and V, both of which have bent W--H--W linkages (less than W--H--W in the range 125-130 0 ), there is conclusive evidence for the existence of a closed three-center W--H--W bond with significant metal-metal interaction. Such is the case, because extensions of the axial W--C and W--N bonds trans to the hydride intersect at a point near the center of the W--H--W triangle. The geometry of VI, which also contains a bent M--H--M bond, is consistent with that of IV and V. Bridging M--H bonds in these second- and third-row hydrides range in length from 1.85 to 1.89 A, compared to 1.75 A in the first-row polynuclear complex VII. For metals of corresponding rows, bridging M--H bonds are about 0.1 A longer than terminal bonds, which are classified as single covalent bonds

  6. Energetic Surface Smoothing of Complex Metal-Oxide Thin Films

    Willmott, P.R.; Herger, R.; Schlepuetz, C.M.; Martoccia, D.; Patterson, B.D.

    2006-01-01

    A novel energetic smoothing mechanism in the growth of complex metal-oxide thin films is reported from in situ kinetic studies of pulsed laser deposition of La 1-x Sr x MnO 3 on SrTiO 3 , using x-ray reflectivity. Below 50% monolayer coverage, prompt insertion of energetic impinging species into small-diameter islands causes them to break up to form daughter islands. This smoothing mechanism therefore inhibits the formation of large-diameter 2D islands and the seeding of 3D growth. Above 50% coverage, islands begin to coalesce and their breakup is thereby suppressed. The energy of the incident flux is instead rechanneled into enhanced surface diffusion, which leads to an increase in the effective surface temperature of ΔT≅500 K. These results have important implications on optimal conditions for nanoscale device fabrication using these materials

  7. Electron spin resonance of radicals and metal complexes

    1993-01-01

    The materials are a collection of extended synopsis of papers presented at the conference sessions. The broad area of magnetic techniques applications has been described as well as their spectra interpretation methods. The ESR, NMR, ENDOR and spin echo were applied for studying the radiation and UV induced radicals in chemical and biological systems. Also in the study of complexes of metallic ions (having the paramagnetic properties) and their interaction with the matrix, the magnetic techniques has been commonly used. They are also very convenient tool for the study of reaction kinetics and mechanism as well as interaction of paramagnetic species with themselves and crystal lattice or with the surface as for thee catalytic processes

  8. Friction and solid-solid adhesion on complex metallic alloys

    Dubois, Jean-Marie; Belin-Ferré, Esther

    2014-01-01

    The discovery in 1987 of stable quasicrystals in the Al–Cu–Fe system was soon exploited to patent specific coatings that showed reduced friction in ambient air against hard antagonists. Henceforth, it was possible to develop a number of applications, potential or commercially exploited to date, that will be alluded to in this topical review. A deeper understanding of the characteristics of complex metallic alloys (CMAs) may explain why material made of metals like Al, Cu and Fe offers reduced friction; low solid–solid adhesion came later. It is linked to the surface energy being significantly lower on those materials, in which translational symmetry has become a weak property, that is determined by the depth of the pseudo-gap at the Fermi energy. As a result, friction is anisotropic in CMAs that builds up according to the translation symmetry along one direction, but is aperiodic along the other two directions. A review is given in this article of the most salient data found along these lines during the past two decades or so. PMID:27877675

  9. Radical bonding: structure and stability of bis(phenalenyl) complexes of divalent metals from across the periodic table.

    Craciun, Smaranda; Donald, Kelling J

    2009-07-06

    We examine the bonding possibilities of the bis(phenalenyl) MP(2) sandwich complexes of the divalent metals M = Be, Mg, Ca, Sr, Ba, Zn, Cd, and Hg, at the B3LYP level of theory. The outcome is an extraordinarily diverse class of low symmetry bis(phenalenyl)metal complexes in which bonding preferences and binding enthalpies differ dramatically. The lowest energy group 2 metal MP(2) complexes include an intriguing eta(1),eta(3) BeP(2) structure, and bent eta(6),eta(6) systems for M = Ca, Sr, and Ba. The group 12 bis(phenalenyl) complexes are thermodynamically unstable eta(1),eta(1) slip-sandwich structures. To better understand changes in the structural preferences going from the (eta(6),eta(6)) group 2 to the (eta(1),eta(1)) group 12 complexes, we explored the bonding in the bis(phenalenyl) complexes of transition metals with stable +2 oxidations states between Ca and Zn in period 4. The computed binding enthalpies are large and negative for nearly all of the minimum energy bis(phenalenyl) complexes of the group 2 and the transition metals; they are tiny for MgP(2), and are quite positive for the group 12 systems. The structural preferences and stability of the complexes is a subtle negotiation of several influences: the (un)availability of (n - 1)d and np, orbitals for bonding, the cost of the rehybridization at carbon sites in the phenalenyl rings in preparation for bonding to the metals, and the (P---P) interaction between the phenalenyl radicals.

  10. Technical project of complex fast cycle heat treatment of hydrogenous coal preparation

    Moiseev, V. A.; Andrienko, V. G.; Pileckij, V. G.; Urvancev, A. I.; Gvozdyakov, Dmitry Vasilievich; Gubin, Vladimir Evgenievich; Matveev, Aleksandr Sergeevich; Savostiyanova, Ludmila Viktorovna

    2015-01-01

    Problems of heat-treated milled hydrogenous coal preparation site creation in leading fast cycle heat treatment complex were considered. Conditions for effective use of electrostatic methods of heat-treated milled hydrogenous coal preparation were set. Technical project of heat treatment of milled hydrogenous coal preparation site was developed including coupling of working equipment complex on fast heat treatment and experimental samples of equipment being designed for manufacturing. It was ...

  11. Metal retention in human transferrin: consequences of solvent composition in analytical sample preparation methods.

    Quarles, C Derrick; Randunu, K Manoj; Brumaghim, Julia L; Marcus, R Kenneth

    2011-10-01

    The analysis of metal-binding proteins requires careful sample manipulation to ensure that the metal-protein complex remains in its native state and the metal retention is preserved during sample preparation or analysis. Chemical analysis for the metal content in proteins typically involves some type of liquid chromatography/electrophoresis separation step coupled with an atomic (i.e., inductively coupled plasma-optical emission spectroscopy or -mass spectrometry) or molecular (i.e., electrospray ionization-mass spectrometry) analysis step that requires altered-solvent introduction techniques. UV-VIS absorbance is employed here to monitor the iron content in human holo-transferrin (Tf) under various solvent conditions, changing polarity, pH, ionic strength, and the ionic and hydrophobic environment of the protein. Iron loading percentages (i.e. 100% loading equates to 2 Fe(3+):1 Tf) were quantitatively determined to evaluate the effect of solvent composition on the retention of Fe(3+) in Tf. Maximum retention of Fe(3+) was found in buffered (20 mM Tris) solutions (96 ± 1%). Exposure to organic solvents and deionized H(2)O caused release of ~23-36% of the Fe(3+) from the binding pocket(s) at physiological pH (7.4). Salt concentrations similar to separation conditions used for ion exchange had little to no effect on Fe(3+) retention in holo-Tf. Unsurprisingly, changes in ionic strength caused by additions of guanidine HCl (0-10 M) to holo-Tf resulted in unfolding of the protein and loss of Fe(3+) from Tf; however, denaturing and metal loss was found not to be an instantaneous process for additions of 1-5 M guanidinium to Tf. In contrast, complete denaturing and loss of Fe(3+) was instantaneous with ≥6 M additions of guanidinium, and denaturing and loss of iron from Tf occurred in parallel proportions. Changes to the hydrophobicity of Tf (via addition of 0-14 M urea) had less effect on denaturing and release of Fe(3+) from the Tf binding pocket compared to changes

  12. Effect of the type of metal on the electrical conductivity and thermal properties of metal complexes: The relation between ionic radius of metal complexes and electrical conductivity

    Morgan, Sh. M.; El-Ghamaz, N. A.; Diab, M. A.

    2018-05-01

    Co(II) complexes (1-4) and Ni(II) complexes (5-8) were prepared and characterized by elemental analysis, IR spectra and thermal analysis data. Thermal decomposition of all complexes was discussed using thermogravimetric analysis. The dielectric properties and alternating current conductivity were investigated in the frequency range 0.1-100 kHz and temperature range 300-660 K. The thermal activation energies of electrical conductivity (ΔE1 and ΔE2) values for complexes were calculated and discussed. The values of ΔE1 and ΔE2 for complexes (1-8) were found to decrease with increasing the frequency. Ac electrical conductivity (σac) values increases with increasing temperatures and the values of σac for Co(II) complexes are greater than Ni(II) complexes. Co(II) complexes showed a higher conductivity than other Ni(II) complexes due to the higher crystallinity as confirmed by X-ray diffraction analysis.

  13. A detailed in vitro study of naproxen metal complexes in quest of ...

    Md. Sharif Hasan

    2016-07-01

    Jul 1, 2016 ... possibilities of using Naproxen metal complexes for different therapeutic ..... FTIR spectra, scanning electron microscopy and HPLC study of Naproxen metal ..... aminobenzoic acid and 2-aminophenol and their coordination.

  14. Propellant Preparation Laboratory Complex (Area1-21)

    Federal Laboratory Consortium — Description: Area 1-21 is an explosion resistant complex of nine cells built into the side of a granite ridge. Three solid propellant cutting cells are housed in the...

  15. Hydrothermal preparation and physicochemical studies of new copper nano-complexes for antitumor application

    Saif, M.; El-Shafiy, Hoda F.; Mashaly, Mahmoud M.; Eid, Mohamed F.; Nabeel, A. I.; Fouad, R.

    2018-03-01

    Two novel nano-complexes [(Cu)2(L) (NO3)2(OH2)] (CuH) and [Cu(HL) (OH2)2(NO3)] (CuCTH)were synthesized by hydrothermal method at 200 °C for 48 h in absence and presence of surfactant (CTAB), respectively. Introducing surfactant (CTAB) leads to changing stoichiometric metal/ligand ratio from binuclear (CuH) to mononuclear (CuCTH) nano-complexes. CuH shows irregular nano-flake shape while CuCTH have separately uniform nano-spherical morphology. Thermal analysis revealed that CuCTH is thermally stable in comparison with CuH Nano-complex. CuCTH absorption peak shifted to shorter wavelength (blue shift) and sharpness of the peak also decreased in presence of CTAB. The role of CTAB in the crystal growth is discussed. CuH and CuCTH nano-complexes were tested for their in vitro cytotoxicity against Ehrlich Ascites Carcinoma cell line (E.A.C.). Both nano-complexes effectively inhibited E.A.C. growth with IC50value of 37 and 25 μM for CuH and CuCTH, respectively. The high antitumor activity of CuCTH was attributed to several factors such as spherical morphology, smaller size, chemical structure, and geometry. The LD50 for high cytotoxic CuCTH nano-complex on mice was found to be 100 mg/kg with strong abscess in abdomen side effect. To overcome this side effect, different molar ratio of CuCTH and previously prepared ZnNano-complexes were tested for their in vitrocytotoxicity and in vivo toxicity. Obtained results show that the 2:8 M ratio between CuCTH and Zn nano-complexes gives very low toxicity without any side effects. Also, geometric optimization and conformational analysis were performed using semi-empirical PM3 method. Energy gap (ΔE), dipole moment, and structure activity relationship were performed and discussed.

  16. Precision analysis in billet preparation for micro bulk metal forming

    Mahshid, Rasoul; Hansen, Hans N.

    2015-01-01

    The purpose of this research is to fabricate billets for an automated transfer press for micro forming. High performance transfer presses are wellknown in conventional metal forming and distinguished from their automation and mass production. The press used in this research is a vertical mechanical...... press. When using a vertical mechanical press, the material is fed as billets into the forming zone. Therefore, a large number of highly uniform billets are required to run mass production in such a setup. Shearing technique was used for manufacturing the billets. The efficiency of the shearing tool...

  17. Method for the preparation of metal colloids in inverse micelles and product preferred by the method

    Wilcoxon, Jess P.

    1992-01-01

    A method is provided for preparing catalytic elemental metal colloidal particles (e.g. gold, palladium, silver, rhodium, iridium, nickel, iron, platinum, molybdenum) or colloidal alloy particles (silver/iridium or platinum/gold). A homogeneous inverse micelle solution of a metal salt is first formed in a metal-salt solvent comprised of a surfactant (e.g. a nonionic or cationic surfactant) and an organic solvent. The size and number of inverse micelles is controlled by the proportions of the surfactant and the solvent. Then, the metal salt is reduced (by chemical reduction or by a pulsed or continuous wave UV laser) to colloidal particles of elemental metal. After their formation, the colloidal metal particles can be stabilized by reaction with materials that permanently add surface stabilizing groups to the surface of the colloidal metal particles. The sizes of the colloidal elemental metal particles and their size distribution is determined by the size and number of the inverse micelles. A second salt can be added with further reduction to form the colloidal alloy particles. After the colloidal elemental metal particles are formed, the homogeneous solution distributes to two phases, one phase rich in colloidal elemental metal particles and the other phase rich in surfactant. The colloidal elemental metal particles from one phase can be dried to form a powder useful as a catalyst. Surfactant can be recovered and recycled from the phase rich in surfactant.

  18. Stimulated X-Ray Emission Spectroscopy in Transition Metal Complexes

    Kroll, Thomas; Weninger, Clemens; Alonso-Mori, Roberto; Sokaras, Dimosthenis; Zhu, Diling; Mercadier, Laurent; Majety, Vinay P.; Marinelli, Agostino; Lutman, Alberto; Guetg, Marc W.; Decker, Franz-Josef; Boutet, Sébastien; Aquila, Andy; Koglin, Jason; Koralek, Jake; DePonte, Daniel P.; Kern, Jan; Fuller, Franklin D.; Pastor, Ernest; Fransson, Thomas; Zhang, Yu; Yano, Junko; Yachandra, Vittal K.; Rohringer, Nina; Bergmann, Uwe

    2018-03-01

    We report the observation and analysis of the gain curve of amplified K α x-ray emission from solutions of Mn(II) and Mn(VII) complexes using an x-ray free electron laser to create the 1 s core-hole population inversion. We find spectra at amplification levels extending over 4 orders of magnitude until saturation. We observe bandwidths below the Mn 1 s core-hole lifetime broadening in the onset of the stimulated emission. In the exponential amplification regime the resolution corrected spectral width of ˜1.7 eV FWHM is constant over 3 orders of magnitude, pointing to the buildup of transform limited pulses of ˜1 fs duration. Driving the amplification into saturation leads to broadening and a shift of the line. Importantly, the chemical sensitivity of the stimulated x-ray emission to the Mn oxidation state is preserved at power densities of ˜1020 W /cm2 for the incoming x-ray pulses. Differences in signal sensitivity and spectral information compared to conventional (spontaneous) x-ray emission spectroscopy are discussed. Our findings build a baseline for nonlinear x-ray spectroscopy for a wide range of transition metal complexes in inorganic chemistry, catalysis, and materials science.

  19. Concurrent coordination of ligand in metal chloride complexes with 1-vinyl-2-(2-pyridyl)benzimidazole

    Bajkalov, L.V.; Domnina, E.S.

    1996-01-01

    The properties and structure of bivalent cadmium and 1-vinyl-2-(2-pyridyl)benzimidazole chloride complexes, which have been prepared for the first time, have been studied by the methods of potentiometric titration and PMR, 35 Cl NQR, UV and IR spectroscopy. For the complexes above di- and polymeric structures in crystal phase are suggested, where ligand plays the role of a bridge. N,N-bidentate ligand. In solution the complexes dissociate with formation of monomeric coordination compounds, their metal being bound by different ways, stemming from participation of N benzimidazole or pyridine fragment of the ligand. Adducts of ionic type with second sphere 1-vinyl-2-(2-pyridyl)benzimidazole cation have been obtained in the course of hydrochlorination of the complexes prepared

  20. [COMPUTER ASSISTED DESIGN AND ELECTRON BEAMMELTING RAPID PROTOTYPING METAL THREE-DIMENSIONAL PRINTING TECHNOLOGY FOR PREPARATION OF INDIVIDUALIZED FEMORAL PROSTHESIS].

    Liu, Hongwei; Weng, Yiping; Zhang, Yunkun; Xu, Nanwei; Tong, Jing; Wang, Caimei

    2015-09-01

    To study the feasibility of preparation of the individualized femoral prosthesis through computer assisted design and electron beammelting rapid prototyping (EBM-RP) metal three-dimensional (3D) printing technology. One adult male left femur specimen was used for scanning with 64-slice spiral CT; tomographic image data were imported into Mimics15.0 software to reconstruct femoral 3D model, then the 3D model of individualized femoral prosthesis was designed through UG8.0 software. Finally the 3D model data were imported into EBM-RP metal 3D printer to print the individualized sleeve. According to the 3D model of individualized prosthesis, customized sleeve was successfully prepared through the EBM-RP metal 3D printing technology, assembled with the standard handle component of SR modular femoral prosthesis to make the individualized femoral prosthesis. Customized femoral prosthesis accurately matching with metaphyseal cavity can be designed through the thin slice CT scanning and computer assisted design technology. Titanium alloy personalized prosthesis with complex 3D shape, pore surface, and good matching with metaphyseal cavity can be manufactured by the technology of EBM-RP metal 3D printing, and the technology has convenient, rapid, and accurate advantages.

  1. Metal based biologically active compounds: Design, synthesis, DNA binding and antidiabetic activity of 6-methyl-3-formyl chromone derived hydrazones and their metal (II) complexes.

    Philip, Jessica Elizabeth; Shahid, Muhammad; Prathapachandra Kurup, M R; Velayudhan, Mohanan Puzhavoorparambil

    2017-10-01

    Two chromone hydrazone ligands HL 1 and HL 2 were synthesized and characterized by elemental analyses, IR, 1 H NMR & 13 C NMR, electronic absorption and mass spectra. The reactions of the chromone hydrazones with transition metals such as Ni, Cu, and Zn (II) salts of acetate afforded mononuclear metal complexes. Characterization and structure elucidation of the prepared chromone hydrazone metal (II) complexes were done by elemental, IR, electronic, EPR spectra and thermo gravimetric analyses as well as conductivity and magnetic susceptibility measurements. The spectroscopic data showed that the ligand acts as a mono basic bidentate with coordination sites are azomethine nitrogen and hydrazonic oxygen, and they exhibited distorted geometry. The biological studies involved antidiabetic activity i.e. enzyme inhibition of α-amylase and α-glucosidase, Calf Thymus - DNA (CT-DNA) interaction and molecular docking. Potential capacity of synthesized compounds to inhibit the α-amylase and α-glucosidase activity was assayed whereas DNA interaction studies were carried out with the help UV-Vis absorption titration and viscosity method. The docking studies of chromone hydrazones show that they are minor groove binders. Complexes were found to be good DNA - intercalates. Chromone hydrazones and its transition metal complexes have shown comparable antidiabetic activity with a standard drug acarbose. Copyright © 2017 Elsevier B.V. All rights reserved.

  2. The preparation of primary standard solutions for each of the noble metals

    Mallett, R.C.; Wall, G.J.; Jones, E.A.; Royal, S.J.

    1977-01-01

    A revised method for the preparation of primary standard solutions for each of the noble metals is described. It is now recommended that standard noble-metal solutions should be made from the pure metals and not from salts as previously described. Metals should have a certified purity of 99,95 per cent or better, and the purity should be confirmed by analysis, the techniques of emission spectography or spark-source mass spectrography being used. After the metals have been dissolved, the solutions are made up to volume and the metal content of the standard solutions is checked. For most instrumental techniques for which the standards are intended, the check analysis should be within 0,3 per cent of the certified value

  3. Highly efficient one-step synthesis of carbon encapsulated nanocrystals by the oxidation of metal π-complexes

    Liu, Boyang; Shao, Yingfeng; Xiang, Xin; Zhang, Fuhua; Yan, Shengchang; Li, Wenge

    2017-08-01

    Various carbon encapsulated nanocrystals, including MnS and MnO, Cr2O3, MoO2, Fe7S8 and Fe3O4, and ZrO2, are prepared in one step and in situ by a simple and highly efficient synthesis approach. The nanocrystals have an equiaxed morphology and a median size smaller than 30 nm. Tens and hundreds of these nanocrystals are entirely encapsulated by a wormlike amorphous carbon shell. The formation of a core-shell structure depends on the strongly exothermic reaction of metal π-complexes with ammonium persulfate in an autoclave at below 200 °C. During the oxidation process, the generated significant amounts of heat will destroy the molecular structure of the metal π-complex and cleave the ligands into small carbon fragments, which further transform into an amorphous carbon shell. The central metal atoms are oxidized to metal oxide/sulfide nanocrystals. The formation of a core-shell structure is independent of the numbers of ligands and carbon atoms as well as the metal types, implying that any metal π-complex can serve as a precursor and that various carbon encapsulated nanocrystals can be synthesized by this method.

  4. Coordination kinetics of different metal ions with the amidoximated polyacrylonitrile nanofibrous membranes and catalytic behaviors of their complexes

    Li, Fu; Dong, Yong Chun; Kang, Wei Min; Cheng, Bowen; Qu, Xiang; Cui, Guixin [School of Textiles, Tianjin Polytechnic University, Tianjin (China)

    2016-12-15

    Two transition metal ions (Fe{sup 3+} and Cu{sup 2+}) and a rare earth metal ion (Ce{sup 3+}) were selected to coordinate with amidoximated polyacrylonitrile (PAN) nanofibrous membrane for preparing three metal modified PAN nanofibrous membrane complexes (M-AO-n-PANs, M = Fe, Cu, or Ce) as the heterogeneous Fenton catalysts for the dye degradation in water under visible irradiation. The coordination kinetics of three metal ions with modified PAN nanofibrous membranes was studied and the catalytic properties of the resulting complexes were also compared. The results indicated that increasing metal ion concentrations in solution or higher coordination temperature led to a significant increase in metal content, particularly in Fe and Cu contents of the complexes. Their coordination process could be described using Langmuir isotherm and pseudo-second-order kinetic equations. Moreover, Fe-AO-n-PAN had the best photocatalytic efficiency for the dye degradation in acidic medium, but a lower photocatalytic activity than Cu-AO-n-PAN in alkali medium.

  5. Preparation of Glucose Sensor Using Polydimethylsiloxane / Polypyrrole Complex

    Yasuzawa, Mikito; Inoue, Shigeru; Imai, Shinji

    New glucose oxidase (GOD) immobilized glucose sensors were prepared by the electropolymerization of 1-(6-D-gluconamidohexyl) pyrrole (GHP) on the platinum wire electrode precoated with the mixture solution of pyrrole derivative GHP, polydimethylsiloxane (PDS) and Nafion. The addition of Nafion into the precoating mixture solution was essential to obtain suitable sensor sensitivity. However, the sensitivity was about the half of that of the electrode without PDS precoating. Although, the introduction of Nafion was effective to improve the long-term stability of the enzyme-immobilized electrode, the electrode prepared using Nafion, PDS and GHP performed excellent long-term stability even at the measurement and storage temperatures of 40°C. Relatively constant response current was obtained over 30 days under the condition of 40°C and over 9 months measured at 25°C. Moreover, the GOD-immobilized GHP polymer film prepared on the electrode precoated with GHP, PDS and Nafion solution, was found to have excellent hemocompatibility from the result of platelet rich plasma contacting test.

  6. Metal–Organic Frameworks Stabilize Mono(phosphine)–Metal Complexes for Broad-Scope Catalytic Reactions

    Sawano, Takahiro; Lin, Zekai; Boures, Dean; An, Bing; Wang, Cheng; Lin, Wenbin (UC); (Xiamen)

    2016-08-10

    Mono(phosphine)–M (M–PR3; M = Rh and Ir) complexes selectively prepared by postsynthetic metalation of a porous triarylphosphine-based metal–organic framework (MOF) exhibited excellent activity in the hydrosilylation of ketones and alkenes, the hydrogenation of alkenes, and the C–H borylation of arenes. The recyclable and reusable MOF catalysts significantly outperformed their homogeneous counterparts, presumably via stabilizing M–PR3 intermediates by preventing deleterious disproportionation reactions/ligand exchanges in the catalytic cycles.

  7. Interaction of Cr (III), Ni (II), Pb (II) with DTPA complexes of essential metal ions

    Gulzar, S.; Zahida; Maqsood, T.; Naqvi, R.R.

    2002-01-01

    With the increase of anthropogenic activities in the environment, heavy metal toxicity (Chromium, Nickel and Lead) is more common now. DTPA (diethylene triamine pentaacetic acid) a polyamino carboxylic acid is widely used to form hydrophilic and stable complexes with most of the metal ions. In this spectrophotometric study, concentration of Cr(III), Ni(II) and Pb(II) (toxic metal ions) exchanged with Fe(III), Zn(II) and Ca(II) from their DTPA complexes were estimated at pH 4,7 and 9. Concentration of added metal was varied from 1-4 times to that of complexed metal. (author)

  8. Complex Nanostructures from Materials based on Metal-Organic Frameworks for Electrochemical Energy Storage and Conversion.

    Guan, Bu Yuan; Yu, Xin Yao; Wu, Hao Bin; Lou, Xiong Wen David

    2017-12-01

    Metal-organic frameworks (MOFs) have drawn tremendous attention because of their abundant diversity in structure and composition. Recently, there has been growing research interest in deriving advanced nanomaterials with complex architectures and tailored chemical compositions from MOF-based precursors for electrochemical energy storage and conversion. Here, a comprehensive overview of the synthesis and energy-related applications of complex nanostructures derived from MOF-based precursors is provided. After a brief summary of synthetic methods of MOF-based templates and their conversion to desirable nanostructures, delicate designs and preparation of complex architectures from MOFs or their composites are described in detail, including porous structures, single-shelled hollow structures, and multishelled hollow structures, as well as other unusual complex structures. Afterward, their applications are discussed as electrode materials or catalysts for lithium-ion batteries, hybrid supercapacitors, water-splitting devices, and fuel cells. Lastly, the research challenges and possible development directions of complex nanostructures derived from MOF-based-templates for electrochemical energy storage and conversion applications are outlined. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Preparation of metallic nanoparticles by irradiation in starch aqueous solution

    Nemţanu, Monica R., E-mail: monica.nemtanu@inflpr.ro; Braşoveanu, Mirela, E-mail: monica.nemtanu@inflpr.ro; Iacob, Nicuşor, E-mail: monica.nemtanu@inflpr.ro [National Institute for Lasers, Plasma and Radiation Physics, Electron Accelerators Laboratory, 409 Atomiştilor St., PO Box MG-36, 077125, Bucharest-Măgurele (Romania)

    2014-11-24

    Colloidal silver nanoparticles (AgNPs) were synthesized in a single step by electron beam irradiation reduction of silver ions in aqueous solution containing starch. The nanoparticles were characterized by spectrophotocolorimetry and compared with those obtained by chemical (thermal) reduction method. The results showed that the smaller sizes of AgNPs were prepared with higher yields as the irradiation dose increased. The broadening of particle size distribution occurred by increasing of irradiation dose and dose rate. Chromatic parameters such as b* (yellow-blue coordinate), C* (chroma) and ΔE{sub ab} (total color difference) could characterize the nanoparticles with respect of their concentration. Hue angle h{sup o} was correlated to the particle size distribution. Experimental data of the irradiated samples were also subjected to factor analysis using principal component extraction and varimax rotation in order to reveal the relation between dependent variables and independent variables and to reduce their number. The radiation-based method provided silver nanoparticles with higher concentration and narrower size distribution than those produced by chemical reduction method. Therefore, the electron beam irradiation is effective for preparation of silver nanoparticles using starch aqueous solution as dispersion medium.

  10. Preparation of transition metal sulfide nanoparticles via hydrothermal route

    Fei-Ling, P.; Chin-Hua, C.; Sarani Zakaria; Tze-Khong, L.; Mohd Ambar Yarmo; Nay-Ming, H.

    2010-01-01

    Nano sized copper sulfide, iron sulfide and molybdenum sulfide were successfully synthesised via a simple hydrothermal method. Sodium thiosulfate pentahydrate (Na 2 S 2 O 3 ·5H 2 O) and hydroxylamine sulfate ((H 3 NO) 2 ·H 2 SO 4 ) were used as the starting materials and reacted with the transition metal source at 200 degree Celsius for 90 min. The products were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDX) and Fourier transform infrared spectroscopy (FTIR). Spherical shape CuS and FeS 2 nanoparticles with high crystallinity were successfully produced. The transmission electron micrographs revealed the well-dispersibility of the produced nanoparticles. Scanning electron micrograph showed the MoS 2 nanoparticles possessed a spherical shape with sheet-like structure covering on the outer surface of the particles. (author)

  11. Direct synthesis of metal complexes starting from zero-valent metals

    Gojon-Zorrilla, Gabriel; Kharisov, Boris I. [Universidad Autonoma de Nuevo Leon, Monterrey, Nuevo Leon (Mexico); Garnovskii, Alexander D. [Institute of Physical and Organic Chemistry (Russian Federation)

    1996-06-01

    The recent (1980-1994) literature on metal-vapor synthesis of coordination and organometallic compounds is reviewed. An account is given of the high-and low-temperature reactions between free metal atoms and a large variety of substrates, mainly alkenes, alkynes, dienes, arenes, funtionalized arenes, alkyl halides {beta}-diketones and simple inorganic molecules. The main experimental methods are described, as well as the results obtained thereby. It is shown that in many instances these methods present significant advantages over conventional synthetic procedures, offering unique access to some metal complexes. [Spanish] Se reviso la literatura reciente (1980-1994) sobre la sintesis de compuestos de coordinacion y compuestos organometalicos a partir de vapores metalicos. Se examinan las reacciones de los atomos metalicos libres con una gran variedad de substratos, principalmente alquenos, alquinos, dienos, hidrocarburos aromaticos y sus derivados, haluros de alquilo y arilo, {beta}-dicetonas y moleculas inorganicas simples. Se presentan los principales metodos experimentales, asi como los resultados obtenidos; se concluye que la crisintesis presenta en muchos casos ventajas significativas sobre los procedimientos sinteticos tradicionales, constituyendo frecuentemente la unica opcion disponible.

  12. Preparation, characterization, and kinetics of thermolysis of nickel and copper nitrate complexes with 2,2 Prime -bipyridine ligand

    Kumar, Dinesh; Kapoor, I.P.S. [Department of Chemistry, DDU Gorakhpur University, Gorakhpur 273 009 (India); Singh, Gurdip, E-mail: gsingh4us@yahoo.com [Department of Chemistry, DDU Gorakhpur University, Gorakhpur 273 009 (India); Froehlich, Roland [Institut fuer Organische Chemie, Universitaet Muenster, D-48149 Muenster (Germany)

    2012-10-10

    Graphical abstract: Nickel and copper nitrate complexes with 2,2 Prime -bipyridine, nitrate and water ligands have been prepared and characterized by single crystal X-ray diffraction, FT-IR and CHN analyses. Thermolysis was performed by using TG, DTA and ignition delay measurements. The kinetics of thermolysis were also evaluated. Highlights: Black-Right-Pointing-Pointer Preparation and characterization of Ni and Cu nitrate complexes have been reported. Black-Right-Pointing-Pointer Thermolysis has been carried out using TG-DTA and ignition delay measurements. Black-Right-Pointing-Pointer Their thermal decomposition pathways have been proposed. Black-Right-Pointing-Pointer Oxides residues as end product of thermolysis were revealed by XRD patterns. Black-Right-Pointing-Pointer Kinetics of their isothermal decomposition was evaluated. - Abstract: Nickel and copper nitrate complexes with 2,2 Prime -bipyridine (bipy) as a N donor and nitrate and water as oxygen donor ligands of the general formula [M(NO{sub 3})(C{sub 10}H{sub 8}N{sub 2})(H{sub 2}O){sub 3}](NO{sub 3}), where M = Ni and Cu, have been obtained from the corresponding metal nitrate salts. These complexes were characterized by X-ray crystallography, FT-IR, and CHN analysis. Both the complexes have been found to be six coordinated. Their thermal decomposition behaviour was investigated by TG, DTA, and ignition delay measurements. TG-DTA examinations of these complexes revealed multistep thermal decomposition. The corresponding metal oxide residues obtained after thermolysis were identified from their X-ray diffraction patterns (XRD). Kinetics of isothermal decomposition of the complexes was established from both the model-fitting as well as isoconversional methods.

  13. Metal nanoparticles (other than gold or silver) prepared using plant extracts for medical applications

    Pasca, Roxana-Diana; Santa, Szabolcs; Racz, Levente Zsolt; Racz, Csaba Pal

    2016-12-01

    There are many modalities to prepare metal nanoparticles, but the reducing of the metal ions with plant extracts is one of the most promising because it is considerate less toxic for the environment, suitable for the use of those nanoparticles in vivo and not very expensive. Various metal ions have been already studied such as: cobalt, copper, iron, platinum, palladium, zinc, indium, manganese and mercury and the number of plant extracts used is continuously increasing. The prepared systems were characterized afterwards with a great number of methods of investigation: both spectroscopic (especially UV-Vis spectroscopy) and microscopic (in principal, electron microscopy-TEM) methods. The applications of the metal nanoparticles obtained are diverse and not completely known, but the medical applications of such nanoparticles occupy a central place, due to their nontoxic components, but some diverse industrial applications do not have to be forgotten.

  14. Preparation of thin actinide metal disks using a multiple disk casting technique

    Conner, W.V.

    1975-01-01

    A casting technique has been developed for preparing multiple actinide metal disks which have a minimum thickness of 0.006 inch. This technique was based on an injection casting procedure which utilizes the weight of a tantalum metal rod to force the molten metal into the mold cavity. Using the proper mold design and casting parameters, it has been possible to prepare ten 1/2 inch diameter neptunium or plutonium metal disks in a single casting, This casting technique is capable of producing disks which are very uniform. The average thickness of the disks from a typical casting will vary no more than 0.001 inch and the variation in the thickness of the individual disks will range from 0.0001 to 0.0005 inch. (Auth.)

  15. Preparation of thin actinide metal disks using a multiple disk casting technique

    Conner, W.V.

    1976-01-01

    A casting technique has been developed for preparing multiple actinide metal disks which have a minimum thickness of 0.006 inch. This technique was based on an injection casting procedure which utilizes the weight of a tantalum metal rod to force the molten metal into the mold cavity. Using the proper mold design and casting parameters, it has been possible to prepare ten 1/2 inch diameter neptunium or plutonium metal disks in a single casting. This casting technique is capable of producing disks which are very uniform. The average thickness of the disks from a typical casting will vary no more than 0.001 inch and the variation in the thickness of the individual disks will range from 0.0001 to 0.0005 inch. (author)

  16. Factors influencing Complexity in Financial Report preparation - Evidence from the Banking Sector in Kenya

    A.Mutiso

    2013-06-01

    Full Text Available The current developments in the business environment as well as in the accountancy profession have significantly affected the way the financial reports are prepared. This study sought to assess the factors influencing complexity of preparing financial reports in the banking sector in Kenya. The objectives included assessing whether disclosures, adoption of International financial Reporting Standard, regulations and lack of competence by the preparers have contributed to the complexity of preparing financial statements. Using a descriptive study design, data was collected from ten banks registered in the Nairobi Capital Market. The study found out that the identified variables positively contributed to complications in the preparation of financial reports. Management interference, lack of guidance on interpretations and frequent updates of the standards were identified as the main challenges in preparing financial reports. Several recommendations were given to help simplify the process of preparing financial statements.

  17. Preparation of metal adsorbents from chitin/chitosan by radiation technology

    Nguyen Van Suc; Nguyen Quoc Hien; Ngo Quang Huy; Thai My Phe; Dao Van Hoang; Nguyen Van Hung

    2004-01-01

    The methods of preparation of metal adsorbents basing on chitin/chitosan were developed. That include the adsorbent from chitin grafted with acrylic acid by different irradiation doses; the clinging chitosan gel beads; the coagulable solution and the chitosan composite filter. The process of metal adsorption for each adsorbent was studied as adsorption kinetic, isothermal adsorption. The results have been applied for removal of some elements as Hg, Pb, Cd, U, Cu, ect. in the wastewater. (NHA)

  18. Preparation and adsorption properties of nano magnetite chitosan films for heavy metal ions from aqueous solution

    Lasheen, M.R., E-mail: ragaei24@link.net [Water Pollution Research Department, Environmental Research Division, National Research Centre, 33-El Buhoth St., Dokki, Cairo, 12311 (Egypt); El-Sherif, Iman Y., E-mail: iman57us@yahoo.com [Water Pollution Research Department, Environmental Research Division, National Research Centre, 33-El Buhoth St., Dokki, Cairo, 12311 (Egypt); Tawfik, Magda E., E-mail: magdaemileta@yahoo.com [Polymers and Pigments Department, National Research Centre, 33-El Buhoth St., Dokki, Cairo, 12311 (Egypt); El-Wakeel, S.T., E-mail: shaimaa_tw@yahoo.com [Water Pollution Research Department, Environmental Research Division, National Research Centre, 33-El Buhoth St., Dokki, Cairo, 12311 (Egypt); El-Shahat, M.F., E-mail: elshahatmf@hotmail.com [Faculty of Science, Ain Shams University, Khalifa El-Maamon St., Abbasiya Sq., 11566, Cairo (Egypt)

    2016-08-15

    Highlights: • Nano magnetite–chitosan films were prepared by casting method. • The efficiency of the prepared films for removing heavy metals was investigated. • The adsorption mechanism was studied using different isotherm and kinetic models. • Films reuse and metals recovery were studied. - Abstract: Nano magnetite chitosan (NMag–CS) film was prepared and characterized with different analytical methods. X-ray diffraction (XRD) patterns confirmed the formation of a pure magnetite structure and NMag–CS nanocomposite. TEM image of the film, revealed the uniform dispersion of magnetite nanoparticles inside chitosan matrix. The adsorption properties of the prepared film for copper, lead, cadmium, chromium and nickel metal ions were evaluated. Different factors affecting the uptake behavior by the composite films such as time, initial pH and film dose were investigated. The adsorption equilibrium attained using 2 g/L of the film after 120 min of reaction. The equilibrium data were analyzed using Langmuir and Freundlich models. The adsorption kinetics followed the mechanism of the pseudo-second-order equation for all metals. The metals regenerated from films with an efficiency greater than 95% using 0.1 M ethylene diamine tetra acetic acid (EDTA) and films were successfully reused for adsorption.

  19. Method for preparation of melts of alkali metal chlorides with highly volatile polyvalent metal chlorides

    Salyulev, A.B.; Kudyakov, V.Ya.

    1990-01-01

    A method for production of alkali metal (Cs, Rb, K) chloride melts with highly volatile polyvalent metal chlorides is suggested. The method consists, in saturation of alkali metal chlorides, preheated to the melting point, by volatile component vapours (titanium tetrachloride, molybdenum or tantalum pentachloride) in proportion, corresponding to the composition reguired. The saturation is realized in an evacuated vessel with two heating areas for 1-1.5 h. After gradual levelling of temperature in both areas the product is rapidly cooled. 1 fig.; 1 tab

  20. Contributions to the preparation of 241americium metal and a few 241americium silicides

    Wittmann, F.D.

    1980-01-01

    In order to take a closer look at the americium-silicon system, three further silicides of americium: Am 5 Si 3 , Am 2 Si 3 and AmSi 2 were prepared in addition to the already known americium monosilicide and starting from the knowledge gained from the latters preparation. Radiographic investigations were carried out into the temperature region of 900 0 C. They showed no change of structure in the three compounds. It was possible to prepare residue-free americium metal by reducing AmF 3 with Si, whereby the SiF 4 formed can be easily separated off as volatile compound, and the Am metal is brought into a very pure form by sublimation suitable for spectrochemical investigations. Attempts to prepare binary germanides and gallides of 241 americium were unsuccessful. (RB) [de

  1. Preparation and characterization of metallic supported thin Pd-Ag membranes for hydrogen separation

    Fernandez, Ekain; Medrano, Jose Antonio; Melendez, Jon; Parco, Maria; Viviente, J.L.; van Sint Annaland, Martin; Gallucci, Fausto; Pacheco Tanaka, David A.

    2015-01-01

    This paper reports the preparation and characterization of thin-film (4-5 µm thick) Pd-Ag metallic supported membranes for high temperature applications. Various thin film membranes have been prepared by depositing a ceramic interdiffusion barrier layer prior to the simultaneous Pd-Ag electroless plating deposition. Two deposition techniques for ceramic layers (made of zirconia and alumina) have been evaluated: atmospheric plasma spraying and dip coating of a powder suspension. Initially, the...

  2. Synthesis, characterization and anti-bacterial activity of divalent transition metal complexes of hydrazine and trimesic acid

    K. Kumar

    2018-01-01

    Full Text Available Transition metal complexes of trimesic acid and hydrazine mixed-ligands with a general formula M(Htma(N2H42, where, M = Mn, Co, Ni, Cu and Zn; H3tma = trimesic acid, have been prepared and characterized by elemental, structural, spectral and thermal analyses. For the complexes, the carboxylate νasym and νsym stretchings are observed at about 1626 and 1367 cm−1 respectively, with Δν between them of ∼260 cm−1, showing the unidentate coordination of each carboxylate group. The hydrazine moieties are present as bridging bidentates. Electronic and EPR spectral studies suggest an octahedral geometry for the complexes. All these complexes show three steps of decomposition in TGA/DTA. SEM images of CuO and MnO residues obtained from the complexes show nano-sized clusters suggesting that the complexes may be used as precursors for nano-CuO and nano-MnO preparation. The antimicrobial activities of the prepared complexes, against four bacteria have been evaluated.

  3. Sustainable preparation of supported metal nanoparticles and their applications in catalysis.

    Campelo, Juan M; Luna, Diego; Luque, Rafael; Marinas, José M; Romero, Antonio A

    2009-01-01

    Metal nanoparticles have attracted much attention over the last decade owing to their unique properties as compared to their bulk metal equivalents, including a large surface-to-volume ratio and tunable shapes. To control the properties of nanoparticles with particular respect to shape, size and dispersity is imperative, as these will determine the activity in the desired application. Supported metal nanoparticles are widely employed in catalysis. Recent advances in controlling the shape and size of nanoparticles have opened the possibility to optimise the particle geometry for enhanced catalytic activity, providing the optimum size and surface properties for specific applications. This Review describes the state of the art with respect to the preparation and use of supported metal nanoparticles in catalysis. The main groups of such nanoparticles (noble and transition metal nanoparticles) are highlighted and future prospects are discussed.

  4. Photoluminescent properties of complex metal oxide nanopowders for gas sensing

    Bovhyra, R. V.; Mudry, S. I.; Popovych, D. I.; Savka, S. S.; Serednytski, A. S.; Venhryn, Yu. I.

    2018-03-01

    This work carried out research on the features of photoluminescence of the mixed and complex metal oxide nanopowders (ZnO/TiO2, ZnO/SnO2, Zn2SiO4) in vacuum and gaseous ambient. The nanopowders were obtained using pulsed laser reactive technology. The synthesized nanoparticles were characterized by X-ray diffractometry, energy-dispersive X-ray analysis, and scanning and transmission electron microscopy analysis for their sizes, shapes and collocation. The influence of gas environment on the photoluminescence intensity was investigated. A change of ambient gas composition leads to a rather significant change in the intensity of the photoluminescence spectrum and its deformation. The most significant changes in the photoluminescent spectrum were observed for mixed ZnO/TiO2 nanopowders. This obviously is the result of a redistribution of existing centers of luminescence and the appearance of new adsorption centers of luminescence on the surface of nanopowders. The investigated nanopowders can be effectively used as sensing materials for the construction of the multi-component photoluminescent sensing matrix.

  5. Principles of big data preparing, sharing, and analyzing complex information

    Berman, Jules J

    2013-01-01

    Principles of Big Data helps readers avoid the common mistakes that endanger all Big Data projects. By stressing simple, fundamental concepts, this book teaches readers how to organize large volumes of complex data, and how to achieve data permanence when the content of the data is constantly changing. General methods for data verification and validation, as specifically applied to Big Data resources, are stressed throughout the book. The book demonstrates how adept analysts can find relationships among data objects held in disparate Big Data resources, when the data objects are endo

  6. Metal ion-improved complexation countercurrent chromatography for enantioseparation of dihydroflavone enantiomers.

    Han, Chao; Wang, Wenli; Xue, Guimin; Xu, Dingqiao; Zhu, Tianyu; Wang, Shanshan; Cai, Pei; Luo, Jianguang; Kong, Lingyi

    2018-01-12

    Cu(II) ion was selected as an additive to improve the enantioseparation efficiency of three dihydroflavone enantiomers in high-speed counter-current chromatography (HSCCC), using hydroxypropyl-β-cyclodextrin (HP-β-CyD) as the chiral selector. The influences of important parameters, including the metal ion, the concentrations of HP-β-CyD and the Cu(II) ion, and the sample size were investigated. Under optimal conditions, three dihydroflavone enantiomers, including (±)-hesperetin, (±)-naringenin, and (±)-farrerol, were successfully enantioseparated. The chiral recognition mechanism was investigated. The enantioseparation was attributed to the different thermodynamic stabilities of the binary complexes of HP-β-CyD and (±)-hesperetin, and Cu(II) ion could enhance this difference by forming ternary complexes with the binary complexes. This Cu(II) ion-improved complexation HSCCC system exhibited improved performance for chiral separation, and therefore it has great application potential in the preparative enantioseparation of other compounds with similar skeletons. Copyright © 2017 Elsevier B.V. All rights reserved.

  7. Metal doped fluorocarbon polymer films prepared by plasma polymerization using an RF planar magnetron target

    Biederman, H.; Holland, L. (Sussex Univ., Brighton (UK). Lab. for Plasma Materials Processing)

    1983-07-01

    Fluorocarbon films have been prepared by plasma polymerization of CF/sub 4/ using an RF planar magnetron with an aluminium target. More than one order of magnitude higher deposition rate has been achieved in comparison with an R.F. diode system operated under similar conditions of monomer pressure and flow rate and power input. A glow discharge in a CF/sub 4/(25%)-argon(75%) mixture was used to incorporate aluminium from a target electrode into the polymer films. The foregoing mixture and another based on CF/sub 4/(87%)-argon(13%) were used in the RF discharge with a copper target. Some experiments with a gold target and pure CF/sub 4/ as the inlet gas were also made. The film structure was examined by SEM and TEM and characteristic micrographs are presented here. The composition of the films was estimated from an EAS study. The sheet resistivity of the metal/polymer film complexes was determined.

  8. 'Pincer' dicarbene complexes of some early transition metals and uranium.

    Pugh, David; Wright, Joseph A; Freeman, Sandra; Danopoulos, Andreas A

    2006-02-14

    The complexes [(C-N-C)MX(n)(thf)(m)] with the 'pincer' 2,6-bis(imidazolylidene)pyridine, (C-N-C) = 2,6-bis(arylimidazol-2-ylidene)pyridine, aryl = 2,6-Pr(i)2C6H3, M = V, X = Cl, n = 2, m = 1 1a; M = Cr, X = Cl, n = 2, m = 0, 2a, X = Br, 2b; M = Mn, X = Br, n = 2, m = 0, 3; M = Nb, X = Cl, n = 3, m = 0, 4; and M = U, X = Cl, n = 4, m = 0, 5, were synthesised by (a) substitution of labile tmed (1a), thf (2a, 3, 5) or dme (4) by free (C-N-C) or by (b) reaction of the bisimidazolium salt (CH-N-CH)Br2 with {Cr[N(SiMe3)2]2(thf)2} followed by amine elimination (2b). Attempted alkylation of 1a, 2, 3a and 4 with Grignard or alkyl lithiums gave intractable mixtures, and in one case [reaction of 1a with (mesityl)MgBr] resulted in exchange of Cl by Br (1b). Oxidation of 1a or [(C-N-C)VCl3] with 4-methylmorpholine N-oxide afforded the trans-V(C-N-C)(=O)Cl2, 6, which by reaction with AgBF4 in MeCN gave trans-[V(C-N-C)(=O)(MeCN)2][BF4]2, 7. Reaction of 1a with p-tolyl azide gave trans-V(C-N-C)(=N-p-tolyl)Cl2 8. The complex trans-Ti(C-N-C)(=NBu(t))Cl2, 9, was prepared by substitution of the pyridine ligands in Ti(NBu(t))Cl2(py)3 by C-N-C.

  9. Preparation, characterization and in vitro dissolution study of Nitrazepam: Cyclodextrin inclusion complex

    J S Patel

    2012-01-01

    Full Text Available The objectives of this research were to prepare and characterize inclusion complexes of Nitrazepam with Hydroxypropyl-β-cyclodextrin (HPβCD and Sulfobutyl ether β-cyclodextrin (SBEβCD to study the effect of complexation on the dissolution rate of Nitrazepam, a water-insoluble drug. The phase solubility profile of Nitrazepam with Hydroxypropyl- β-cyclodextrin and Sulfobutyl ether β-cyclodextrin was an AP-type, indicating the formation of 2:1 stoichiometric inclusion complexes. Gibbs free energy values were all negative, indicating the spontaneous nature Nitrazepam solubilization and their value decreased with increase in the cyclodextrin concentration, demonstrating that the reaction conditions became more favorable as the concentration of cyclodextrins increased. Complexes of Nitrazepam were prepared with cyclodextrin using various methods such as physical mixing, kneading, spray-drying and lyophilization. The complexes were characterized by Differential scanning calorimetry, Fourier-transform infrared, scanning electron microscopy and powder X-ray diffraction studies. These studies indicated that a complex prepared by lyophilization had successful inclusion of the Nitrazepam molecule into the cyclodextrin cavity. Complexation resulted in a marked improvement in the solubility and wettability of Nitrazepam. Among all the samples, a complex prepared with Sulfobutyl ether β-cyclodextrin by lyophilization had the greatest improvement in the in vitro rate of Nitrazepam dissolution. The mean dissolution time for Nitrazepam decreased significantly after preparing complexes. The similarity factor indicated a significant difference between the release profiles of Nitrazepam from complexes, physical mixtures and plain Nitrazepam. To conclude that, the tablets containing complexes prepared with Cyclodextrins had significant improvement in the release profile of Nitrazepam as compared to tablets containing Nitrazepam without cyclodextrin.

  10. Preparation and characterization of some pyridine-2,6-dicarboxylato thorium(IV) complexes

    Degetto, S; Baracco, L [Consiglio Nazionale delle Ricerche, Padua (Italy). Lab. di Chimica e Tecnologia dei Radioelementi; Graziani, R [Padua Univ. (Italy). Istituto di Chimica Generale ed Inorganica; Celon, E [Padua Univ. (Italy). Istituto di Chimica Organica

    1978-12-01

    The preparation of complexes of pyridine-2,6-dicarboxylic acid (H/sub 2/PDC) with thorium(IV) is reported and discussed. The reactivity of Th(PDC)/sub 2/(H/sub 2/O)/sub 4/ was tested by preparing adducts with some neutral ligands. The complexes were characterized by i.r. spectroscopy, elemental analysis and thermal behaviour. Preliminary information on the structure obtained by x-ray analysis is also reported.

  11. FT-IR Spectroscopic study on the 4-(3-Cyclohexen-1-yl)pyridine metal (II) tetracyanonickelate complex

    Parlak, C.

    2005-01-01

    New Hofmann type complex in the form of M(4-Chpy) 2 Ni(CN) 4 (where 4-Chpy=4-(3- Cyclohexen-1-yl)pyridine and M = Ni) was prepared in powder form and its infrared spectra is reported in the range of 4000-400 cm - 1. The spectral findings suggest that this compound is similar in structure to the Hofmann type complexes and its structure consists of polymeric layers | M-Ni(CN) 4 |∞ with the 4-(3-Cyclohexen-1-yl)pyridine molecule bound to the metal atom (M)

  12. Preparation of high purity metallic protactinium. Crystal structure and dissolution enthalpy of the metal

    Bohet, J.

    1977-01-01

    Some 300 mg of Pa have been produced in a high purity metallic state. Protactinium monocarbide has been obtained by the carboreduction of Pa 2 O 5 . Protactinium iodide, produced by the direct reaction of iodine on the carbide, has been sublimated at 420 0 C and thermally dissociated at 1200 0 C on a W wire. In these conditions Pa metal has been deposited with a yield greater than 85% and presents a bct structure stable at room temperature (a=3.921+-0.001A and c=3.235+-0.001A). The fcc phase (Fm3m type) (a=5.018+-0.001A) has been obtained by quenching metallic samples (bct) heated in argon at 1500 0 C. The chemical analysis and the transformation of the fcc into bct phase by controlled heat treatments show the presence of this high temperature phase in the metal. Protactinium mononitride (5.58% N) produced by direct reaction of N on Pa at 1100 0 C presents the same fcc crystal structure but the lattice parameter is higher (a=5.047+-0.001A). The dissolution heat of metallic Pa (bct) has been determined in the aqueous solution HCl 12M - HF 0.05M at 298.15+-0.05 K. The standard formation enthalpies of the ionic species Pa(IV) and Pa(V) are respectively equal to -672+-15 kJ.mol -1 and -821+-15 kJ.mol -1

  13. Complexity of food preparation and food security status in low-income young women.

    Engler-Stringer, Rachel; Stringer, Bernadette; Haines, Ted

    2011-01-01

    This study was conducted to explore whether preparing more complex meals was associated with higher food security status. This mixed-methods, community-based study involved the use of semistructured interviews to examine the cooking practices of a group of young, low-income women in Montreal. Fifty participants aged 18 to 35 were recruited at 10 locations in five low-income neighbourhoods. Food security status was the main outcome measure and the main exposure variable, "complex food preparation," combined the preparation of three specific food types (soups, sauces, and baked goods) using basic ingredients. Low-income women preparing a variety of meals using basic ingredients at least three times a week were more than twice as likely to be food secure as were women preparing more complex meals less frequently. Women who prepared more complex meals more frequently had higher food security. Whether this means that preparing more complex foods results in greater food security remains unclear, as this was an exploratory study.

  14. Catalytic polarographic currents of platinum metal complexes and their application to determination of trace concentrations of the elements

    Ezerskaya, N.A.; Kiseleva, I.N.

    1984-01-01

    Several types of catalytic electrode processes with the participation of platinum metal complexes and used for the determination of the element microconcentrations have been considered in the review. It is pointed out that to measure catalytic currents of hydrogen solutions nitroso compounds, which are prepared by heating chloride complexes of Ru(3) and (4) with NaNO 2 are used. The method is applicable for ruthenium determination in commercial nitric acid solutions. Ru determination in solution of ruthenium (4) dimeric chloride complex on graphite electrode, using catalytic currents of hydrogen, surpasses in sensitivity the determination of the element, using the method of inversion voltammetry. Certain other complexes of Ru and determination methods of ruthenium in them are considered. Hydrogen catalytic currents in the complexes solutions with organic ligands are the most perspective for analysis

  15. Hydrogen storage in metal hydrides and complex hydrides; Wasserstoffspeicherung in Metall- und komplexen Hydriden - Schlussbericht

    Bielmann, M.; Zuettel, A.

    2007-07-01

    This final report for the Swiss Federal Office of Energy (SFOE), reports on work done in 2007 at the Swiss Federal Laboratories for Materials Science and Technology EMPA on the storage of hydrogen in metal hydrides and complex hydrides. In particular, the use of tetrahydroborates is noted. The potential of this class of materials is stressed. The structures at room-temperature were examined using neutron and X-ray diffraction methods. Thermodynamic methods helped determine the thermodynamic stability of the materials. Also, a complete energy diagram for the materials was developed. The use of silicon oxide to reduce activation energy and its catalytic effects are discussed. The challenges placed by desorption mechanisms are noted. The authors note that reversibility is basically proven.

  16. Sliding wear resistance of metal matrix composite layers prepared by high power laser

    Ocelik, Vaclav; Matthews, D; de Hosson, Jeff

    2005-01-01

    Two laser surface engineering techniques, Laser Cladding and Laser Melt Injection (LMI), were used to prepare three different metal matrix composite layers with a thickness of about 1 mm and approximately 25-30% volume fraction of ceramic particles. SiC/Al-8Si, WC/Ti-6Al-4V and TiB2/Ti-6Al-4V layers

  17. Wood metal. A material of interest for the preparation of individual collimators and radiation protective means

    Schumann, E.; Keiner, P.; Klose, E.

    1978-01-01

    On the grounds of its physical properties Wood metal is suitable for the preparation of individual collimators, shields and other radiation protective means in clinical radiology. Advantages and disadvantages of these self-made protective means are discussed. Its use for constructing special shielding elements and filters applied in radiotherapy as well as for shielding syringes applied in nuclear medicine is demonstrated. (author)

  18. On the possibility of removing of transition metal ions from sewage using polymeric complexes

    Tazhibaeva, S.M.; Abilov, Zh.A.; Musabekov, K.V.

    1997-01-01

    The possibility of using of complexation in the system polyethylene-imine transition metal ions (Cu 2+ , Ni 2+ , Co 2+ )-surface active substance for removing of metal ions from solution and sewage has been investigated. It is shown, that pH of medium, hydro-fugitive of system and ratio between component of the triply complex effect on purification of solution. (author)

  19. Complexation with dissolved organic matter and solubility control of heavy metals in sandy soil

    Weng, L.; Temminghoff, E.J.M.; Lofts, S.; Tipping, E.; Riemsdijk, van W.H.

    2002-01-01

    The complexation of heavy metals with dissolved organic matter (DOM) in the environment influences the solubility and mobility of these metals. In this paper, we measured the complexation of Cu, Cd, Zn, Ni, and Pb with DOM in the soil solution at pH 3.7-6.1 using a Donnan membrane technique. The

  20. Reactivity of olefin and allyl ligands in π-complexes of metals

    Kukushkin, Yu.N.

    1987-01-01

    The data on reactivity of olefin and allyl ligands in transition metal (Ru, W) π-complexes, published up to 1984 are presented. Metal ion coordination of olefins causes their appreciable reactivity change. Transformations of π-olefin ligands into σ-alkyl ones, interaction of π-complexes with oxygen nucleophilic reagents, amines, halogenides and pseudohalogenides are considered

  1. Metal-Insulator-Metal Single Electron Transistors with Tunnel Barriers Prepared by Atomic Layer Deposition

    Golnaz Karbasian

    2017-03-01

    Full Text Available Single electron transistors are nanoscale electron devices that require thin, high-quality tunnel barriers to operate and have potential applications in sensing, metrology and beyond-CMOS computing schemes. Given that atomic layer deposition is used to form CMOS gate stacks with low trap densities and excellent thickness control, it is well-suited as a technique to form a variety of tunnel barriers. This work is a review of our recent research on atomic layer deposition and post-fabrication treatments to fabricate metallic single electron transistors with a variety of metals and dielectrics.

  2. Metal oxide nanostructures: preparation, characterization and functional applications as chemical sensors.

    Zappa, Dario; Bertuna, Angela; Comini, Elisabetta; Kaur, Navpreet; Poli, Nicola; Sberveglieri, Veronica; Sberveglieri, Giorgio

    2017-01-01

    Preparation and characterization of different metal oxide (NiO, WO 3 , ZnO, SnO 2 and Nb 2 O 5 ) nanostructures for chemical sensing are presented. p-Type (NiO) and n-type (WO 3 , SnO 2 , ZnO and Nb 2 O 5 ) metal oxide nanostructures were grown on alumina substrates using evaporation-condensation, thermal oxidation and hydrothermal techniques. Surface morphologies and crystal structures were investigated through scanning electron microscopy and Raman spectroscopy. Furthermore, different batches of sensors have been prepared, and their sensing performances towards carbon monoxide and nitrogen dioxide have been explored. Moreover, metal oxide nanowires have been integrated into an electronic nose and successfully applied to discriminate between drinking and contaminated water.

  3. Preparation and pattern recognition of metallic Ni ultrafine powders by electroless plating

    Zhang, H.J.; Zhang, H.T.; Wu, X.W.; Wang, Z.L.; Jia, Q.L.; Jia, X.L.

    2006-01-01

    Using hydrazine hydrate as reductant, metallic Ni ultrafine powders were prepared from NiSO 4 aqueous solution by electroless plating method. The factors including concentration of NiSO 4 , bathing temperature, ratio of hydrazine hydrate to NiSO 4 , the pH of the solution, etc., on influence of the yield and average particle size of metallic Ni ultrafine powders were studied in detail. X-ray powders diffraction patterns show that the nickel powders are cubic crystallite. The average crystalline size of the ultrafine nickel powders is about 30 nm. The dielectric and magnetic loss of ultrafine Ni powders-paraffin wax composites were measured by the rectangle waveguide method in the range 8.2-12.4 GHz. The factors for Ni ultrafine powders preparation are optimized by computer pattern recognition program based on principal component analysis, the optimum factors regions with higher yield of metallic Ni ultrafine powders are indicated by this way

  4. Metallic complexes with glyphosate: a review; Complexos metalicos com o herbicida glifosato: revisao

    Coutinho, Claudia F.B.; Mazo, Luiz Henrique [Sao Paulo Univ., Sao Carlos, SP (Brazil). Inst. de Quimica]. E-mail: claudiabreda@iqsc.usp.br

    2005-11-15

    We present studies involving metallic ions and the herbicide glyphosate. The metallic complexes of Cu(II), Zn(II), Mn(II), Ni(II), Cd(II), Pb(II), Cr(III), Fe(III), Co(III), ammonium, sodium, Ag(I), alkaline earth metals and of some lanthanides ions are described. The complexes are discussed in terms of their synthesis, identification, stability and structural properties, based on data from the current literature. (author)

  5. Comparison of sample preparation procedures on metal(loid) fractionation patterns in lichens.

    Kroukamp, E M; Godeto, T W; Forbes, P B C

    2017-08-13

    The effects of different sample preparation strategies and storage on metal(loid) fractionation trends in plant material is largely underresearched. In this study, a bulk sample of lichen Parmotrema austrosinense (Zahlbr.) Hale was analysed for its total extractable metal(loid) content by ICP-MS, and was determined to be adequately homogenous (sample were prepared utilising a range of sample preservation techniques and subjected to a modified sequential extraction procedure or to total metal extraction. Both experiments were repeated after 1-month storage at 4 °C. Cryogenic freezing gave the best reproducibility for total extractable elemental concentrations between months, indicating this to be the most suitable method of sample preparation in such studies. The combined extraction efficiencies were >82% for As, Cu, Mn, Pb, Sr and Zn but poor for other elements, where sample preparation strategies 'no sample preparation' and 'dried in a desiccator' had the best extraction recoveries. Cryogenic freezing procedures had a significantly (p sample cleaning and preservation when species fractionation patterns are of interest. This study also shows that the assumption that species stability can be ensured through cryopreservation and freeze drying techniques needs to be revisited.

  6. Export control guide: Spent nuclear fuel reprocessing and preparation of plutonium metal

    1993-10-01

    The international Treaty on the Non-Proliferation of Nuclear Weapons, also referred to as the Non-Proliferation Treaty (NPT), states in Article III, paragraph 2(b) that open-quotes Each State Party to the Treaty undertakes not to provide . . . equipment or material especially designed or prepared for the processing, use or production of special fissionable material to any non-nuclear-weapon State for peaceful purposes, unless the source or special fissionable material shall be subject to the safeguards required by this Article.close quotes This guide was prepared to assist export control officials in the interpretation, understanding, and implementation of export laws and controls relating to the international Trigger List for irradiated nuclear fuel reprocessing equipment, components, and materials. The guide also contains information related to the production of plutonium metal. Reprocessing and its place in the nuclear fuel cycle are described briefly; the standard procedure to prepare metallic plutonium is discussed; steps used to prepare Trigger List controls are cited; descriptions of controlled items are given; and special materials of construction are noted. This is followed by a comprehensive description of especially designed or prepared equipment, materials, and components of reprocessing and plutonium metal processes and includes photographs and/or pictorial representations. The nomenclature of the Trigger List has been retained in the numbered sections of this document for clarity

  7. Controlled metal nitrate decomposition for the preparation of supported metal Catalysts

    Wolters, M.

    2010-01-01

    High surface area supported metal (oxide) catalysts are essential for the production of fuels, chemicals, pharmaceuticals and the abatement of environmental pollution. Impregnation of high surface area supports, often silica or alumina, followed by drying, calcination and reduction is one of the

  8. The use of metal alkoxides in the preparation of ceramic powders

    Chetcuti, A.M.; Woolfrey, J.L.

    1982-01-01

    The production of fine, chemically homogeneous and highly reactive powder is particularly desirable where the synthesis and fabrication of multicomponent ceramic systems, such as SYNROC, are concerned. To produce good sinterable material, a preparation technique that allows intimate mixing of all reacting species is desirable. Traditional routes for preparing fine powders have involved ball-milling metal oxides and spray-drying or flash-drying the resulting oxide slurries. The hydrolysis of metal alkoxides has been investigated as a technique to produce fine powders. The preparation of SYNROC B powder from alkoxides involves hydrolysing a mixture of titanium and zirconium alkoxides. The precipitated product is then blended with Al 3 + , Ba 2 + and Ca 2 + nitrate solution

  9. Solid state and solution photoluminescence properties of a novel meso–meso-linked porphyrin dimer Schiff base ligand and its metal complexes

    Tümer, Mehmet, E-mail: mtumer@ksu.edu.tr; Ali Güngör, S.; Raşit Çiftaslan, A.

    2016-02-15

    We prepared novel meso-meso linked 4-bromo-2,6-bis[5-(4-iminophenyl)-10,15,20-triphenylporphyrin]phenol (HL) and its Cu(II), Fe(III), Mn(III), Pt(II) and Zn(II) transition metal complexes. Structural characterizations of the ligand (HL) and its metal complexes were done by the spectroscopic and analytical methods. The electronic absorption and photoluminescence spectra of the ligand, its metal complexes and the metal salts used for preparing of the complexes were investigated in the solid and solution state. The emission and excitation data of the CuCl{sub 2}·2H{sub 2}O in both solid and the solution state were obsrved in the longest wavelenght. On the other hand, the emission value of the ZnCl{sub 2} salt was shown at the shortest wavelenght. The emission values of the [LCu{sub 4}Cl{sub 3}(H{sub 2}O){sub 2}]H{sub 2}O and LPt{sub 4}Cl{sub 3} complexes in the solid state are bigger than the other metal salts. The ligand and its metal complexes show the very interesting absorption spectral properties in the solid state. Metal complexes have less number Q bands in the solid state. The electrochemical properties of the ligand and its metal complexes were investigated and found that they show the reversible or irreversible redox processes at the different scan rates. Thermal properties of the compopunds were investigated in the 20–900 °C temperature range.

  10. Some physico-chemical and radiation properties of plutonium-238 metal prepared by electrochemical amalgamation

    Peretrukhin, V.F. [A.N. Frumkin Institute of Physical Chemistry and Electrochemistry, Russian Academy of Sciences, 31 Leninsky Prospect, Moscow 119991 (Russian Federation)], E-mail: vperet@ipc.rssi.ru; Rovny, S.I. [Production Association ' Mayak' , 31 Prospect Lenin, Ozersk, Chelyabinsk Region 456784 (Russian Federation); Maslennikov, A.G. [A.N. Frumkin Institute of Physical Chemistry and Electrochemistry, Russian Academy of Sciences, 31 Leninsky Prospect, Moscow 119991 (Russian Federation); Ershov, V.V.; Chinenov, P.P.; Kapitonov, V.I.; Kuvaev, V.L. [Production Association ' Mayak' , 31 Prospect Lenin, Ozersk, Chelyabinsk Region 456784 (Russian Federation)

    2007-10-11

    Pu-238 metal was prepared by electrolytic amalgamation from Pu(III) acetate aqueous solution and by followed by the thermal decomposition of the Pu amalgam. The density, specific heat power, {gamma}-spectra, neutron flux, and corrosion kinetics in dry air at ambient temperature of the prepared {sup 238}Pu metal were measured. The neutron flux and {gamma}-spectra from {sup 238}Pu metal have been attributed to spontaneous and induced fission and to ({alpha},{alpha}'{gamma}), ({alpha},p{gamma}), and ({alpha},n{gamma}) nuclear reactions on light nuclei. The electrochemically prepared {sup 238}Pu metal was shown to generate fewer neutrons, produce less gamma radiation, and contains lower {sup 10}B, {sup 19}F, and {sup 28}Si impurities in comparison with biomedical {sup 238}PuO{sub 2}. The increase of neutron flux from the sample due to the reaction {sup 18}O({alpha},n{gamma}) {sup 21}Ne was shown to be proportional to the increase of the mass of the {sup 238}Pu metal with time due to corrosion in dry air. {sup 238}Pu metal corrosion rate maximum and average values (1.1 x 10{sup -2} and 4.7 x 10{sup -3} mg cm{sup -2} h{sup -1}, respectively) obtained in dry air were an order of magnitude higher than the rates published for {sup 239}Pu under similar experiment conditions. The difference between the {sup 239}Pu and {sup 238}Pu metal corrosion rate and mechanism is proposed to be due to the greater radiation effects and temperature on the {sup 238}Pu surface.

  11. On the capacity to the complexing of alkaline earth metal and magnesium chromates

    Orekhov, O.L.

    1978-01-01

    Considered is the capacity to the complexing of magnesium chromates and alkaline earth metal chromates with ammonium chromates in aqueous solutions. It has been established that the complexing of alkaline earth metal and magnesium chromates is effected by a nature of initial salts as well as their solubilities and the presence of crystallization water. Capacity of magnesium ions and alkaline rare earth metals to the complexing decreases in a series of Mg-Ca-Sr-Ba. Ca complexes exceed magnesium derivatives in respect of stability

  12. Preparation and photoluminescence enhancement in terbium(III ternary complexes with β-diketone and monodentate auxiliary ligands

    Devender Singh

    2016-12-01

    Full Text Available A series of new solid ternary complexes of terbium(III ion based on β-diketone ligand acetylacetone (acac and monodentate auxiliary ligands (aqua/urea/triphenylphosphineoxide/pyridine-N-oxide had been prepared. The structural characterizations of synthesized ternary compounds were studied by means of elemental analysis, infrared (IR, and proton nuclear magnetic resonance (NMR spectral techniques. The optical characteristics were investigated with absorption as well as photoluminescence spectroscopy. Thermal behavior of compounds was examined by TGA/DTA analysis and all metal complexes were found to have good thermal stability. The luminescence decay time of complexes were also calculated by monitoring at emission wavelength corresponding to 5D4 → 7F5 transition. A comparative inspection of the luminescent behavior of prepared ternary compounds was performed in order to determine the function of auxiliary ligands in the enhancement of luminescence intensity produced by central terbium(III ion. The color coordinates values suggested that compounds showed bright green emission in visible region in electromagnetic spectrum. Complexes producing green light could play a significant role in the fabrication of efficient light conversion molecular devices for display purposes and lightning systems.

  13. Speciation Studies of Some Toxic Metal Complexes of Glycylglycine ...

    NICO

    mixtures apart from its established utility in understanding ... Chemical speciation of metals is important for an understand- ... Titrations with differ- ent ratios (1:2.5, 1:3.5 and 1:5) of metal-ligand were performed with 0.4 mol L–1 sodium hydroxide solution. The mixtures obtained from PG and water are non-ideal due.

  14. Studies on the preparation of thorium metal sponge from thorium oxalate

    Vijay, P.L.; Sehra, J.C.; Sundaram, C.V.; Gurumurthy, K.R.; Raghavan, R.V.

    1978-01-01

    The results of investigations carried out on the production of high purity thorium metal sponge, starting with thorium oxalate are presented. The flow sheet includes chlorination of thorium oxalate, purification of raw thorium tetrachloride, magnesium reduction of anhydrous thorium tetrachloride, slag metal separation, vacuum distillation for removal of residual MgCl 2 and excess magnesium, and consolidation of the metal sponge. Studies have been carried out to investigate the optimum chlorination efficiency and chlorine utilization attainable using different chlorinating agents, and to compare the quality of the sponge obtained with single and double distilled chloride. The overall process efficiency under optimum conditions was 81%. The thorium metal button, prepared from the sponge by arc-melting, analysed : O 2 - 847, N 2 - 20, C - 179, Mg - 100, Fe - 49, Ni<50, Al - 11, Cr - 7 (expressed in parts per million parts of thorium). The button could be further purified by electron beam melting to improve its ductility. (author)

  15. Synthesis, spectral studies and biological evaluation of 2-aminonicotinic acid metal complexes

    Nawaz, Muhammad; Abbasi, Muhammad Waseem; Hisaindee, Soleiman; Zaki, Muhammad Javed; Abbas, Hira Fatima; Mengting, Hu; Ahmed, M. Arif

    2016-05-01

    We synthesized 2-aminonicotinic acid (2-ANA) complexes with metals such as Co(II), Fe(III), Ni(II), Mn(II), Zn(II), Ag(I),Cr(III), Cd(II) and Cu(II) in aqueous media. The complexes were characterized and elucidated using FT-IR, UV-Vis, a fluorescence spectrophotometer and thermo gravimetric analysis (TGA). TGA data showed that the stoichiometry of complexes was 1:2 metal/ligand except for Ag(I) and Mn(II) where the ratio was 1:1. The metal complexes showed varied antibacterial, fungicidal and nematicidal activities. The silver and zinc complexes showed highest activity against Bacillus subtilis and Bacillus licheniformis respectively. Fusarium oxysporum was highly susceptible to nickel and copper complexes whereas Macrophomina phaseolina was completely inert to the complexes. The silver and cadmium complexes were effective against the root-knot nematode Meloidogyne javanica.

  16. Synthesis, spectral studies and biological evaluation of 2-aminonicotinic acid metal complexes.

    Nawaz, Muhammad; Abbasi, Muhammad Waseem; Hisaindee, Soleiman; Zaki, Muhammad Javed; Abbas, Hira Fatima; Mengting, Hu; Ahmed, M Arif

    2016-05-15

    We synthesized 2-aminonicotinic acid (2-ANA) complexes with metals such as Co(II), Fe(III), Ni(II), Mn(II), Zn(II), Ag(I),Cr(III), Cd(II) and Cu(II) in aqueous media. The complexes were characterized and elucidated using FT-IR, UV-Vis, a fluorescence spectrophotometer and thermo gravimetric analysis (TGA). TGA data showed that the stoichiometry of complexes was 1:2 metal/ligand except for Ag(I) and Mn(II) where the ratio was 1:1. The metal complexes showed varied antibacterial, fungicidal and nematicidal activities. The silver and zinc complexes showed highest activity against Bacillus subtilis and Bacillus licheniformis respectively. Fusarium oxysporum was highly susceptible to nickel and copper complexes whereas Macrophomina phaseolina was completely inert to the complexes. The silver and cadmium complexes were effective against the root-knot nematode Meloidogyne javanica. Copyright © 2016 Elsevier B.V. All rights reserved.

  17. PREPARATION AND PROPERTY OF POLYMERIC PENDANT Ru(bpy)32+ COMPLEXES

    HOU Xiaohuai; Masao Kaneko; Akira Yamada

    1984-01-01

    Polymeric pendant Ru(bpy)32+ complexes were prepared from homopolymer and copolymers of 4-methyl-4'-vinyl-2,2'-bipyridine (Vbpy). Vbpy was prepared from 4-methylpyridine. The comonomers were styrene (St), acrylic acid (AA), N-vinylpyrrolidone (Pyr), 4-vinylpyridine (Vpy), methyl methacrylate (MMA), 2-hydroxyethyl methacrylate (HEMA), acrylonitrile (AN) and N-ethyl-4-vinylpyridium bromide (EQ-Vpy). The fraction of the pendant Ru(bpy)32+ repeating unit in the polymeric complex was 0.022 to 0.052. Absorption maximum, molar extinction coefficient, emission maximum and relative emission intensity of the polymeric complexes were studied.

  18. Some transition metal complexes derived from mono- and di-ethynyl perfluorobenzenes.

    Armitt, David J; Bruce, Michael I; Gaudio, Maryka; Zaitseva, Natasha N; Skelton, Brian W; White, Allan H; Le Guennic, Boris; Halet, Jean-François; Fox, Mark A; Roberts, Rachel L; Hartl, Frantisek; Low, Paul J

    2008-12-21

    Transition metal alkynyl complexes containing perfluoroaryl groups have been prepared directly from trimethylsilyl-protected mono- and di-ethynyl perfluoroarenes by simple desilylation/metallation reaction sequences. Reactions between Me(3)SiC[triple bond, length as m-dash]CC(6)F(5) and RuCl(dppe)Cp' [Cp' = Cp, Cp*] in the presence of KF in MeOH give the monoruthenium complexes Ru(C[triple bond, length as m-dash]CC(6)F(5))(dppe)Cp' [Cp' = Cp (); Cp* ()], which are related to the known compound Ru(C[triple bond, length as m-dash]CC(6)F(5))(PPh(3))(2)Cp (). Treatment of Me(3)SiC[triple bond, length as m-dash]CC(6)F(5) with Pt(2)(mu-dppm)(2)Cl(2) in the presence of NaOMe in MeOH gave the bis(alkynyl) complex Pt(2)(mu-dppm)(2)(C[triple bond, length as m-dash]CC(6)F(5))(2) (). The Pd(0)/Cu(i)-catalysed reactions between Au(C[triple bond, length as m-dash]CC(6)F(5))(PPh(3)) and Mo( identical withCBr)(CO)(2)Tp* [Tp* = hydridotris(3.5-dimethylpyrazoyl)borate], Co(3)(mu(3)-CBr)(mu-dppm)(CO)(7) or IC[triple bond, length as m-dash]CFc [Fc = (eta(5)-C(5)H(4))FeCp] afford Mo( identical withCC[triple bond, length as m-dash]CC(6)F(5))(CO)(2)Tp* (), Co(3)(mu(3)-CC[triple bond, length as m-dash]CC(6)F(5))(mu-dppm)(CO)(7) () and FcC[triple bond, length as m-dash]CC[triple bond, length as m-dash]CC(6)F(5) (), respectively. The diruthenium complexes 1,4-{Cp'(PP)RuC[triple bond, length as m-dash]C}(2)C(6)F(4) [(PP)Cp' = (PPh(3))(2)Cp (); (dppe)Cp (); (dppe)Cp* ()] are prepared from 1,4-(Me(3)SiC[triple bond, length as m-dash]C)(2)C(6)F(4) in a manner similar to that described for the monoruthenium complexes -. The non-fluorinated complexes 1,4-{Cp'(PP)RuC[triple bond, length as m-dash]C}(2)C(6)H(4) [(PP)Cp' = (PPh(3))(2)Cp (); (dppe)Cp (); (dppe)Cp* ()], prepared for comparison, are obtained from 1,4-(Me(3)SiC[triple bond, length as m-dash]C)(2)C(6)H(4). Spectro-electrochemical studies of the ruthenium aryl and arylene alkynyl complexes - and -, together with DFT-based computational

  19. Magnetite–hematite nanoparticles prepared by green methods for heavy metal ions removal from water

    Ahmed, M.A.; Ali, S.M.; El-Dek, S.I.; Galal, A.

    2013-01-01

    Graphical abstract: The negatively charged cubic magnetite nanoparticles, prepared by the coprecipitation method in N 2 atmosphere, can adsorb up to 99% of the positively charged toxic heavy metal ions at a proper pH value. -- Highlights: • Mixed magnetite–hematite nanoparticles were synthesized via different routes. • Prepared samples were characterized by XRD, HRTEM, BET and magnetic hysteresis. • The material was employed as a sorbent for removal of some heavy metal ions from water. • The effects of pH and the contact time on the adsorption process were studied and optimized. -- Abstract: Mixed magnetite–hematite nanoparticles were synthesized via different routes such as, coprecipitation in air and N 2 atmosphere, citrate–nitrate, glycine–nitrate and microwave-assisted citrate methods. The prepared samples were characterized by X-ray diffraction (XRD), high resolution transmission electron microscope (HRTEM), BET measurements and magnetic hysteresis. XRD data showed the formation of magnetite–hematite mixture with different compositions according to the synthesis method. The particle size was in the range of 4–52 nm for all the prepared samples. From HRTEM micrographs, it was found that, the synthesis method affects the moropholgy of the prepared samples in terms of crystallinity and porosity. The magnetite–hematite mixture was employed as a sorbent material for removal of some heavy metal ions from water such as lead(II), cadmium(II) and chromium(III). The effects of pH value and the contact time on the adsorption process were studied and optimized in order to obtain the highest possible adsorption efficiency of the magnetite–hematite mixture. The effect of the synthesis method of the magnetite–hematite mixture on the adsorption process was also investigated. It was found that samples prepared by the coprecipitation method had better adsorption efficiency than those prepared by other combustion methods

  20. Preparation of new phthalocyanine complexes of some rare-earth elements

    Sugimoto, Hiroshi; Higashi, Teruaki; Mori, Masayasu

    1982-01-01

    The reaction of tris(1,3-diphenyl-1,3-propanedionato) complexes of heavier rare-earth elements, M 3+ (dbm) 3 and lithium phthalocyaninato (2-), Li 2 (pc) gave two types of new stable phthalocyanine complexes, [M 3+ (pc)(dbm)(dbmH)] and [M 3+ (pc)(dbm)] depending on the solvents used for the preparation. The structure of both types of complexes are tentatively proposed. (author)

  1. A method for the preparation of lipophilic macrocyclic technetium-99m complexes

    Troutner, D.E.; Volkert, W.A.

    1991-01-01

    A procedure for the preparation of technetium complexes applicable as diagnostic radiopharmaceuticals is suggested and documented with 27 examples. Technetium-99m is reacted with a suitable complexant selected from the class of alkylenamine oximes containing 2 or 3 carbon atoms in the alkylene group. The lipophilic macrocyclic complexes possess an amine, amide, carboxy, carboxy ester, hydroxy or alkoxy group or a suitable electron acceptor group. (M.D.). 7 tabs

  2. Preparation, characterization and in vitro dissolution study of Nitrazepam: Cyclodextrin inclusion complex

    Patel, J. S.; Patel, R. P.

    2012-01-01

    The objectives of this research were to prepare and characterize inclusion complexes of Nitrazepam with Hydroxypropyl-β-cyclodextrin (HPβCD) and Sulfobutyl ether β-cyclodextrin (SBEβCD) to study the effect of complexation on the dissolution rate of Nitrazepam, a water-insoluble drug. The phase solubility profile of Nitrazepam with Hydroxypropyl- β-cyclodextrin and Sulfobutyl ether β-cyclodextrin was an AP-type, indicating the formation of 2:1 stoichiometric inclusion complexes. Gibbs free ene...

  3. Preparation and Heat-Treatment of DWPF Simulants With and Without Co-Precipitated Noble Metals

    Koopman, David C.:Eibling, Russel E

    2005-01-01

    The Savannah River National Laboratory is in the process of investigating factors suspected of impacting catalytic hydrogen generation in the Chemical Process Cell of the Defense Waste Processing Facility, DWPF. Noble metal catalyzed hydrogen generation in simulation work constrains the allowable acid addition operating window in DWPF. This constraint potentially impacts washing strategies during sludge batch preparation. It can also influence decisions related to the addition of secondary waste streams to a sludge batch. Noble metals have historically been added as trim chemicals to process simulations. The present study investigated the potential conservatism that might be present from adding the catalytic species as trim chemicals to the final sludge simulant versus co-precipitating the noble metals into the insoluble sludge solids matrix. Parallel preparations of two sludge simulants targeting the composition of Sludge Batch 3 were performed in order to evaluate the impact of the form of noble metals. Identical steps were used except that one simulant had dissolved palladium, rhodium, and ruthenium present during the precipitation of the insoluble solids. Noble metals were trimmed into the other stimulant prior to process tests. Portions of both sludge simulants were held at 97 C for about eight hours to qualitatively simulate the effects of long term storage on particle morphology and speciation. The simulants were used as feeds for Sludge Receipt and Adjustment Tank, SRAT, process simulations. The following conclusions were drawn from the simulant preparation work: (1) The first preparation of a waste slurry simulant with co-precipitated noble metals was successful, based on the data obtained. It appears that 99+% of the noble metals were retained in the simulant. (2) Better control of carbonate, hydroxide, and post-wash trim chemical additions is needed before the new method of simulant preparation will be as reproducible as the old method. (3) The two new

  4. Multiheteromacrocycles that Complex Metal Ions. Sixth Progress Report, 1 May 1979-30 April 1980

    Cram, D. J.

    1980-01-15

    Objective is to design synthesize, and evaluate cyclic and polycyclic host organic compounds for their abilities to complex and lipophilize guest metal ions, their complexes, and their clusters. Host organic compounds consist of strategically placed solvating, coordinating, and ion-pairing sites tied together by covalent bonds through hydrocarbon units around cavities shaped to be occupied by guest metal ions or by metal ions plus their ligands. Specificity in complexation is sought by matching the following properties of host and guest: cavity and metal ion sizes; geometric arrangements of binding sites; number of binding sites; character of binding sites; and valences. During this period, hemispherands based on an aryloxy or cyclic urea unit, spherands based on aryloxyl units only, and their complexes with alkali metals and alkaline earths were investigated. An attempt to separate {sup 6}Li and {sup 7}Li by gel permeation chromatography of lithiospherium chloride failed. (DLC)

  5. Structure and catalytic properties of metal β-diketonate complexes with oxygen-containing compounds

    Nizel'skij, Yu.N.; Ishchenko, S.S.; Lipatova, T.Eh.

    1985-01-01

    The results of researches published in recent 15-20 years of complexes of metal β-diketonates (including Cr 3+ , VO 2+ , MoOΛ2 2+ , Co 3+ , Mn 3+ , Ni 2+ , Fe 3+ ) with oxygen-containing compounds (alcohols, glycols, phenols, hydroperoxides, aldehydes, esters, etc.) playing an important role in catalytic processes of oxidation, addition, polymerization and copolymerization are reviewed. Data on the nature of chemical bond of oxygen-containing reacting agents with metal β-diketonates, on structure of metal β-diketonate complexes with oxygen-containing reacting agents and thermodynamics of complexing as well as on activation of reacting agents in complexes and catalytic properties of metal β-diketonates are discussed. Stored materials make it possible to exercise directed control of metal β-diketonate activity

  6. Preparation of Zeolite/Zinc Oxide Nanocomposites for toxic metals removal from water

    Abdullah A. Alswata

    Full Text Available This research work has proposed preparation of Zeolite/Zinc Oxide Nanocomposite (Zeolite/ZnO NCs by using a co-precipitation method. Then, the prepared Nanocomposite has been tested for adsorption of Lead Pb (II and Arsenic As (V from aqueous solution under the room pressure and temperature. After that, the prepared adsorbent has been studied by several techniques. For adsorption process; the effect of the adsorbent masses, contact time, PH and initial metals concentration as well as, the kinetics and isotherm for adsorption process have been investigated. The results revealed that; ZnO nanoparticles (NPs with average diameter 4.5 nm have successfully been loaded into Zeolite. The optimum parameters for the removal of the toxic metals 93% and 89% of Pb (II and As (V, respectively, in 100 mg/L aqua solutions were pH4, 0.15 g and 30 min. According to the obtained results; pseudo second-order kinetic and Langmuir isotherm model have higher correlation coefficients and provided a better agreement with the experimental data. The prepared sorbent showed an economical and effective way to remove the heavy toxic metals due to its ambient operation conditions, low- consumption energy and facile regeneration method. Keywords: Zeolite, ZnO, Nanocomposites, Adsorbent, Kinetic, Isotherm

  7. Removal of Heavy Metals from Drinking Water by Magnetic Carbon Nanostructures Prepared from Biomass

    Muhammad Muneeb Ur Rahman Khattak

    2017-01-01

    Full Text Available Heavy metals contamination of drinking water has significant adverse effects on human health due to their toxic nature. In this study a new adsorbent, magnetic graphitic nanostructures were prepared from watermelon waste. The adsorbent was characterized by different instrumental techniques (surface area analyzer, FTIR, XRD, EDX, SEM, and TG/DTA and was used for the removal of heavy metals (As, Cr, Cu, Pb, and Zn from water. The adsorption parameters were determined for heavy metals adsorption using Freundlich and Langmuir isotherms. The adsorption kinetics and effect of time, pH, and temperature on heavy metal ions were also determined. The best fits were obtained for Freundlich isotherm. The percent adsorption showed a decline at high pH. Best fit was obtained with second-order kinetics model for the kinetics experiments. The values of ΔH° and ΔG° were negative while that of ΔS° was positive. The prepared adsorbent has high adsorption capacities and can be efficiently used for the removal of heavy metals from water.

  8. Molecular nanomagnets: Syntheses and characterization of high nuclearity transition metal complexes

    Foguet-Albiol, Maria D.

    2006-12-01

    High nuclearity transition metal complexes have attracted a lot of attention because of their aesthetically pleasant structures and/or their potential applications. The fusion of the world of magnetism with the exciting research in physics and chemistry led to the realization of interesting types of materials that can function as nanoscale magnetic particles. The study of the magnetism of inorganic complexes and especially the study of these molecular nanomagnets (or single-molecule magnets, SMMs) is a field that has generated intense interest in the scientific community. Interest in these molecular nanomagnets arises as part of a broader investigation of nanomagnetism (and nanotechnology), as these represent the ultimate step in device miniaturization. The primary purpose of this dissertation is the development of new synthetic methods intended for the preparation of novel single-molecule magnets (SMMs). The definition of the "bottom-up approach" is to increase the size of molecules by adding new magnetic centers; this is attractive but does not actually reflect how the chemistry takes place. Various strategies have been employed in developing the aforementioned synthetic methods which include the use of mononuclear as well as preformed clusters as starting materials; and the introduction of new alcohol based ligands as N-methyldiethanolamine (mdaH2) and triethanolamine (teaH3), since currently only a few alcohol based ligands have been used by different research groups. Many of these efforts have led to the isolation of new polynuclear Mn clusters with nuclearities ranging all the way from four to thirty-one. Additionally, a family of related Fe7 complexes has been synthesized. The transition metal cluster chemistry has also been extended to nickel-containing species. Many of these polynulear transition metal complexes function as single-molecule magnets. An additional research direction discussed herein is the study of the exchange-coupled dimer of single

  9. Purification of Ovine Respiratory Complex I Results in a Highly Active and Stable Preparation*

    Letts, James A.; Degliesposti, Gianluca; Fiedorczuk, Karol; Skehel, Mark; Sazanov, Leonid A.

    2016-01-01

    NADH-ubiquinone oxidoreductase (complex I) is the largest (∼1 MDa) and the least characterized complex of the mitochondrial electron transport chain. Because of the ease of sample availability, previous work has focused almost exclusively on bovine complex I. However, only medium resolution structural analyses of this complex have been reported. Working with other mammalian complex I homologues is a potential approach for overcoming these limitations. Due to the inherent difficulty of expressing large membrane protein complexes, screening of complex I homologues is limited to large mammals reared for human consumption. The high sequence identity among these available sources may preclude the benefits of screening. Here, we report the characterization of complex I purified from Ovis aries (ovine) heart mitochondria. All 44 unique subunits of the intact complex were identified by mass spectrometry. We identified differences in the subunit composition of subcomplexes of ovine complex I as compared with bovine, suggesting differential stability of inter-subunit interactions within the complex. Furthermore, the 42-kDa subunit, which is easily lost from the bovine enzyme, remains tightly bound to ovine complex I. Additionally, we developed a novel purification protocol for highly active and stable mitochondrial complex I using the branched-chain detergent lauryl maltose neopentyl glycol. Our data demonstrate that, although closely related, significant differences exist between the biochemical properties of complex I prepared from ovine and bovine mitochondria and that ovine complex I represents a suitable alternative target for further structural studies. PMID:27672209

  10. studies on transition metal complexes of herbicidal compounds. ii

    a

    derivative of 2-chloro-4-ethylamino-6-isopropylamino-s-triazine, atrazine (ATZ) --- a well known herbicide has ... development while the other is the metal ion associated degradation or deactivation of the herbicides .... Colour M.p./decomp.

  11. Transition metal complexes with oxygen donor ligands: a synthesis, spectral, thermal and antimicrobial study

    VAIBHAV N. PATANGE

    2008-10-01

    Full Text Available Transition metal complexes of chalcones derived from the conden¬sation of 3-acetyl-6-methyl-2H-pyran-2,4(3H-dione (dehydroacetic acid and p-methoxybenzaldehyde (HL1 or p-nitrobenzaldehyde (HL2 were synthesized and characterized by elemental analysis, conductometry, thermal analysis, magnetic measurements, IR, 1H-NMR, UV–Vis spectroscopy and a microbial study. From the analytical and thermal data, the stoichiometry of the complexes was found to be 1:2 (metal:ligand. The molar conductance data revealed that all the metal chelates were non-electrolytes. The thermal stability of the complexes was studied by thermogravimetry and the decomposition schemes of the complexes are given. The ligands and their metal complexes were screened for antibacterial activity against Staphylococcus aureus and Escherichia coli, and fungicidal activity against Aspergillus flavus, Curvularia lunata and Penicillium notatum.

  12. Determination of stability constants of aminoglycoside antibiotics with their metal complexes

    Tiwow, Vanny M. A.

    2014-03-01

    One group of aminoglycoside antibiotics contains aminosugars. The aminosugar neomycin B with its derivate product neamine (2-Deoxy-4-0-(2,6-diamino-2,6-dideoxy-α-D-glucopyranosyl)-D-Streptamine) was identified as a free ligands and metal complexes. In particular, the stability constants of metal complexes by potentiometric titration techniques were investigated. Our previous study had determined the acid dissociation constants of these aminosugars with few metal complexes in fair depth. In this work, the complexation of two pyridine-containing amino alcohols and an amino sugar (neamine) have been measured potentiometrically. For instance, the stability constant of copper(II) complexation were determine and the model system generated an excellent fit. Stability constants with several metals have been determined and will be reported.

  13. Insights into the superhydrophobicity of metallic surfaces prepared by electrodeposition involving spontaneous adsorption of airborne hydrocarbons

    Liu, Peng; Cao, Ling; Zhao, Wei; Xia, Yue; Huang, Wei; Li, Zelin

    2015-01-01

    Graphical abstract: - Highlights: • Several superhydrophobic metallic surfaces were fabricated by fast electrodeposition. • Both micro/nanostructures and adsorption of airborne hydrocarbons make contributions. • XPS analyses confirm presence of airborne hydrocarbons on these metallic surfaces. • The adsorption of airborne hydrocarbons on the clean metal Au surface was very quick. • UV-O 3 treatment oxidized the hydrocarbons to hydrophilic oxygen-containing organics. - Abstract: Electrochemical fabrication of micro/nanostructured metallic surfaces with superhydrophobicity has recently aroused great attention. However, the origin still remains unclear why smooth hydrophilic metal surfaces become superhydrophobic by making micro/nanostructures without additional surface modifications. In this work, several superhydrophobic micro/nanostructured metal surfaces were prepared by a facile one-step electrodeposition process, including non-noble and noble metals such as copper, nickel, cadmium, zinc, gold, and palladium with (e.g. Cu) or without (e.g. Au) surface oxide films. We demonstrated by SEM and XPS that both hierarchical micro/nanostructures and spontaneous adsorption of airborne hydrocarbons endowed these surfaces with excellent superhydrophobicity. We revealed by XPS that the adsorption of airborne hydrocarbons at the Ar + -etched clean Au surface was rather quick, such that organic contamination can hardly be prevented in practical operation of surface wetting investigation. We also confirmed by XPS that ultraviolet-O 3 treatment of the superhydrophobic metal surfaces did not remove the adsorbed hydrocarbons completely, but mainly oxidized them into hydrophilic oxygen-containing organic substances. We hope our findings here shed new light on deeper understanding of superhydrophobicity for micro/nanostructured metal surfaces with and without surface oxide films

  14. Modulation of solubility and dissolution of furosemide by preparation of phospholipid complex

    Mona Semalty

    2014-01-01

    Full Text Available Aim: The aim of this study is to improve the solubility and dissolution of furosemide (a potent high ceiling diuretic used for the treatment of hypertension and a Class IV drug that is low solubility and low permeability drug as per the Biopharmaceutical Classification System by preparing its phospholipid complexes or pharmacosomes. Materials and Methods: Furosemide was complexed with phosphatidylcholine in four different molar ratios (1:1, 1:2, 1:3 and 1:4 by conventional solvent-evaporation technique. The pharmacosomes prepared were evaluated for drug content, solubility, X-ray powder diffraction (XRPD and in-vitro dissolution study. Results: Pharmacosomes of furosemide showed high drug content ranging from 88.30% to 100%. XRPD studies confirmed the formation of phospholipid complex and the amorphization of drug in the complex. The water solubility was found to be increased up to six-fold in the complexes. The octanol solubility also increased in the complexes indicating the probable increase in permeability. The in-vitro dissolution profile of the prepared complexes was found to be much better than furosemide. Conclusion: It was concluded that the phospholipid complexes can be effectively used for improving the solubility, dissolution, permeability and hence the bioavailability of furosemide like Class IV drugs.

  15. Atomic absorption determination of metals in soils using ultrasonic sample preparation

    Chmilenko, F.A.; Smityuk, N.M.; Baklanov, A.N.

    2002-01-01

    It was shown that ultrasonic treatment accelerates sample preparation of soil extracts from chernozem into different solvents by a factor of 6 to 60. These extracts are used for the atomic absorption determination of soluble species of Cd, Co, Cr, Cu, Ni, Pb, and Zn. The optimum ultrasound parameters (frequency, intensity, and treatment time) were found for preparing soil extracts containing analytes in concentrations required in agrochemical procedures. Different extractants used to extract soluble heavy metals from soils of an ordinary chernozem type in agrochemical procedures using ultrasonic treatment were classified in accordance with the element nature [ru

  16. Metal-ion complexes of functionalised 1,10-Phenanthrolines as hydrolytic synzymes

    Weijnen, J.G.J.

    1993-01-01

    In this thesis metal-ion complexes of functionalised 1,10-phenanthroline derivatives have been studied as model systems for hydrolytic metallo-enzymes. Amphiphilic metallo- complexes incorporated into micelles or vesicles and water-soluble complexes in pure aqueous buffer solutions, have

  17. Synthesis, spectral, thermal, potentiometric and antimicrobial studies of transition metal complexes of tridentate ligand

    Sarika M. Jadhav

    2014-01-01

    Full Text Available A series of metal complexes of Cu(II, Ni(II, Co(II, Fe(III and Mn(II have been synthesized with newly synthesized biologically active tridentate ligand. The ligand was synthesized by condensation of dehydroacetic acid (3-acetyl-6-methyl-(2H pyran-2,4(3H-dione or DHA, o-phenylene diamine and fluoro benzaldehyde and characterized by elemental analysis, molar conductivity, magnetic susceptibility, thermal analysis, X-ray diffraction, IR, 1H-NMR, UV–Vis spectroscopy and mass spectra. From the analytical data, the stoichiometry of the complexes was found to be 1:2 (metal:ligand with octahedral geometry. The molar conductance values suggest the non-electrolyte nature of metal complexes. The IR spectral data suggest that the ligand behaves as a dibasic tridentate ligand with ONN donor atoms sequence towards central metal ion. Thermal behaviour (TG/DTA and kinetic parameters calculated by the Coats–Redfern and Horowitz–Metzger method suggest more ordered activated state in complex formation. To investigate the relationship between stability constants of metal complexes and antimicrobial activity, the dissociation constants of Schiff bases and stability constants of their binary metal complexes have been determined potentiometrically in THF–water (60:40% solution at 25 ± 1 °C and at 0.1 M NaClO4 ionic strength. The potentiometric study suggests 1:1 and 1:2 complexation. Antibacterial and antifungal activities in vitro were performed against Staphylococcus aureus, Escherichia coli and Aspergillus niger, Trichoderma, respectively. The stability constants of the metal complexes were calculated by the Irving–Rosotti method. A relation between the stability constant and antimicrobial activity of complexes has been discussed. It is observed that the activity enhances upon complexation and the order of antifungal activity is in accordance with stability order of metal ions.

  18. Self-Assembly of Discrete Metal Complexes in Aqueous Solution via Block Copolypeptide Amphiphiles

    Timothy J. Deming

    2013-01-01

    Full Text Available The integration of discrete metal complexes has been attracting significant interest due to the potential of these materials for soft metal-metal interactions and supramolecular assembly. Additionally, block copolypeptide amphiphiles have been investigated concerning their capacity for self-assembly into structures such as nanoparticles, nanosheets and nanofibers. In this study, we combined these two concepts by investigating the self-assembly of discrete metal complexes in aqueous solution using block copolypeptides. Normally, discrete metal complexes such as [Au(CN2]−, when molecularly dispersed in water, cannot interact with one another. Our results demonstrated, however, that the addition of block copolypeptide amphiphiles such as K183L19 to [Au(CN2]− solutions induced one-dimensional integration of the discrete metal complex, resulting in photoluminescence originating from multinuclear complexes with metal-metal interactions. Transmission electron microscopy (TEM showed a fibrous nanostructure with lengths and widths of approximately 100 and 20 nm, respectively, which grew to form advanced nanoarchitectures, including those resembling the weave patterns of Waraji (traditional Japanese straw sandals. This concept of combining block copolypeptide amphiphiles with discrete coordination compounds allows the design of flexible and functional supramolecular coordination systems in water.

  19. On Metal Segregation of Bimetallic Nanocatalysts Prepared by a One-Pot Method in Microemulsions

    Concha Tojo

    2017-02-01

    Full Text Available A comparative study on different bimetallic nanocatalysts prepared from microemulsions using a one-pot method has been carried out. The analysis of experimental observations, complemented by simulation studies, provides detailed insight into the factors affecting nanoparticle architecture: (1 The metal segregation in a bimetallic nanocatalysts is the result of the combination of three main kinetic parameters: the reduction rate of metal precursors (related to reduction standard potentials, the material intermicellar exchange rate (determined by microemulsion composition, and the metal precursors concentration; (2 A minimum difference between the reduction standard potentials of the two metals of 0.20 V is needed to obtain a core-shell structure. For values ∆ε0 smaller than 0.20 V the obtaining of alloys cannot be avoided, neither by changing the microemulsion nor by increasing metal concentration; (3 As a rule, the higher the film flexibility around the micelles, the higher the degree of mixture in the nanocatalyst; (4 A minimum concentration of metal precursors is required to get a core-shell structure. This minimum concentration depends on the microemulsion flexibility and on the difference in reduction rates.

  20. Co3O4 protective coatings prepared by Pulsed Injection Metal Organic Chemical Vapour Deposition

    Burriel, M.; Garcia, G.; Santiso, J.

    2005-01-01

    of deposition temperature. Pure Co3O4 spinel structure was found for deposition temperatures ranging from 360 to 540 degreesC. The optimum experimental parameters to prepare dense layers with a high growth rate were determined and used to prepare corrosion protective coatings for Fe-22Cr metallic interconnects......Cobalt oxide films were grown by Pulsed Injection Metal Organic Chemical Vapour Deposition (PI-MOCVD) using Co(acac)(3) (acac=acetylacetonate) precursor dissolved in toluene. The structure, morphology and growth rate of the layers deposited on silicon substrates were studied as a function......, to be used in Intermediate Temperature Solid Oxide Fuel Cells. (C) 2004 Elsevier B.V. All rights reserved....

  1. Studies on the complexation of diclofenac sodium with β-cyclodextrin: Influence of method of preparation

    Das, Subhraseema; Subuddhi, Usharani

    2015-11-01

    Inclusion complexes of diclofenac sodium (DS) with β-cyclodextrin (β-CD) were prepared in order to improve the solubility, dissolution and oral bioavailability of the poorly water soluble drug. The effect of method of preparation of the DS/β-CD inclusion complexes (ICs) was investigated. The ICs were prepared by microwave irradiation and also by the conventional methods of kneading, co-precipitation and freeze drying. Though freeze drying method is usually referred to as the gold standard among all the conventional methods, its long processing time limits the utility. Microwave irradiation accomplishes the process in a very short span of time and is a more environmentally benign method. Better efficacy of the microwaved inclusion product (MW) was observed in terms of dissolution, antimicrobial activity and antibiofilm properties of the drug. Thus microwave irradiation can be utilized as an improved, time-saving and cost-effective method for the generation of DS/β-CD inclusion complexes.

  2. Advances in modern sample preparation techniques using microwaves assisted chemistry for metal species determination (W1)

    Ponard, O.F.X.

    2002-01-01

    Full text: Sample preparation has long been the bottleneck of environmental analysis for both total and species specific analysis. Digestion, extraction and preparation of the analytes are relying on a series of chemical reactions. The introduction of microwave assisted sample preparation has first been viewed as a mean to accelerate the kinetics of digestion of the matrix for total elements and fast samples preparation procedures. However, the extensive development and success of microwave digestion procedures in total elemental analysis has now allowed to have a larger insight of the perspectives offered by this technique. Microwave technologies now offer to have a precise control of the temperature and indirectly control the reaction kinetics taking place during the sample preparation procedures. Microwave assisted chemistry permits to perform simultaneously the fundamental steps required for metal species extraction and derivatization. The number of sample preparation steps used for organotin or organomercury species have been reduced to one and the total time of sample preparation brought down for a few hours to some minutes. Further, the developments of GC/ICP/MS techniques allow to routinely use speciated isotopic dilution methods has internal probe of the chemical reactions. These new approaches allow us to use the addition of the labeled species for isotopic dilution as a mean to evaluate and follow the chemical processes taking place during the extraction procedure. These procedures will help us to understand and check for the stability of the analytes during the chemistry of the sample preparation procedure and bring some insights of the chemistry taking place during the extraction. Understanding the different mechanisms involved in the sample preparation steps will allow us in return to further improve all theses procedures and bring us to the horizon of 'on-line sample preparation and detection'. (author)

  3. The complex synthesis and solid state chemistry of ceria-lanthana solid solutions prepared via a hexamethylenetetramine precipitation

    Fleming, P.G.; Holmes, J.D.; Otway, D.J.; Morris, M.A.

    2011-01-01

    Mixed oxide solid solutions are becoming ever more commercially important across a range of applications. However, their synthesis can be problematical. Here, we show that ceria-lanthana solid solutions can be readily prepared via simple precipitation using hexamethylenetetramine. However, the solution chemistry can be complex, which results in the precipitated particles having a complex structure and morphology. Great care must be taken in both the synthesis and characterisation to quantify the complexity of the product. Even very high heat treatments were not able to produce highly homogeneous materials and X-ray diffractions reveals the non-equilibrium form of particles prepared in this way. Unexpected crystal structures are revealed including a new metastable cubic La 2 O 3 phase. - Graphical abstract: The suggested mechanism for the formation of dual fluorite phase particles, where Step 1 corresponds to room temperature aging, Step 2; heating the solution to 90 deg. C, Step 3; cooling of the solution to room temperature, Step 4; calcination to 500 deg. C, Step 5; calcination to 700 deg. C and Step 6; calcination to 1300 deg. C. The terminology of e.g. La 1-x Ce x (OH) 3 is used to indicate the formation of a mixed oxy-hydroxy participate rather than a definitive assignment of stoichiometry. Similarly, La 1-y Ce y O 2 only implies a mixed solid solution. Highlights: → Mol% of prepared Ce-La oxides did not follow that of reactant mol%. → Complex reaction pathway found to be dependent on metal solution concentrations. → At certain concentrations core shell particles were found to form. → A reaction model was produced based on cationic solubility. → Report lanthana solubility higher than previously reported in CeO 2 .

  4. Nitrido-technetium(V) complexes with amino acids: Preparation and X-ray crystal structure of the L-cysteinate ethyl ester technetium(V) complex

    Marchi, A.; Rossi, R.; Marvelli, L.; Bertolasi, V.

    1993-01-01

    Technetium-99m is the radionuclide of choice in diagnostic nuclear medicine due to its ideal photon energy of 140 keV and half-life of 6 h. Neutral, stable, and lipophilic technetium complexes with diamino dithiol ligands (DADT) have been widely studied as potential brain perfusion agents and a 99m Tc complex of N,N'-1,2-ethylenediylbis(L-cysteine diethyl ester) (L,L-ECD) has been proposed as a marker of regional cerebral blood flow. It crosses the blood brain barrier (BBB) and is retained in the brain owing to enzymatic hydrolysis of one ester group yielding to a more polar species. More recently, 99m Tc-cysteine complex has been evaluated in animal distribution studies for tumor diagnosis, but its chemical structure has not been determined. A large number of transition metal complexes with amino acids and peptides have been synthesized and structurally characterized to understand their interactions with proteins and antibodies, as well as biocatalytic processes, but only a limited number of rhenium and technetium compounds have been reported. Up to now, the only technetium complex to be characterized by X-ray analysis that contains amino acids as ligand is [TcO(L,L-ECD)]. The author's interest in the nitrido-technetium chemistry is due to the discovery of a new method for preparing radiopharmaceuticals containing the [ 99m Tc triple-bond N] 2+ core. In this communication the authors report the synthesis and characterization of nitrido-technetium complexes with L-cysteine ethyl ester (CYS-OEt), L-cysteine (CYS) and cysteamine (CSA) and the first X-ray crystal structure of a [TcN] 2+ -amino acid complex

  5. Metal complexes of alkyl-aryl dithiocarbamates: Structural studies, anticancer potentials and applications as precursors for semiconductor nanocrystals

    Andrew, Fartisincha P.; Ajibade, Peter A.

    2018-03-01

    Dithiocarbamates are versatile ligands able to stabilize wide range of metal ions in their various oxidation states with the partial double bond character of Csbnd N and Csbnd S of thioureide moiety. Variation of the substituents attached to the nitrogen atom of dithiocarbamate moiety generates various intermolecular interactions, which lead to different structural arrangement in the solid state. The presence of bulky substituents on the N atom obviates the supramolecular aggregation via secondary Msbnd S interactions whereas smaller substituents encourage such aggregation that results in their wide properties and applications. Over the past decades, the synthesis and structural studies of metal complexes of dithiocarbamates have received considerable attention as potential anticancer agents with various degree of DNA binding affinity and cytotoxicity and as single molecule precursors for the preparation of semiconductor nanocrystals. In this paper, we review the synthesis, structural studies, anticancer potency and the use of alkyl-phenyl dithiocarbamate complexes as precursors for the preparation of semiconductor nanocrystals. The properties of these compounds and activities are ascribed to be due to either the dithiocarbamate moieties, the nature or type of the substituents around the dithiocarbamate backbone and the central metal ions or combination of these factors.

  6. Lanthanide Single-Molecule Magnets Framed by Alkali Metals & Magnetic and Spectroscopic Studies of 3d Transition Metal Complexes

    Konstantatos, Andreas

    -molecule magnets (SMMs). Starting from the archetype SMM Mn12 we present the details of the mechanisms governing the relaxation of the magnetization of these systems. In Chapter 2 we present our work on the coordination chemistry of lanthanides with a new Schiff-base ligand, H3L [(E)-3-((2-hydroxyphenyl...... complexes of M3+ or M2+ metal ions (M: 3d transition metal) with the preference to either approximate octahedral or trigonal prismatic coordination geometry. A detailed magnetic characterization for most of the complexes is presented where a trinuclear Co2+ cluster stands out for its pronounced SMM...

  7. Preparation Methods of Metal Organic Frameworks and Their Capture of CO2

    Zhang, Linjian; Liand, Fangqin; Luo, Liangfei

    2018-01-01

    The increasingly serious greenhouse effect makes people pay more attention to the capture and storage technology of CO2. Metal organic frameworks (MOFs) have the advantages of high specific surface area, porous structure and controllable structure, and become the research focus of CO2 emission reduction technology in recent years. In this paper, the characteristics, preparation methods and application of MOFs in the field of CO2 adsorption and separation are discussed, especially the application of flue gas environment in power plants.

  8. Synthesis and Crystal Structures of Two Metal Complexes Incorporating Malonate and Organodiamine Ligands

    Zhang, Quan Zheng; Yang, Wen Bin; Chen, Shu Mei; Lu, Can Zhong

    2005-01-01

    In the present work we report the synthesis and X-ray crystal structures of two new malonato complexes incorporating organodiamine ligands: [Ni(phen)(mal)(H_2O)_2]·3H_2O (H_2mal = malonic acid, phen = 1,10-phenanthroline) and [Zn(bpy)(H_2O)]_2[Zn(bpy)(mal)(H_2O)_2]_2(NO_3)_4·4H_2O (bpy = 2,2'-bipyridine). Investigation on novel organic-inorganic hybrid framework assemblies represents one of the most active areas of material science and chemical research. Major advances have been made in these materials due to their interesting properties and potential in various applications, e. g., electrical conductivity, magnetism, host-guest chemistry, ion exchange, catalysis, nonlinear optics, etc. Moreover, discovery and design of such new materials with specific networks remain of a particularly important and active subject in the field of supramolecuar chemistry and crystal engineering. A variety of complexes with interesting compositions and topologies have been prepared through taking certain factors into account, such as the coordination nature of the metal ion and the shape, functionality, flexibility, and symmetry of organic ligand. Recently, some dicarboxylate ligands, such as oxalate, malonate, and terephthalate, have been widely used in the construction of these interesting structures

  9. Synthesis and Biological Activities on Metal Complexes of 2,5-Diamino-1,3,4-thiadiazole Derived from Semicarbazide Hydrochloride

    Matthew A. Adebayo

    2011-07-01

    Full Text Available A bioactive ligand, 2,5-diamino-1,3,4-thiadiazole (L, derived from semicarbazide hydrochloride, and its metal complexes were prepared and characterized. The complexes were characterized using elemental, infra-red, ultraviolet/visible, magnetic moment, atomic absorption, thin layer chromatography and molar conductance measurements. The IR data revealed that the ligand (L behaved as a tridentate neutral ligand. It coordinated to the metal ion via sulphur and nitrogen of the amines. The molar conductance data reveal that the chelates are non-electrolytes. From the Ultraviolet/Visible spectra and magnetic moment data, the complexes were found to have octahedral geometrical structure. In vivo evaluation of the antimicrobial activities of the metal complexes and the ligands showed greater activity against some micro-organisms when compared to the parent compounds. The chelates do not show toxicity against the activities of enzymes from homogenates of liver, kidney and serum in experimental rats.

  10. The application of prepared porous carbon materials: Effect of different components on the heavy metal adsorption.

    Song, Min; Wei, Yuexing; Yu, Lei; Tang, Xinhong

    2016-06-01

    In this study, five typical municipal solid waste (MSW) components (tyres, cardboard, polyvinyl chloride (PVC), acrylic textile, toilet paper) were used as raw materials to prepare four kinds of MSW-based carbon materials (paperboard-based carbon materials (AC1); the tyres and paperboard-based carbon materials (AC2); the tyres, paperboard and PVC-based carbon materials (AC3); the tyres, paperboard, toilet paper, PVC and acrylic textile-based carbon materials (AC4)) by the KOH activation method. The characteristic results illustrate that the prepared carbon adsorbents exhibited a large pore volume, high surface area and sufficient oxygen functional groups. Furthermore, the application of AC1, AC2, AC3, AC4 on different heavy metal (Cu(2+), Zn(2+), Pb(2+), Cr(3+)) removals was explored to investigate their adsorption properties. The effects of reaction time, pH, temperature and adsorbent dosage on the adsorption capability of heavy metals were investigated. Comparisons of heavy metal adsorption on carbon of different components were carried out. Among the four samples, AC1 exhibits the highest adsorption capacity for Cu(2+); the highest adsorption capacities of Pb(2+) and Zn(2+) are obtained for AC2; that of Cr(3+) are obtained for AC4. In addition, the carbon materials exhibit better adsorption capability of Cu(2+) and Pb(2+) than the other two kind of metal ions (Zn(2+) and Cr(3+)). © The Author(s) 2016.

  11. Effects of complexing compounds on sorption of metal ions to cement

    Loevgren, Lars [Umeaa Univ. (Sweden). Inorganic chemistry

    2005-12-15

    This present report is a literature review addressing the effects of complexing ligands on the sorption of radionuclides to solid materials of importance for repositories of radioactive waste. Focus is put on laboratory studies of metal ion adsorption to cement in presence of chelating agents under strongly alkaline conditions. As background information, metal sorption to different mineral and cement phases in ligand free systems is described. Furthermore, surface complexation model (SCM) theories are introduced. According to surface complexation theories these interactions occur at specific binding sites at the particle/water interface. Adsorption of cationic metals is stronger at high pH, and the adsorption of anions occurs preferentially at low pH. The adsorption of ions to mineral surfaces is a result of both chemical bonding and electrostatic attraction between the ions and charged mineral surfaces. By combining uptake data with spectroscopic information the sorption can be explained on a molecular level by structurally sound surface complexation models. Most of the metal sorption studies reviewed are dealing with minerals exhibiting oxygen atoms at their surfaces, mainly oxides of Fe(II,III) and Al(III), and aluminosilicates. Investigations of radionuclides are focused on clay minerals, above all montmorillonite and illite. Which mechanism that is governing the metal ion adsorption to a given mineral is to a large extent depending on the metal adsorbed. For instance, sorption of Ni to montmorillonite can occur by formation of inner-sphere mononuclear surface complexes located at the edges of montmorillonite platelets and by formation of a Ni phyllosilicate phase parallel to montmorillonite layers. Also metal uptake to cement materials can occur by different mechanisms. Cationic metals can both be attached to cement (calcium silicate hydrate, CSH) and hardened cement paste (HCP) by formation of inner-sphere complexes at specific surface sites and by

  12. Heterobimetallic transition metal/rare earth metal bifunctional catalysis: a Cu/Sm/Schiff base complex for syn-selective catalytic asymmetric nitro-Mannich reaction.

    Handa, Shinya; Gnanadesikan, Vijay; Matsunaga, Shigeki; Shibasaki, Masakatsu

    2010-04-07

    The full details of a catalytic asymmetric syn-selective nitro-Mannich reaction promoted by heterobimetallic Cu/Sm/dinucleating Schiff base complexes are described, demonstrating the effectiveness of the heterobimetallic transition metal/rare earth metal bifunctional catalysis. The first-generation system prepared from Cu(OAc)(2)/Sm(O-iPr)(3)/Schiff base 1a = 1:1:1 with an achiral phenol additive was partially successful for achieving the syn-selective catalytic asymmetric nitro-Mannich reaction. The substrate scope and limitations of the first-generation system remained problematic. After mechanistic studies on the catalyst prepared from Sm(O-iPr)(3), we reoptimized the catalyst preparation method, and a catalyst derived from Sm(5)O(O-iPr)(13) showed broader substrate generality as well as higher reactivity and stereoselectivity compared to Sm(O-iPr)(3). The optimal system with Sm(5)O(O-iPr)(13) was applicable to various aromatic, heteroaromatic, and isomerizable aliphatic N-Boc imines, giving products in 66-99% ee and syn/anti = >20:1-13:1. Catalytic asymmetric synthesis of nemonapride is also demonstrated using the catalyst derived from Sm(5)O(O-iPr)(13).

  13. Studies on the Use of Gamma Radiation-Induced for Preparation of Some Modified Resins for the Separation of Some Metal Ions

    Abo-Zahra, S.F.

    2012-01-01

    The work carried out in the present thesis is based on preparation, characterization and applications of some modified resins such as: poly(acrylamide)/poly(maleic acid) P(AAm)/P(MA) interpolymer complex (resin), poly(acrylamide-acrylic acid-amidoxime) P(AAm-AA-AO) resin and poly(hydroxamic acid) P(HA) resin. Poly(acrylamide)/poly(maleic acid) P(AAm)/P(MA) interpolymer complex (resin) was prepared by template polymerization of maleic acid (MA) monomer on poly(acrylamide) P(AAm) hydrogel as a template polymer in the presence of N,N'-methylenebisacrylamide (NMBA) as a crosslinker using gamma radiation-induced technique. Poly(acrylamide-acrylic acid-amidoxime) P(AAm-AA-AO) resin was prepared by template polymerization of acrylic acid (AA) and acrylonitrile (AN) monomers on P(AAm) hydrogel as a template polymer in the presence of NMBA as a crosslinker using gamma radiation-induced technique. The conversion of nitrile group to amidoxime one was carried out by the treatment of the prepared resin with an alkaline solution of hydroxylamine. Poly(hydroxamic acid) P(HA) resin was prepared from the reaction of the corresponding water-soluble P(AAm) previously prepared by gamma radiation-induced with hydroxylamine hydrochloride in an alkaline medium. The functional groups on the prepared polymeric resins were confirmed by using Fourier transform infrared (FTIR) spectra. Thermogravimetric analysis (TGA), differential scanning calorimetry (DSC) measurements, scanning electron microscopy (SEM) and electron spin resonance (ESR) measurements were performed to evaluate the properties of the prepared polymeric resins, free or complexed with metal ions such as Cu 2+ metal ions.

  14. Anodic electrode position of cyanometallates as sample preparation for the determination of transition metals from water samples using X-ray fluorescence analysis

    Wundt, K.; Duschner, H.; Starke, K.

    1978-01-01

    The anodic separation of cyanometallates of propanol -2/Water mixtures at high electrical field strengths was developed as new technique for sample preparation. The optimization of the parameters of the system (high voltage applied, current density, separation time and composition of the solution) resulted in quantitative precipitation of the metallates of Fe, Co, Ni, Cu, Zn, Cd and Ag in homogeneous, thin and strong-adhering layer with mass densities of between 1 nmol cm -2 and 1 μmol cm -2 on high-purity aluminium foils. Metals not forming anionic complexes remain in solution with simualtaneous quantitative multielement separation. The described technique is part of a method to determine heavy metal traces in water samples. It comprises the nonspecific sorption on cation exchangers, the elution of the transition metals as cyanometallates, their electrode position on aluminium foil and the determination by X-ray fluorescence analysis. Model experiments illustrate the possible applications of the method. (orig.) [de

  15. Preparations, structures and properties of heterobimetallic complexes based on tetrahydrofuran-2,3,4,5-tetracarboxylate

    Jia, Tian-Jing; Li, Shu-Mu; Cao, Wei; Li, Li-Cun; Zheng, Xiang-Jun; Yuan, Da-Qiang

    2013-01-01

    Transition heterobimetallic metal-organic frameworks based on tetrahydrofuran-2,3,4,5-tetracarboxylicate (FTA), namely [M(H 2 O) 6 ][Cu 2 M(FTA) 2 (H 2 O) 2 ]·4H 2 O [M=Mn (1), Co (2)], and [CuZn(FTA)(H 2 O) 5 ]·H 2 O (3) have been synthesized and characterized. Single-crystal X-ray diffraction indicates that complexes 1 and 2 are isomorphic. In 1 and 2, FTA ligand links the metal ions to a 2-D wave-like negative-charged layer with a topology of (4;6 2 ) 2 (4;6 3 ;8 2 ) 2 (6). They possess 1-D channels with [M(H 2 O) 6 ] 2+ and lattice water molecules enclathrated. While in the complex 3, Cu 2+ and Zn 2+ ions are bridged by FTA to a 2-D neutral layer structure with a (8) 2 (8 4 ;12 2 ) topology. Magnetic properties of 1–3 were analyzed in connection with their structures, which show that there exist weak antiferromagnetic interactions between metal ions. - Graphical abstract: Three heterobimetallic MOFs were constructed through the size-selectivity of TFA coordination sites for different transition metal ions based on the concept of “Hard and Soft Acids and Bases”. Highlights: ► Complexes 1 and 3 contain 2-D wave-like negative-charged layers. ► Complex 2 is a 2-D neutral layer structure with a (8) 2 (8 4 ;12 2 ) topology. ► Complexes 1–3 are the first example of heterobimetallic MOFs based on FTA. ► The coordination sites of FTA show size-selectivity to metal ions

  16. Preparations, structures and properties of heterobimetallic complexes based on tetrahydrofuran-2,3,4,5-tetracarboxylate

    Jia, Tian-Jing; Li, Shu-Mu; Cao, Wei [College of Chemistry, Beijing Normal University, Beijing 100875 (China); Li, Li-Cun [College of Chemistry, Nankai University, Tianjin 300071 (China); Zheng, Xiang-Jun, E-mail: xjzheng@bnu.edu.cn [College of Chemistry, Beijing Normal University, Beijing 100875 (China); Yuan, Da-Qiang [State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou, Fujian 350002 (China)

    2013-05-01

    Transition heterobimetallic metal-organic frameworks based on tetrahydrofuran-2,3,4,5-tetracarboxylicate (FTA), namely [M(H₂O)₆][Cu₂M(FTA)₂(H₂O)₂]·4H₂O [M=Mn (1), Co (2)], and [CuZn(FTA)(H₂O)₅]·H₂O (3) have been synthesized and characterized. Single-crystal X-ray diffraction indicates that complexes 1 and 2 are isomorphic. In 1 and 2, FTA ligand links the metal ions to a 2-D wave-like negative-charged layer with a topology of (4;6²)₂(4;6³;8²)₂(6). They possess 1-D channels with [M(H₂O)₆]²⁺ and lattice water molecules enclathrated. While in the complex 3, Cu²⁺ and Zn²⁺ ions are bridged by FTA to a 2-D neutral layer structure with a (8)₂(8⁴;12²) topology. Magnetic properties of 1–3 were analyzed in connection with their structures, which show that there exist weak antiferromagnetic interactions between metal ions. - Graphical abstract: Three heterobimetallic MOFs were constructed through the size-selectivity of TFA coordination sites for different transition metal ions based on the concept of “Hard and Soft Acids and Bases”. Highlights: • Complexes 1 and 3 contain 2-D wave-like negative-charged layers. • Complex 2 is a 2-D neutral layer structure with a (8)₂(8⁴;12²) topology. • Complexes 1–3 are the first example of heterobimetallic MOFs based on FTA. • The coordination sites of FTA show size-selectivity to metal ions.

  17. Preparation of low valent technetium metal-metal bonded species via solvothermal reduction of pertechnetate salts

    Kerlin, W.M.; Poineau, F.; Forster, P.M.; Czerwinski, K.R.; Sattelberger, A.P.

    2013-01-01

    A new one-step solvothermal synthesis route for reduction of pertechnetate salts to low valent technetium metal-metal bonded dimers will be presented. The reaction of potassium pertechnetate with glacial acetic acid plus either halo acids or halo salts under in-situ hydrogen production by sodium borohydride at various temperatures yields multiple products consisting of tetraacetate Tc-Tc (II,III) and Tc-Tc (III,III) paddle wheel dimers. Solid products isolated and analyzed via Single Crystal X-ray Diffraction (SC-XRD) in these reactions consist of polymeric chains Tc 2 +5 core: Tc 2 (μ-O 2 CCH 3 ) 4 (O 2 CCH 3 ), Tc 2 (μ-O 2 CCH 3 ) 4 Cl, Tc 2 (μ-O 2 CCH 3 ) 4 Br, Tc 2 (μ-O 2 CCH 3 ) 4 I, molecular Tc 2 +5 core: Tc 2 (μ-O 2 CCH 3 ) 3 Cl 2 (H 2 O) 2 ·H 2 O, K[Tc 2 (μ-O 2 CCH 3 ) 4 Br 2 ], and molecular Tc 2 +6 core: Tc 2 (μ-O 2 CCH 3 ) 4 Cl 2 , Tc 2 (μ-O 2 CCH 3 ) 4 Br 2 . Of the compounds listed, four are newly discovered using the one-step technique and two more additions to crystal database. Additional spectroscopic (X-ray Absorbance Fine Structure, UV-Vis, and FT-IR) characterization of the new compounds will be shown and used to propose a mechanism. Analysis of the mother liquor of each reaction by UV-Vis and formation of crystals over time due to oxidation of solutions affords a possible insight into mechanism of the Tc 2 +5 to Tc 2 +6 core formation. The oxidation states of Tc-Tc dimers formed is also dependent on temperature and pH of the starting solutions and will be explained in extensive detail. These one step reactions of reducing Tc(VII) to low valent technetium provides high yield intermediates for potential waste forms, use in nuclear fuel cycle separations, and radiopharmaceuticals. (author)

  18. Reactions of transition metal complexes with cyclic ethers

    Milstein, D.

    1977-02-01

    Three novel reactions of epoxides with homogeneous transition-metal catalysts have been explored: (a) the selective rearrangement of internal epoxides to ketones; (b) the cleavage of C-C bond in epoxides having electron-attracting substituents; (c) the transformation of terminal epoxides into esters. Based on an intensive kinetic study, a general mechanism for the transformations of epoxides is postulated

  19. Biological activities of some Fluoroquinolones-metal complexes

    McRoy

    Background: Metal ions play a vital role in the design of more biologically active drugs. Aim: The paper reviewed the .... 2H2O by direct reaction of copper(II) sulphate pentahydrate with ciprofloxacin in distilled water. ... membered ring and the chloride ion completes the seven coordination around the Ca2+ion.[37-39].

  20. Theoretical NMR spectroscopy of N-heterocyclic carbenes and their metal complexes

    Falivene, Laura; Cavallo, Luigi

    2016-01-01

    Recent theoretical analysis of the NMR properties of free N-heterocyclic carbenes (NHC) and Metal-NHC complexes has complemented experiments, allowing the establishment of structure/property relationships and the rationalization of otherwise

  1. Basic deuteroexchange in complexes of transition metals with nitrogen-containing aromatic heterocycles

    Tupitsyn, I.F.

    1986-01-01

    A study was made of the kinetics of deuteroexchange in the methyl group in complexes of one metal [nickel(II)] with different methyl-substituted aromatic heterocycles and in isostructural complexes of one ligand (2-methylquinoline) with different central metal atoms (Mn 2+ , Ni 2+ , Cu 2+ , Zn 2+ ). The order in which the structures of the ligands influence the rate of deuteroexchange in the complexes does not correspond qualitatively with the order of increase in the rate of deuteroexchange in the noncoordinated ligands. The rate of deuteroexchange is only weakly influenced by change in the identity of the metal complex former. A deuteroexchange mechanism is proposed and discussed. A structure arising in the course of the exchange process with transfer of electron density from the heterocyclic ligand to the metal ion forms the transition state of the reaction

  2. Basic deuteroexchange in transition metal complexes with nitrogen-containing aromatic heterocycles

    Tupitsyn, I.F.

    1986-01-01

    Kinetics of deuteroexchange in the methyl group of nitrate complexes of a metal - nickel (2) - with different methyl-substituted aromatic heterocycles and isostructural complexes of a ligand - 2 - methyl quinoline - with different central metal atoms (Mn(2), Ni(2), Cu(2), Zn(2)) is studied. Series for influence of ligand structure on deuteroexchange rate in complexes doesn't correspond qualitatively to series for deuteroexchange rate increase in noncoordinated ligands. Deuteroexchange rate is weakly subjected to influence of exchange in metal-complexing agent. Deuteroexchange mechanism is suggested and discussed. According to this mechanism the structure developed in the course of the exchange process with electron density transfer from the heterocyclic ligand to a metal ion is a transition state of the reaction

  3. Multiheteromacrocycles that complex metal ions. Third progress report, 1 May 1976--30 April 1977

    Cram, D.J.

    1977-01-01

    The overall objective of this research is to design, synthesize and evaluate cyclic and polycyclic host organic compounds for their abilities to complex and lipophilize guest metal ions, their complexes and clusters. Host organic compounds consist of strategically placed solvating, coordinating and ion-pairing sites tied together by covalent bonds through hydrocarbon units around cavities shaped to be occupied by guest metal ions, or metal ions plus their ligands. Specificity in complexation is sought by matching the following properties of host and guest: cavity and metal ion sizes; geometric arrangements of binding sites; numbers of binding sites; characters of binding sites; and valences. The specific compounds synthesized and their complexing and lipophilizing properties are summarized

  4. Density functional study of isoguanine tetrad and pentad sandwich complexes with alkali metal ions.

    Meyer, Michael; Steinke, Thomas; Sühnel, Jürgen

    2007-02-01

    Isoguanine tetraplexes and pentaplexes contain two or more stacked polyads with intercalating metal ions. We report here the results of a density functional study of sandwiched isoguanine tetrad and pentad complexes consisting of two polyads with Na(+), K(+) and Rb(+) ions at the B3LYP level. In comparison to single polyad metal ion complexes, there is a trend towards increased non-planarity of the polyads in the sandwich complexes. In general, the pentad sandwiches have relatively planar polyad structures, whereas the tetrad complexes contain highly non-planar polyad building blocks. As in other sandwich complexes and in metal ion complexes with single polyads, the metal ion-base interaction energy plays an essential role. In iG sandwich structures, this interaction energy is slightly larger than in the corresponding guanine sandwich complexes. Because the base-base interaction energy is even more increased in passing from guanine to isoguanine, the isoguanine sandwiches are thus far the only examples where the base-base interaction energy is larger than the base-metal ion interaction energy. Stacking interactions have been studied in smaller models consisting of two bases, retaining the geometry from the complete complex structures. From the data obtained at the B3LYP and BH&H levels and with Møller-Plesset perturbation theory, one can conclude that the B3LYP method overestimates the repulsion in stacked base dimers. For the complexes studied in this work, this is only of minor importance because the direct inter-tetrad or inter-pentad interaction is supplemented by a strong metal ion-base interaction. Using a microsolvation model, the metal ion preference K(+) approximately Rb(+) > Na(+) is found for tetrad complexes. On the other hand, for pentads the ordering is Rb(+) > K(+) > Na(+). In the latter case experimental data are available that agree with this prediction.

  5. Preparation of complexes of zirconium and hafnium tetrachlorides with phosphorus oxychloride

    McLaughlin, D.F.

    1989-01-01

    This patent describes an improvement in a method for separating hafnium tetrachloride from zirconium tetrachloride where a complex of zirconium-hafnium tetrachlorides and phosphorus oxychloride is prepared from zirconium-hafnium tetrachlorides and the complex of zirconium-hafnium tetrachlorides and phosphorus oxychloride is introduced into a distillation column, which distillation column has a reboiler connected at the bottom and a reflux condenser connected at the top and where a hafnium tetrachloride enriched stream is taken from the top of the column and a zirconium enriched tetrachloride stream is taken from the bottom of the column. The improvement comprising: prepurifying the zirconium-hafnium tetrachlorides, prior to preparation of the complex and introduction of the complex into a distillation column, to substantially eliminate iron chloride from the zirconium hafnium tetrachlorides, whereby buildup or iron chloride in the distillation column and in the reboiler is substantially eliminated and the column can be operated in a continuous, stable and efficient manner

  6. Preparation, characterization, and thermal stability of β-cyclodextrin/soybean lecithin inclusion complex.

    Wang, Xinge; Luo, Zhigang; Xiao, Zhigang

    2014-01-30

    β-Cyclodextrin (β-CD), which is widely used to increase the stability, solubility, and bioavailability of guests, can form host-guest inclusion complexes with a wide variety of organic molecules. In this study the β-CD/soybean lecithin inclusion complex was prepared. The effect of reaction parameters such as reaction temperature, reaction time and the molar ratio of β-CD/soybean lecithin on inclusion ratio were studied. The inclusion ratio of the product prepared under the optimal conditions of β-CD/soybean lecithin molar ratio 2:1, reaction temperature 60°C reaction time 2h was 40.2%. The results of UV-vis, DSC, XRD and FT-IR spectrum indicated the formation of inclusion complex. The thermal stability experiment indicated that the thermal stability of soybean lecithin in inclusion complex was significantly improved compared with free soybean lecithin. Copyright © 2013 Elsevier Ltd. All rights reserved.

  7. Insights into aquatic toxicities of the antibiotics oxytetracycline and ciprofloxacin in the presence of metal: Complexation versus mixture

    Zhang Yu; Cai Xiyun; Lang Xianming; Qiao Xianliang; Li Xuehua; Chen Jingwen

    2012-01-01

    Co-contamination of ligand-like antibiotics (e.g., tetracyclines and quinolones) and heavy metals prevails in the environment, and thus the complexation between them is involved in environmental risks of antibiotics. To understand toxicological significance of the complex, effects of metal coordination on antibiotics' toxicity were investigated. The complexation of two antibiotics, oxytetracycline and ciprofloxacin, with three heavy metals, copper, zinc, and cadmium, was verified by spectroscopic techniques. The antibiotics bound metals via multiple coordination sites and rendered a mixture of various complexation speciations. Toxicity analysis indicated that metal coordination did modify the toxicity of the antibiotics and that antibiotic, metal, and their complex acted primarily as concentration addition. Comparison of EC 50 values revealed that the complex commonly was highest toxic and predominately correlated in toxicity to the mixture. Finally, environmental scenario analysis demonstrated that ignoring complexation would improperly classify environmental risks of the antibiotics. - Highlights: ► The complex of antibiotic with metal is a mixture of various complexation modes. ► Antibiotic and metal act as various combined interactions when their complexation is ignored. ► Antibiotic, metal, and their complex act as concentration addition interaction. ► Complex commonly is the highest toxicant. ► Neglecting complexation renders improper classification of risks for antibiotics. - Antibiotic, heavy metal and their complex act primarily as concentration addition interaction and the complex commonly is highest toxic.

  8. Insights into aquatic toxicities of the antibiotics oxytetracycline and ciprofloxacin in the presence of metal: Complexation versus mixture

    Yu, Zhang [Key Laboratory of Industrial Ecology and Environmental Engineering (Ministry of Education), School of Environmental Science and Technology, Dalian University of Technology, Dalian 116024 (China); Cai Xiyun, E-mail: xiyuncai@dlut.edu.cn [Key Laboratory of Industrial Ecology and Environmental Engineering (Ministry of Education), School of Environmental Science and Technology, Dalian University of Technology, Dalian 116024 (China); Xianming, Lang [Liaoning Academy of Environmental Sciences, Shenyang 110031 (China); Xianliang, Qiao; Xuehua, Li; Jingwen, Chen [Key Laboratory of Industrial Ecology and Environmental Engineering (Ministry of Education), School of Environmental Science and Technology, Dalian University of Technology, Dalian 116024 (China)

    2012-07-15

    Co-contamination of ligand-like antibiotics (e.g., tetracyclines and quinolones) and heavy metals prevails in the environment, and thus the complexation between them is involved in environmental risks of antibiotics. To understand toxicological significance of the complex, effects of metal coordination on antibiotics' toxicity were investigated. The complexation of two antibiotics, oxytetracycline and ciprofloxacin, with three heavy metals, copper, zinc, and cadmium, was verified by spectroscopic techniques. The antibiotics bound metals via multiple coordination sites and rendered a mixture of various complexation speciations. Toxicity analysis indicated that metal coordination did modify the toxicity of the antibiotics and that antibiotic, metal, and their complex acted primarily as concentration addition. Comparison of EC{sub 50} values revealed that the complex commonly was highest toxic and predominately correlated in toxicity to the mixture. Finally, environmental scenario analysis demonstrated that ignoring complexation would improperly classify environmental risks of the antibiotics. - Highlights: Black-Right-Pointing-Pointer The complex of antibiotic with metal is a mixture of various complexation modes. Black-Right-Pointing-Pointer Antibiotic and metal act as various combined interactions when their complexation is ignored. Black-Right-Pointing-Pointer Antibiotic, metal, and their complex act as concentration addition interaction. Black-Right-Pointing-Pointer Complex commonly is the highest toxicant. Black-Right-Pointing-Pointer Neglecting complexation renders improper classification of risks for antibiotics. - Antibiotic, heavy metal and their complex act primarily as concentration addition interaction and the complex commonly is highest toxic.

  9. Shrinking the Synchrotron : Tabletop Extreme Ultraviolet Absorption of Transition-Metal Complexes

    Zhang, Kaili; Lin, Ming Fu; Ryland, Elizabeth S.; Verkamp, Max A.; Benke, Kristin; De Groot, Frank M F; Girolami, Gregory S.; Vura-Weis, Josh

    2016-01-01

    We show that the electronic structure of molecular first-row transition-metal complexes can be reliably measured using tabletop high-harmonic XANES at the metal M2,3 edge. Extreme ultraviolet photons in the 50-70 eV energy range probe 3p → 3d transitions, with the same selection rules as soft X-ray

  10. Study of the competitive reaction ability of harmine and harmaline during complex formation with transition metals

    Chepulsky, S.A.; Kadirova, Z.Ch.; Parpiev, N.A.

    2006-01-01

    New coordination compounds of d-metals (Zn(II), Co(II), Mn(II), Mo(VI), Cr(VI)) β-carboline alkaloids were synthesized. The structure of obtained substances was established by IR, PMR spectroscopy. The quantum-chemical assessment of the harmine and harmaline reactivity in complexation reactions with d-metals was carried out. (author)

  11. Difficulties in preparing a standard sample of uranium metal having traces of nitrogen

    Toteja, R.S.D.; Jangida, B.L.; Sundaresan, M.

    1991-01-01

    Normally in the analysis of uranium for nitrogen, the nitrides are hydrolysed to give NH 3 and that for standardisation purposes to approximate the closest conditions of analysis of ammonia, NH 4 Cl is added to the sample and the recovery is tested. An appropriate method will be to have a standard sample of uranium with known amounts of nitrogen to be used as reference sample. The present work describes the efforts made in the preparation of such a reference sample and a general assessment of such methods available. In present work, known microamounts of nitrogen in an enclosed volume were allowed to react at a temperature of 773 K with a fixed amount of uranium metal of nitrogen content determined chemically. As the reaction of nitrogen with uranium is essentially a surface reaction, a sample had to be homogenised by allowing the nitrided sample to melt at about 1500 K and allow the nitrogen to diffuse through so that the concentration gradient along the profile will disappear. Attempts were made to prepare such samples in the range to 40 to 100 ppm of nitrogen. The density differences of uranium nitride and uranium metal made this diffusion and homogenisation process difficult. The prepared samples were analysed by the micro-kjeldahl's method and the recoveries tested. The equipment used for the preparation of the nitrided samples, for homogenisation and analysis of the results obtained are detailed in the paper together with the assessment of the general methods. (author). 2 refs., 1 fig., 1 tab

  12. Proton magnetic resonance spectra of metal ammine complexes, 8

    Taura, Toshiaki; Sakaguchi, Ushio; Yoneda, Hayami

    1976-01-01

    The rates of amine hydrogen isotopic exchange in the [Co(O) 2 (N) 4 ] + complex ions, where (O) 2 represents carbonate, oxalate, or malonate ions, and (N) 4 , tetraamine, bis(ethylenediamine), or bis(trimethylenediamine), were measured in D 2 O at 35 0 C by the PMR technique. It was found that: (1) the rates for trans (to oxygen) amines are faster than those for cis amines; (2) the rates, especially for trans amines, in the carbonato complexes are slower than those in the oxalato and malonato analogs, and (3) the difference between the rates for cis and trans amines is smaller in the bis(diamine) complexes than in the tetraammine complexes. These results are discussed in terms of the influence of the chelate geometry in the complex on the exchange reaction. (auth.)

  13. Preparation and characterization of complexes of RE3+ with furfural modified water-soluble chitosan

    WANG Maoyuan; QIU Ligan; MA Guilin

    2008-01-01

    Degraded chitosan, with highly water-solubility, was obtained by the oxidation of chitosan with H2O2, and then reacted with furfural The final product coordinated with the rare earth ions (RE3+ = Sm3+,Eu3+), which led to the formation of the complexes. The prepared complexes were characterized with Inflated Spectroscopy (IR), Ultra Violet (UV), fluorescence, X-Ray Diffraction (XRD), and Thermogravimetric-Differential Scanning Calorimetry (TG-DSC) measurements.

  14. Modulation of solubility and dissolution of furosemide by preparation of phospholipid complex

    Mona Semalty; Prateeksha Badoni; Devendra Singh; Ajay Semalty

    2014-01-01

    Aim: The aim of this study is to improve the solubility and dissolution of furosemide (a potent high ceiling diuretic used for the treatment of hypertension and a Class IV drug that is low solubility and low permeability drug as per the Biopharmaceutical Classification System) by preparing its phospholipid complexes or pharmacosomes. Materials and Methods: Furosemide was complexed with phosphatidylcholine in four different molar ratios (1:1, 1:2, 1:3 and 1:4) by conventional solvent-evaporati...

  15. Effects of preparation method and active metal content on of Ni/kieselguhr catalyst activity

    Galuh Widiyarti; Wuryaningsih Sri Rahayu

    2010-01-01

    The preparation and the active metal content influence the activity of catalyst. Study has been conducted to see the activity of Ni/kieselguhr based on preparation method and Nickel (Ni) contents in the catalyst in the laboratory scale. The Ni/kieselguhr catalyst were prepared by impregnation and precipitation methods, with Ni active contents of 10, 20, and 30 % by weight. The catalysts characterization was analyzed using X-Ray Diffraction (XRD). Catalysts activities were analyzed based on decreasing of iodine number from hydrogenation of crude palm oil for 2 hours. The activity tests results show that precipitation catalysts are more active than impregnation catalysts. The decreasing in iodine number of fatty acid after 2 hours of hydrogenation process using precipitation catalysts and impregnation catalysts are 51.53 and 21.85 %, respectively. In addition, the catalysts are more active with increasing Ni contents. (author)

  16. Preparation of Metallic and Polymer Nanoparticles, Responsive Nanogels and Nanofibers by Radiation Initiated Reactions

    Lee, K. -Pill; Gopalan, A. I. [Department of Chemistry Education, Kyungpook National University (Korea, Republic of)

    2009-07-01

    Synthesis of nanomaterials have become the focus of intensive research due to their numerous applications in diverse fields such as electronics, optics, ceramics, metallurgy, pulp and paper, environmental, pharmaceutics, biotechnology and biomedical fields. Due to expanding demand for the nanomaterials with defined properties, extensive research activities have been focused on the synthesis and characterization of “functional nanomaterials”. Our research group launched into research activities on the preparation of varieties of functional materials using radiation as the source for inducing functionalities ino these new nanomaterials. Importantly, we kept final goals for specific applications. Thus, we have prepared few interesting functional nanomaterials such as metal nanoparticles decorated multi wall carbon nanotubes, pore filled functional electrospun nanofibers and nanocables based on conducting polymer and carbon nanotubes and demonstrated their applications toward electrocatalysts, polymer electrolyte in energy devices and biosensors. In the forthcoming sections, a brief outline on the use of radiation for the preparation of those functional nanomaterials are presented. (author)

  17. Wear Behavior of Aluminium Metal Matrix Composite Prepared from Industrial Waste

    L. Francis Xavier

    2016-01-01

    Full Text Available With an increase in the population and industrialization, a lot of valuable natural resources are depleted to prepare and manufacture products. However industrialization on the other hand has waste disposal issues, causing dust and environmental pollution. In this work, Aluminium Metal Matrix Composite is prepared by reinforcing 10 wt% and 20 wt% of wet grinder stone dust particles an industrial waste obtained during processing of quarry rocks which are available in nature. In the composite materials design wear is a very important criterion requiring consideration which ensures the materials reliability in applications where they come in contact with the environment and other surfaces. Dry sliding wear test was carried out using pin-on-disc apparatus on the prepared composites. The results reveal that increasing the reinforcement content from 10 wt% to 20 wt% increases the resistance to wear rate.

  18. Chiral phosphites as ligands in asymmetric metal complex catalysis and synthesis of coordination compounds

    Gavrilov, Konstantin N; Bondarev, Oleg G; Polosukhin, Aleksei I

    2004-01-01

    The data published during the last five years on the application of chiral derivatives of phosphorous acid in coordination chemistry and enantioselective catalysis are summarised and discussed. The effect of the nature of these ligands on the structure of metal complexes and on the efficiency of catalytic organic syntheses is shown. Hydroformylation, hydrogenation, allylic substitution and conjugate addition catalysed by transition metal complexes with optically active phosphites and hydrophosphoranes are considered. The prospects for the development of this field of research are demonstrated.

  19. Synthesis, physico-chemical characterization and biological activity of 2-aminobenzimidazole complexes with different metal ions

    Podunavac-Kuzmanović Sanja O.

    2004-01-01

    Full Text Available Complexes of 2-aminobenzimidazole (L with nitrates of cobalt(II nickel(II, copper (II, zinc(II and silver(I were synthesized. The molar ratio metal:ligand in the reaction of the complex formation was 1:2. It should be noticed, that the reaction of all the metal salts yielded bis(ligand complexes of the general formula M(L2(NO32 × nH2O (M=Co, Ni Cu, Zn or Ag; n=0, 1, 2 or 6. The complexes were characterized by elemental analysis of the metal, molar conductivity, magnetic susceptibility measurements and IR spectra. Co(II, Ni(II and Cu(II complexes behave as non-electrolytes, whilst Zn(II and Ag(I are 1:1 electrolytes. Cu(II complex has a square-planar stereochemistry, Ag(I complex is linear, whilst the Co(II, Ni(II and Zn(II complexes have a tetrahedral configuration. In all the complexes ligand is coordinated by participation of the pyridine nitrogen of the benzimidazole ring. The antimicrobial activity of the ligand and its complexes against Pseudomonas aeruginosa, Bacillus sp. Staphylococcus aureus and Saccharomyces cerevisiae was investigated. The effect of metal on the ligand antimicrobial activity is discussed.

  20. High density crystalline boron prepared by hot isostatic pressing in refractory metal containers

    Hoenig, C.L.

    1993-08-31

    Boron powder is hot isostatically pressed in a refractory metal container to produce a solid boron monolith with a bulk density at least 2.22 g/cc and up to or greater than 2.34 g/cc. The refractory metal container is formed of tantalum, niobium, tungsten, molybdenum or alloys thereof in the form of a canister or alternatively plasma sprayed or chemical vapor deposited onto a powder compact. Hot isostatic pressing at 1,800 C and 30 PSI (206.8 MPa) argon pressure for four hours produces a bulk density of 2.34 g/cc. Complex shapes can be made.

  1. 3d/4f Metal Complexes of Phenolic Oximes New Binding Sites on Anderson Polyoxometalates Metal Complexes of the New THAME Ligand

    Sethi, Waqas

    to be coordinatedto SMMs as well as onto other transition metal complexes, via different synthetic strategies. These synthetic routes did not result in the crystallisation of any new compounds. A new hexadentate ligand tris(((2-hydroxyethyl)-amino)methyl)ethane (THAME) was synthesised and characterised. THAME...

  2. The acidic complexation of tetracycline with sucralfate for its mucoadhesive preparation.

    Higo, Shoichi; Takeuchi, Hirofumi; Yamamoto, Hiromitsu; Hino, Tomoaki; Kawashima, Yoshiaki

    2004-08-01

    The complex of antibiotics with sucralfate (SF) was prepared with acid. The mechanism of the complexation and some factors concerning the preparation, which influence the mucoadhering property, were studied. The complexation was confirmed by the change in color and instrumental analysis. The acidic complex appeared to be produced by reagglomeration of SF preliminary particles. It was suggested that the amide or amine groups of tetracycline (TC) and aluminum moieties of SF serve as the binding sites. The potential of multiple binding sites and a priority in them were suggested by the Scatchard plot analysis. The additional amounts of acid and the increase in the surface area increased the number of sites. The amount of the additional acid appeared to be the most important factor during the preparation of the acidic complex. The appropriate amount of acid added appeared to produce a complex rich in TC. However, an excess amount might cause the excess dissociation of aluminum moieties, which destroys the mucoadhesive paste-forming property.

  3. Synthesis, Characterization and Spectral Studies of Noble Heterobinuclear Complexes of Transition Metal Ions and their Biological Activity

    Netra Pal Singh

    2011-01-01

    Full Text Available Some noble heterobinuclear complexes of transition metal ions with bis(salicylaldehydemalonyl-dihydrazone in the presence of 5-nitroindazole Cu(II / Ni(II- chloride of the type [ML1M‘L2Cl2] or [ML1FeL2Cl2]Cl, where M = Ni(II, Cu(II and M' = Mn(II, Co(II, have been prepared. All the complexes have been characterized by IR, UV vis and EPR spectroscopy, elemental analysis, magnetic moment and molar conductance measurement. Spectral studies and magnetic moment measurement in DMF suggest the covalent nature of the complexes, except the [ML1FeL2Cl2]Cl complex which is 1:1 electrolyte. An octahedral geometry is proposed for M‘ and square planer for M for the heterobinuclear complexes. The low value of magnetic moment and overlapping EPR signals are due to spin crossover since both of the metals have unpaired electrons with same molecular symmetry. The lowering of the magnetic moment has been discussed. The biological activity (antifungal and antibacterial of the represented compounds has been studied.

  4. Preparation of Conductive Organometallic Complexes and Their Pastes or Inks Using the Electron Beam Apparatus

    Gu, Ja Min; Lee, Hyosun; Lee, Byung Cheol; Park, Ji Hyun

    2011-01-01

    We have synthesized the silver and copper complexes using the ligands, amine derivatives Ν-methylhydantoin amine, Ν-triethanol amine, the copper complexes are prepared depending on the equivalents of starting materials, however the silver complexes failed. In case of terephthalic acid, glutaric acid, we have synthesized silver and copper complexes successfully. We have measured conductivity of silver and copper complexes paste and ink themselves by thermal reduction using PULSE UV method. A couple of synthesized copper complex's paste have shown some resistance which is not enough for the conductive materials. Commercially silver pastes composed of silver oxide and silver salt of carboxylic acid, applied to the printed transistor circuits with suitable process, i. e. thermal reduction. This process substituted for electron beam brings a simplification of process, economical, environmental friendly process and a development of in the application of flexible substrate

  5. Studies on unusually reactive metal powders. Preparation of new organometallic and organic compounds including potential new catalysts. Final report, July 1, 1980-December 31, 1984

    Rieke, R.D.

    1985-06-01

    This research project was involved with the preparation and study of highly reactive metal powders prepared by the reduction of metal salts with alkali metals. Studies concentrated on nickel, copper, cadmium, uranium, iron, and magnesium. The nickel powders have been found to react rapidly with benzylic halides, and the resulting organonickel complexes yield dibenzyl. Aryl halides react rapidly with the nickel powders to produce biaryl compounds in high yields. Benzylic halides react with the nickel powders in the presence of acylhalides to produce benzyl ketones in high yields. Reactions of ROCOCOC1 and benzylic halides with nickel powders yield benzyl ketones. These reactions proceed with a wide variety of substituents on the phenyl ring of the benzylic halides. Highly reactive uranium has been prepared, and found to react with a variety of oxygen containing substrates, such as nitrobenzene to yield azo benzene. Highly reactive magnesium has opened up a totally new area of low temperature Grignard chemistry. The preparation of highly reactive copper has allowed the direct preparation of organocopper species directly from organic halides. 16 refs., 6 tabs

  6. Near-infrared dichroism of a mesogenic transition metal complex and its solubility in nematic hosts

    Marshall, K.L.; Jacobs, S.D.

    1987-01-01

    A transition metal complex possessing the nematic phase, bis (p-n-butylstyryl-1, 2-dithiolato) nickel, was synthesized and its optical properties and solubility in the nematic hosts K15 and MBBA were investigated. The metal complex displayed a high solubility in both host materials (up to 10% wt/wt) and a strong near-infrared absorption band centered at 860 nm. A blocking extinction of greater than OD = 3 was obtained with a 100 micron pathlength of a 0.5% wt/wt mixture of the nematic metal complex in K15, suggesting its usefulness for passive blocking of near infrared radiation. A 24 micron thick, homogeneously aligned guest-host cell containing a 1% wt/wt mixture of the metal complex in K15 possessed a contrast ratio of nearly 5:1 and a blocking extinction of OD = 3.5 at 860 nm, demonstrating for the first time the existence of near-infrared dichroism in this class of materials. The solubility and blocking extinction of the mesogenic metal complex in K15 was considerably superior to the non-mesogenic near ir laser dye bis(dimethylaminodithiobenzil) nickel in the same host. An interaction of the nematic metal complex in mixtures with MBBA which resulted in the creation of a new absorption band at 1050 nm was also observed. 21 refs., 9 figs

  7. Using metal complex-labeled peptides for charge transfer-based biosensing with semiconductor quantum dots

    Medintz, Igor L.; Pons, Thomas; Trammell, Scott A.; Blanco-Canosa, Juan B.; Dawson, Philip E.; Mattoussi, Hedi

    2009-02-01

    Luminescent colloidal semiconductor quantum dots (QDs) have unique optical and photonic properties and are highly sensitive to charge transfer in their surrounding environment. In this study we used synthetic peptides as physical bridges between CdSe-ZnS core-shell QDs and some of the most common redox-active metal complexes to understand the charge transfer interactions between the metal complexes and QDs. We found that QD emission underwent quenching that was highly dependent on the choice of metal complex used. We also found that quenching traces the valence or number of metal complexes brought into close proximity of the nanocrystal surface. Monitoring of the QD absorption bleaching in the presence of the metal complex provided insight into the charge transfer mechanism. The data suggest that two distinct charge transfer mechanisms can take place. One directly to the QD core states for neutral capping ligands and a second to surface states for negatively charged capping ligands. A basic understanding of the proximity driven charge-transfer and quenching interactions allowed us to construct proteolytic enzyme sensing assemblies with the QD-peptide-metal complex conjugates.

  8. Dissolution of Fe(III) (hydr) oxides by metal-EDTA complexes

    Ngwack, Bernd; Sigg, Laura

    1997-03-01

    The dissolution of Fe(III)(hydr)oxides (goethite and hydrous ferric oxide) by metal-EDTA complexes occurs by ligand-promoted dissolution. The process is initiated by the adsorption of metal-EDTA complexes to the surface and is followed by the dissociation of the complex at the surface and the release of Fe(III)EDTA into solution. The dissolution rate is decreased to a great extent if EDTA is complexed by metals in comparison to the uncomplexed EDTA. The rate decreases in the order EDTA CaEDTA ≫ PbEDTA > ZnEDTA > CuEDTA > Co(II)EDTA > NiEDTA. Two different rate-limiting steps determine the dissolution process: (1) detachment of Fe(III) from the oxide-structure and (2) dissociation of the metal-EDTA complexes. In the case of goethite, step 1 is slower than step 2 and the dissolution rates by various metals are similar. In the case of hydrous ferric oxide, step 2 is rate-limiting and the effect of the complexed metal is very pronounced.

  9. ESR investigation of alkali metal complexes of galvinoxyl-labeled benzo-15-crown-5 in frozen solution

    Mukai, Kazuo; Iida, Nobuhito; Ishizu, Kazuhiko

    1982-01-01

    A stable galvinoxyl derivative (1) of benzo-15-crown-5 was prepared and the complex formation between the spin labeled crown ether 1 and the alkali metal and ammonium salts was studied by the ESR technique. Existence of the (2:1) complex of 1 with potassium, rubidium, and ammonium salts was confirmed by the observation of the triplet ESR spectra in ethanol rigid matrix at 77K. Essentially the same g- and D-tensor values are observed for all the (2:1) complexes, indicating similar conformation of the ligand mole cule 1. The zero-field splitting parameters (D and E) are calculated on the basis of the spin distribution of 1 and the assumed molecular structures for the (2:1) complex. By comparing the observed D and E parameters with the calculated ones, the structure of the (2:1) complex in ethanol rigid matrix is discussed. On the other hand, the sodium complexes of 1 show a slightly asymmetric single line, suggesting the (1:1) complex formation btween 1 and the sodium salts. No anions (SCN - , Br - , and I - ) have any appreciable effect on the ESR spectra of both the (2:1) and (1:1) complexes. (author)

  10. Removal of some metal ions by activated carbon prepared from Phaseolus aureus hulls.

    Rao, M Madhava; Ramana, D K; Seshaiah, K; Wang, M C; Chien, S W Chang

    2009-07-30

    Removal of lead [Pb(II)], zinc [Zn(II)], copper [Cu(II)], and cadmium [Cd(II)] from aqueous solutions using activated carbon prepared from Phaseolus aureus hulls (ACPAH), an agricultural waste was studied. The influence of various parameters such as effect of pH, contact time, adsorbent dose, and initial concentration of metal ions on the removal was evaluated by batch method. The removal of metal ions by ACPAH was pH dependent and the optimum pH values were 7.0, 8.0, 7.0 and 6.0 for Cu(II), Cd(II), Zn(II), and Pb(II), respectively. The sorption isotherms were studied using Langmuir, Freundlich, Dubinin-Radushkevich (D-R), and Temkin isotherm models. The maximum adsorption capacity values of ACPAH for metal ions were 21.8 mg g(-1) for Pb(II), 21.2 mg g(-1) for Zn(II), 19.5 mg g(-1) for Cu(II), and 15.7 mg g(-1) for Cd(II). The experiments demonstrated that the removal of metal ions followed the pseudo-second-order kinetic model. Desorption experiments were carried out using HCl solution with a view to regenerate the spent adsorbent and to recover the adsorbed metal ions.

  11. Removal of some metal ions by activated carbon prepared from Phaseolus aureus hulls

    Rao, M. Madhava; Ramana, D.K.; Seshaiah, K.; Wang, M.C.; Chien, S.W. Chang

    2009-01-01

    Removal of lead [Pb(II)], zinc [Zn(II)], copper [Cu(II)], and cadmium [Cd(II)] from aqueous solutions using activated carbon prepared from Phaseolus aureus hulls (ACPAH), an agricultural waste was studied. The influence of various parameters such as effect of pH, contact time, adsorbent dose, and initial concentration of metal ions on the removal was evaluated by batch method. The removal of metal ions by ACPAH was pH dependent and the optimum pH values were 7.0, 8.0, 7.0 and 6.0 for Cu(II), Cd(II), Zn(II), and Pb(II), respectively. The sorption isotherms were studied using Langmuir, Freundlich, Dubinin-Radushkevich (D-R), and Temkin isotherm models. The maximum adsorption capacity values of ACPAH for metal ions were 21.8 mg g -1 for Pb(II), 21.2 mg g -1 for Zn(II), 19.5 mg g -1 for Cu(II), and 15.7 mg g -1 for Cd(II). The experiments demonstrated that the removal of metal ions followed the pseudo-second-order kinetic model. Desorption experiments were carried out using HCl solution with a view to regenerate the spent adsorbent and to recover the adsorbed metal ions.

  12. Solvation Effect on Complexation of Alkali Metal Cations by a Calix[4]arene Ketone Derivative.

    Požar, Josip; Nikšić-Franjić, Ivana; Cvetnić, Marija; Leko, Katarina; Cindro, Nikola; Pičuljan, Katarina; Borilović, Ivana; Frkanec, Leo; Tomišić, Vladislav

    2017-09-14

    The medium effect on the complexation of alkali metal cations with a calix[4]arene ketone derivative (L) was systematically examined in methanol, ethanol, N-methylformamide, N,N-dimethylformamide, dimethyl sulfoxide, and acetonitrile. In all solvents the binding of Na + cation by L was rather efficient, whereas the complexation of other alkali metal cations was observed only in methanol and acetonitrile. Complexation reactions were enthalpically controlled, while ligand dissolution was endothermic in all cases. A notable influence of the solvent on NaL + complex stability could be mainly attributed to the differences in complexation entropies. The higher NaL + stability in comparison to complexes with other alkali metal cations in acetonitrile was predominantly due to a more favorable complexation enthalpy. The 1 H NMR investigations revealed a relatively low affinity of the calixarene sodium complex for inclusion of the solvent molecule in the calixarene hydrophobic cavity, with the exception of acetonitrile. Differences in complex stabilities in the explored solvents, apart from N,N-dimethylformamide and acetonitrile, could be mostly explained by taking into account solely the cation and complex solvation. A considerable solvent effect on the complexation equilibria was proven to be due to an interesting interplay between the transfer enthalpies and entropies of the reactants and the complexes formed.

  13. Ligand combination strategy for the preparation of novel low-dimensional and open-framework metal cluster materials

    Anokhina, Ekaterina V.

    Low-dimensional and open-framework materials containing transition metals have a wide range of applications in redox catalysis, solid-state batteries, and electronic and magnetic devices. This dissertation reports on research carried out with the goal to develop a strategy for the preparation of low-dimensional and open-framework materials using octahedral metal clusters as building blocks. Our approach takes its roots from crystal engineering principles where the desired framework topologies are achieved through building block design. The key idea of this work is to induce directional bonding preferences in the cluster units using a combination of ligands with a large difference in charge density. This investigation led to the preparation and characterization of a new family of niobium oxychloride cluster compounds with original structure types exhibiting 1ow-dimensional or open-framework character. Most of these materials have framework topologies unprecedented in compounds containing octahedral clusters. Comparative analysis of their structural features indicates that the novel cluster connectivity patterns in these systems are the result of complex interplay between the effects of anisotropic ligand arrangement in the cluster unit and optimization of ligand-counterion electrostatic interactions. The important role played by these factors sets niobium oxychloride systems apart from cluster compounds with one ligand type or statistical ligand distribution where the main structure-determining factor is the total number of ligands. These results provide a blueprint for expanding the ligand combination strategy to other transition metal cluster systems and for the future rational design of cluster-based materials.

  14. Features of proteolytic properties of tetraphenylporphyrin complex with lanthanide group metals

    Tobolkina, Elena A.; Skripnikova, Tatiana A.; Starikova, Anna A.; Shumilova, Galina I.; Pendin, Andrey A.

    2018-01-01

    Demetallation of metalloporphyrin molecules is one of the essential degradation reactions in photosynthesis. The effect of metalloporphyrin nature on removal of central metals from tetraphenylporphyrin complexes based on lanthanide group metals (Dy, Er, Lu, Ho) has been studied. pH values, at which the metal ions leave the metalloporphyrin complex were established using two-phase spectrophotometric titration with potentiometric pH-control. The pH values decrease with the increase of atomic numbers of lanthanide groups, as well as with increase of 4f-electrons. The reaction of an extra ligand exchange for the hydroxide ion was studied. For Dy-, Er- and Ho-tetraphenylporphyrin complexes one particle of extra ligand coordinates with one porphyrin complex. A complex with dimeric particles can be formed for the system of Lu-tetraphenylporphyrin. Constants of the ion exchange reactions were calculated.

  15. Transition metal complexes of some biologically active ligands; synthesis characterization and bioactivities

    Rehman, S.; Ali, N.; Nisar, M.

    2009-01-01

    Transition/representative transition metals complexes of biologically active chelating agent 1,2-dipyrolodinoethane were synthesized and characterized through spectral and analytical data. The complexes are of the formula (M(L)X/sub 2/). Where (M = Co (II), Ni (II), Cu (II), Zn (II), Hg (II) and Cd (II) and X = CI, Br, NO/sub 3/). Tetrahedral geometry has been proposed to these-metal complexes with the help of magnetic measurements, elemental analysis, chemical stoichiometry and spectroscopic data Antibacterial activity of the ligand and its metal complexes were screened against Eschereschi coli, Klebsiello pneumonia, Proteus mirabilis, Proteus vulhari, Streptococcus pneumonia, Salmonella Iyphi, Bacilh,s anthrax, Streptococcus fecalis and Staphylococcus aureus. Complexes were found to be active against Eschereschi coli, Klebsiella pneumonia, Proteus mirabilis and Proteus vulharis. (author)

  16. Supercritical CO2-assisted preparation of ibuprofen loaded PEG-PVP complexes

    Labuschagne, Philip W

    2010-06-01

    Full Text Available Stoichiometric ratios of poly (ethylene glycol) (PEG, Mw = 400) with poly(vinylpyrrolidone) (PVP, Mw = ±3.1 x 104 & Mw = 1.25 x 106 Mw) were prepared from ethanol cast solutions and in supercritical CO2. The complex formation was studied via glass...

  17. Purification of Ovine Respiratory Complex I Results in a Highly Active and Stable Preparation.

    Letts, James A; Degliesposti, Gianluca; Fiedorczuk, Karol; Skehel, Mark; Sazanov, Leonid A

    2016-11-18

    NADH-ubiquinone oxidoreductase (complex I) is the largest (∼1 MDa) and the least characterized complex of the mitochondrial electron transport chain. Because of the ease of sample availability, previous work has focused almost exclusively on bovine complex I. However, only medium resolution structural analyses of this complex have been reported. Working with other mammalian complex I homologues is a potential approach for overcoming these limitations. Due to the inherent difficulty of expressing large membrane protein complexes, screening of complex I homologues is limited to large mammals reared for human consumption. The high sequence identity among these available sources may preclude the benefits of screening. Here, we report the characterization of complex I purified from Ovis aries (ovine) heart mitochondria. All 44 unique subunits of the intact complex were identified by mass spectrometry. We identified differences in the subunit composition of subcomplexes of ovine complex I as compared with bovine, suggesting differential stability of inter-subunit interactions within the complex. Furthermore, the 42-kDa subunit, which is easily lost from the bovine enzyme, remains tightly bound to ovine complex I. Additionally, we developed a novel purification protocol for highly active and stable mitochondrial complex I using the branched-chain detergent lauryl maltose neopentyl glycol. Our data demonstrate that, although closely related, significant differences exist between the biochemical properties of complex I prepared from ovine and bovine mitochondria and that ovine complex I represents a suitable alternative target for further structural studies. © 2016 by The American Society for Biochemistry and Molecular Biology, Inc.

  18. High capacity hydrogen absorption in transition-metal ethylene complexes: consequences of nanoclustering

    Phillips, A B; Shivaram, B S

    2009-01-01

    We have recently shown that organo-metallic complexes formed by laser ablating transition metals in ethylene are high hydrogen absorbers at room temperature (Phillips and Shivaram 2008 Phys. Rev. Lett. 100 105505). Here we show that the absorption percentage depends strongly on the ethylene pressure. High ethylene pressures (>100 mTorr) result in a lowered hydrogen uptake. Transmission electron microscopy measurements reveal that while low pressure ablations result in metal atoms dispersed uniformly on a near atomic scale, high pressure ones yield distinct nanoparticles with electron energy-loss spectroscopy demonstrating that the metal atoms are confined solely to the nanoparticles.

  19. Quantitative Interpretation of Multifrequency Multimode EPR Spectra of Metal Containing Proteins, Enzymes, and Biomimetic Complexes.

    Petasis, Doros T; Hendrich, Michael P

    2015-01-01

    Electron paramagnetic resonance (EPR) spectroscopy has long been a primary method for characterization of paramagnetic centers in materials and biological complexes. Transition metals in biological complexes have valence d-orbitals that largely define the chemistry of the metal centers. EPR spectra are distinctive for metal type, oxidation state, protein environment, substrates, and inhibitors. The study of many metal centers in proteins, enzymes, and biomimetic complexes has led to the development of a systematic methodology for quantitative interpretation of EPR spectra from a wide array of metal containing complexes. The methodology is now contained in the computer program SpinCount. SpinCount allows simulation of EPR spectra from any sample containing multiple species composed of one or two metals in any spin state. The simulations are quantitative, thus allowing determination of all species concentrations in a sample directly from spectra. This chapter will focus on applications to transition metals in biological systems using EPR spectra from multiple microwave frequencies and modes. © 2015 Elsevier Inc. All rights reserved.

  20. Preconcentration of metallic elements by complexation with ammonium pyrrolidine dithiocarbamate (APDC) for atomic absorption analysis

    Santos Coelho, Ricardo dos; Dantas, Elizabeth S.K.

    1997-01-01

    Ammonium pyrrolidine dithiocarbamate (APDC) forms stable chelates with many metals being therefore, used in systems of preconcentration for determination of heavy metals in water. In this work, the metals were complexed with APDC and extracted with methyl isobutyl ketone (MIBK). The results showed that the studied metals (Co, Cu, Fe, Ni, Pb, Cr and Cd), in the range of 2 to 5 μg, in 100 ml of sample, were quantitatively extracted in only one stage using 10 ml of MIBK and 5 ml of 4% APDC. The pH must be between 4 and 5. The complexes stability was also studied. The proposed method can be applied to pre concentrate heavy metals in natural waters. (author). 4 refs., 1 fig., 3 tabs

  1. Selective transport of metal ions through cation exchange membrane in the presence of a complexing agent

    Tingchia Huang; Jaukai Wang (National Cheng Kung Univ., Tainan (Taiwan, Province of China))

    1993-01-01

    Selective transport of metal ions through a cation exchange membrane was studied in stirred batch dialyzer for the systems Ni[sup 2+]-Cu[sup 2+] and Cu[sup 2+]-Fe[sup 3+]. Oxalic acid, malonic acid, citric acid, glycine, and ethylenediaminetetraacetic acid were employed as the complexing agents added in the feed solution in order to increase the permselectivity of metal ions. The experimental results show that the selective transport behavior of metal ions depends on the valence and the concentration of metal ions, the stoichiometric ratio of complexing agent to metal ions, and the pH value of the feed solution, but is independent of the concentration of counterion in the stripping phase. A theoretical approach was formulated on the basis of the Nernst-Planck equation and interface quasi-equilibrium. Theoretical solutions obtained from numerical calculation were in agreement with the experimental data.

  2. Mesoporous activated carbons with metal-oxide particles prepared from Morwell coal; Morwell tan wo genryo to shita kinzoku sankabutsu tanji kasseitan no saiko kozo

    Yoshizawa, N.; Yamada, Y.; Shiraishi, M. [National Institute for Resources and Environment, Tsukuba (Japan); Kojima, S.; Tamai, H.; Yasuda, H. [Hiroshima University, Hiroshima (Japan). Faculty of Engineering

    1996-10-28

    The metal dependence of mesoporous activated carbons with various metal acetylacetonate (acac) particles prepared from Morwell coal was studied. In experiment, the mixture of Morwell coal and acac metal complexes were dissipated into tetrahydrofuran, and after agitation in Ar atmosphere, the solvent was removed by vacuum distillation. Coal specimens with Fe(acac)3, Ni(acac)2 and Co(acac)2 as acac complexes were activated by exchanging flow gas with water vapor after heat treatment in N2 gas flow at 900{degree}C. The pore sizes of the specimens were obtained from N2 adsorption isotherms by BET method and BJH method. Conditions of pores and metals in the specimens were examined by XRD measurement and TEM observation. The relation between the above conditions and pore characteristics obtained from adsorption experiment was also examined. As a result, the difference in mesopore ratio between the specimens and blank specimens was larger in the order of Fe, Co and Ni, and the effect of added metal complexes was also larger in this order. 3 refs., 3 figs., 3 tabs.

  3. Surfactant-thermal method to prepare two new cobalt metal-organic frameworks

    Yu, Xianglin [School of Materials Science and Engineering and School of Chemical and Biomedical Engineering, Nanyang Technological University, Singapore 639798 (Singapore); Key Laboratory for Green Chemical Process of Ministry of Education, School of Chemical Engineering and Pharmacy, Wuhan Institute of Technology, Wuhan 430074 (China); Toh, Yong Siang [School of Materials Science and Engineering and School of Chemical and Biomedical Engineering, Nanyang Technological University, Singapore 639798 (Singapore); Zhao, Jun [College of Materials and Chemical Engineering, Hubei Provincial Collaborative Innovation Center for New Energy Microgrid, China Three Gorges University, Yichang 443002 (China); Nie, Lina [School of Materials Science and Engineering and School of Chemical and Biomedical Engineering, Nanyang Technological University, Singapore 639798 (Singapore); Ye, Kaiqi; Wang, Yue [State Key Laboratory of Supramolecular Structure and Materials, College of Chemistry, Jilin University, Changchun 130012 (China); Li, Dongsheng [College of Materials and Chemical Engineering, Hubei Provincial Collaborative Innovation Center for New Energy Microgrid, China Three Gorges University, Yichang 443002 (China); Zhang, Qichun, E-mail: qczhang@ntu.edu.sg [School of Materials Science and Engineering and School of Chemical and Biomedical Engineering, Nanyang Technological University, Singapore 639798 (Singapore); Division of Chemistry and Biological Chemistry, School of Physical and Mathematical Sciences, Nanyang Technological University, Singapore 637371 (Singapore)

    2015-12-15

    Employing surfactants as reaction media, two new metal-organic frameworks (MOFs):(HTEA){sub 3}[Co{sub 3}(BTC){sub 3}] (NTU-Z33) and (HTEA)[Co{sub 3}(HBTC){sub 2}(BTC)] (NTU-Z34) (H{sub 3}BTC=1,3,5-benzenetricarboxylic acid, TEA=trimethylamine, and NTU=Nanyang Technological University), have been successfully synthesized and fully characterized. Note that NTU-Z33 has an unusual trimeric [Co{sub 3}(COO){sub 9}] secondary building unit (SBU). Magnetic characterization suggests that both compounds have weak antiferromagnetic behaviors. Our success in preparing new crystalline Co-BTC based MOFs under different surfactant media could provide a new road to prepare new diverse MOFs through various combinations of surfactants. - Graphical abstract: Employing surfactants as reaction media, two new metal-organic frame-works (MOFs) have been successfully synthesized and magnetic study suggests that both compounds have weak antiferromagnetic behaviors. - Highlights: • Two novel metal-organic frame-works (MOFs). • Synthesis through surfactant-thermal condition. • weak antiferromagnetic behaviors for both compounds.

  4. Surfactant-thermal method to prepare two new cobalt metal-organic frameworks

    Yu, Xianglin; Toh, Yong Siang; Zhao, Jun; Nie, Lina; Ye, Kaiqi; Wang, Yue; Li, Dongsheng; Zhang, Qichun

    2015-01-01

    Employing surfactants as reaction media, two new metal-organic frameworks (MOFs):(HTEA)_3[Co_3(BTC)_3] (NTU-Z33) and (HTEA)[Co_3(HBTC)_2(BTC)] (NTU-Z34) (H_3BTC=1,3,5-benzenetricarboxylic acid, TEA=trimethylamine, and NTU=Nanyang Technological University), have been successfully synthesized and fully characterized. Note that NTU-Z33 has an unusual trimeric [Co_3(COO)_9] secondary building unit (SBU). Magnetic characterization suggests that both compounds have weak antiferromagnetic behaviors. Our success in preparing new crystalline Co-BTC based MOFs under different surfactant media could provide a new road to prepare new diverse MOFs through various combinations of surfactants. - Graphical abstract: Employing surfactants as reaction media, two new metal-organic frame-works (MOFs) have been successfully synthesized and magnetic study suggests that both compounds have weak antiferromagnetic behaviors. - Highlights: • Two novel metal-organic frame-works (MOFs). • Synthesis through surfactant-thermal condition. • weak antiferromagnetic behaviors for both compounds.

  5. A Plasma-Assisted Route to the Rapid Preparation of Transition-Metal Phosphides for Energy Conversion and Storage

    Liang, Hanfeng; Alshareef, Husam N.

    2017-01-01

    with the method of preparation as the electronic, catalytic, and magnetic properties of the metal phosphides strongly depend on their synthesis routes. Commonly practiced processes such as solid-state synthesis and ball milling have proven to be reliable routes

  6. Facile preparation of highly hydrophilic, recyclable high-performance polyimide adsorbents for the removal of heavy metal ions

    Huang, Jieyang; Zheng, Yaxin; Luo, Longbo; Feng, Yan [State Key Laboratory of Polymer Material and Engineering, College of Polymer Science and Engineering, Sichuan University, Chengdu 610065 (China); Zhang, Chaoliang [State Key Laboratory of Oral Diseases, West China College of Stomatology, Sichuan University, Chengdu 610041 (China); Wang, Xu, E-mail: wx19861027@163.com [State Key Laboratory of Polymer Material and Engineering, College of Polymer Science and Engineering, Sichuan University, Chengdu 610065 (China); Liu, Xiangyang, E-mail: lxy6912@sina.com [State Key Laboratory of Polymer Material and Engineering, College of Polymer Science and Engineering, Sichuan University, Chengdu 610065 (China)

    2016-04-05

    Highlights: • High-performance polyimide was used as heavy metal adsorbents. • The contradiction between hydrophilicity and high performance of PI was solved. • Adsorption amount for Cu{sup 2+} of PI/silica was 77 times higher than that of PI. • The adsorption ability remained steady for more than 50 recycling processes. - Abstract: To obtain high-performance adsorbents that combine excellent adsorption ability, thermal stability, service life and recycling ability, polyimide (PI)/silica powders were prepared via a facile one-pot coprecipitation process. A benzimidazole unit was introduced into the PI backbone as the adsorption site. The benzimidazole unit induced more hydroxyls onto the silica, which provided hydrophilic sites for access by heavy metal ions. By comprehensively analyzing the effect of hydrophilcity, agglomeration, silica polycondensation, specific surface area and PI crystallinity, 10% was demonstrated to be the most proper feed silica content. The equilibrium adsorption amount (Q{sub e}) for Cu{sup 2+} of PI/silica adsorbents was 77 times higher than that of pure PI. Hydrogen chloride (HCl) was used as a desorbent for heavy metal ions and could be decomplexed with benzimidazole unit at around 300 °C, which was lower than the glass transition temperature of PI. The complexation and decomplexation process of HCl made PI/silica adsorbents recyclable, and the adsorption ability remained steady for more than 50 recycling processes. As PI/silica adsorbents possess excellent thermal stability, chemical resistance and radiation resistance and hydrophilicity, they have potential as superior recyclable adsorbents for collecting heavy metal ions from waste water in extreme environments.

  7. Preparation of a novel breviscapine-loaded halloysite nanotubes complex for controlled release of breviscapine

    Gao, Min; Lu, Liqian; Wang, Xiaoyue; Lin, Houke; Zhou, Qingsong

    2017-11-01

    For sustain the release rate and prolong half-life of breviscapine in vivo, the breviscapine-loaded halloysite nanotubes complex was prepared. The breviscapine was encapsulated into halloysite nanotubes (HNTs) using a vacuum process. The complex were investigated by scanning electron microscopy (SEM), differential scanning calorimetry (DSC), transmission electron microscope (TEM), X-ray diffraction (XRD) and fourier transform infrared spectroscopy(FT-IR). The formation of breviscapine-loaded HNTs complex was proved by the test results of SEM, DSC, TEM and IR analysise. The results confirmed that breviscapine was successfully loaded in the halloysite nanotubes. Additionally, the in vitro drug release of breviscapine from breviscapine-loaded HNTs complex was investigated, the result indicated this complex has apparent sustained-release effect.

  8. Light induced electron transfer reactions of metal complexes

    Sutin, N.; Creutz, C.

    1980-01-01

    Properties of the excited states of tris(2,2'-bipyridine) and tris(1,10-phenanthroline) complexes of chromium(III), iron(II), ruthenium(II), osmium(II), rhodium(III), and iridium(III) are described. The electron transfer reactions of the ground and excited states are discussed and interpreted in terms of the driving force for the reaction and the distortions of the excited states relative to the corresponding ground states. General considerations relevant to the conversion of light into chemical energy are presented and progress in the use of polypyridine complexes to effect the light decomposition of water into hydrogen and oxygen is reviewed

  9. Electron transfer reactions of metal complexes in solution

    Sutin, N.

    1977-01-01

    A few representative electron-transfer reactions are selected and their kinetic parameters compared with the predictions of activated complex models. Since Taube has presented an elegant treatment of intramolecular electron-transfer reactions, emphasis is on bimolecular reactions. The latter electron-transfer reactions are more complicated to treat theoretically since the geometries of their activated complexes are not as well known as for the intramolecular case. In addition in biomolecular reactions, the work required to bring the two reactants together needs to be calculated. Since both reactants generally carry charges this presents a non-trivial problem at the ionic strengths usually used to study bimolecular electron transfer

  10. Confirmation of molecular formulas of metallic complexes through X-ray fluorescence quantitative analysis

    Filgueiras, C.A.L.; Marques, E.V.; Machado, R.M.

    1984-01-01

    X-ray fluorescence spectrophotometry was employed to determined the metal content in a series of five transition element complexes (Mn, Ti, Zn, V). The results confirmed the molecular formulas of these complexes, already proposed on the basis of elemental microanalysis, solution condutimetry and other analytical methods. (C.L.B.) [pt

  11. Hydrogen storage material and process using graphite additive with metal-doped complex hydrides

    Zidan, Ragaiy [Aiken, SC; Ritter, James A [Lexington, SC; Ebner, Armin D [Lexington, SC; Wang, Jun [Columbia, SC; Holland, Charles E [Cayce, SC

    2008-06-10

    A hydrogen storage material having improved hydrogen absorbtion and desorption kinetics is provided by adding graphite to a complex hydride such as a metal-doped alanate, i.e., NaAlH.sub.4. The incorporation of graphite into the complex hydride significantly enhances the rate of hydrogen absorbtion and desorption and lowers the desorption temperature needed to release stored hydrogen.

  12. Bioassay studies of metal(II) complexes of 2,2'-(ethane-1,2 ...

    ethane-1,2-diyldiimino)diacetic acid (EDDA) were prepared and characterized. Coordination complexes of the EDDA were characterized by physical measurements including elemental analysis, IR, UV-Visible, magnetic susceptibilities and ...

  13. Preparation of large-area molecular junctions with metallic conducting Langmuir–Blodgett films

    Mochizuki, Kengo [Division of Marine Technology, Tokyo University of Marine Science and Technology, 2-1-6 Etchujima Koto-ku, Tokyo 135-8533 (Japan); Ohnuki, Hitoshi, E-mail: ohnuki@kaiyodai.ac.jp [Division of Marine Technology, Tokyo University of Marine Science and Technology, 2-1-6 Etchujima Koto-ku, Tokyo 135-8533 (Japan); Shimizu, Daisuke [Division of Marine Technology, Tokyo University of Marine Science and Technology, 2-1-6 Etchujima Koto-ku, Tokyo 135-8533 (Japan); Imakubo, Tatsuro [Department of Materials and Technology, Nagaoka University of Technology, 1603-1 Kamitomioka, Nagaoka, Niigata 940-2188 (Japan); Tsuya, Daiju [National Institute for Materials Science,1-2-1 Sengen, Tsukuba, Ibaraki 305-0047 (Japan); Izumi, Mitsuru [Division of Marine Technology, Tokyo University of Marine Science and Technology, 2-1-6 Etchujima Koto-ku, Tokyo 135-8533 (Japan)

    2014-03-03

    Metallic conducting Langmuir–Blodgett (LB) films were used as soft electrodes to fabricate molecular junctions with self-assembled monolayers (SAMs) of alkanethiols (CH{sub 3}(CH{sub 2}){sub n−1}SH) on an Au surface. Alkanethiols can form highly ordered, stable dielectric SAMs on metal surfaces over large areas. However, it is difficult to establish electrical contacts on such SAMs, which has limited their application. In this work, we used metallic conducting LB films composed of bis(ethylenedioxy)tetrathiafulvalene and stearic acid as a soft electrode onto alkanethiol SAMs (C{sub n}-SAM, n = 12, 14, 16, 18) to prepare Au/SAM/metal junctions of relatively large size (∼ 15.6 × 10{sup 3} μm{sup 2}). The current density–voltage (J–V) characteristics across the junctions exhibited rectifying behavior with a ratio R of ∼ 5 (R = |J(V)|/|J(− V)| at ± 1 V). The lower transfer rate corresponding to the electron transport from Au to the LB films exhibited nonlinear J–V characteristics, while the higher transfer rate of electrons from the LB film to Au showed linear J–V characteristics. Kelvin probe force microscopy revealed that the work function of the metallic LB films was smaller than that of Au. The observed rectification behavior is probably caused by different electron transport mechanisms between the two current directions. - Highlights: • Metallic Langmuir–Blodgett (LB) films were used as soft electrodes. • Molecular junctions of metal–alkanethiol–LB films were fabricated. • The current–voltage curve across the junctions exhibited rectifying behavior. • This is the first observation for alkanethiol monolayer junctions. • The work function difference between the electrodes induces the rectification.

  14. The chemical and catalytic properties of nanocrystalline metal oxides prepared through modified sol-gel synthesis

    Carnes, Corrie Leigh

    The goal of this research was to synthesize, characterize and study the chemical properties of nanocrystalline metal oxides. Nanocrystalline (NC) ZnO, CuO, NiO, Al2O3, and the binary Al2O 3/MgO and ZnO/CuO were prepared through modified sol gel methods. These NC metal oxides were studied in comparison to the commercial (CM) metal oxides. The samples were characterized by XRD, TGA, FTIR, BET, and TEM. The NC samples were all accompanied by a significant increase in surface area and decrease in crystallite size. Several chemical reactions were studied to compare the NC samples to the CM samples. One of the reactions involved a high temperature reaction between carbon tetrachloride and the oxide to form carbon dioxide and the corresponding metal chloride. A similar high temperature reaction was conducted between the metal oxide and hydrogen sulfide to form water and the corresponding metal sulfide. A room temperature gas phase adsorption was studied where SO2 was adsorbed onto the oxide. A liquid phase adsorption conducted at room temperature was the destructive adsorption of paraoxon (a toxic insecticide). In all reactions the NC samples exhibited greater activity, destroying or adsorbing a larger amount of the toxins compared to the CM samples. To better study surface area effects catalytic reactions were also studied. The catalysis of methanol was studied over the nanocrystalline ZnO, CuO, NiO, and ZnO/CuO samples in comparison to their commercial counterparts. In most cases the NC samples proved to be more active catalysts, having higher percent conversions and turnover numbers. A second catalytic reaction was also studied, this reaction was investigated to look at the support effects. The catalysis of cyclopropane to propane was studied over Pt and Co catalysts. These catalysts were supported onto NC and CM alumina by impregnation. By observing differences in the catalytic behavior, support effects have become apparent.

  15. Electrode-analytical properties of polyvinylchloride membranes based on triple metal-polymeric complexes

    Katerina V. Matorina

    2015-10-01

    Full Text Available The influence of the nature of the electrode-active substances (EAS, the composition of the external and internal solutions on the formation of the analytical signal of polyvinylchloride (PVC membranes based on associates and triple metal-polymeric complexes (TMPC was established. Dehumidification of synthesized membranes increases with the content of polyvinylpyrrolidone (PVP. The value of the swelling degree is more than two times greater for membranes, which contain as EAS TMPC, relative to membranes based on associates. The value of water absorption of membranes is determined by the nature of EAS. They formed a series of increasing of the swelling degree such as associate < background membrane < TMPC. Swelling of the background membrane is explained by the physical sorption of water molecules on the surface of plasticized membrane. Hydration of PVP macromolecules varies with the introduction of metal ions, macromolecules unit undergoes a conformational transition. PVP macromolecules form tunnels or cavities where complex particles distributed and additional water accumulated through the second coordination layer. Constructed sensors based on TMPC have slope of electrode function equal to 25 mV/pC. Linear dependence of potential on the polymer concentration is observed in the range of 5–7 pC units. Sensors based on associates have slope of the electrode function of 20–25 mV/pC that can be varied depending on the nature of the EAS. Working range is 4–8 pC. Response time of sensor is less than 1 min. The optimal time for conditioning of the synthesized PVC membrane is 24 hours. Potentiometric sensors have been developed for the determination of residual amounts of low molecular PVP which is a food additive E 1201 commonly used for thickening, stabilizing and clarifying of food products. The content of PVP was determined in real objects (apple juice, beer, red wine and cognac with using the polyvinylpyrrolidone sensors (Sr < 0.08. The

  16. Synthesis and Spectral Characterization of Antifungal Sensitive Schiff Base Transition Metal Complexes

    Sakthivel, A.; Rajasekaran, K.

    2007-01-01

    New N2O2 donor type Schiff base has been designed and synthesized by condensing acetoacetanilido-4-aminoantipyrine with 2-aminobenzoic acid in ethanol. Solid metal complexes of the Schiff base with Cu(II), Ni(II), Co(II), Mn(II), Zn(II), VO(IV), Hg(II) and Cd(II) metal ions were synthesized and characterized by elemental analyses, magnetic susceptibility, molar conduction, fast atom bombardment (FAB) mass, IR, UV-Vis, and 1H NMR spectral studies. The data show that the complexes have the composition of ML type. The UV-Vis. and magnetic susceptibility data of the complexes suggest a square-planar geometry around the central metal ion except VO(IV) complex which has square-pyramidal geometry. The in vitro antifungal activities of the compounds were tested against fungi such as Aspergillus niger, Aspergillus flavus, Rhizopus stolonifer, Candida albicans, Rhizoctonia bataicola and Trichoderma harizanum. All the metal complexes showed stronger antifungal activities than the free ligand. The minimum inhibitory concentrations (MIC) of the metal complexes were found in the range of 10~31 µg/ml. PMID:24015086

  17. Humic substances in natural waters and their complexation with trace metals and radionuclides: a review

    Boggs, S. Jr.; Livermore, D.; Seitz, M.G.

    1985-07-01

    Dissolved humic substances (humic and fulvic acids) occur in surface waters and groundwaters in concentrations ranging from less than 1 mg(C)/L to more than 100 mg(C)/L. Humic substances are strong complexing agents for many trace metals in the environment and are also capable of forming stable soluble complexes or chelates with radionuclides. Concentrations of humic materials as low as 1 mg(C)/L can produce a detectable increase in the mobility of some actinide elements by forming soluble complexes that inhibit sorption of the radionuclides onto rock materials. The stability of trace metal- or radionuclide-organic complexes is commonly measured by an empirically determined conditional stability constant (K'), which is based on the ratio of complexed metal (radionuclide) in solution to the product concentration of uncomplexed metal and humic complexant. Larger values of stability constants indicate greater complex stability. The stability of radionuclide-organic complexes is affected both by concentration variables and envionmental factors. In general, complexing is favored by increased of radionuclide, increased pH, and decreased ionic strength. Actinide elements are generally most soluble in their higher oxidation states. Radionuclides can also form stable, insoluble complexes with humic materials that tend to reduce radionuclide mobility. These insoluble complexes may be radionuclide-humate colloids that subsequently precipitate from solution, or complexes of radionuclides and humic substances that sorb to clay minerals or other soil particulates strongly enough to immobilize the radionuclides. Colloid formation appears to be favored by increased radionuclide concentration and lowered pH; however, the conditions that favor formation of insoluble complexes that sorb to particulates are still poorly understood. 129 refs., 25 figs., 19 tabs

  18. Evaluation of marginal fit of single implant-supported metal-ceramic crowns prepared by using presintered metal blocks.

    Pasali, Baris; Sarac, Duygu; Kaleli, Necati; Sarac, Yakup Sinasi

    2018-02-01

    Recently, presintered metal blocks for nonprecious and precious metal implant-supported restorations have gained popularity in computer-aided design and computer-aided manufacturing (CAD-CAM) systems. However, few studies have evaluated the marginal discrepancy of implant-supported restorations made with these new alloy systems. The purpose of this in vitro study was to compare the milling-sintering method with the lost-wax and milling methods in terms of the marginal fit of implant-supported metal-ceramic restorations. Thirty implant abutments screwed to implant analogs were embedded into acrylic resin to investigate marginal fit and then divided according to fabrication methods into the following 3 groups (n=10): lost-wax (LW; control group), milling (M), and milling-sintering (MS). Porcelain material was applied to all specimens after completion of the fabrication process. Subsequently, all specimens were cemented to implant abutments for the measurement of marginal discrepancies. Twelve marginal discrepancy measurements were recorded on each implant abutment by using a stereomicroscope. The arithmetic mean of these 12 measurements was considered the mean marginal discrepancy value of each abutment. Data were statistically analyzed by using 1-way ANOVA and Tukey honest significant difference tests (α=.05). The lowest mean marginal discrepancy values (81 ±2 μm) were observed in the M group, which was significantly different (Pmarginal discrepancy values (99 ±2 μm) were observed in the MS group. The results revealed that restorations prepared by the milling-sintering method provided clinically acceptable results (marginal fit. Copyright © 2017 Editorial Council for the Journal of Prosthetic Dentistry. Published by Elsevier Inc. All rights reserved.

  19. A comprehensive in vitro biological investigation of metal complexes ...

    Md. Mahabob Ullah Mazumder

    ... Journal of Medicine journal homepage: http://www.elsevier.com/locate/ajme .... two new complexes containing Fe (III) and Mo(VI) of two tridentate ONO donor · sets ligands. Der Chem Sin. .... Pharmaceuticals (Basel). 2014;7(4):453–463. 13.

  20. Synthesis of first row transition metal carboxylate complexes by ring ...

    tion of pyromellitic dianhydride with methanol and ring opening of pyromellitic dianhydride takes place. The corresponding carboxylate complex formed dur- ing the process can be crystallised by adding biden- tate nitrogen donor ligands such as 1,10-phenanthroline or 2,2 - bipyridine.20 From the reaction with 1,10-.

  1. Stability constant of the trisglycinto metal complexes | Na'aliya ...

    The stability constants of iron, manganese, cobalt, and nickel complexes of glycine have been determined in aqueous solution by potentiometric titration with standard sodium hydroxide solution. The values of the stepwise stability constants were obtained by ORIGIN '50' program. The overall stability constants of the ...

  2. Preparation of the Nanostructured Radioisotope Metallic Oxide by Neutron Irradiation for Use as Radiotracers

    Sang-Ei Seo

    2017-10-01

    Full Text Available Metallic oxides manganese dioxide (MnO2, samarium oxide (Sm2O3, and dysprosium oxide (Dy2O3 with nanorod-like structures were synthesized by the hydrothermal synthesis method, respectively. Subsequently, the nanostructured radioisotopes MnO2 with Mn-56, Sm2O3 with Sm-153, and Dy2O3 with Dy-165 were prepared by neutron irradiation from the HANARO research reactor, respectively. The three different elements, Mn, Sm, and Dy, were selected as radiotracers because these elements can be easily gamma-activated from neutrons (activation limits: 1 picogram (Dy, 1–10 picogram (Mn, 10–100 picogram (Sm. Furthermore, the synthesized radioisotopes can be used as radiotracers in Prompt Gamma Neutron Activation Analysis as the rare earth metals Dy and Sm were not present in the Korean environment. The successful synthesis of the radioisotope metallic oxides was confirmed by Transmission Electron Microscopy (TEM, Energy Dispersive X-ray Spectrometry (EDS, X-ray Diffraction (XRD analysis, and gamma spectroscopy analysis. The synthesized nanostructured radioisotope metallic oxides may be used as radiotracers in scientific, environmental, engineering, and industrial fields.

  3. Preparation and properties of mononuclear and binuclear uranyl(VI), thorium(IV) and transition d ions complexes with multidentate Schiff bases

    Vidali, M; Casellato, U; Vigato, P A; Doretti, L; Madalosso, F [Consiglio Nazionale delle Ricerche, Padua (Italy). Lab. di Chimica e Tecnologia dei Radioelementi

    1977-01-01

    The preparation, physical and chemical properties of a variety of mononuclear and binuclear complexes containing Schiff base ligands derived from 3-formylsalicylic acid and diamines are reported. The Schiff bases have six potential donor atoms and can function as tetrabasic ligands. In the mononuclear complexes the copper(II) and nickel(II) ions occupy the N/sub 2/O/sub 2/ donor set and the uranyl(VI) ion the O/sub 2/O/sub 2/ one. Both types of complexes can act as ligand toward transition metal ions to form complexes with a binuclear structure connected by two phenolic oxygens. The complexes have been characterized by magnetic measurements and by IR and visible spectral methods.

  4. Quantification of trace metals in water using complexation and filter concentration.

    Dolgin, Bella; Bulatov, Valery; Japarov, Julia; Elish, Eyal; Edri, Elad; Schechter, Israel

    2010-06-15

    Various metals undergo complexation with organic reagents, resulting in colored products. In practice, their molar absorptivities allow for quantification in the ppm range. However, a proper pre-concentration of the colored complex on paper filter lowers the quantification limit to the low ppb range. In this study, several pre-concentration techniques have been examined and compared: filtering the already complexed mixture, complexation on filter, and dipping of dye-covered filter in solution. The best quantification has been based on the ratio of filter reflectance at a certain wavelength to that at zero metal concentration. The studied complex formations (Ni ions with TAN and Cd ions with PAN) involve production of nanoparticle suspensions, which are associated with complicated kinetics. The kinetics of the complexation of Ni ions with TAN has been investigated and optimum timing could be found. Kinetic optimization in regard to some interferences has also been suggested.

  5. Optimization of a method for preparing solid complexes of essential clove oil with β-cyclodextrins.

    Hernández-Sánchez, Pilar; López-Miranda, Santiago; Guardiola, Lucía; Serrano-Martínez, Ana; Gabaldón, José Antonio; Nuñez-Delicado, Estrella

    2017-01-01

    Clove oil (CO) is an aromatic oily liquid used in the food, cosmetics and pharmaceutical industries for its functional properties. However, its disadvantages of pungent taste, volatility, light sensitivity and poor water solubility can be solved by applying microencapsulation or complexation techniques. Essential CO was successfully solubilized in aqueous solution by forming inclusion complexes with β-cyclodextrins (β-CDs). Moreover, phase solubility studies demonstrated that essential CO also forms insoluble complexes with β-CDs. Based on these results, essential CO-β-CD solid complexes were prepared by the novel approach of microwave irradiation (MWI), followed by three different drying methods: vacuum oven drying (VO), freeze-drying (FD) or spray-drying (SD). FD was the best option for drying the CO-β-CD solid complexes, followed by VO and SD. MWI can be used efficiently to prepare essential CO-β-CD complexes with good yield on an industrial scale. © 2016 Society of Chemical Industry. © 2016 Society of Chemical Industry.

  6. Sample preparation of waste water to determine metallic contaminants by X-ray fluorescence spectroscopy

    Gonzalez Olivos, Javier.

    1987-01-01

    Trace X-ray fluorescence spectroscopy analysis in liquid samples is preceded by sample preparation, which usually consists in the precipitation of the metallic ions and concentration over a thin cellulose filter. The samples preparation of waste water by this method is not efficient, due to the great amount of organic and insoluble matter that they contain. The purpose of this work was to determine the optimal value of pH in order to adsorbe all the insoluble matter contained in a waste water sample in the activated charcoal, so that the metallic ions could be precipitated and concentrated on a thin filter and determinated by X-ray fluorescence spectroscopy. A survey about the adsorption of some ions in activated charcoal in function of the pH was made for the following: Cr 3+ , Fe 3+ , Ni 2+ , Cu 2+ , Zn 2+ , Se 2+ , Hg 2+ , and Pb 2+ . It was observed that at pH 0, the ions are not adsorbed, but Cu 2+ and Zn 2+ are adsorbed in small amount; at pH 14, the ions are adsorbed, excluding Se, which is not adsorbed at any value of pH. If a waste water sample is treated at pH 0 with activated charcoal to adsorbe the organic and insoluble matter, most of the metallic ions are not adsorbed by the activated charcoal and could be precipitated with APDC (ammonium 1-pirrolidine dithio carbamate salt) and concentrated on a thin filter. The analysis of the metallic ions contained on the filter and those adsorbed in the activated charcoal by X-ray fluorescence spectroscopy, gave the total amount of the ions in the sample. (author)

  7. [Progress in sample preparation and analytical methods for trace polar small molecules in complex samples].

    Zhang, Qianchun; Luo, Xialin; Li, Gongke; Xiao, Xiaohua

    2015-09-01

    Small polar molecules such as nucleosides, amines, amino acids are important analytes in biological, food, environmental, and other fields. It is necessary to develop efficient sample preparation and sensitive analytical methods for rapid analysis of these polar small molecules in complex matrices. Some typical materials in sample preparation, including silica, polymer, carbon, boric acid and so on, are introduced in this paper. Meanwhile, the applications and developments of analytical methods of polar small molecules, such as reversed-phase liquid chromatography, hydrophilic interaction chromatography, etc., are also reviewed.

  8. Preparation of organogel with tea polyphenols complex for enhancing the antioxidation properties of edible oil.

    Shi, Rong; Zhang, Qiuyue; Vriesekoop, Frank; Yuan, Qipeng; Liang, Hao

    2014-08-20

    Food-grade organogels are semisolid systems with immobilized liquid edible oil in a three-dimensional network of self-assembled gelators, and they are supposed to have a broad range of potential applications in food industries. In this work, an edible organogel with tea polyphenols was developed, which possesses a highly effective antioxidative function. To enhance the dispersibility of the tea polyphenols in the oil phase, a solid lipid-surfactant-tea polyphenols complex (organogel complex) was first prepared according to a novel method. Then, a food-grade organogel was prepared by mixing this organogel complex with fresh peanut oil. Compared with adding free tea polyphenols, the organogel complex could be more homogeneously distributed in the prepared organogel system, especially under heating condition. Furthermore, the organogel loading of tea polyphenols performed a 2.5-fold higher antioxidation compared with other chemically synthesized antioxidants (butylated hydroxytoluene and propyl gallate) by evaluating the peroxide value of the fresh peanut oil based organogel in accelerated oxidation conditions.

  9. A novel method for the preparation of uranium metal, oxide and carbide via electrolytic amalgamation

    Wang, L.C.; Lee, H.C.; Lee, T.S.; Lai, W.C.; Chang, C.T.

    1978-01-01

    A solid uranium amalgam was prepared electrolytically using a two-compartment cell separated with an ion exchange membrane for the purpose of regulating pH value within a narrowly restricted region of 2 to 3. The mercury cathode was kept at -1.8V vs SCE during electrolysis. The thereby obtained amalgam containing as high as 1.9gm U/ml Hg is easily converted into uranium metal by heating in vacuo above 1300 0 C. Uranium dioxide and uranium monocarbide could be easily obtained at relatively low temperature by reacting the amalgam with water vapor and methane. (author)

  10. Supercapacitors Based on Metal Electrodes Prepared from Nanoparticle Mixtures at Room Temperature

    Nakanishi, Hideyuki [Northwestern Univ., Evanston, IL (United States); Grzybowski, Bartosz A. [Northwestern Univ., Evanston, IL (United States)

    2010-01-01

    Films comprising Au and Ag nanoparticles are transformed into porous metal electrodes by desorption of weak organic ligands followed by wet chemical etching of silver. Thus prepared electrodes provide the basis for supercapacitors whose specific capacitances approach 70 F/g. Cyclic voltammetry measurement yield “rectangular” I-V curves even at high scan rates, indicating that the supercapacitors have low internal resistance. Owing to this property, the supercapacitors have a high power density ~12 kW/kg, comparable with that of the state-of-the-art carbon-based devices. The entire assembly protocol does not require high-temperature processing or the use of organic binders.

  11. Preparation of iron metal nano solution by anodic dissolution with high voltage

    Nguyen Duc Hung; Do Thanh Tuan

    2012-01-01

    Iron nano metal solution is prepared from anodic dissolution process with ultra- high Dc voltage. The size and shape of iron nanoparticles determined by Tem images and particle size distribution on the device LA-950 Laser Scattering Particle Distribution Analyzer V2. The concentration of nano-iron solution was determined by the analytical methods AAS atomic absorption spectrometry and Faraday's law. The difference in concentration of both methods demonstrated outside the anodic dissolution process has created the water electrolysis to form H 2 and O 2 gases and heating the solution. (author)

  12. A simple method to prepare self-assembled organic-organic heterobilayers on metal substrates

    L. D. Sun

    2011-06-01

    Full Text Available We demonstrate a self-assembly based simple method to prepare organic-organic heterobilayers on a metal substrate. By either sequential- or co-deposition of para-sexiphenyl (p-6P and pentacene molecules onto the Cu(110 surface in ultrahigh vacuum, p-6P/pentacene/Cu(110 heterobilayer is synthesized at room temperature. The layer sequence of the heterostructure is independent of the growth scenario indicating the p-6P/pentacene/Cu(110 is a self-assembled structure with lowest energy. Besides, the bilayer shows a very high orientational ordering and is thermally stable up to 430K.

  13. Selective Decontamination Effect of Metal Ions in Soil Using Supercritical CO2 and TBP Complex

    Park, Jihye; Park, Kwangheon; Jung, Wonyoung

    2014-01-01

    Decontamination of soil pollution is difficult because the type of contamination largely depends on the characteristics of the pollutant and the area. Also, existing soil decontamination methods generate large quantities of secondary waste and additional process costs. For this reason, new decontamination methods are always under active investigation. A method involving the use of supercritical carbon dioxide with excellent permeability in place of chemical solvents is currently being studied. Unlike other heavy metals in fission products, uranium is used as fuel, and must be handled carefully. Therefore, in this paper, we studied a supercritical carbon dioxide method for decontaminating heavy metal ions in soil using tri-n-butyl phosphate(TBP), which is well known as a ligand for the extraction of metal ions of actinium. We investigated the decontamination effect of heavy metal ions in the soil using TBP-HNO 3 Complex and supercritical carbon dioxide. The study results showed that when heavy metals in soil are extracted using supercritical carbon dioxide, the extraction efficiency is different according to the type of pollutant metal ions in the soil. When TBP-HNO 3 Complex is used with an extractant, uranium extraction is very effective, but lithium, strontium, and cesium extraction is not effective. Therefore, in the case of a mixture of uranium and other metals such as lithium, strontium, cesium, and so on in soil contaminated by fission product leaks from nuclear power plants, we can selectively decontaminate uranium with supercritical carbon dioxide and TBP-HNO 3 Complex

  14. Lutetium-177 complexation of DOTA and DTPA in the presence of competing metals

    Watanabe, Satoshi; Ishioka, Noriko S.; Hashimoto, Kazuyuki

    2013-01-01

    177 Lu complexation of DOTA and DTPA is investigated by the addition of Ca(II), Fe(II) and Zn(II). The 177 Lu complexation yield of DTPA was higher than that of DOTA in the presence of Ca(II), Fe(II) and Zn(II). Therefore, it was found that the 177 Lu complexation of DTPA was more advantageous compared with DOTA in the presence of competing metals, Ca, Fe and Zn. (author)

  15. Optical characterization and blu-ray recording properties of metal(II) azo barbituric acid complex films

    Li, X.Y. [Shanghai Institute of Optics and Fine Mechanics, Chinese Academy of Sciences, Shanghai 201800 (China)], E-mail: xyli@siom.ac.cn; Wu, Y.Q. [Shanghai Institute of Optics and Fine Mechanics, Chinese Academy of Sciences, Shanghai 201800 (China); Key Lab of Functional Inorganic Material Chemistry (Heilongjiang University), Ministry of Education, Haerbin 150080 (China)], E-mail: yqwu@siom.ac.cn; Gu, D.D.; Gan, F.X. [Shanghai Institute of Optics and Fine Mechanics, Chinese Academy of Sciences, Shanghai 201800 (China)

    2009-02-25

    Smooth thin films of nickel(II), cobalt(II) and zinc(II) complexes with azo barbituric acid were prepared by the spin-coating method. Absorption spectra of the thin films on K9 glass substrates in 300-700 nm wavelength region were measured. Optical constants (complex refractive index N = n + ik) of the thin films prepared on single-crystal silicon substrates in 275-695 nm wavelength region were investigated on rotating analyzer-polarizer type of scanning ellipsometer, and dielectric constant {epsilon} ({epsilon} = {epsilon}{sub 1} + i{epsilon}{sub 2}) as well as absorption coefficient {alpha} of thin films were calculated at 405 nm. In addition, static optical recording properties of the cobalt(II) complex thin film with an Ag reflective layer was carried out using a 406.7 nm blue-violet laser and a high numerical aperture (NA) of 0.90. Clear recording marks with high reflectivity contrast (>60%) at proper laser power and pulse width were obtained, and the size of recording mark was as small as 250 nm. The results indicate that these metal(II) complexes are promising organic recording medium for the blu-ray optical storage system.

  16. Synthesis of complex plutonium oxides with alkaline-earth metals

    Suzuki, Yasufumi; Nakajima, Kunihisa; Iwai, Takashi; Ohmichi, Toshihiko; Yamawaki, Michio.

    1995-03-01

    Complex plutonium(IV) oxides with strontium and barium, SuPuO 3 and BaPuO 3 , were synthesized and their crystal structure was analyzed. Compacted mixture of plutonium dioxide powder and the carbonate of strontium or barium was heated in a stream of argon gas using a cell with a small orifice. The products obtained were found to be composed of a nearly single phase showing the structure of orthorhombic slightly distorted from cubic. (author)

  17. Poly-functional description of metal complexation by natural organic matter: theory and practice

    Buffle, J.; Filella, M.; Altmann, R.S.

    1995-01-01

    The Differential Equilibrium Function (DEF) approach to metal complexation interpretation and prediction is compared to other models or approaches. The basic features of DEF are summarized, both from the experimental and theoretical points of view. The relation of DEF with key environmental concepts or parameters, in particular minor vs major complexing sites, the buffering intensity of natural organic matter (NOM), and their poly functional vs polyelectrolyte properties, is discussed. The relation between DEF and Freundlich isotherm is described quantitatively. The practical applications of DEF are discussed for (i) interpretation of metal complexation by NOM, and (ii) prediction of metal complexation by NOM. It is shown that DEF (i.e. sound extrapolation is possible with care). DEF cans be readily incorporated in metal species distribution codes (e.g. MINEQL). DEF is not equivalent to a molecular complexation model which describes complexation at each individual site; DEF gives a rigorous representation of complexation by NOM as a whole chemical system. (authors). 23 refs., 6 figs

  18. Efficient sample preparation from complex biological samples using a sliding lid for immobilized droplet extractions.

    Casavant, Benjamin P; Guckenberger, David J; Beebe, David J; Berry, Scott M

    2014-07-01

    Sample preparation is a major bottleneck in many biological processes. Paramagnetic particles (PMPs) are a ubiquitous method for isolating analytes of interest from biological samples and are used for their ability to thoroughly sample a solution and be easily collected with a magnet. There are three main methods by which PMPs are used for sample preparation: (1) removal of fluid from the analyte-bound PMPs, (2) removal of analyte-bound PMPs from the solution, and (3) removal of the substrate (with immobilized analyte-bound PMPs). In this paper, we explore the third and least studied method for PMP-based sample preparation using a platform termed Sliding Lid for Immobilized Droplet Extractions (SLIDE). SLIDE leverages principles of surface tension and patterned hydrophobicity to create a simple-to-operate platform for sample isolation (cells, DNA, RNA, protein) and preparation (cell staining) without the need for time-intensive wash steps, use of immiscible fluids, or precise pinning geometries. Compared to other standard isolation protocols using PMPs, SLIDE is able to perform rapid sample preparation with low (0.6%) carryover of contaminants from the original sample. The natural recirculation occurring within the pinned droplets of SLIDE make possible the performance of multistep cell staining protocols within the SLIDE by simply resting the lid over the various sample droplets. SLIDE demonstrates a simple easy to use platform for sample preparation on a range of complex biological samples.

  19. Sample preparation technique for transmission electron microscopy anodized Al-Li-SiC metal matrix composite

    Shahid, M.; Thomson, G.E.

    1997-01-01

    Along with improved mechanical properties, metal matrix composites (MMC) have a disadvantage of enhanced corrosion susceptibility in aggressive environments. Recent studies on corrosion behaviour of an Al-alloy 8090/SiC MMC, revealed considerably high corrosion rates of the MMC in near neutral solutions containing chloride ions. Anodizing is one of the potential surface treatment for the MMC to provide protective coating against corrosion. The surface and cross section of the anodized MMC can easily be observed using scanning electron microscope. The anodizing behaviour of the MMC can be understood further if the anodized cross section in examined under transmission electron microscope (TEM). However, it is relatively difficult to prepare small (3 mm diameter) electron transparent specimens of the MMC supporting an anodic film. In the present study a technique has been developed for preparing thin electron transparent specimens of the anodized MMC. This technique employed conventional ion beam thinning process but the preparation of small discs was a problem. A MMMC consisting of Al-alloy 8090 with 20 % (by weight) SiC particulate with an average size of 5 Mu m, was anodized and observed in TEM after preparing the samples using the above mentioned techniques. (author)

  20. Pt-Rh/g Al2O3 Influence of Catalyst Preparation Methods on Metallic Particle Dispersion and Size Distribution

    N.M. da Fonseca

    1998-06-01

    Full Text Available - Pt-Rh/Al2O3 catalysts were prepared by successive incipient impregnations or coimpregnation. Characterization was achieved by H2 chemisorption and transmission electron microscopy. It was verified that method of preparation, ratio of metal weights and sequence of deposition are factors that result in very distinct catalysts.

  1. Molecular Speciation of Trace Metal Organic Complexes in the Pacific Ocean

    Repeta, D.; Boiteau, R. M.; Bundy, R. M.; Babcock-Adams, L.

    2017-12-01

    Microbial production across approximately one third of the surface ocean is limited by extraordinarily low (picomolar) concentrations of dissolved iron, essentially all of which is complexed to strong organic ligands of unknown composition. Other biologically important trace metals (cobalt, copper, zinc, nickel) are also complexed to strong organic ligands, which again have not been extensively characterized. Nevertheless, organic ligands exert a strong influence on metal bioavailability and toxicity. For example, amendment experiments using commercially available siderophores, organic compounds synthesized by microbes to facilitate iron uptake, show these ligands can both facilitate or impede iron uptake depending on the siderophore composition and available uptake pathways. Over the past few years we have developed analytical techniques using high pressure liquid chromatography interfaced with inductively coupled plasma and electrospray ionization mass spectrometry to identify and quantify trace metal organic complexes in laboratory cultures of marine microbes and in seawater. We found siderophores to be widely distributed in the ocean, particularly in regions characterized by low iron concentrations. We also find chemically distinct complexes of copper, zinc, colbalt and nickel that we have yet to fully characterize. We will discuss some of our recent work on trace metal organic speciation in seawater and laboratory cultures, and outline future efforts to better understand the microbial cycling of trace metal organic complexes in the sea.

  2. Selective polymerization catalysis: controlling the metal chain end group to prepare block copolyesters.

    Zhu, Yunqing; Romain, Charles; Williams, Charlotte K

    2015-09-30

    Selective catalysis is used to prepare block copolyesters by combining ring-opening polymerization of lactones and ring-opening copolymerization of epoxides/anhydrides. By using a dizinc complex with mixtures of up to three different monomers and controlling the chemistry of the Zn-O(polymer chain) it is possible to select for a particular polymerization route and thereby control the composition of block copolyesters.

  3. Preparation and structural studies on organotin(IV) complexes with flavonoids

    Nagy, L.; Christy, A.A.; Sletten, E.; Andersen, Q.M.; Edelmann, F.T.

    1998-01-01

    Fourteen complexes of di-n-butyltin(IV) 2+ cations with flavonoid glycosides (rutin, hesperidin, 2',4',3-trihydroxy-5',4-dimetoxychalkone 4-rutinoside) and flavonoid aglycones (quercetin, morin, hesperitin and sorte flavones) were prepared. The composition of the complexes was determined by standard analytical methods. The results showed that complexes containing diorganotin(IV) 2+ moiety and the ligand in 1:1, 2:1 or 3:1 ratio are formed. The FTIR spectra were consistent with the presence of Sn-O (phenol or carbohydrate) vibration in the compounds. The structure of the complexes was measured by Moessbauer spectroscopy. Comparison of the experimental quadrupole splitting with those calculated on the basis of partial quadrupole splitting concept revealed that the complexes are of four types: with the central tin atoms surrounded by donor atoms in a purely trigonal-bipyramidal, octahedral+trigonal-bipyramidal, trigonal-bipyramidal+tetrahedral and octahedral+tetrahedral arrangement. This procedure also distinguished between the different structural isomers of both trigonal-bipyramidal and octahedral complexes. Conclusions could therefore be drawn on the factors determining which of the isomers are formed in the systems. The Moessbauer parameters obtained for organotin(IV)-flavonoid complexes were compared with those measured for organotin(IV)-carbohydrate complexes. (author)

  4. Preparation of Some Novel Copper(I) Complexes and their Molar Conductances in Organic Solvents

    Gill, Dip Singh; Rana, Dilbag

    2009-04-01

    Attempts have been made to prepare some novel copper(I) nitrate, sulfate, and perchlorate complexes. Molar conductances of these complexes have been measured in organic solvents like acetonitrile (AN), acetone (AC), methanol (MeOH), N,N-dimethylformamide (DMF), N,Ndimethylacetamide (DMA), and dimethylsulfoxide (DMSO) at 298 K. The molar conductance data have been analyzed to obtain limiting molar conductances (λ0) and ion association constants (KA) of the electrolytes. The results showed that all these complexes are strong electrolytes in all organic solvents. The limiting ionic molar conductances (λo± ) for various ions have been calculated using Bu4NBPh4 as reference electrolyte. The actual radii for copper(I) complex ions are very large and different in different solvents and indicate some solvation effects in each solvent system

  5. Preparation and characterization of bi-metallic nanoparticle catalyst having better anti-coking properties using reverse micelle technique

    Zacharia, Thomas

    Energy needs are rising on an exponential basis. The mammoth energy sources like coal, natural gas and petroleum are the cause of pollution. The large outcry for an alternate energy source which is environmentally friendly and energy efficient is heard during the past few years. This is where “Clean-Fuel” like hydrogen gained its ground. Hydrogen is mainly produced by steam methane reforming (SMR). An alternate sustainable process which can reduce the cost as well as eliminate the waste products is Tri-reforming. In both these reforming processes nickel is used as catalyst. However as the process goes on the catalyst gets deactivated due to coking on the catalytic surface. This goal of this thesis work was to develop a bi-metallic catalyst which has better anti-coking properties compared to the conventional nickel catalyst. Tin was used to dope nickel. It was found that Ni3Sn complex around a core of Ni is coking resistant compared to pure nickel catalyst. Reverse micelle synthesis of catalyst preparation was used to control the size and shape of catalytic particles. These studies will benefit researches on hydrogen production and catalyst manufactures who work on different bi-metallic combinations.

  6. Metal complexes in cancer therapy – an update from drug design perspective

    Ndagi U

    2017-03-01

    Full Text Available Umar Ndagi, Ndumiso Mhlongo, Mahmoud E Soliman Molecular Modelling and Drug Design Research Group, School of Health Sciences, University of KwaZulu-Natal, Westville, Durban, South Africa Abstract: In the past, metal-based compounds were widely used in the treatment of disease conditions, but the lack of clear distinction between the therapeutic and toxic doses was a major challenge. With the discovery of cisplatin by Barnett Rosenberg in 1960, a milestone in the history of metal-based compounds used in the treatment of cancers was witnessed. This forms the foundation for the modern era of the metal-based anticancer drugs. Platinum drugs, such as cisplatin, carboplatin and oxaliplatin, are the mainstay of the metal-based compounds in the treatment of cancer, but the delay in the therapeutic accomplishment of other metal-based compounds hampered the progress of research in this field. Recently, however, there has been an upsurge of activities relying on the structural information, aimed at improving and developing other forms of metal-based compounds and nonclassical platinum complexes whose mechanism of action is distinct from known drugs such as cisplatin. In line with this, many more metal-based compounds have been synthesized by redesigning the existing chemical structure through ligand substitution or building the entire new compound with enhanced safety and cytotoxic profile. However, because of increased emphasis on the clinical relevance of metal-based complexes, a few of these drugs are currently on clinical trial and many more are awaiting ethical approval to join the trial. In this review, we seek to give an overview of previous reviews on the cytotoxic effect of metal-based complexes while focusing more on newly designed metal-based complexes and their cytotoxic effect on the cancer cell lines, as well as on new approach to metal-based drug design and molecular target in cancer therapy. We are optimistic that the concept of selective

  7. Characterization of the Unusual Product from the Reaction between Cobalt(II) Chloride, Ethane-1,2-diamine, and Hydrochloric Acid: An Undergraduate Project Involving an Unknown Metal Complex.

    Curtis, Neil F.; And Others

    1986-01-01

    Discusses the need for student research-type chemistry projects based upon "unknown" metal complexes. Describes an experiment involving the product from the reaction between cobalt(II) chloride, ethane-1,2-diamine (en) and concentrated hydrochloric acid. Outlines the preparation of the cobalt complex, along with procedure, results and…

  8. Preparation and toxicity evaluation of a novel nattokinase-tauroursodeoxycholate complex

    Rui Feng

    2018-03-01

    Full Text Available Nattokinase (NK, which has been identified as a potent fibrinolytic protease, has remarkable potential in treatment of thrombolysis, and even has the ability to ameliorate chronic vein thrombosis. To reduce the hemorrhagic risk from an intravenous injection of NK, nattokinase-tauroursodeoxycholate (NK-TUDCA complex was prepared at different pH values and with different ratios of NK and TUDCA. When assessing survival time, survival state, tail injury, and the body weight of mice, it was found that the NK-TUDCA complex (NK: 10 kIU/ml; TUDCA: 10 mg/ml; pH 5.0 had a lower toxicity when administered at an NK dosage of 130 kIU/kg in the acute toxicity test and 13 kIU/kg in the repeated low-dose challenge. From the results of the in vitro thrombolytic test and characterization of NK-TUDCA, we speculated that the delayed release of NK-TUDCA might be the main cause of toxicity reduction by the complex. This study described the preparation of an NK complex with low toxicity following intravenous administration, which could be utilized for further clinical study of NK. Keywords: Nattokinase, Tauroursodeoxycholate, Complex, Toxicity test, In vitro thrombolytic test

  9. Preparation, characterization, and anti-Helicobacter pylori activity of Bi3+-Hericium erinaceus polysaccharide complex.

    Zhu, Yang; Chen, Yao; Li, Qian; Zhao, Ting; Zhang, Ming; Feng, Weiwei; Takase, Mohammed; Wu, Xueshan; Zhou, Zhaoxiang; Yang, Liuqing; Wu, Xiangyang

    2014-09-22

    Two new Bi3+-Hericium erinaceus polysaccharide (BiHEP) complexes were prepared using Bi3+ and two purified polysaccharides from H. erinaceus (HEPs), respectively. The complexes were characterized by elemental analysis, FT-IR, CD, SEM, AFM, XRD, and TG. The anti-Helicobacter pylori (Hp) activities in vitro by agar dilution assay of the complexes were evaluated. The molecular weights of HEPs were 197 and 20 kDa, respectively. All the analyses confirmed the formation of new BiHEP complexes with lower content of Bi3+ compared with colloidal bismuth subcitrate (CBS), the most utilized bismuth preparation clinically. Furthermore, HEPs themselves have definite inhibition effects on Hp, and BiHEP complexes have lower content of Bi exhibited strong inhibition effects on Hp (MIC=20 μg/mL), similar to that of CBS with higher content of Bi. The study provides a basis for further development of multiple treatments of Hp infection or new medicines. Copyright © 2014 Elsevier Ltd. All rights reserved.

  10. Interaction of natural complexing agents with soil bound heavy metals -geochemical and environmental technical aspects

    Fischer, K.

    1994-01-01

    The sanitation of heavy metal polluted soils requires the application of an adequate technology, which should be consistent in its ecological aims and methodology. Therefore a research programme has been developed at the 'Institute of Ecological Chemistry' of the 'GSF-Research Center', Neuherberg, which has its starting point in the study of influences of natural organic complexing agents on the chemical activity and dynamic of heavy metals in soils. The groundlaying idea is to elevate the concentration of complexing agents in the soil solution by additional application and possible stimulation of their microbial production to such an extent, that heavy metals will be enhanced solubilized, mobilized and removed together with the seepage water. Batch experiments in order to extract heavy metals from typical soil components (bentonite, peat) by amino acids demonstrate, that removal rates up to 95% can be obtained. (orig.) [de

  11. A molecular mechanics (MM3(96)) force field for metal-amide complexes

    Hay, B.P.; Clement, O.; Sandrone, G.; Dixon, D.A.

    1998-01-01

    A molecular mechanics (MM3(96)) force field is reported for modeling metal complexes of amides in which the amide is coordinated through oxygen. This model uses a points-on-a-sphere approach which involves the parameterization of the Msingle bondO stretch, the Msingle bondO double-bond C bend, and the Msingle bondO double-bond Csingle bondX (X = C, H, N) torsion interactions. Relationships between force field parameters and metal ion properties (charge, ionic radius, and electronegativity) are presented that allow the application of this model to a wide range of metal ions. The model satisfactorily reproduces the structures of over fifty amide complexes with the alkaline earths, transition metals, lanthanides, and actinides

  12. Preparation of tin -heparin complex to be applied for myocardial infarct diagnosis

    Badi, J. M.; Al-Azzawi, H. A.; Resen, H. M.; Abed, I. G.; Owiad, H.; Manji, A. N.

    2012-12-01

    Tin-heparin complex has been prepared (liquid form) to be labeled with technetium-99 can be applied for diagnosis of myocardial infarcts vascular diseases and deep vein thrombosis. The preparation contents are 0.1mg tin chloride dehydrate and 1250 1.U of heparin. The results of the pH effect on the labeling yield indicated that high percentage of labeling yield (96.1%) was obtained in the optimal pH (5.50). The obtained results showed that the quantity of reducing agent (tin chloride dehydrate) and chelating agent (heparin) has no effect on the labeling yield. Results of radio analytical studies by paper chromatography technique wear confirmed by data obtained by Gel chromatography column scanning techniques. These techniques showed the high labeling yield of the tin-heparin complex. The persistence of high labeling yield for 8 hours is a good indication for its stability and efficiency for radio diagnosis examination in nuclear medicine centers. (Author)

  13. Preparation of lanthanum sulfide nanoparticles by thermal decomposition of lanthanum complex

    LI Peisen; LI Huanyong; JIE Wanqi

    2011-01-01

    γ-La2S3 nanoparticles were successfully prepared by thermal decomposition of lanthanum complex La(Et2S2CN)3·phen at low temperature. The obtained sample was characterized by the X-ray powder diffraction (XRD), scanning electron microscopy (SEM) and element analysis. The decomposition mechanism of lanthanum complex was studied by thermogravimetric analyses (TGA). The results showed that the obtained samples were cubic phase particles with uniform sizes among 10-30 nm and γ-La2S3 was prepared by decomposition of La(Et2S2CN)3 phen via La4(Et2S2CN)3 as an intermediate product. The band gap of γ-La2S3 was 2.97 eV, which was bigger than bulk crystal because of pronounced quantum confinement effect.

  14. Influence of cueing on the preparation and execution of untrained and trained complex motor responses

    S.R. Alouche

    2012-05-01

    Full Text Available This study investigated the influence of cueing on the performance of untrained and trained complex motor responses. Healthy adults responded to a visual target by performing four sequential movements (complex response or a single movement (simple response of their middle finger. A visual cue preceded the target by an interval of 300, 1000, or 2000 ms. In Experiment 1, the complex and simple responses were not previously trained. During the testing session, the complex response pattern varied on a trial-by-trial basis following the indication provided by the visual cue. In Experiment 2, the complex response and the simple response were extensively trained beforehand. During the testing session, the trained complex response pattern was performed in all trials. The latency of the untrained and trained complex responses decreased from the short to the medium and long cue-target intervals. The latency of the complex response was longer than that of the simple response, except in the case of the trained responses and the long cue-target interval. These results suggest that the preparation of untrained complex responses cannot be completed in advance, this being possible, however, for trained complex responses when enough time is available. The duration of the 1st submovement, 1st pause and 2nd submovement of the untrained and the trained complex responses increased from the short to the long cue-target interval, suggesting that there is an increase of online programming of the response possibly related to the degree of certainty about the moment of target appearance.

  15. Metal distributions in complexes with Chlorella vulgaris in seawater and wastewater

    Pascucci, P.R.; Kowalak, A.D.

    1999-10-01

    Divalent cadmium (Cd), copper (Cu), iron (Fe), nickel (Ni), lead (Pb), and zinc (Zn) simultaneous complexes with an algal biomass Chlorella vulgaris were studied for bioremediation purposes in various aqueous media: distilled-deionized water (DDIW), seawater, nuclear-reactor pool water, and process wastewater. Reactions were monitored using various dry masses of algae at constant temperature and constant metal concentrations for reaction times ranging from 0 to 150 minutes. Complexes occurred within 30 minutes and reached a steady state after 80 to 120 minutes. Distribution constants (K{prime}{sub d}) were calculated for the complexes and relative orders of K{prime}{sub d} were reported. The K{prime}{sub d} are used to evaluate relative efficiency of metal remediation from waters. Lead, Cu, and Ni complexes had the greatest K{prime}{sub d} values and those metals were most efficiently removed from these waters. Zinc and Fe formed the most labile complexes. The order of K{prime}{sub d} values for complexes in DDIW was Pb > Cu > Cd > Zn, then Cu > Cd > Zn in seawater, Cd > Cu > Zn in reactor pool water, and Ni > Cd > Cu > Zn > Fe in wastewater. C. vulgaris biomass may potentially be used as an alternative to traditional water treatment methods for simultaneous extraction of metals from seawater, process wastewater, or drinking water.

  16. Synthesis, Characterization and Biological Evaluation of Transition Metal Complexes Derived from N, S Bidentate Ligands

    Enis Nadia Md Yusof

    2015-05-01

    Full Text Available Two bidentate NS ligands were synthesized by the condensation reaction of S-2-methylbenzyldithiocarbazate (S2MBDTC with 2-methoxybenzaldehyde (2MB and 3-methoxybenzaldehyde (3MB. The ligands were reacted separately with acetates of Cu(II, Ni(II and Zn(II yielding 1:2 (metal:ligand complexes. The metal complexes formed were expected to have a general formula of [M(NS2] where M = Cu2+, Ni2+, and Zn2+. These compounds were characterized by elemental analysis, molar conductivity, magnetic susceptibility and various spectroscopic techniques. The magnetic susceptibility measurements and spectral results supported the predicted coordination geometry in which the Schiff bases behaved as bidentate NS donor ligands coordinating via the azomethine nitrogen and thiolate sulfur. The molecular structures of the isomeric S2M2MBH (1 and S2M3MBH (2 were established by X-ray crystallography to have very similar l-shaped structures. The Schiff bases and their metal complexes were evaluated for their biological activities against estrogen receptor-positive (MCF-7 and estrogen receptor-negative (MDA-MB-231 breast cancer cell lines. Only the Cu(II complexes showed marked cytotoxicity against the cancer cell lines. Both Schiff bases and other metal complexes were found to be inactive. In concordance with the cytotoxicity studies, the DNA binding studies indicated that Cu(II complexes have a strong DNA binding affinity.

  17. Preparation and Property of Acrylic Acid Rare Earth Complex and Its Hydrosilylation

    Zhang Ming; Chen Haiyan; Chen Xiaosong; Dai Shaojun; Inoue Shinich; Okamoto Hiroshi

    2004-01-01

    Acrylic acid rare earth complex was prepared. Its chemical composition was determined by chemical and elemental analysis, and its structure as well as properties was characterized using IR, Fluorescence and UV spectrum, and its solubility was also investigated. Meanwhile a kind of elastic functional polymer with rare earth units in the side chains was produced. It is confirmed by IR spectrum that the Si-H bonds really react with acrylic acid rare earth.

  18. Polyelectrolyte Complex Nanoparticles of Poly(ethyleneimine) and Poly(acrylic acid): Preparation and Applications

    Martin Müller; Bernd Keßler; Sebastian Poeschla; Bernhard Torger; Johanna Fröhlich

    2011-01-01

    In this contribution we outline polyelectrolyte (PEL) complex (PEC) nanoparticles, prepared by mixing solutions of the low cost PEL components poly(ethyleneimine) (PEI) and poly(acrylic acid) (PAC). It was found, that the size and internal structure of PEI/PAC particles can be regulated by process, media and structural parameters. Especially, mixing order, mixing ratio, PEL concentration, pH and molecular weight, were found to be sensible parameters to regulate the size (diameter) of spherica...

  19. Preparation and Characterization of Starch-g-PVA/Nano-hydroxyapatite Complex Hydrogel

    2005-01-01

    Starch-g-PVA/hydroxyapatite complex hydrogel was prepared with two-repeated freezing/ thawing circles. SEM observation results exhibits that hydroxyapatite is dispersed in starch-g-PVA in nanoscale. Thermogravimetric analysis curves show that the remained fraction keeps the same at the temperatures higher than 490℃ . It was found the dried starch-g- PVA/ hydroxyapatite films could reswell within 12 minutes.

  20. Physical-chemical and biocatalytic properties of a proteolytic complex of the preparation "Protepsin"

    L. V. Antipova

    2016-01-01

    Full Text Available Enzymatic technologies were included strongly into practical activities of the person, the volume of the world market constantly grows and is updated. However the domestic production of enzymatic preparations very lags behind world level that is in many respects connected with insufficient scientific and technical base for a wide circulation of technologies in large-scale production. At the same time there were Russian producers of enzymatic preparations from animal fabrics and bodies for processing of raw materials of an animal origin, according to forecasts, of interest in rational use of resources of an animal origin. In article data on research of properties of the enzymatic preparation "Protepsin" and an assessment of prospects of application are provided in processing of raw materials of an animal origin. The enzymatic preparation "Protepsin" made in the conditions of JSC Plant of Endocrine Enzymes (Rzhavki, Moscow region activity at action on proteins of meat shows, including the strengthened structure, has milk-clotting effect, is active in the field of pH 4,0-6,0 and temperature 20-45zs. The proteinaceous complex includes 4 fractions, 2 from which possess the general proteolytic activity. One of them shows the general proteolytic and milk-clotting activity. Enzymes differ in an amino-acid set and molecular weight. The method of a disk electrophoresis determined molecular-mass structure of "Protepsin". The preparation inactivation conditions guaranteeing its safety in the production technology of foodstuff as active proteolytic enzymes in the course of digestion can cause violations of integrity of fabrics and corresponding diseases are shown. Thus, conditions of use of a perspective proteolytic preparation in technology of a wide range of food of an animal origin are in a complex proved and picked up.

  1. Nanocomposite metal/plasma polymer films prepared by means of gas aggregation cluster source

    Polonskyi, O.; Solar, P.; Kylian, O.; Drabik, M.; Artemenko, A.; Kousal, J.; Hanus, J.; Pesicka, J.; Matolinova, I. [Charles University in Prague, Faculty of Mathematics and Physics, V Holesovickach 2, 18000 Prague 8 (Czech Republic); Kolibalova, E. [Tescan, Libusina trida 21, 632 00 Brno (Czech Republic); Slavinska, D. [Charles University in Prague, Faculty of Mathematics and Physics, V Holesovickach 2, 18000 Prague 8 (Czech Republic); Biederman, H., E-mail: bieder@kmf.troja.mff.cuni.cz [Charles University in Prague, Faculty of Mathematics and Physics, V Holesovickach 2, 18000 Prague 8 (Czech Republic)

    2012-04-02

    Nanocomposite metal/plasma polymer films have been prepared by simultaneous plasma polymerization using a mixture of Ar/n-hexane and metal cluster beams. A simple compact cluster gas aggregation source is described and characterized with emphasis on the determination of the amount of charged clusters and their size distribution. It is shown that the fraction of neutral, positively and negatively charged nanoclusters leaving the gas aggregation source is largely influenced by used operational conditions. In addition, it is demonstrated that a large portion of Ag clusters is positively charged, especially when higher currents are used for their production. Deposition of nanocomposite Ag/C:H plasma polymer films is described in detail by means of cluster gas aggregation source. Basic characterization of the films is performed using transmission electron microscopy, ultraviolet-visible and Fourier-transform infrared spectroscopies. It is shown that the morphology, structure and optical properties of such prepared nanocomposites differ significantly from the ones fabricated by means of magnetron sputtering of Ag target in Ar/n-hexane mixture.

  2. Highly Active Non-PGM Catalysts Prepared from Metal Organic Frameworks

    Heather M. Barkholtz

    2015-06-01

    Full Text Available Finding inexpensive alternatives to platinum group metals (PGMs is essential for reducing the cost of proton exchange membrane fuel cells (PEMFCs. Numerous materials have been investigated as potential replacements of Pt, of which the transition metal and nitrogen-doped carbon composites (TM/Nx/C prepared from iron doped zeolitic imidazolate frameworks (ZIFs are among the most active ones in catalyzing the oxygen reduction reaction based on recent studies. In this report, we demonstrate that the catalytic activity of ZIF-based TM/Nx/C composites can be substantially improved through optimization of synthesis and post-treatment processing conditions. Ultimately, oxygen reduction reaction (ORR electrocatalytic activity must be demonstrated in membrane-electrode assemblies (MEAs of fuel cells. The process of preparing MEAs using ZIF-based non-PGM electrocatalysts involves many additional factors which may influence the overall catalytic activity at the fuel cell level. Evaluation of parameters such as catalyst loading and perfluorosulfonic acid ionomer to catalyst ratio were optimized. Our overall efforts to optimize both the catalyst and MEA construction process have yielded impressive ORR activity when tested in a fuel cell system.

  3. Synthesis, structure, DNA/BSA binding and antibacterial studies of NNO tridentate Schiff base metal complexes

    Sakthi, Marimuthu; Ramu, Andy

    2017-12-01

    A new salicylaldehyde derived 2,4-diiodo-6-((2-phenylaminoethylimino)methyl)phenol Schiff base(L) and its transition metal complexes of the type MLCl where, M = Cu(II), Ni(II), Co(II), Mn(II) and Zn(II) have been synthesized. The coordination mode of Schiff base holding NNO donor atoms with metal ions was well investigated by elemental analysis, ESI-mass as well as IR, UV-vis, CV and NMR spectral studies. The binding efficiency and mode of these complexes with biological macromolecules viz., herring sperm DNA (HS- DNA) and bovine serum albumin (BSA) have been explored through various spectroscopic techniques. The characteristic changes in absorption, emission and, circular dichroism spectra of the complexes with DNA indicate the noticeable interaction between them. From the all spectral information complexes could interact with DNA via non-intercalation mode of binding. The hyperchromisim in absorption band and hypochromisim in emission intensity of BSA with different complex concentrations shown significant information, and the binding affinity value has been predicted from Stern-Volmer plots. Further, all the complexes could cleave the circular plasmid pUC19 DNA efficiently by using an activator H2O2. The ligand and all metal(II) complexes showed good antibacterial activities. The molecular docking studies of the complexes with DNA were performed in order to make a comparison and conclusion with spectral technic results.

  4. Preparation and Properties of 3D Printed Alginate–Chitosan Polyion Complex Hydrogels for Tissue Engineering

    Qiongqiong Liu

    2018-06-01

    Full Text Available Three-dimensional (3D printing holds great potential for preparing sophisticated scaffolds for tissue engineering. As a result of the shear thinning properties of an alginate solution, it is often used as 3D printing ink. However, it is difficult to prepare scaffolds with complexity structure and high fidelity, because the alginate solution has a low viscosity and alginate hydrogels prepared with Ca2+ crosslinking are mechanically weak. In this work, chitosan powders were dispersed and swelled in an alginate solution, which could effectively improve the viscosity of an alginate solution by 1.5–4 times. With the increase of chitosan content, the shape fidelity of the 3D printed alginate–chitosan polyion complex (AlCh PIC hydrogels were improved. Scanning electron microscope (SEM photographs showed that the lateral pore structure of 3D printed hydrogels was becoming more obvious. As a result of the increased reaction ion pairs in comparison to the alginate hydrogels that were prepared with Ca2+ crosslinking, AlCh PIC hydrogels were mechanically strong, and the compression stress of hydrogels at a 90% strain could achieve 1.4 MPa without breaking. In addition, human adipose derived stem cells (hASCs adhered to the 3D printed AlCh PIC hydrogels and proliferated with time, which indicated that the obtained hydrogels were biocompatible and could potentially be used as scaffolds for tissue engineering.

  5. High-performance liquid chromatography of metal complexes of pheophytins a and b

    Brykina, G.D.; Lazareva, E.E.; Uvarova, M.I.; Shpigun, O.A.

    1997-01-01

    Cu(2), Zn(2), Pb(2), Hg(2), and Ce(4) complexes of phenophytins a and b were synthesized. The chromatographic retention parameters of pheophytins a and b, chlorophylls a and b, and the above complexes were determined under conditions of normal-phase and reversed-phase high-performance liquid chromatography (HPLC). The adsorption of metal pheophytinates in the hexane-n-butanol (96:4)-Silasorb 600 and acetonitrile-ethanol-acetic acid (40:40:16)-Nucleosil C 18 systems was studied by HPLC. Factors that affect the chromatographic and adsorption characteristics of compounds (structural differences between pheophytinates of the a and b series, the nature of the central metal atom, and the nature of the mobile and stationary phases) are discussed. It is demonstrated that pheophytins a and b their metal complexes can be identified and quantiatively determined by HPLC in the concentration range (0.6-44.0)[10 -6 M

  6. Structural and Spectral Properties of Curcumin and Metal- Curcumin Complex Derived from Turmeric (Curcuma longa)

    Bich, Vu Thi; Thuy, Nguyen Thi; Binh, Nguyen Thanh; Huong, Nguyen Thi Mai; Yen, Pham Nguyen Dong; Luong, Tran Thanh

    Structural and spectral properties of curcumin and metal- curcumin complex derived from turmeric (Curcuma longa) were studied by SEM and vibrational (FTIR and Raman) techniques. By comparison between curcumin commercial, fresh turmeric and a yellow powder obtained via extraction and purification of turmeric, we have found that this insoluble powder in water is curcumin. The yellow compound could complex with certain ion metal and this metal-curcumin coloring complex is water soluble and capable of producing varying hues of the same colors and having antimicrobial, cytotoxicity activities for use in foodstuffs and pharmacy. The result also demonstrates that Micro-Raman spec-troscopy is a valuable non-destructive tool and fast for investigation of a natural plant even when occurring in low concentrations.

  7. New trends in the optical and electronic applications of polymers containing transition-metal complexes.

    Liu, Shu-Juan; Chen, Yang; Xu, Wen-Juan; Zhao, Qiang; Huang, Wei

    2012-04-13

    Polymers containing transition-metal complexes exhibit excellent optical and electronic properties, which are different from those of polymers with a pure organic skeleton and combine the advantages of both polymers and metal complexes. Hence, research about this class of polymers has attracted more and more interest in recent years. Up to now, a number of novel polymers containing transition-metal complexes have been exploited, and significant advances in their optical and electronic applications have been achieved. In this article, we summarize some new research trends in the applications of this important class of optoelectronic polymers, such as chemo/biosensors, electronic memory devices and photovoltaic devices. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Kinetic studies of the solvent extraction of metal complexes

    Mirza, M.Y.; Nwabue, F.I.; Okafo, E.N.

    1981-01-01

    The rate of forward extraction of Zr(IV) from 2M sulphuric acid into 1-phenyl-3-methyl-4-benzoyl-pyrazole-5-one (HPsub (z)) dissolved in chloroform and backward extraction of the tetrakis-chelate, Zr(Pz) 4 have been measured under various conditions. The rate of forward reaction is proportional to [Zr 4+ ], [HPsub(z)] 2 and [H + ] -2 , while that of back extraction to [Zr(Pz) 4 ]sub(org), [HPsub(z)] -2 sub(org) and [H + ] 2 . The rate determining step in the forward extraction is established to be the formation of the second complex between the dissociated form of HPz, Pz - and the Zr(H 2 O) 2 SO 4 Pz + species in the aqueous phase while it is the reverse in the backward extraction. The velocity constants for both rate controlling steps have been determined and the extraction constant agrees with the value obtained from the equilibrium data. (author)

  9. Paramagnetic metal complexes as potential relaxation agents for NMR imaging

    Coroiu, Ilioara; Demco, D. E.; Darabont, Al.; Bogdan, M.

    1997-01-01

    The development of nuclear magnetic resonance (NMR) imaging technique as a clinical diagnostic modality has prompted the need for a new class of pharmaceuticals. These drugs must be administered to a patient in order to enhance the image contrast between the normal and diseased tissue and/or indicate the status of organ function or blood flow. Paramagnetic compounds are presently undergoing extensive evaluation as contrast agents in magnetic resonance imaging (MRI). These agents increase contrast in MRI by differentially localizing in tissue where they increase the relaxation rates of nearby water protons. The longitudinal R 1 and transverse R 2 relaxivities were measured as a function of molar concentrations for some new paramagnetic complexes like the following: dysprosium, erbium and gadolinium citrates, gadolinium methylene diphosphonate, dysprosium and gadolinium iminodiacetate, manganese para-aminobenzoate and copper nicotinate. The available theoretical approaches for quantitative understanding are presented. (authors)

  10. Alkali Metal Variation and Twisting of the FeNNFe Core in Bridging Diiron Dinitrogen Complexes.

    McWilliams, Sean F; Rodgers, Kenton R; Lukat-Rodgers, Gudrun; Mercado, Brandon Q; Grubel, Katarzyna; Holland, Patrick L

    2016-03-21

    Alkali metal cations can interact with Fe-N2 complexes, potentially enhancing back-bonding or influencing the geometry of the iron atom. These influences are relevant to large-scale N2 reduction by iron, such as in the FeMoco of nitrogenase and the alkali-promoted Haber-Bosch process. However, to our knowledge there have been no systematic studies of a large range of alkali metals regarding their influence on transition metal-dinitrogen complexes. In this work, we varied the alkali metal in [alkali cation]2[LFeNNFeL] complexes (L = bulky β-diketiminate ligand) through the size range from Na(+) to K(+), Rb(+), and Cs(+). The FeNNFe cores have similar Fe-N and N-N distances and N-N stretching frequencies despite the drastic change in alkali metal cation size. The two diketiminates twist relative to one another, with larger dihedral angles accommodating the larger cations. In order to explain why the twisting has so little influence on the core, we performed density functional theory calculations on a simplified LFeNNFeL model, which show that the two metals surprisingly do not compete for back-bonding to the same π* orbital of N2, even when the ligand planes are parallel. This diiron system can tolerate distortion of the ligand planes through compensating orbital energy changes, and thus, a range of ligand orientations can give very similar energies.

  11. Preparation and characterization of simvastatin/DMβCD complex and its pharmacokinetics in rats

    Gu Fugen

    2018-06-01

    Full Text Available Simvastatin is poorly bioavailable because it is practically insoluble in water and shows dissolution rate-limited absorption. Solubilizing effects of several β-cyclodextrin (βCD derivatives such as HPβCD, SBEβCD and DMβCD on simvastatin in aqueous solution were investigated using the phase solubility technique. The solubility diagram of simvastatin with each βCD derivative could be classified as AL-type, indicating soluble complex formation of 1:1 stoichiometry. Among the above βCD derivatives DMβCD was found to be the ideal complexing agent for improving drug solubility. The simvastatin complex with DMβCD was prepared using the co-evaporation method and was then characterized by differential scanning calorimetry (DSC, Fourier-transform infrared spectroscopy (FT-IR and in vitro dissolution. Dissolution and pharmacokinetic studies indicated that the simvastatin/DMβCD complex exhibited an increased dissolution rate, rapid absorption, and improved bioavailability in rats compared to free drug. Maximum plasma concentration (cmax and the time to reach it (tmax were 21.86 μg mL−1 and 1.4 h for the drug complex, 8.25 μg mL−1 and 3.0 h for free drug, respectively. Main pharmacokinetic parameters such as tmax, cmax were significantly different (p < 0.01 between the simvastatin complex and free drug. Bioavailability of the simvastatin complex relative to free drug was up to 167.0 %.

  12. Preparation and characterization of expanded graphite/metal oxides for antimicrobial application.

    Hung, Wei-Che; Wu, Kuo-Hui; Lyu, Dong-Yi; Cheng, Ken-Fa; Huang, Wen-Chien

    2017-06-01

    Composite materials based on expanded graphite (EG) and metal oxide (MO) particles was prepared by an explosive combustion and blending method. The objective of the study was to develop EG impregnated with metal oxide particulates (Ag 2 O, CuO and ZnO) and evaluate the level of protection the materials conferred against biological agents. The physical properties of the EG/MO composites were examined using SEM, EDX and XRD spectroscopy, and the results indicated that the MO particles were incorporated into the EG matrix after impregnation. The antimicrobial activities of the EG/MO composites against Gram-positive bacteria, Gram-negative bacteria and Bacillus anthracis were investigated using zone of inhibition, minimum inhibitory concentration (MIC), minimum bactericidal concentration (MBC) and plate-counting methods. EG/Ag 2 O exhibited a stronger antibacterial activity than EG/CuO and EG/ZnO, with a MIC of 0.3mg/mL and a MBC of 0.5mg/mL. To the best of our knowledge, few studies have demonstrated that EG/MO composites can inhibit the growth of Bacillus anthracis-adhered cells, thus preventing the process of biofilm formation. Nanoscale metal oxides display enhanced reactive properties toward bacteria due to their high surface area, large number of highly reactive edges, corner defect sites and high surface to volume ratio. Copyright © 2017 Elsevier B.V. All rights reserved.

  13. Visible light active TiO2 films prepared by electron beam deposition of noble metals

    Hou Xinggang; Ma Jun; Liu Andong; Li Dejun; Huang Meidong; Deng Xiangyun

    2010-01-01

    TiO 2 films prepared by sol-gel method were modified by electron beam deposition of noble metals (Pt, Pd, and Ag). Effects of noble metals on the chemical and surface characteristics of the films were studied using XPS, TEM and UV-Vis spectroscopy techniques. Photocatalytic activity of modified TiO 2 films was evaluated by studying the degradation of methyl orange dye solution under visible light UV irradiation. The result of TEM reveals that most of the surface area of TiO 2 is covered by tiny particles of noble metals with diameter less than 1 nm. Broad red shift of UV-Visible absorption band of modified photocatalysts was observed. The catalytic degradation of methyl orange in aqueous solutions under visible light illumination demonstrates a significant enhancement of photocatalytic activity of these films compared with the un-loaded films. The photocatalytic efficiency of modified TiO 2 films by this method is affected by the concentration of impregnating solution.

  14. Preparation, thermal stability, and magnetic properties of Fe-Zr-Mo-W-B bulk metallic glass

    Liu, D.Y.; Sun, W.S.; Wang, A.M.; Zhang, H.F.; Hu, Z.Q.

    2004-01-01

    A bulk metallic glass (BMG) cylinder of Fe 60 Co 8 Zr 10 Mo 5 W 2 B 15 with a diameter of 1.5 mm was prepared by copper mould casting of industrial raw materials. The amorphous state and the crystallization behavior were investigated by X-ray diffraction (XRD). The thermal stability parameters, such as glass transition temperature (T g ), crystallization temperature (T x ), supercooled liquid region (ΔT x ) between T g and T x , and reduced glass transition temperature T rg (T g /T m ) were measured by differential scanning calorimetry (DSC) to be 891, 950, 59 K, and 0.62, respectively. The crystallization process took place through a single stage, and involved crystallization of the phases α-Fe, ZrFe 2 , Fe 3 B, MoB 2 , Mo 2 FeB 2 , and an unknown phase, as determined by X-ray analysis of the sample annealed for 1.5 ks at 1023 K, 50 K above the DSC peak temperature of crystallization. Moessbauer spectroscopy was studied for this alloy. The spectra exhibit a broadened and asymmetric doublet-like structure that indicated paramagnetic behavior and a fully amorphous structure. α-Fe was found in the amorphous matrix for a cylinder with a diameter of 2.5 mm. The success of synthesis of the Fe-based bulk metallic glass from industrial materials is important for the future progress in research and practical application of new bulk metallic glasses

  15. Preparation and characterisation of biodegradable pollen-chitosan microcapsules and its application in heavy metal removal.

    Sargın, İdris; Kaya, Murat; Arslan, Gulsin; Baran, Talat; Ceter, Talip

    2015-02-01

    Biosorbents have been widely used in heavy metal removal. New resources should be exploited to develop more efficient biosorbents. This study reports the preparation of three novel chitosan microcapsules from pollens of three common, wind-pollinated plants (Acer negundo, Cupressus sempervirens and Populus nigra). The microcapsules were characterized (Fourier transform infrared spectroscopy, thermogravimetric analysis, scanning electron microscopy and elemental analysis) and used in removal of heavy metal ions: Cd(II), Cr(III), Cu(II), Ni(II) and Zn(II). Their sorption capacities were compared to those of cross-linked chitosan beads without pollen grains. C. sempervirens-chitosan microcapsules exhibited better performance (Cd(II): 65.98; Cu(II): 67.10 and Zn(II): 49.55 mg g(-1)) than the other microcapsules and the cross-linked beads. A. negundo-chitosan microcapsules were more efficient in Cr(III) (70.40 mg g(-1)) removal. P. nigra-chitosan microcapsules were found to be less efficient. Chitosan-pollen microcapsules (except P. nigra-chitosan microcapsules) can be used in heavy metal removal. Copyright © 2014 Elsevier Ltd. All rights reserved.

  16. Nanotubes within transition metal silicate hollow spheres: Facile preparation and superior lithium storage performances

    Zhang, Fan; An, Yongling; Zhai, Wei; Gao, Xueping [Key Laboratory for Liquid–Solid Structural Evolution & Processing of Materials (Ministry of Education), Jinan 250100 (China); Feng, Jinkui, E-mail: jinkui@sdu.edu.cn [Key Laboratory for Liquid–Solid Structural Evolution & Processing of Materials (Ministry of Education), Jinan 250100 (China); Ci, Lijie [Key Laboratory for Liquid–Solid Structural Evolution & Processing of Materials (Ministry of Education), Jinan 250100 (China); Xiong, Shenglin [School of Materials Science and Engineering, School of Chemistry and Chemical Engineering, Shandong University, Jinan 250100 (China)

    2015-10-15

    Highlights: • The hollow Co{sub 2}SiO{sub 4}, MnSiO{sub 3} and CuSiO{sub 3} were successfully prepared by a facile hydrothermal method using SiO{sub 2} nanosphere. • The hollow Co{sub 2}SiO{sub 4}, MnSiO{sub 3} and CuSiO{sub 3} were tested as anode materials for lithium batteries. • The hollow Co{sub 2}SiO{sub 4}, MnSiO{sub 3} and CuSiO{sub 3} delivered superior electrochemical performance. • The lithium storage mechanism is probe via cyclic voltammetry and XPS. - Abstract: A series of transition metal silicate hollow spheres, including cobalt silicate (Co{sub 2}SiO{sub 4}), manganese silicate (MnSiO{sub 3}) and copper silicate (CuSiO{sub 3}.2H{sub 2}O, CuSiO{sub 3} as abbreviation in the text) were prepared via a simple and economic hydrothermal method by using silica spheres as chemical template. Time-dependent experiments confirmed that the resultants formed a novel type of hierarchical structure, hollow spheres assembled by numerous one-dimensional (1D) nanotubes building blocks. For the first time, the transition metal silicate hollow spheres were characterized as novel anode materials of Li-ion battery, which presented superior lithium storage capacities, cycle performance and rate performance. The 1D nanotubes assembly and hollow interior endow this kind of material facilitate fast lithium ion and electron transport and accommodate the big volume change during the conversion reactions. Our study shows that low-cost transition metal silicate with rationally designed nanostructures can be promising anode materials for high capacity lithium-ion battery.

  17. A novel method for preparation of HAMLET-like protein complexes.

    Permyakov, Sergei E; Knyazeva, Ekaterina L; Leonteva, Marina V; Fadeev, Roman S; Chekanov, Aleksei V; Zhadan, Andrei P; Håkansson, Anders P; Akatov, Vladimir S; Permyakov, Eugene A

    2011-09-01

    Some natural proteins induce tumor-selective apoptosis. α-Lactalbumin (α-LA), a milk calcium-binding protein, is converted into an antitumor form, called HAMLET/BAMLET, via partial unfolding and association with oleic acid (OA). Besides triggering multiple cell death mechanisms in tumor cells, HAMLET exhibits bactericidal activity against Streptococcus pneumoniae. The existing methods for preparation of active complexes of α-LA with OA employ neutral pH solutions, which greatly limit water solubility of OA. Therefore these methods suffer from low scalability and/or heterogeneity of the resulting α-LA - OA samples. In this study we present a novel method for preparation of α-LA - OA complexes using alkaline conditions that favor aqueous solubility of OA. The unbound OA is removed by precipitation under acidic conditions. The resulting sample, bLA-OA-45, bears 11 OA molecules and exhibits physico-chemical properties similar to those of BAMLET. Cytotoxic activities of bLA-OA-45 against human epidermoid larynx carcinoma and S. pneumoniae D39 cells are close to those of HAMLET. Treatment of S. pneumoniae with bLA-OA-45 or HAMLET induces depolarization and rupture of the membrane. The cells are markedly rescued from death upon pretreatment with an inhibitor of Ca(2+) transport. Hence, the activation mechanisms of S. pneumoniae death are analogous for these two complexes. The developed express method for preparation of active α-LA - OA complex is high-throughput and suited for development of other protein complexes with low-molecular-weight amphiphilic substances possessing valuable cytotoxic properties. Copyright © 2011 Elsevier Masson SAS. All rights reserved.

  18. Pesticides Curbing Soil Fertility: Effect of Complexation of Free Metal Ions

    Kaur, Sukhmanpreet

    2017-07-04

    Researchers have suggested that the reason behind infertility is pernicious effect of broad spectrum pesticides on non target, beneficial microorganism of soil. Here, studying the chelating effect of selective organophosphate and carbamate pesticides with essential metal ions, at all possible combinations of three different pH (4 ± 0.05, 7 ± 0.05 and 9 ± 0.05) and three different temperatures (15 ± 0.5°C, 30 ± 0.5°C and 45 ± 0.5°C), shows very fast rate of reaction which further increases with increase of pH and temperature. Carbonyl oxygen of carbamate and phosphate oxygen of organophosphate were found to be common ligating sites among all the complexes. Formed metal complexes were found to be highly stable and water insoluble on interaction with essential metal ions in solvent medium as well as over silica. Density functional theory (DFT) calculations not only reinforced the experimental observations, but, after a wide computational conformational analysis, unraveled the nature of the high stable undesired species that consist of pesticides complexed by metal ions from the soil. All in all, apart from the direct toxicity of pesticides, the indirect effect by means of complexation of free metal ions impoverishes the soil.

  19. Pesticides Curbing Soil Fertility: Effect of Complexation of Free Metal Ions

    Kaur, Sukhmanpreet; Kumar, Vijay; Chawla, Mohit; Cavallo, Luigi; Poater, Albert; Upadhyay, Niraj

    2017-07-01

    Researchers have suggested that the reason behind infertility is pernicious effect of broad spectrum pesticides on non target, beneficial microorganism of soil. Here, studying the chelating effect of selective organophosphate and carbamate pesticides with essential metal ions, at all possible combinations of three different pH (4±0.05, 7±0.05 and 9±0.05) and three different temperatures (15±0.5°C, 30±0.5°C and 45±0.5°C), shows very fast rate of reaction which further increases with increase of pH and temperature. Carbonyl oxygen of carbamate and phosphate oxygen of organophosphate were found to be common ligating sites among all the complexes. Formed metal complexes were found to be highly stable and water insoluble on interaction with essential metal ions in solvent medium as well as over silica. Density functional theory (DFT) calculations not only reinforced the experimental observations, but, after a wide computational conformational analysis, unraveled the nature of the high stable undesired species that consist of pesticides complexed by metal ions from the soil. All in all, apart from the direct toxicity of pesticides, the indirect effect by means of complexation of free metal ions impoverishes the soil.

  20. Pesticides Curbing Soil Fertility: Effect of Complexation of Free Metal Ions

    Kaur, Sukhmanpreet; Kumar, Vijay; Chawla, Mohit; Cavallo, Luigi; Poater, Albert; Upadhyay, Niraj

    2017-01-01

    Researchers have suggested that the reason behind infertility is pernicious effect of broad spectrum pesticides on non target, beneficial microorganism of soil. Here, studying the chelating effect of selective organophosphate and carbamate pesticides with essential metal ions, at all possible combinations of three different pH (4 ± 0.05, 7 ± 0.05 and 9 ± 0.05) and three different temperatures (15 ± 0.5°C, 30 ± 0.5°C and 45 ± 0.5°C), shows very fast rate of reaction which further increases with increase of pH and temperature. Carbonyl oxygen of carbamate and phosphate oxygen of organophosphate were found to be common ligating sites among all the complexes. Formed metal complexes were found to be highly stable and water insoluble on interaction with essential metal ions in solvent medium as well as over silica. Density functional theory (DFT) calculations not only reinforced the experimental observations, but, after a wide computational conformational analysis, unraveled the nature of the high stable undesired species that consist of pesticides complexed by metal ions from the soil. All in all, apart from the direct toxicity of pesticides, the indirect effect by means of complexation of free metal ions impoverishes the soil.