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Sample records for chemical synthesis characterization

  1. Synthesis and Characterization of Chemically Etched Nanostructured Silicon

    KAUST Repository

    Mughal, Asad Jahangir

    2012-05-01

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

  2. Chemical Synthesis and Electrochemical Characterization of Nanoporous Gold films

    DEFF Research Database (Denmark)

    Christiansen, Mikkel U-B; Seselj, Nedjeljko; Engelbrekt, Christian

    Nanoporous gold (NPG) is conventionally made via dealloying methods1. We present an alternative method for bottom-up chemical synthesis of nanoporous gold film (cNPGF), with properties resembling those of dealloyed NPG. The developed procedure is simple and only benign chemicals are used....... Chloroauric acid is reduced to nanoparticles (NPs) by 2-(N-morpholino)ethanesulfonate, acting also as a protecting agent for the NPs and as a pH buffer, while potassium chloride is used to control ionic strength. The film formation is controlled by parameters such as temperature, ionic strength...... and protonation of the buffer. Therefore, it is possible to influence the trapping of nanoparticles at the air-liquid interface, yielding porous thin film structures, Figure 1A. The produced cNPGFs have been investigated by atomic force microscopy (AFM), transmission electron microscopy (TEM) and cyclic...

  3. Radiation chemical synthesis and characterization of UO 2 nanoparticles

    Science.gov (United States)

    Roth, Olivia; Hasselberg, Hanna; Jonsson, Mats

    2009-01-01

    In a deep repository for spent nuclear fuel, U(VI)(aq) released upon dissolution of the fuel matrix could, in reducing parts of the system, be converted to U(IV) species which might coalesce and form nanometer-sized UO 2 particles. This type of particles is expected to have different properties compared to bulk UO 2(s). Hence, their properties, in particular the capacity for oxidant consumption, must be investigated in order to assess the effects of formation of such particles in a deep repository. In this work, methods for radiation chemical synthesis of nanometer-sized UO 2 particles, by electron- and γ-irradiation of U(VI) solutions, are presented. Electron-irradiation proved to be the most efficient method, showing high conversions of U(VI) and yielding small particles with a narrow size distribution (22-35 nm). Stable colloidal suspensions were obtained at low pH and ionic strength (pH 3, I = 0.03). Furthermore, the reactivity of the produced UO 2 particles towards H 2O 2 is investigated. The U(IV) fraction in the produced particles was found to be ˜20% of the total uranium content, and the results show that the UO 2 nanoparticles are significantly more reactive than micrometer-sized UO 2 when it comes to H 2O 2 consumption, the major part of the H 2O 2 being catalytically decomposed on the particle surface.

  4. Synthesis and characterization of nanoparticles of CZTSe by microwave-assited chemical synthesis

    Science.gov (United States)

    Reyes Vallejo, O.; Sánchez, Mónica; Pal, Mou; Espinal, R.; Llorca, Jordi; Sebastian, P. J.

    2016-12-01

    In this study we present the synthesis of Cu2ZnSnSe4 (CZTSe) nanoparticles by microwave-assisted chemical synthesis employing organic solvents. The effect of reaction time, reactant concentration, solvent and additives (inorganic material) was studied on the structural and optical properties of the nanomaterials. The powder samples were analyzed by x-ray diffraction, Raman spectroscopy, x-ray energy dispersive spectroscopy and x-ray photoelectron spectroscopy. The results show that the synthesis performed with triethanolamine and deionized water is better than others solvents, producing nanocrystals of quaternary phase (CZTSe) with stoichiometric relations similar to the reported research in the literature, which falls in the range of Cu/(Zn+Sn): 0.8-1.0, Zn/Sn: 1.0-1.20. The nanoparticles of CZTSe synthesized in this study present desirable properties in order to use them in solar cell and photoelectrochemical cell applications.

  5. Synthesis and characterization of carbon nanofilms for chemical sensing

    Science.gov (United States)

    Kumar, Vivek

    Carbon nanofilms obtained by high temperature graphitization of diamond surface in inert atmospheres or vacuum are modified by treatment in plasma of different precursor gases. At temperatures above 1000 °C, a stable conductive film of thickness between 10 - 100 nm and specific resistivity 10-3-10-4 Ωm, depending upon the heating conditions and the growth atmosphere, is formed on diamond surface. A gray, thin film of high surface resistivity is obtained in high vacuum, while at low vacuum (below 10-4 mbar), a thick black film of low surface resistivity forms. It is observed that the exposure to plasma reduces the surface conductance of carbon nanofilms as result of a partial removal of carbon and the plasma-stimulated amorphization. The rate of the reduction of conductance and hence the etching ability of plasma depends on the type of precursor gas. Hydrogen reveals the strongest etching ability, followed by oxygen and argon, whereas SF6 is ineffective. The carbon nanofilms show significant sensitivity of their electrical conductance to temperature and exposure to the vapors of common organic compounds. The oxygen plasma treated films exhibit selective response to acetone and water vapors. The fast response and recovery of the conductance are the features of the carbon nanofilms. The plasma-treated carbon nanofilm on graphitized diamond surface is discussed as a promising sensing material for development of all-carbon chemical sensors, which may be suitable for biological and medical applications. An alternative approach of fabrication of temperature and chemical sensitive carbon nanofilms on insulating substrates is proposed. The films are obtained by direct deposition of sputtered carbon on highly polished quartz substrates followed by subsequent annealing at temperatures above 400 °C. It is observed that the as-deposited films are essentially amorphous, while the heating induces irreversible structural ordering and gradual conversion of amorphous carbon in

  6. Chemical synthesis and characterization of highly soluble conducting polyaniline in the mixtures of common solvents

    Directory of Open Access Journals (Sweden)

    Zeghioud Hichem

    2015-01-01

    Full Text Available This work presents the synthesis and characterization of soluble and conducting polyaniline PANI-PIA according to chemical polymerization route. This polymerization pathway leads to the formation of poly(itaconic acid doped polyaniline salts, which are highly soluble in a number of mixtures between organic common polar solvents and water, the solubility reaches 4 mg mL-1. The effect of synthesis parameters such as doping level on the conductivity and the study of solubility and other properties of the resulting PANI salts were also undertaken. The maximum of conductivity was found equal to 2.48×10-4 S cm-1 for fully protonated PANI-EB. In addition, various characterizations of the synthesized materials were also done with the help of viscosity measurements, UV-vis spectroscopy, XRD, FTIR and finally TGA for the thermal properties behaviour.

  7. Physical-chemical characterization of Tunisian clays for the synthesis of geopolymers materials

    Science.gov (United States)

    Selmani, S.; Essaidi, N.; Gouny, F.; Bouaziz, S.; Joussein, E.; Driss, A.; Sdiri, A.; Rossignol, S.

    2015-03-01

    Natural clay materials from Tunisia were examined as an aluminosilicate source for the synthesis of consolidated materials at low temperatures. Three clay samples were collected from the El Kef, Douiret and Gafsa basins and calcined at different temperatures. All of the samples were characterized using chemical and mineralogical analyses, thermogravimetry, dilatometry, and Fourier transform infrared spectroscopy (FTIR) measurements. The chemical (XRF) and mineralogical analyses (XRD and FTIR) indicated that all of the samples contained various amounts of kaolinite and quartz, followed by calcite, mica, palygorskite and gypsum. Curing produced a binder which did not significantly affect the physic-chemical properties of these clays. The obtained materials heterogeneous did not reach the geopolymerization stage, most likely because of their low kaolinite content. The addition of a suitable aluminosilicate to these clays is therefore recommended to produce homogeneous consolidated geopolymers. The synthesized materials obtained after the addition of metakaolin to the formulation to improve reactivity have interesting properties, thereby providing good potential for Tunisian clays in the synthesis of geopolymers.

  8. Graphene Synthesis and Characterization

    Science.gov (United States)

    2015-04-08

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

  9. Magnetite Fe3O4 nanoparticles synthesis by wet chemical reduction and their characterization

    Science.gov (United States)

    Chaki, S. H.; Malek, Tasmira J.; Chaudhary, M. D.; Tailor, J. P.; Deshpande, M. P.

    2015-09-01

    The authors report the synthesis of Fe3O4 nanoparticles by wet chemical reduction technique at ambient temperature and its characterization. Ferric chloride hexa-hydrate (FeCl3 · 6H2O) and sodium boro-hydrate (NaBH4) were used for synthesis of Fe3O4 nanoparticles at ambient temperature. The elemental composition of the synthesized Fe3O4 nanoparticles was determined by energy dispersive analysis of x-rays technique. The x-ray diffraction (XRD) technique was used for structural characterization of the nanoparticles. The crystallite size of the nanoparticles was determined using XRD data employing Scherrer’s formula and Hall-Williamson’s plot. Surface morphology of as-synthesized Fe3O4 nanoparticles was studied by scanning electron microscopy. High resolution transmission electron microscopy analysis of the as-synthesized Fe3O4 nanoparticles showed narrow range of particles size distribution. The optical absorption of the synthesized Fe3O4 nanoparticles was studied by UV-vis-NIR spectroscopy. The as-synthesized nanoparticles were analyzed by Fourier transform infrared spectroscopy technique for absorption band study in the infrared region. The magnetic properties of the as-synthesized Fe3O4 nanoparticles were evaluated by vibrating sample magnetometer technique. The thermal stability of the as-synthesized Fe3O4 nanoparticles was studied by thermogravimetric technique. The obtained results are elaborated and discussed in details in this paper.

  10. Copper Nanoparticles Mediated by Chitosan: Synthesis and Characterization via Chemical Methods

    Directory of Open Access Journals (Sweden)

    Muhammad Sani Usman

    2012-12-01

    Full Text Available Herein we report a synthesis of copper nanoparticles (Cu-NPs in chitosan (Cts media via a chemical reaction method. The nanoparticles were synthesized in an aqueous solution in the presence of Cts as stabilizer and CuSO4·5H2O precursor. The synthesis proceeded with addition of NaOH as pH moderator, ascorbic acid as antioxidant and hydrazine as the reducing agent. The characterization of the prepared NPs was done using ultraviolet-visible spectroscopy, which showed a 593 nm copper band. The Field Emission Scanning Electron Microscope (FESEM images were also observed, and found to be in agreement with the UV-Vis result, confirming the formation of metallic Cu-NPs. The mean size of the Cu-NPs was estimated to be in the range of 35–75 nm using X-ray diffraction. XRD was also used in analysis of the crystal structure of the NPs. The interaction between the chitosan and the synthesized NPs was studied using Fourier transform infrared (FT-IR spectroscopy, which showed the capping of the NPs by Cts.

  11. Synthesis and characterization of chemically anchored adenosine with PHEMA grafted gold nanoparticles

    Science.gov (United States)

    Bach, Long Giang; Islam, Md. Rafiqul; Jeong, Yeon Tae; Gal, Yeong Soon; Lim, Kwon Taek

    2012-01-01

    The synthesis of chemically anchored adenosine with biocompatible poly(2-hydroxylethyl methacrylate) grafted gold nanoparticles (Ado-i-PHEMA-g-AuNPs) was realized by employing a simple strategy. Disulfide-containing poly(2-hydroxylethyl methacrylate) (DT-PHEMA) was initially synthesized by atom transfer radical polymerization (ATRP). The formation of DT-PHEMA was confirmed by 1H-NMR and FT-IR. The molecular weight and molecular weight distribution were found to be 9.6 kg/mol and 1.40 from GPC analysis. DT-PHEMA was subsequently used for the synthesis of PHEMA-g-AuNPs by a grafting to protocol. The grafting of DT-PHEMA on the surface of AuNPs was confirmed by FT-IR, TGA, XPS, and EDX analyses. The particle size of the PHEMA-g-AuNPs was found to be ca. 5.0 nm from HR-TEM analysis. Boronic acid was used for functionalization of PHEMA-g-AuNPs, which was then subjected for covalent immobilization with adenosine via strong interaction between free hydroxyl groups of adenosine and boronic acid. Characterization and properties of the Ado-i-PHEMA-g-AuNPs were investigated by taking advantage from FT-IR, XPS, EDX, and UV-visible spectroscopy. The Ado-i-PHEMA-g-AuNPs nanocomposite exhibits a surface plasmon resonance peak at 586 nm which is red shifted from AuNPs (521 nm), indicating significant changes of surface property upon PHEMA-adenosine immobilization onto the surface of AuNPs.

  12. Synthesis and Characterization of Tin(IV) Oxide Obtained by Chemical Vapor Deposition Method

    Science.gov (United States)

    Nagirnyak, Svitlana V.; Lutz, Victoriya A.; Dontsova, Tatiana A.; Astrelin, Igor M.

    2016-07-01

    The effect of precursors on the characteristics of tin oxide obtained by chemical vapor deposition (CVD) method was investigated. The synthesis of nanosized tin(IV) oxide was carried out with the use of two different precursors: tin(II) oxalate obtained using tin chloride(II) and oxalic acid; tin(II) oxalate obtained using tin chloride(II); and ammonium oxalate. The synthesized tin(IV) oxide samples were studied by electron microscopy, X-ray diffraction and optical spectra. The lattice parameters of tin(IV) oxide samples were defined, the bandgap of samples were calculated.

  13. Synthesis and Characterization of Tin(IV) Oxide Obtained by Chemical Vapor Deposition Method

    OpenAIRE

    Nagirnyak, Svitlana V.; Lutz, Victoriya A.; Dontsova, Tatiana A.; Astrelin, Igor M.

    2016-01-01

    The effect of precursors on the characteristics of tin oxide obtained by chemical vapor deposition (CVD) method was investigated. The synthesis of nanosized tin(IV) oxide was carried out with the use of two different precursors: tin(II) oxalate obtained using tin chloride(II) and oxalic acid; tin(II) oxalate obtained using tin chloride(II); and ammonium oxalate. The synthesized tin(IV) oxide samples were studied by electron microscopy, X-ray diffraction and optical spectra. The lattice parame...

  14. Chemical Capping Synthesis of Nickel Oxide Nanoparticles and their Characterizations Studies

    CERN Document Server

    rifaya, M Nowsath; Alagar, M; 10.5923/j.nn.20120205.01

    2012-01-01

    This work reports aspect related to chemical capping synthesis of nano-sized particles of nickel oxide. It is a simple, novel and cost effective method. The average particle size, specific surface area, crystallinity index are estimated from XRD analysis. The structural, functional groups and optical characters are analyzed with using of SEM, FTIR and UV- visible techniques. XRD studies confirm the presence of high degree of crystallinity nature of nickel oxide nanoparticles. Their particle size is found to be 12 nm and specific surface area (SSA) is 74m2 g-1. The optical band gap energy value 3.83ev has also been determined from UV-vis spectrum.

  15. Chemical Precipitation Synthesis of Ferric Chloride Doped Zinc Sulphide Nanoparticles and Their Characterization Studies

    OpenAIRE

    Theivasanthi, T.; Kartheeswari, N.; Alagar, M.

    2013-01-01

    Nanoparticles of Ferric Chloride doped ZnS has been synthesized by simple chemical precipitation method and characterized by XRD, SEM, UV-Vis analysis, Differential Thermal Analysis, Thermo Gravimetric Analysis and Differential Scanning Calorimetry. XRD patterns of the samples reveal particle size, specific surface area and the formation of cubic structure. The SEM images show that the cauliflower likes structure. Optical band gap values have been obtained from UV-Vis absorption spectra. It h...

  16. Chemical Oxidative Polymerization of 2-Aminothiazole in Aqueous Solution: Synthesis, Characterization and Kinetics Study

    Directory of Open Access Journals (Sweden)

    Hua Zou

    2016-11-01

    Full Text Available The chemical oxidative polymerization of 2-aminothiazole (AT was studied in aqueous solution using copper chloride (CuCl2 as an oxidant. The effect of varying the reaction temperature, reaction time and oxidant/monomer molar ratio on the polymer yield was investigated. The resulting poly(2-aminothiazoles (PATs were characterized by FTIR, 1H NMR, UV-vis, gel permeation chromatography, scanning electron microscopy, thermogravimetric analysis and four-point probe electrical conductivity measurements. Compared with a previous study, PATs with higher yield (81% and better thermal stability could be synthesized. The chemical oxidative polymerization kinetics of AT were studied for the first time. The orders of the polymerization reaction with respect to monomer concentration and oxidant concentration were found to be 1.14 and 0.97, respectively, and the apparent activation energy of the polymerization reaction was determined to be 21.57 kJ/mol.

  17. Studies on the chemical synthesis and characterization of lead oxide nanoparticles with different organic capping agents

    Energy Technology Data Exchange (ETDEWEB)

    Arulmozhi, K. T., E-mail: arulsheelphy@gmail.com [Physics Wing (DDE), Annamalai University, Tamil Nadu, India - 608 002 (India); Mythili, N. [Department of Physics, Annamalai University, Tamil Nadu, India - 608 002 (India)

    2013-12-15

    Lead oxide (PbO) nanoparticles were chemically synthesized using Lead (II) acetate as precursor. The effects of organic capping agents such as Oleic acid, Ethylene Diamine Tetra Acetic acid (EDTA) and Cetryl Tri Methyl Butoxide (CTAB) on the size and morphology of the nanoparticles were studied. Characterization techniques such as X-ray diffraction (XRD), Fourier Transform-Infrared spectroscopy (FT-IR), Photoluminescence (PL) Field Emission Scanning Electron Microscopy (FE-SEM), Energy Dispersive Spectroscopy (EDS) and Transmission Electron Microscopy (TEM) were used to analyse the prepared nanoparticles for their physical, structural and optical properties. The characterization studies reveal that the synthesized PbO nanoparticles had well defined crystalline structure and sizes in the range of 25 nm to 36 nm for capping agents used and 40 nm for pure PbO nanoparticles.

  18. Studies on the chemical synthesis and characterization of lead oxide nanoparticles with different organic capping agents

    Directory of Open Access Journals (Sweden)

    K. T. Arulmozhi

    2013-12-01

    Full Text Available Lead oxide (PbO nanoparticles were chemically synthesized using Lead (II acetate as precursor. The effects of organic capping agents such as Oleic acid, Ethylene Diamine Tetra Acetic acid (EDTA and Cetryl Tri Methyl Butoxide (CTAB on the size and morphology of the nanoparticles were studied. Characterization techniques such as X-ray diffraction (XRD, Fourier Transform-Infrared spectroscopy (FT-IR, Photoluminescence (PL Field Emission Scanning Electron Microscopy (FE-SEM, Energy Dispersive Spectroscopy (EDS and Transmission Electron Microscopy (TEM were used to analyse the prepared nanoparticles for their physical, structural and optical properties. The characterization studies reveal that the synthesized PbO nanoparticles had well defined crystalline structure and sizes in the range of 25 nm to 36 nm for capping agents used and 40 nm for pure PbO nanoparticles.

  19. Chemical synthesis and characterization of bismuth oxychloride BiOCl nanoparticles

    Science.gov (United States)

    Ascencio-Aguirre, Francisco Miguel; Bazán-Díaz, Lourdes; Mendoza-Cruz, Rubén; Santana-Vázquez, Maricela; Ovalle-Encinia, Oscar; Gómez-Rodríguez, Alfredo; Herrera-Becerra, Raúl

    2017-03-01

    Bismuth oxychloride (BiOCl) nanoparticles were synthesized using bismuth nitrate pentahydrate (Bi (NO3)3*5H2O) and tannic acid (C76H52O46), the latter playing the role of stabilizing agent in a highly acid environment. For the characterization of the particles several techniques were used. The X-ray diffraction patterns (XRD) confirmed the formation of BiOCl nanocrystals with an average size of 15.33 ± 0.16 nm. Raman spectroscopy showed the characteristic A1g and Eg vibrational normal modes of BiOCl. Through electron microscopy studies (SEM and TEM) the formation of nanosized particles was confirmed. The average particle size measured from TEM images was 22.11 ± 0.29 nm, in good agreement with the one calculated from XRD data. The synthesis method was performed in aqueous solution and it represents an easy and low-cost protocol for the production of BiOCl nanoparticles.

  20. Polymeric imidazolium ionic liquids as valuable stationary phases in gas chromatography: chemical synthesis and full characterization.

    Science.gov (United States)

    González-Álvarez, Jaime; Blanco-Gomis, Domingo; Arias-Abrodo, Pilar; Díaz-Llorente, Daniel; Ríos-Lombardía, Nicolás; Busto, Eduardo; Gotor-Fernández, Vicente; Gutiérrez-Álvarez, María Dolores

    2012-04-06

    Seven new functionalized polymerizable ionic liquids were chemically prepared, and later applied for the preparation of polymeric stationary phases in gas chromatography. These coated GC columns, which exhibited good thermal stabilities (240-300°C) and very high efficiencies (3120-4200 plates/m), have been characterized using the Abraham solvation parameter model. The chromatographic behavior of these polymeric IL columns has been deeply studied observing excellent selectivities in the separation of many organic substances such as alkanes, ketones, alcohols, amines or esters in mixtures of polar and non polar solvents or fragrances. Remarkably, the challenging separation of xylene isomers has been possible using a bis(trifluoromethylsulfonyl)amide based imidazolium IL coated column as a gas chromatography stationary phase.

  1. Synthesis and Characterization of Mass Produced High Quality Few Layered Graphene Sheets via a Chemical Method

    KAUST Repository

    Khenfouch, Mohammed

    2014-04-01

    Graphene is a two-dimensional crystal of carbon atoms arranged in a honeycomb lattice. It is a zero band gap semimetal with very unique physical and chemical properties which make it useful for many applications such as ultra-high-speed field-effect transistors, p-n junction diodes, terahertz oscillators, and low-noise electronic, NEMS and sensors. When the high quality mass production of this nanomaterial is still a big challenge, we developed a process which will be an important step to achieve this goal. Atomic Force Microscopy, Scanning Electron Microscopy, Scanning tunneling microscopy, High Resolution Transmission Electron Microscopy, X-Ray Diffraction, Raman spectroscopy, Energy Dispersive X-ray system were investigated to characterize and examine the quality of this product.

  2. Synthesis and Characterization of SnO2 Thin Films by Chemical Bath Deposition

    Science.gov (United States)

    Rifai, Aditia; Iqbal, Muhammad; Nugraha; Nuruddin, Ahmad; Suyatman; Yuliarto, Brian

    2011-12-01

    SnO2 thin films were deposited on glass substrate by chemical bath deposition (CBD) with stannous chloride (SnCl2..2H2O) as a precursor and urea (CO(NH2)2) as a buffer. X-Ray Diffraction (XRD) are used to characterize the structure of the films; the surface morphology of the films were observed by Scanning Electron Microscope (SEM). Using this techniques, we specify the effect of stannous chloride concentration and weight ratio of urea/H2O on the crystallinity and morphology of these films. The rutile structure corresponding (110), (101) and (211) planes of SnO2 is obtained. The increasing of stannous chloride concentration and the decreasing weight ratio of urea/H2O is found to improve the crystallinity of the film. The average diameter of grain size is about 96 nm.

  3. Chemical Precipitation Synthesis of Ferric Chloride Doped Zinc Sulphide Nanoparticles and Their Characterization Studies

    CERN Document Server

    Theivasanthi, T; Alagar, M; 10.7598/cst2013.207

    2013-01-01

    Nanoparticles of Ferric Chloride doped ZnS has been synthesized by simple chemical precipitation method and characterized by XRD, SEM, UV-Vis analysis, Differential Thermal Analysis, Thermo Gravimetric Analysis and Differential Scanning Calorimetry. XRD patterns of the samples reveal particle size, specific surface area and the formation of cubic structure. The SEM images show that the cauliflower likes structure. Optical band gap values have been obtained from UV-Vis absorption spectra. It has also been found that energy band gap (Eg) increases with the increase in molar concentration of reactant solution. Thermal analysis measurement of the prepared sample shows that the thermal stability of pure ZnS is decreased due to increase in Ferric Chloride concentration. Undoped ZnS is more thermal stable when compared to FeCl3 doped ZnS.

  4. A novel chemical synthesis and characterization of Mn 3O 4 thin films for supercapacitor application

    Science.gov (United States)

    Dubal, D. P.; Dhawale, D. S.; Salunkhe, R. R.; Pawar, S. M.; Lokhande, C. D.

    2010-05-01

    Mn 3O 4 thin films have been prepared by novel chemical successive ionic layer adsorption and reaction (SILAR) method. Further these films were characterized for their structural, morphological and optical properties by means of X-ray diffraction (XRD), Fourier transform infrared spectrum (FTIR), field emission scanning electron microscopy (FESEM), wettability test and optical absorption studies. The XRD pattern showed that the Mn 3O 4 films exhibit tetragonal hausmannite structure. Formation of manganese oxide compound was confirmed from FTIR studies. The optical absorption showed existence of direct optical band gap of energy 2.30 eV. Mn 3O 4 film surface showed hydrophilic nature with water contact angle of 55°. The supercapacitive properties of Mn 3O 4 thin film investigated in 1 M Na 2SO 4 electrolyte showed maximum supercapacitance of 314 F g -1 at scan rate 5 mV s -1.

  5. Synthesis and characterization studies of MgO:CuO nanocrystals by wet-chemical method

    Science.gov (United States)

    Kaviyarasu, K.; Maria Magdalane, C.; Anand, K.; Manikandan, E.; Maaza, M.

    2015-05-01

    In this report, we examine the progress in adapting these nanomaterials for several predominantly photonics device fabrication by wet-chemical method. Nanocomposite of magnesium oxide (MgO) with copper oxide (CuO) doped nanoparticles were characterized by X-ray powder diffraction (XRD) and the observed peaks are quite agreeable with the pure phase cubic structure. High-resolution transmission electron microscopic (HR-TEM) results reveal that the resultant nanopowders are porous and agglomerated with polycrystalline nano-entities. Field emission of selected-area electron diffraction (SAED) studies showed that the average size of the nanoparticles were 20 nm. Photoluminescence spectra of MgO:CuO were investigated, showing emission peaks around 375 nm relating to new energy levels induced by defects or defect levels generation and confocal micro-Raman images indicated that the chemical molecular vibrational band structure and morphology of the product which is spherical shaped nanoparticles with an average particle size of ∼25 nm with standard deviation. The electrochemical response of MgO:CuO which is proves that the nano-copper/magnesium has high functionality due to the small size and it has higher electrochemical activity without any modifications.

  6. Synthesis and characterization of silver/talc nanocomposites using the wet chemical reduction method.

    Science.gov (United States)

    Shameli, Kamyar; Ahmad, Mansor Bin; Yunus, Wan Zin Wan; Ibrahim, Nor Azowa; Darroudi, Majid

    2010-10-05

    In this study, silver nanoparticles (Ag-NPs) were synthesized using the wet chemical reduction method on the external surface layer of talc mineral as a solid support. Silver nitrate and sodium borohydride were used as the silver precursor and reducing agent in talc. The talc was suspended in aqueous AgNO(3) solution. After the absorption of Ag(+) on the surface, the ions were reduced with NaBH(4). The interlamellar space limits were without many changes (d(s) = 9.34-9.19 A(º)); therefore, Ag-NPs formed on the exterior surface of talc, with d(ave) = 7.60-13.11 nm in diameter. The properties of Ag/talc nanocomposites (Ag/talc-NCs) and the diameters of the Ag-NPs prepared in this way depended on the primary AgNO(3) concentration. The prepared Ag-NPs were characterized by ultraviolet-visible spectroscopy, powder X-ray diffraction, transmission electron microscopy, scanning electron microscopy, and Fourier transform infrared. These Ag/talc-NCs may have potential applications in the chemical and biological industries.

  7. Synthesis and characterization of silver/talc nanocomposites using the wet chemical reduction method

    Directory of Open Access Journals (Sweden)

    Kamyar Shameli

    2010-09-01

    Full Text Available Kamyar Shameli1, Mansor Bin Ahmad1, Wan Zin Wan Yunus1, Nor Azowa Ibrahim1, Majid Darroudi21Department of Chemistry, Faculty of Science, 2Advanced Materials and Nanotechnology Laboratory, Institute of Advanced Technology, Universiti Putra Malaysia, Selangor, MalaysiaAbstract: In this study, silver nanoparticles (Ag-NPs were synthesized using the wet chemical reduction method on the external surface layer of talc mineral as a solid support. Silver nitrate and sodium borohydride were used as the silver precursor and reducing agent in talc. The talc was suspended in aqueous AgNO3 solution. After the absorption of Ag+ on the surface, the ions were reduced with NaBH4. The interlamellar space limits were without many changes (ds = 9.34–9.19 Aº; therefore, Ag-NPs formed on the exterior surface of talc, with dave = 7.60–13.11 nm in diameter. The properties of Ag/talc nanocomposites (Ag/talc-NCs and the diameters of the Ag-NPs prepared in this way depended on the primary AgNO3 concentration. The prepared Ag-NPs were characterized by ultraviolet-visible spectroscopy, powder X-ray diffraction, transmission electron microscopy, scanning electron microscopy, and Fourier transform infrared. These Ag/talc-NCs may have potential applications in the chemical and biological industries.Keywords: nanocomposites, silver nanoparticles, talc, powder X-ray diffraction, scanning electron microscopy

  8. Chemical synthesis and characterization of hydrous tin oxide (SnO2:H2O) thin films

    Indian Academy of Sciences (India)

    S N Pusawale; P R Deshmukh; C D Lokhande

    2011-10-01

    In the present investigation, we report chemical synthesis of hydrous tin oxide (SnO2:H2O) thin films by successive ionic layer adsorption and reaction (SILAR) method at room temperature (∼300 K). The films are characterized for their structural and surface morphological properties. The formation of nanocrystalline SnO2 with porous and agglomerated particle morphology is revealed from X-ray diffraction (XRD) and scanning electron microscopy (SEM) studies, respectively. The Fourier transform infrared spectroscopy (FTIR) study confirmed the formation of Sn–O phase and hydrous nature of the deposited film. Static water contact angle studies showed the hydrophilic nature of SnO2:H2O thin film. Electrical resistivity showed the semiconducting behaviour with room temperature electrical resistivity of 105 cm. The electrochemical properties studied in 0.5 M Na2SO4 electrolyte showed a specific capacitance of 25 F g-1 at 5 mVs-1 scan rate.

  9. Synthesis and Characterization of Cadmium Sulfide Nanoparticles by Chemical Precipitation Method.

    Science.gov (United States)

    Devi, R Aruna; Latha, M; Velumani, S; Oza, Goldie; Reyes-Figueroa, P; Rohini, M; Becerril-Juarez, I G; Lee, Jae-Hyeong; Yi, Junsin

    2015-11-01

    Cadmium sulfide (CdS) nanoparticles were synthesized by chemical precipitation method using cadmium chloride (CdCl2), sodium sulfide (Na2S) and water as a solvent by varying temperatures from 20-80 degrees C. The nanoparticles were characterized by X-ray diffraction (XRD), Raman spectroscopy, field emission scanning electron microscopy (FE-SEM), energy dispersive spectroscopy (EDS), High-resolution transmission electron microscopy (HR-TEM) and UV-Visible spectroscopy. XRD pattern revealed cubic crystal structure for all the synthesized CdS nanoparticles. Raman spectra showed first and second order longitudinal optical (LO) phonon vibrational modes of CdS. The size of CdS nanoparticles was found to be in the range of 15-80 nm by FE-SEM analysis, in all cases. The atomic percentage of cadmium and sulfur was confirmed to be 1:1 from EDS analysis. TEM micrograph depicts the spherical shape of the particles and the size is in the range of 15-85 nm while HR-TEM images of CdS nanoparticles exhibit well-resolved lattice fringes of the cubic structure of CdS. The optical properties of CdS were examined by UV-Visible spectroscopy which showed variation in absorption band from 460-480 nm. The band gap was calculated from the absorption edge and found to be in the range of 3.2-3.5 eV which is greater than the bulk CdS.

  10. Functionalized tellurols: synthesis, spectroscopic characterization by photoelectron spectroscopy, and quantum chemical study.

    Science.gov (United States)

    Khater, Brahim; Guillemin, Jean-Claude; Bajor, Gábor; Veszprémi, Tamás

    2008-03-03

    Ethene-, cyclopropane-, 3-butene-, and cyclopropanemethanetellurol have been synthesized by reaction of tributyltin hydride with the corresponding ditellurides and characterized by 1H, 13C, and 125Te NMR spectroscopy and high-resolution mass spectrometry. The tellurols of this series, with a gradually increasing distance between the tellurium atom and the unsaturated group, have been studied by photoelectron spectroscopy and quantum chemical calculations. Two stable conformations of ethenetellurol and cyclopropanetellurol, five of allyltellurol, and four of cyclopropanemethanetellurol were found. In the photoelectron spectrum of vinyltellurol, the huge split between the first two bands indicates a direct interaction between the tellurium lone electron pair and the double bond. In the allyl derivative, a hyperconjugation effect was found for the most stable conformers. In contrast to the vinyl compounds, no direct interaction between the lone electron pair of X (X = O, S, Se, and Te) and the three-membered ring could be observed in the cyclopropyl derivatives. A hyperconjugation-like effect, which is independent of the relative orientation of the X-H group, is found to increase from S to Te. Thus, the type and extent of the interaction between the TeH group and an unsaturated or cyclopropyl moiety are clarified while the first comparison of interactions between the nonradioactive unsaturated chalcogen derivatives is performed.

  11. Synthesis and Characterization of Vanadium Doped Zinc Oxide Thick Film for Chemical Sensor Application

    Directory of Open Access Journals (Sweden)

    Rayees Ahmad Zargar

    2015-01-01

    Full Text Available Zinc oxide and vanadium pentoxide nanoparticles derived by chemical coprecipitation route were used to cast Zn0.96V0.04O thick film by screen printing method. The structural, morphological, optical, and electrical properties of the film were characterized by powder XRD, SEM, Raman, UV-VIS, and DC conductivity techniques. XRD pattern, SEM image, and Raman spectrum of the film confirm the single phase formation of Wurtzite structure with preferential orientation along [101] plane, minor variation in lattice parameters, and vanadium ions substitution at zinc sites. Zn0.96V0.04O pellet has been used for sensing ammonia vapor concentrations in 20–50°C temperature range which exhibits maximum responsiveness and sensitivity at 30°C. The minor variations in resistance are observed with ammonia vapor concentration. The adsorption of ammonia vapors through weak hydrogen bonding and its insertion into lattice by nitrogen lone pairs donation at vacant/defect sites in lattice caused by vanadium doping are considered to explain gas sensing mechanism.

  12. Poly Meta-Aminophenol: Chemical Synthesis, Characterization and Ac Impedance Study

    Directory of Open Access Journals (Sweden)

    Thenmozhi Gopalasamy

    2014-01-01

    Full Text Available The present work is an investigation of AC impedance behaviour of poly(meta-aminophenol. The polymer was prepared by oxidative chemical polymerization of meta-aminophenol in aqueous HCl using ammonium persulfate as an oxidant at 0–3°C. The synthesized polymer was characterized by GPC, Elemental analysis, UV-VIS-NIR, FT-IR, 1H NMR, XRD, SEM, and TGA-DTA. The AC conductivity and dielectric response were measured at a temperature range from 303 to 383 K in the frequency range of 20 Hz to 106 Hz. The AC conductivity data could be described by the relation σacω=AωS, where the parameter “S” and Rb values decrease in the entire range of study and hence follow Correlated Barrier Hopping conduction mechanism. Both dielectric constant and dielectric loss increase with the decrease of frequency exhibiting strong interfacial polarization at low frequency and the dissipation factor also decreases with frequency. Complex electric modulus and dissipation factor exhibit two relaxation peaks, indicating two-phase structure as indicated by a bimodal distribution of relaxation process. The activation energies corresponding to these two relaxation processes were found to be 0.07 and 0.1 eV.

  13. Leiurotoxin I (scyllatoxin), a peptide ligand for Ca2(+)-activated K+ channels. Chemical synthesis, radiolabeling, and receptor characterization

    Energy Technology Data Exchange (ETDEWEB)

    Auguste, P.; Hugues, M.; Grave, B.; Gesquiere, J.C.; Maes, P.; Tartar, A.; Romey, G.; Schweitz, H.; Lazdunski, M. (Institut de Pharmacologie du Centre National de la Recherche Scientifique, Valbonne (France))

    1990-03-15

    Leiurotoxin I (scyllatoxin) is a 31-amino acid polypeptide from the venom of the scorpion Leiurus quinquestriatus hebraeus which has been previously isolated and sequenced by others. This paper reports (i) the total synthesis of this scorpion neurotoxin as well as some aspects of its structure-function relationships; (ii) the synthesis of the analog (Tyr2)leiurotoxin I (scyllatoxin) that has been monoiodinated at high specific radioactivity (2000 Ci/mmol) and has served for the characterization of the properties of {sup 125}I-(Tyr2)leiurotoxin I binding sites (Kd = 80 pM, molecular mass of 27 and 57 kDa for two polypeptides in the leiurotoxin I binding protein); (iii) the similarity of physiological actions between leiurotoxin I and apamin. Both toxins contract Taenia coli previously relaxed with epinephrine, both toxins block the after-hyperpolarization due to Ca2(+)-activated K+ channel activity in muscle cells in culture; (iv) the probable identity of binding sites for apamin and leiurotoxin I. In spite of a different chemical structure apamin competitively inhibits {sup 125}I-(Tyr2) leiurotoxin I binding and vice versa. Moreover, the peculiar effects of K+ on {sup 125}I-(Tyr2)leiurotoxin I binding are identical to those previously observed for {sup 125}I-apamin binding.

  14. Synthesis and Characterization of Silver/Clay Nanocomposites by Chemical Reduction Method

    Directory of Open Access Journals (Sweden)

    Mansor B. Ahmad

    2009-01-01

    Full Text Available Problem statement: Silver Nanoparticles (Ag-NPs have been synthesized by using chemical reduction method into the interlayer space of a Montmorillonite (MMT as a solid support which is used to antibacterial application and polymer nanocomposites for fabrication of medical devices. Approach: AgNO3 and NaBH4 were used as a silver precursor and reducing agent, respectively. The properties of Ag/MMT nanocomposites were studied as a function of the AgNO3 concentration. The crystalline structure, d-spacing of interlayer of MMT, the size distributions and surface plasmon resonance of synthesized Ag-NPs were characterized using Powder X-Ray Diffraction (PXRD, Transmission Electron Microscopy (TEM and UV-vis spectroscopy. Results: The results obtained from UV-vis spectroscopy of synthesized Ag-NPs showed that the intensity of the maximum wavelength of the plasmon peaks were increased with the increasing in the AgNO3 concentration. The obtained information from UV-vis spectra of Ag-NPs was in an excellent agreement with the obtained microstructures studies performed by Transmission Electron Microscopy (TEM and their size distributions. The prepared Ag/MMT nanocomposites are very stable over a long period of time in aqueous solution. Conclusion: The synthesized Ag/MMT nanocomposites are very stable in aqueous solution over a long period of time without any sign of precipitation. Silver nanoparticles in MMT suspension could be suitable to use antibacterial applications, since MMT is viewed as ecologically and environmentally inert material and used for biological application such as cosmetics and pharmaceutical usage.

  15. Chemically Modified Starch; Allyl- and Epoxy-Starch Derivatives: Their Synthesis and Characterization

    NARCIS (Netherlands)

    Franssen, M.C.R.; Boeriu, C.

    2014-01-01

    Both native and modified starches, such as starch that is pregelatinized, extruded, acid-converted, cross-linked, and substituted, are widely used in industry. This chapter describes a mild two-step process for the synthesis of novel, highly reactive granular epoxy-starch derivatives. Via this metho

  16. Synthesis and characterization of a novel chemically designed (Globo3–DTPA–KLH antigen

    Directory of Open Access Journals (Sweden)

    Hajmohammadi M

    2014-12-01

    Full Text Available Mehdi Hajmohammadi,1 Seyed Davar Siadat,2 Masoud Ghorbani,3,4,* Mehdi Shafiee Ardestani,5,* Shahram Teimourian,6 Vahid Asgari,3 Reza Ahangari Cohan,3 Mostafa Hajmohammadi,5 Akram Hajmohammadi,7 Ramezan Behzadi,8 Saied Rajab Nezhad,9 Nabiollah Namvar Asl10 1Department of Research and Biotechnology, 2Department of Microbiology, 3Department of Virology, Pasteur Institute of Iran, Tehran Iran; 4Department of Virology, University of Ottawa, Ottawa, ON, Canada; 5Department of Radiopharmacy, Faculty of Pharmacy, Tehran University of Medical Sciences, Tehran, Iran; 6Department of Medical Genetics, Iran University of Medical Sciences, Tehran, 7Faculty of Pharmacy, Ahvaz Jundishapur University of Medical Sciences, Ahvaz, 8Laboratory Animal Management of North Research Center, Pasteur Institute of Iran, 9Department of Research and Development, Alhavi Pharmaceutical, Tehran, 10Pasteur Institute of Iran, Department of Animal Sciences, Karaj, Iran *These authors contributed equally to this work Abstract: In recent years, many experiments have been conducted for the production and evaluation of anticancer glycoconjugated vaccines in developed countries and many achievements have been accomplished with Globo H derivatives. In the current experiment, a new chemically designed triplicate version of (Globo H3–diethylenetriamine pentaacetic acid (DTPA–KLH antigen was synthesized and characterized. Immunization with (Globo H3-DTPA-KLH, a hexasaccharide that is a member of a family of antigenic carbohydrates that are highly expressed in various types of cancers conjugated with DTPA and KLH protein, induced a high level of antibody titer along with an elevated level of IL-4 in mice. Treatment of tumors with the collected sera from immunized mice decreased the tumor size in nude mice as well. None of the immunized mice illustrated any sign of tumor growth after injection of MCF-7 cells compared to the control animals. These findings, based on the newly presented

  17. Cobalt-doped ZnO nanowires on quartz: Synthesis by simple chemical method and characterization

    Science.gov (United States)

    Vempati, Sesha; Shetty, Amitha; Dawson, P.; Nanda, Karunakar; Krupanidhi, S. B.

    2012-03-01

    The synthesis of cobalt-doped ZnO nanowires is achieved using a simple, metal salt decomposition growth technique. A sequence of drop casting on a quartz substrate held at 100 °C and annealing results in the growth of nanowires of average (modal) length ˜200 nm and diameter of 15±4 nm and consequently an aspect ratio of ˜13. A variation in the synthesis process, where the solution of mixed salts is deposited on the substrate at 25 °C, yields a grainy film structure which constitutes a useful comparator case. X-ray diffraction shows a preferred [0001] growth direction for the nanowires while a small unit cell volume contraction for Co-doped samples and data from Raman spectroscopy indicate incorporation of the Co dopant into the lattice; neither technique shows explicit evidence of cobalt oxides. Also the nanowire samples display excellent optical transmission across the entire visible range, as well as strong photoluminescence (exciton emission) in the near UV, centered at 3.25 eV.

  18. Synthesis and characterization of well-aligned carbon nitrogen nanotubes by microwave plasma chemical vapor deposition

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    Well-aligned carbon nitrogen nanotube films have been synthesized successfully on mesoporous silica substrates by microwave plasma chemical vapor deposition (MWPCVD) method. Studies on their morphology, structure, and composition by scanning electron microscopy (SEM), transmission electron microscopy (TEM), and energy dispersive X-ray spectroscopy (EDX), respectively, indicate that these nanotubes consist of linearly polymerized carbon nitrogen nanobells, and the nitrogen atoms have been doped into carbon netweork to form a new structure C1-xNx (x=0.16±0.01). X-ray photoelectron spectroscopy (XPS) results of the samples further demonstrate that carbon bonds covalently with nitrogen in all the carbon nitrogen nanotube films.

  19. Chemical Synthesis of Nano-Sized particles of Lead Oxide and their Characterization Studies

    CERN Document Server

    Alagar, M; Raja, A Kubera; 10.3923/jas.2012.398.401

    2012-01-01

    The quantum dots of semiconductor display novel and interesting phenomena that have not been in the bulk material. The color tunability is one of the most attractive characteristics in II-VI semiconductor nanoparticles such as CdS, ZnS, CdSe, ZnSe and PbO. In this work, the semiconductor lead oxide nanoparticles are prepared by chemical method. The average particle size, specific surface area, crystallinity index are estimated from XRD analysis. The structural, functional groups and optical characters are analyzed with using of SEM, FTIR and UV- Visible techniques. The optical band gap value has also been determined.

  20. Synthesis and characterization of chemically deposited CdS thin films without toxic precursors.

    Science.gov (United States)

    Fernández-Pérez, A.; Sandoval-Paz, M. G.

    2016-05-01

    Al doped and undoped CdS thin films (CdS:Al) were deposited on glass, copper and bronze substrates by chemical bath deposition technique in an ammonia-free cadmium-sodium citrate system. The structural and optical properties of the CdS films were determined by X-ray diffraction (XRD), scanning electron microscope (SEM), and simultaneous transmission- reflection spectroscopy. It was found that the properties of the films depend on the amount of Al in the growth solutions and deposition time. The increase in Al content in the reaction solution led to a smaller crystallite size and higher energy band gap that varies in the range 2.42 eV - 2.59 eV depending on the Al content.

  1. Synthesis and characterization of well-aligned carbon nitrogen nanotubes by microwave plasma chemical vapor deposition

    Institute of Scientific and Technical Information of China (English)

    马旭村; 徐贵昌; 王恩哥

    2000-01-01

    Well-aligned carbon nitrogen nanotube films have been synthesized successfully on meso-porous silica substrates by microwave plasma chemical vapor deposition (MWPCVD) method. Studies on their morphology, structure, and composition by scanning electron microscopy (SEM), transmission electron microscopy (TEM), and energy dispersive X-ray spectroscopy (EDX), respectively, indicate that these nanotubes consist of linearly polymerized carbon nitrogen nanobells, and the nitrogen atoms have been doped into carbon netweork to form a new structure C1-xNx( x = 0.16±0.01). X-ray photoelectron spectroscopy (XPS) results of the samples further demonstrate that carbon bonds cova-lently with nitrogen in all the carbon nitrogen nanotube films.

  2. Synthesis and Characterization of Cellulose from Green Bamboo by Chemical Treatment with Mechanical Process

    Directory of Open Access Journals (Sweden)

    Fui Kiew Liew

    2015-01-01

    Full Text Available Bamboo cellulose was prepared by chemical process involving dewaxing, delignification, and mercerization process. Four samples namely, green bamboo fiber (GBF, dewaxed bamboo fiber (DBF, delignified bamboo fiber (DLBF, and cellulose fiber (CF had been analysed. FTIR and TGA analysis confirmed the removal of hemicellulose and lignin at the end stage of the process. FTIR results reveal that the D-cellulose OH group occurred at 1639 cm−1 region. SEM micrograph showed that mercerization leads to fibrillation and breakage of the fiber into smaller pieces which promote the effective surface area available for contact. Barrer, Joiyner, and Halenda (BJH method confirmed that the effective surface area of CF is two times larger compared to GBF. CF showed the highest activation energy compared to GBF. It indicates that CF was thermally stable.

  3. New methods for chemical protein synthesis.

    Science.gov (United States)

    Guan, Xiaoyang; Chaffey, Patrick K; Zeng, Chen; Tan, Zhongping

    2015-01-01

    Chemical protein synthesis is a useful tool to generate pure proteins which are otherwise difficult to obtain in sufficient amounts for structure and property analysis. Additionally, because of the precise and flexible nature of chemical synthesis, it allows for controllable variation of protein sequences, which is valuable for understanding the relationships between protein structure and function. Despite the usefulness of chemical protein synthesis, it has not been widely adopted as a tool for protein characterization, mainly because of the lack of general and efficient methods for the preparation and coupling of peptide fragments and for the folding of polypeptide chains. To address these issues, many new methods have recently been developed in the areas of solid-phase peptide synthesis, peptide fragment assembly, and protein folding. Here we review these recent technological advances and highlight the gaps needing to be addressed in future research.

  4. Green chemistry for chemical synthesis

    OpenAIRE

    Li, Chao-Jun; Trost, Barry M.

    2008-01-01

    Green chemistry for chemical synthesis addresses our future challenges in working with chemical processes and products by inventing novel reactions that can maximize the desired products and minimize by-products, designing new synthetic schemes and apparati that can simplify operations in chemical productions, and seeking greener solvents that are inherently environmentally and ecologically benign.

  5. Green chemistry for chemical synthesis

    Science.gov (United States)

    Li, Chao-Jun; Trost, Barry M.

    2008-01-01

    Green chemistry for chemical synthesis addresses our future challenges in working with chemical processes and products by inventing novel reactions that can maximize the desired products and minimize by-products, designing new synthetic schemes and apparati that can simplify operations in chemical productions, and seeking greener solvents that are inherently environmentally and ecologically benign. PMID:18768813

  6. Synthesis, physico-chemical characterization and biological activity of 2-aminobenzimidazole complexes with different metal ions

    Directory of Open Access Journals (Sweden)

    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.

  7. Chemical synthesis on SU-8

    DEFF Research Database (Denmark)

    Qvortrup, Katrine; Taveras, Kennedy; Thastrup, Ole;

    2011-01-01

    In this paper we describe a highly effective surface modification of SU-8 microparticles, the attachment of appropriate linkers for solid-supported synthesis, and the successful chemical modification of these particles via controlled multi-step organic synthesis leading to molecules attached...

  8. Synthesis and characterization of bulk Cu{sub 2}ZnSnX{sub 4} (X: S, Se) via thermodynamically supported mechano-chemical process

    Energy Technology Data Exchange (ETDEWEB)

    Pareek, Devendra, E-mail: devpareek@iitb.ac.in; Balasubramaniam, K.R.; Sharma, Pratibha

    2015-05-15

    Materials with the general formula, Cu{sub 2}ZnSnX{sub 4} (CZTX; X: Group 16 elements), with X being S/Se, have been receiving considerable attention due to their utility as an absorber layer in solar photovoltaics (PV). This paper reports on the synthesis of CZTSe and CZTS nanocrystalline powders at low temperatures, starting from elemental metal and chalcogen powders, via the low cost, scalable technique of ball milling. The prepared samples were well characterized using the different characterization tools. XRD, Raman, SEM and TEM studies confirm the formation of single-phase, stoichiometric, nano-crystalline kesterite CZTS and CZTSe powders. The low temperature phase selection of the complex quaternary compound in this system is seen as a direct consequence of the thermodynamic facilitation, coupled with the capability of mechano-chemical synthesis to aid in overcoming kinetic constraints. The optical bandgap of the various samples of CZTS was observed in the range of 1.4–1.6 eV and corresponding values for CZTSe was observed to be in the range of 1.08–1.18 eV. Our work provides a pathway for developing cheap, scalable, and ink-based techniques for low cost solar PV. - Graphical abstract: Display Omitted - Highlights: • A scalable route for synthesis of near phase pure CZTS/Se nano-crystals has been demonstrated. • Stoichiometric CZTS and CZTSe were synthesized via mechano-chemical synthesis route. • Synthesis at near room temperature is supported by thermodynamic calculations.

  9. Synthesis and characterization of graphene layers prepared by low-pressure chemical vapor deposition using triphenylphosphine as precursor

    Energy Technology Data Exchange (ETDEWEB)

    Mastrapa, G.C.; Maia da Costa, M.E.H. Maia [Departamento de Física, Pontifícia Universidade Católica do Rio de Janeiro, 22451-900, Rio de Janeiro, RJ (Brazil); Larrude, D.G., E-mail: dunigl@vdg.fis.puc-rio.br [Departamento de Física, Pontifícia Universidade Católica do Rio de Janeiro, 22451-900, Rio de Janeiro, RJ (Brazil); Freire, F.L. [Departamento de Física, Pontifícia Universidade Católica do Rio de Janeiro, 22451-900, Rio de Janeiro, RJ (Brazil); Brazilian Center for Physical Research, 22290-180, Rio de Janeiro, RJ (Brazil)

    2015-09-15

    The synthesis of a single-layer graphene using a low-pressure Chemical Vapor Deposition (CVD) system with triphenylphosphine as precursor is reported. The amount of triphenylphosphine used as precursor was in the range of 10–40 mg. Raman spectroscopy was employed to analyze samples prepared with 10 mg of the precursor, and these spectra were found typical of graphene. The Raman measurements indicate that the progressive degradation of graphene occurs as the amount of triphenylphosphine increases. X-ray photoelectron spectroscopy measurements were performed to investigate the different chemical environments involving carbon and phosphorous atoms. Scanning electron microscopy and transmission electron microscopy were also employed and the results reveal the formation of dispersed nanostructures on top of the graphene layer, In addition, the number of these nanostructures is directly related to the amount of precursor used for sample growth. - Highlights: • We grow graphene using the solid precursor triphenylphosphine. • Raman analysis confirms the presence of monolayer graphene. • SEM images show the presence of small dark areas dispersed on the graphene surface. • Raman I{sub D}/I{sub G} ratio increases in the dark region of the graphene surface.

  10. Chemical Synthesis of Glycosaminoglycans.

    Science.gov (United States)

    Mende, Marco; Bednarek, Christin; Wawryszyn, Mirella; Sauter, Paul; Biskup, Moritz B; Schepers, Ute; Bräse, Stefan

    2016-07-27

    Glycosaminoglycans (GAGs) as one major part of the glycocalyx are involved in many essential biological cell processes, as well as in many courses of diseases. Because of the potential therapeutic application of GAG polymers, fragments, and also derivatives toward different diseases (e.g., heparin derivatives against Alzheimer's disease), there is a continual growing demand for new chemical syntheses, which suffice the high claim to stereoselectivity and chemoselectivity. This Review summarizes the progress of chemical syntheses of GAGs over the last 10 years. For each class of the glycosaminoglycans-hyaluronan (HA), heparan sulfate/heparin (HS/HP), chondroitin/dermatan sulfate (CS/DS), and keratan sulfate (KS)-mainly novel glycosylation strategies, elongation sequences, and protecting group patterns are discussed, but also (semi)automated syntheses, enzymatic approaches, and functionalizations of synthesized or isolated GAGs are considered.

  11. Synthesis and Characterization of In2S3 Thin Films Deposited by Chemical Bath Deposition on Polyethylene Naphthalate Substrates

    Science.gov (United States)

    Castelo-González, O. A.; Santacruz-Ortega, H. C.; Quevedo-López, M. A.; Sotelo-Lerma, M.

    2012-04-01

    Indium sulfide (In2S3) thin films were deposited on polyethylene naphthalate (PEN) by chemical bath deposition (CBD). The materials were characterized by ultraviolet (UV)-visible spectroscopy, x-ray photoelectron spectroscopy (XPS), energy-dispersive x-ray spectroscopy (EDX), scanning electron microscopy (SEM), and x-ray diffraction (XRD) to investigate the influence of the polymeric substrate on the resulting thin In2S3. The films showed polycrystalline (cubic and tetragonal) structure. A reduction of the ordering of the polymeric chains at the surface of the PEN was also observed, demonstrated by the appearance of two infrared bands at 1094 cm-1 and 1266 cm-1. Presence of oxygen during the early stages of In2S3 growth was also identified. We propose a reaction mechanism for both the equilibrium and nucleation stages. These results demonstrate that In2S3 can be deposited at room temperature on a flexible substrate.

  12. Hydroxyapatite, a biomaterial: Its chemical synthesis, characterization and study of biocompatibility prepared from shell of garden snail, Helix aspersa

    Indian Academy of Sciences (India)

    Anjuvan Singh

    2012-11-01

    The shell of garden snail (Helix aspersa) is basically made of calcium carbonate. An attempt is made to convert calcium carbonate of garden snail shell to hydroxyapatite. The snail shell was found to decompose within 850°C to all the carbonate phases. The calcined snail shells were then treated with acids followed by different chemicals in ammoniacal media maintaining proper stoichiometry to produce fine hydroxyapatite (HAP) as filter cake with a Ca/P molar ratio of 1.67. The dried HAP powder was extremely pure with a specific surface area of 15 m2/g. The different characterization techniques were adopted both for calcined snail shell and HAP synthesized by X-ray diffraction (XRD), thermal analysis (DTA/TGA), Fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM). The surface area and particle size of HAP powder prepared by chemical precipitation route, were also determined by BET and Malvern particle size analyser, respectively. The synthesized powder was soaked in stimulated body fluid (SBF) medium for various periods of time in order to evaluate its bioactivity. The changes of pH of SBF medium were measured. High bioactivity of prepared HAP powder due to the formation of apatite on its surface was observed.

  13. Synthesis of zeolites from boiler fly ash: physical, chemical and mineralogical characterization; Sintese de zeolitas a partir de cinza volante de caldeiras: caracterizacao fisica, quimica e mineralogica

    Energy Technology Data Exchange (ETDEWEB)

    Rocha Junior, C.A.F.; Santos, S.C.A.; Souza, C.A.G., E-mail: augustorocha2@gmail.com [Programa de Pos Graduacao em Engenharia Quimica (PPEQ-UFPA), Belem, PA (Brazil); Angelica, R.S.; Neves, R.F. [Programa de Pos-Graduacao em Geologia e Geoquimica, Instituto de Geociencias (PPGG-IG-UFPA), Ananindeua, PA (Brazil)

    2012-01-15

    Along the years, worldwide industrial development has causing a growing generation of residues, bringing potentials environmental problems. A study of the characteristics of these wastes, as well as the development of techniques for their use in new processes becomes indispensable for the environment preservation. The main purpose of this work is to evaluate the possible use of two important industrial residues from the Amazon region for zeolite synthesis: (a) the fly ash (particle size < 100 {mu}m) that comes from burning of mineral coal in boiler; and (b) the micro silica, a by-product of the reaction between quartz and coal in the production of metallic silicon and alloys iron-silicon.The following chemical, physical and mineralogical characterization methods were carried out: X-ray diffractometry, X-ray fluorescence, scanning electron microscopy, granulometric analysis, differential thermal and thermogravimetric analysis (DTA-TG). The analyses were carried out at the following conditions: 60, 100, 150 and 190 deg C, Na{sub 2}O/Al{sub 2}O{sub 3} molar ratio of 5 and Si/Al molar ratio ranging from 2.12 to 15, and reaction time of 24 h. The results of the fly characterization demonstrate its enormous potential as raw material for the zeolite synthesis. SiO{sub 2} and Al{sub 2}O{sub 3} represent more than 50% of its composition, mineralogical phases defined, low humidity content, low particle size (d{sub 90} < 10 {mu}m), among others. Mineralogical analyses of the synthesized products showed the formation of some zeolite types, as follow: analcime, phillipsite, sodalite, zeolite P and tobermorite. The results show that the mixture fly ash-micro silica in these reaction conditions point to a promising material for zeolite synthesis (author)

  14. Synthesis and characterization of silver/montmorillonite/chitosan bionanocomposites by chemical reduction method and their antibacterial activity.

    Science.gov (United States)

    Shameli, Kamyar; Bin Ahmad, Mansor; Zargar, Mohsen; Yunus, Wan Md Zin Wan; Ibrahim, Nor Azowa; Shabanzadeh, Parvaneh; Moghaddam, Mansour Ghaffari

    2011-01-01

    Silver nanoparticles (AgNPs) of a small size were successfully synthesized using the wet chemical reduction method into the lamellar space layer of montmorillonite/chitosan (MMT/Cts) as an organomodified mineral solid support in the absence of any heat treatment. AgNO3, MMT, Cts, and NaBH4 were used as the silver precursor, the solid support, the natural polymeric stabilizer, and the chemical reduction agent, respectively. MMT was suspended in aqueous AgNO3/Cts solution. The interlamellar space limits were changed (d-spacing = 1.24-1.54 nm); therefore, AgNPs formed on the interlayer and external surface of MMT/Cts with d-average = 6.28-9.84 nm diameter. Characterizations were done using different methods, ie, ultraviolet-visible spectroscopy, powder X-ray diffraction, transmission electron microscopy, scanning electron microscopy, energy dispersive X-ray fluorescence spectrometry, and Fourier transform infrared spectroscopy. Silver/montmorillonite/chitosan bionanocomposite (Ag/MMT/Cts BNC) systems were examined. The antibacterial activity of AgNPs in MMT/Cts was investigated against Gram-positive bacteria, ie, Staphylococcus aureus and methicillin-resistant S. aureus and Gram-negative bacteria, ie, Escherichia coli, E. coli O157:H7, and Pseudomonas aeruginosa by the disc diffusion method using Mueller Hinton agar at different sizes of AgNPs. All of the synthesized Ag/MMT/Cts BNCs were found to have high antibacterial activity. These results show that Ag/MMT/Cts BNCs can be useful in different biological research and biomedical applications, including surgical devices and drug delivery vehicles.

  15. Wet chemical synthesis of soluble gold nanogaps

    DEFF Research Database (Denmark)

    Jain, Titoo; Tang, Qingxin; Bjørnholm, Thomas;

    2014-01-01

    NRs) in aqueous solution. Through controlled end-to-end assembly of the AuNRs into dimers or chains, facilitated via target molecules, they can be used as electrical contacts. In this way, the preparation of AuNR-molecule-AuNR junctions by wet chemical methods may afford a large number of identical devices...... with little variation in the interface between molecule and electrode (AuNR). In this Account, we highlight recent progress in using chemically synthesized AuNRs as building blocks for molecular electronic applications. We outline the general synthesis and properties of AuNRs and describe the aqueous growth...... in the nanogaps lets us spectroscopically characterize the molecules via surface-enhanced Raman scattering. We discuss the incorporation of oligopeptides functionalized with acetylene units having uniquely identifiable vibrational modes. This acetylene moiety allows chemical reactions to be performed in the gaps...

  16. Synthesis and characterization of ZrO2-CuO co-doped ceria nanoparticles via chemical precipitation method

    Science.gov (United States)

    Viruthagiri, G.; Gopinathan, E.; Shanmugam, N.; Gobi, R.

    2014-10-01

    In the present study, the fluorite cubic phase of bare and ZrO2-CuO co-doped ceria (CeO2) nanoparticles have been synthesized through a simple chemical precipitation method. X-ray diffraction results revealed that average grain sizes of the samples are within 5-6 nm range. The functional groups present in the samples were identified by Fourier Transform Infrared Spectroscopy (FTIR) study. Surface area measurement was carried out for the ceria nanoparticles to characterize the surface properties of the synthesized samples. The direct optical cutoff wavelength from DRS analysis was blue-shifted evidently with respect to the bulk material and indicated quantum-size confinement effect in the nanocrystallites. PL spectra revealed the strong and sharp UV emission at 401 nm. The surface morphology and the element constitution of the pure and doped nanoparticles were studied by scanning electron microscope fitted with energy dispersive X-ray spectrometer arrangement. The thermal decomposition course was followed using thermo gravimetric and differential thermal analyses (TG-DTA).

  17. A novel chemical synthesis and characterization of Mn{sub 3}O{sub 4} thin films for supercapacitor application

    Energy Technology Data Exchange (ETDEWEB)

    Dubal, D.P.; Dhawale, D.S.; Salunkhe, R.R. [Thin Film Physics Laboratory, Department of Physics, Shivaji University, Kolhapur 416004 (M.S) (India); Pawar, S.M. [Photonic and Electronic Thin Film Laboratory, Department of Materials Science and Engineering, Chonnam National University, 300 Yongbong-Dong, Puk-Gu, Gwangju 500-757 (Korea, Republic of); Lokhande, C.D., E-mail: l_chandrakant@yahoo.com [Thin Film Physics Laboratory, Department of Physics, Shivaji University, Kolhapur 416004 (M.S) (India)

    2010-05-01

    Mn{sub 3}O{sub 4} thin films have been prepared by novel chemical successive ionic layer adsorption and reaction (SILAR) method. Further these films were characterized for their structural, morphological and optical properties by means of X-ray diffraction (XRD), Fourier transform infrared spectrum (FTIR), field emission scanning electron microscopy (FESEM), wettability test and optical absorption studies. The XRD pattern showed that the Mn{sub 3}O{sub 4} films exhibit tetragonal hausmannite structure. Formation of manganese oxide compound was confirmed from FTIR studies. The optical absorption showed existence of direct optical band gap of energy 2.30 eV. Mn{sub 3}O{sub 4} film surface showed hydrophilic nature with water contact angle of 55{sup o}. The supercapacitive properties of Mn{sub 3}O{sub 4} thin film investigated in 1 M Na{sub 2}SO{sub 4} electrolyte showed maximum supercapacitance of 314 F g{sup -1} at scan rate 5 mV s{sup -1}.

  18. Synthesis and characterization of flower-like ZnSe nanostructured thin films by chemical bath deposition (CBD) method

    Science.gov (United States)

    Bakiyaraj, G.; Dhanasekaran, R.

    2013-04-01

    Flower-like zinc selenide nanostructured thin films were successfully prepared by a chemical bath deposition method on non-conducting glass substrate in an aqueous alkaline medium using sodium selenosulphate as Se2- ion source. The as-deposited films have been characterized by X-ray diffraction (XRD), high resolution scanning electron microscopy (HRSEM), energy-dispersive X-ray analysis (EDX), optical absorption, and photoluminescence spectroscopy (PL). The XRD studies reveal that the as-deposited ZnSe thin film is nanocrystalline with a face-centered cubic phase. SEM image shows the tens to hundreds of petals are self-assembled within a single nanoflower. The direct optical band gap ` E g' for as-deposited flower-like ZnSe thin films is found to be 2.80 eV. Room temperature PL measurement indicates that the as-deposited cubic ZnSe thin films have a near band edge (NBE) emission peaked at around 440 nm (2.81 eV) and broad weak band emission peak from 552 nm (2.24 eV) to 658 nm (1.88 eV). The strong NBE emission from the flower-like ZnSe nanostructured thin films reveals their potential as building for optoelectronic devices.

  19. Novel chemical synthesis and characterization of copper pyrovanadate nanoparticles and its influence on the flame retardancy of polymeric nanocomposites

    Science.gov (United States)

    Ghiyasiyan-Arani, Maryam; Masjedi-Arani, Maryam; Ghanbari, Davood; Bagheri, Samira; Salavati-Niasari, Masoud

    2016-05-01

    In this work, copper pyrovanadate (Cu3V2O7(OH)2(H2O)2) nanoparticles have been synthesized by a simple and rapid chemical precipitation method. Different copper-organic complexes were used to control the size and morphology of products. The morphology and structure of the as-synthesized products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared (FT-IR) spectrum, electron dispersive X-ray spectroscopy (EDX), thermal gravimetric analysis (TGA), differential thermal analysis (DTA) and photoluminescence (PL) spectroscopy. The influence of copper pyrovanadate nanostructures on the flame retardancy of the polystyrene, poly vinyl alcohol and cellulose acetate was studied. Dispersed nanoparticles play the role of a magnetic barrier layer, which slows down product volatilization and prevents the flame and oxygen from the sample during decomposition of the polymer. Cu3V2O7(OH)2(H2O)2 is converted to Cu3V2O8 with an endothermic reaction which simultaneously releases water and decrease the temperature of the flame region.

  20. Synthesis and characterization of silver/montmorillonite/chitosan bionanocomposites by chemical reduction method and their antibacterial activity

    Directory of Open Access Journals (Sweden)

    Kamyar Shameli

    2011-01-01

    Full Text Available Kamyar Shameli1, Mansor Bin Ahmad1, Mohsen Zargar3, Wan Md Zin Wan Yunus1, Nor Azowa Ibrahim1, Parvaneh Shabanzadeh2, Mansour Ghaffari Moghaddam41Department of Chemistry, Faculty of Science, 2Institute for Mathematical Research, Universiti Putra Malaysia, Selangor, Malaysia; 3Department of Biology, Islamic Azad University, Qum, Iran; 4Department of Chemistry, Faculty of Science, University of Zabol, Zabol, IranAbstract: Silver nanoparticles (AgNPs of a small size were successfully synthesized using the wet chemical reduction method into the lamellar space layer of montmorillonite/chitosan (MMT/Cts as an organomodified mineral solid support in the absence of any heat treatment. AgNO3, MMT, Cts, and NaBH4 were used as the silver precursor, the solid support, the natural polymeric stabilizer, and the chemical reduction agent, respectively. MMT was suspended in aqueous AgNO3/Cts solution. The interlamellar space limits were changed (d-spacing = 1.24–1.54 nm; therefore, AgNPs formed on the interlayer and external surface of MMT/Cts with d-average = 6.28–9.84 nm diameter. Characterizations were done using different methods, ie, ultraviolet-visible spectroscopy, powder X-ray diffraction, transmission electron microscopy, scanning electron microscopy, energy dispersive X-ray fluorescence spectrometry, and Fourier transform infrared spectroscopy. Silver/montmorillonite/chitosan bionanocomposite (Ag/MMT/Cts BNC systems were examined. The antibacterial activity of AgNPs in MMT/Cts was investigated against Gram-positive bacteria, ie, Staphylococcus aureus and methicillin-resistant S. aureus and Gram-negative bacteria, ie, Escherichia coli, E. coli O157:H7, and Pseudomonas aeruginosa by the disc diffusion method using Mueller Hinton agar at different sizes of AgNPs. All of the synthesized Ag/MMT/Cts BNCs were found to have high antibacterial activity. These results show that Ag/MMT/Cts BNCs can be useful in different biological research and biomedical

  1. Standardized chemical synthesis of Pseudomonas aeruginosa pyocyanin

    Directory of Open Access Journals (Sweden)

    Rajkumar Cheluvappa

    2014-01-01

    As we have extracted pyocyanin both from P. aeruginosa cultures, and via chemical synthesis; we know the procedural and product-quality differences. We endorse the relative ease, safety, and convenience of using the chemical synthesis described here. Crucially, our “naturally endotoxin-free” pyocyanin can be extracted easily without using infectious bacteria.

  2. Nanodispersed Oxides-Plasma-Chemical Synthesis and Properties

    Institute of Scientific and Technical Information of China (English)

    Gheorghi VISSOKOV; Katerina ZAHARIEVA

    2007-01-01

    We discuss the plasma-chemical synthesis and the properties of transition metals oxides, Al2O3, SiO2, rare-earth oxides, oxides for ceramics and metal-ceramics, and oxides used as catalysts. Bearing in mind the indisputable advantages of using plasma-chemically synthesized nanodispersed oxides for the needs of various industrial fields, we set out to review the articles published in the past few years devoted to the problems of plasma-chemical synthesis and characterization of nanodispersed oxides.

  3. Synthesis, Characterization, Crystal Structure and Quantum Chemical Calculation of Novel Compound 1,3-Dimethyl-2-ferrocenylmethylbenzimidazolium Iodide

    Institute of Scientific and Technical Information of China (English)

    ZHANG Jing; YANG Bing-Qin; ZHU Hai-Yan; LI Tao; WEN Zhen-Yi

    2006-01-01

    A novel benzimidazole derivative, 1,3-dimethyl-2-ferrocenylmethylbenzimidazolium iodide (1) was synthesized and characterized by elemental analysis, MS, 1H NMR and IR spectra. Its crystal structure was determined by X-ray single crystal diffraction, and the title compound belongs to monoclinic system with space group P2(1)/c.According to the crystal structure, the quantum chemistry calculation was performed by Gaussian 03 program, and full geometry optimizations of the title compound were carried out with DFT method at B3LYP/6-31G level. Its structure, stability, frontier molecular orbital components and net charge distribution were discussed.

  4. Synthesis and characterization of nanoporous strontium-doped lanthanum cobaltite thin film using metal organic chemical solution deposition

    Energy Technology Data Exchange (ETDEWEB)

    Park, Jun-Sik [Department of Mechanical Convergence Engineering, Hanyang University, Seoul 133-791 (Korea, Republic of); Kim, Young-Beom, E-mail: ybkim@hanyang.ac.kr [Department of Mechanical Convergence Engineering, Hanyang University, Seoul 133-791 (Korea, Republic of); Institute of Nano Science and Technology, Hanyang University, Seoul 133-791 (Korea, Republic of)

    2016-01-29

    By employing strontium as a dopant of lanthanum cobaltite (LaCoO{sub 3}), strontium-doped lanthanum cobaltite (La{sub 1−x}Sr{sub x}CoO{sub 3−δ}, LSC) thin film was fabricated using a metal organic chemical solution deposition (MOCSD) method. Lanthanum nitrate hexahydrate [La(NO{sub 3}){sub 3}6H{sub 2}O], strontium acetate [Sr(CH{sub 3}COO){sub 2}], and cobalt acetate tetrahydrate [Co(CH{sub 3}COO){sub 2}4H{sub 2}O] were used as precursors. The coating process was performed through a spin coating method on a substrate, which were then heat treated under various temperature conditions. Electrical properties, microstructures, and crystalline structures with respect to sintering temperature were analyzed. According to these analyses, the change in surface morphology, phase shift, and conductive properties were closely related, which could explain their respective behaviors. Furthermore, sintered strontium-doped lanthanum perovskite oxides showed various conductivities according to the amount of dopant. With the molar ratio of strontium that is stoichiometrically equivalent to lanthanum (La{sub 0.5}Sr{sub 0.5}CoO{sub 3−δ}) thin film showed the best conductivity in the sintering temperature range of 650–700 °C, with perovskite phases formed at this temperature condition. As the electrically conductive properties of the thin film are a function of thickness, the films were coated several times to a thickness of approximately 300 nm, with the lowest resistivity (approximately 9.06 × 10{sup −4} Ω cm) observed at the optimized sintering temperature and solution composition. - Highlights: • LSC thin film was fabricated by metal organic chemical solution deposition (MOCSD). • The film shows good agreement on the electrical conductivity of LSC by conventional methods. • The properties of LSC film are influenced by the surface morphology and crystalline phase. • Optimal molar ratio of strontium for the highest conductivity was investigated.

  5. Synthesis,characterization and swelling properties of a chemically cross-linked poly(vinyl alcohol) hydrogel

    Institute of Scientific and Technical Information of China (English)

    LI Wenbo; XUE Feng; CHENG Rongshi

    2007-01-01

    A poly(vinyl alcohol) hydrogel was prepared by coupling poly(vinyl alcohol) with epichlorohydrin as the cross-linking agent.The structure of the hydrogel was characterized by FTIR and GPC techniques.Various amounts of water were added into the dry gel to swell it,and the quantity of water in various states in the partially swollen hydrogel was determined by DSC technique.The analytical results indicate that the water introduced into the dry gel first combines with the hydrophilic groups of the network chains through hydrogen bond forming non-freezable water.The weight ratio of the non-freezable water to dry gel in the hydrogels is about 0.20.After the non-freezable water is saturated,the additional water penetrates the network space and exists simultaneously both in the freezable and free water states until reaching equilibrium swelling.

  6. Synthesis and Characterization of SiO2 Nanoparticles and Their Efficacy in Chemical Mechanical Polishing Steel Substrate

    Directory of Open Access Journals (Sweden)

    M. J. Kao

    2014-01-01

    Full Text Available Chemical mechanical polishing (CMP technology is extensively used in the global planarization of highly value-added and large components in the aerospace industry. A nanopowder of SiO2 was prepared by the sol-gel method and was compounded into polishing slurry for the CMP of steel substrate. The size of the SiO2 abrasives was controlled by varying the sol-gel reaction conditions. The polishing efficacy of nano-SiO2 was studied, and the CMP mechanism with nanosized abrasives was further investigated. The proposed methods can produce SiO2 abrasives whose size can be controlled by varying the sol-gel reaction conditions. The size of the SiO2 abrasives was controlled in the range from 58 to 684 nm. The roughness of the steel substrate strongly depends on the size of the abrasive, and the surface roughness decreases as the abrasive size declines. A super-smooth surface with a roughness of 8.4 nm is obtained with nanosized SiO2. Ideal CMP slurry can be used to produce material surfaces with low roughness, excellent global planarization, high selectivity, an excellent finish, and a low-defected rate.

  7. Synthesis and characterization of novel bactericidal Cu/HPMC BNCs using chemical reduction method for food packaging.

    Science.gov (United States)

    Ebrahimiasl, Saeideh; Rajabpour, Ataollah

    2015-09-01

    In this research copper nanoparticles (Cu NPs) were incorporated in the biodegradable hydroxypropyl methylcellulose (HPMC) matrix using the simple and low cost chemical reduction method for application as food packaging material. The properties of Cu/HPMC bionanocomposites (BNCs) were studied as a function of the CuSO4 concentration. Surface morphology of the film was investigated by scanning electron microscopy. Mechanical analysis and water vapor barrier properties of HPMC/Cu nanocomposites were analyzed. It was observed that mechanical and water vapor barrier properties of the films were improved by the concentration of CuSO4. The antibacterial activity of HPMC/Cu thin films were evaluated based on the diameter of inhibition zone in a disk diffusion test against Gram positive bacteria, ie, Streptococus A., S. epidermidis, S.aureus , B.cereus and Gram negative bacteria, ie, E. coli, E. faecalis, Salmonella, P. aeruginosa using Mueller Hinton agar at different concentration of CuSO4. The results revealed a greater bactericidal effectiveness for nanocomposite films containing 5 % of CuSO4. Packages prepared from HPMC/Cu nanocomposite films were used for meat packaging. The films were filled with meat and then stored at 4 °C. Microbial stability of the meat was evaluated after 3, 7, 10 and 15 days of storage. The results showed that microbial growth rate significantly reduced as a result of using this nanocomposite packaging material.

  8. Chemical Synthesis, Characterization, and Biocompatibility Study of Hydroxyapatite/Chitosan Phosphate Nanocomposite for Bone Tissue Engineering Applications

    Directory of Open Access Journals (Sweden)

    Nabakumar Pramanik

    2009-01-01

    Full Text Available A novel bioanalogue hydroxyapatite (HAp/chitosan phosphate (CSP nanocomposite has been synthesized by a solution-based chemical methodology with varying HAp contents from 10 to 60% (w/w. The interfacial bonding interaction between HAp and CSP has been investigated through Fourier transform infrared absorption spectra (FTIR and x-ray diffraction (XRD. The surface morphology of the composite and the homogeneous dispersion of nanoparticles in the polymer matrix have been investigated through scanning electron microscopy (SEM and transmission electron microscopy (TEM, respectively. The mechanical properties of the composite are found to be improved significantly with increase in nanoparticle contents. Cytotoxicity test using murine L929 fibroblast confirms that the nanocomposite is cytocompatible. Primary murine osteoblast cell culture study proves that the nanocomposite is osteocompatible and highly in vitro osteogenic. The use of CSP promotes the homogeneous distribution of particles in the polymer matrix through its pendant phosphate groups along with particle-polymer interfacial interactions. The prepared HAp/CSP nanocomposite with uniform microstructure may be used in bone tissue engineering applications.

  9. Production and structural characterization of nanolayers of LiNbO{sub 3} by wet chemical synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Eger, Doreen; Gutmann, Emanuel; Stoecker, Hartmut; Mehner, Erik; Meyer, Dirk-Carl [TU Bergakademie Freiberg, Inst. fuer Experimentelle Physik (Germany)

    2012-07-01

    There are many known applications of pyroelectrics. Some new ideas, e.g. disinfecting and biocatalytic surfaces, require thin pyroelectric layers on a substrate. A substance with high pyroelectric coefficient is lithium niobate. There, basic investigations of a new method for manufacturing thin layers of lithium niobate are presented. The thin layers are produced by dip coating of fused silica in a solvent of lithium niobate. Samples with different drawing speed and reaction temperature are manufactured. The resulting layers are characterized by reflected light microscopy (RLM), atomic force microscopy (AFM) and X-ray diffraction (XRD). It is proven by XRD that the layers consist of lithium niobate. AFM and RLM show that samples with low drawing speed become so thick that clefts are formed. Therefore, the manufacturing of nanolayers of lithium niobate with dip coating is possible and reasonable. For an optimization of process parameters for deposition of a defined layer thickness more improvement of the method is necessary, e.g. adding a wetting agent or a conditioning step of the substrate.

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

    CERN Document Server

    Yihong, Wu; Ting, Yu

    2013-01-01

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

  11. Novel biodegradable aliphatic poly(butylene succinate-co-cyclic carbonate)s with functional carbonate building blocks. 1. Chemical synthesis and their structural and physical characterization.

    Science.gov (United States)

    Yang, Jing; Hao, Qinghui; Liu, Xiaoyun; Ba, Chaoyi; Cao, Amin

    2004-01-01

    This study presents chemical synthesis, structural, and physical characterization of novel biodegradable aliphatic poly(butylene succinate-co-cyclic carbonate)s P(BS-co-CC) bearing functional carbonate building blocks. First, five kinds of six-membered cyclic carbonate monomers, namely, trimethylene carbonate (TMC), 1-methyl-1,3-trimethylene carbonate (MTMC), 2,2-dimethyl-1,3-trimethylene carbonate (DMTMC), 5-benzyloxytrimethylene carbonate (BTMC), and 5-ethyl-5-benzyloxymethyl trimethylene carbonate (EBTMC), were well prepared from ethyl chloroformate and corresponding diols at 0 degrees C in THF solution with our modified synthetic strategies. Then, a series of new P(BS-co-CC)s were synthesized at 210 degrees C through a simple combination of poly-condensation and ring-opening-polymerization (ROP) of hydroxyl capped PBS macromers and the prepared carbonate monomers, and titanium tetra-isopropoxide Ti(i-OPr)4 was used as a more suitable catalyst of 5 candidate catalysts which could concurrently catalyze poly-condensation and ROP. By means of NMR, GPC, FTIR, and thermal analytical instruments, macromolecular structures and physical properties have been characterized for these aliphatic poly(ester carbonate)s. The experimental results indicated that novel biodegradable P(BS-co-CC)s were successfully synthesized with number average molecular weight Mn ranging from 24.3 to 99.6 KDa and various CC molar contents without any detectable decarboxylation and that the more bulky side group was attached to a cyclic carbonate monomer, the lower reactivity for its copolymerization would be observed. The occurrences of 13C NMR signal splitting of succinyl carbonyl attributed to the BS building blocks could be proposed due to the randomized sequences of BS and CC building blocks. FTIR characterization indicated two distinct absorption bands at 1716 and 1733 approximately 1735 cm(-1), respectively, stemming from carbonyl stretching modes for corresponding BS and CC units. With

  12. Synthesis, Characterization, Antimicrobial Studies and Corrosion Inhibition Potential of 1,8-dimethyl-1,3,6,8,10,13-hexaazacyclotetradecane: Experimental and Quantum Chemical Studies

    Directory of Open Access Journals (Sweden)

    Henry U. Nwankwo

    2016-02-01

    Full Text Available The macrocylic ligand, 1,8-dimethyl-1,3,6,8,10,13-hexaazacyclotetradecane (MHACD was synthesized by the demetallation of its freshly synthesized Ni(II complex (NiMHACD. Successful synthesis of NiMHACD and the free ligand (MHACD was confirmed by various characterization techniques, including Fourier transform infra-red (FT-IR, proton nuclear magnetic resonance (1H-NMR, carbon-13 nuclear magnetic resonance (13C-NMR, ultraviolet-visible (UV-vis, and energy dispersive x-ray (EDX spectroscopic techniques. The anti-bacteria activities of MHACD were investigated against Staphylococcus aureus and Enterococcus species and the results showed that MHACD possesses a spectrum of activity against the two bacteria. The electrochemical cyclic voltammetry study on MHACD revealed that it is a redox active compound with promising catalytic properties in electrochemical applications. The inhibition potential of MHACD for mild steel corrosion in 1 M HCl was investigated using potentiodynamic polarization method. The results showed that MHACD inhibits steel corrosion as a mixed-type inhibitor, and the inhibition efficiency increases with increasing concentration of MHACD. The adsorption of MHACD obeys the Langmuir adsorption isotherm; it is spontaneous and involves competitive physisorption and chemisorption mechanisms. Quantum chemical calculations revealed that the energy of the highest occupied molecular orbital (HOMO of MHACD is high enough to favor forward donation of charges to the metal during adsorption and corrosion inhibition. Natural bond orbital (NBO analysis revealed the presence of various orbitals in the MHACD that are capable of donating or accepting electrons under favorable conditions.

  13. Synthesis, chemical characterization, computational studies and biological activity of new DNA methyltransferases (DNMTs) specific inhibitor. Epigenetic regulation as a new and potential approach to cancer therapy.

    Science.gov (United States)

    Pellerito, C; Morana, O; Ferrante, F; Calvaruso, G; Notaro, A; Sabella, S; Fiore, T

    2015-09-01

    This work deals with the synthesis, the chemical characterization of dibutyltin(IV) complex of caffeic acid (Bu2Sn(IV)HCAF, caf1) and its cytotoxic action on tumor cells. The coordination environment at the tin center was investigated by FTIR, (119)Sn{(1)H} cross polarization magic angle spinning, electrospray ionization mass spectroscopy in the solid state and UV-vis, fluorescence and (1)H, (13)C and (119)Sn NMR spectroscopy in solution phases. Density functional theory study confirmed the proposed structures in solution phase and indicated the most probably stable conformation. The effects on viability of breast cancer MDA-MB231, colorectal cancer HCT116, hepatocellular carcinoma HepG2 and Chang liver cells, an immortalized non-tumor hepatic cell line, have been investigated. The effect of a variation in structure of caf1 was found to lead to a change in the respective antiproliferative properties: caf1 induces loss of viability in HCT116, MDA-MB-231, and HepG2; the complex shows only moderate effects in non-tumor Chang liver cells. caf1 exerts lower cytotoxic activity than Bu2SnCl2, suggesting that the binding with H3CAF modulates the marked cytotoxic activity exerted by Bu2SnCl2; caf1 displays a considerably more pronounced antitumoural effect towards cell lines than caffeic acid. It is known that caffeic acid can modulate DNA (cytosine-5)-methyltransferases 1 (DNMT1) mediated DNA methylation. In this paper we demonstrate that caf1 treatment was able to induce a time-dependent reduction of global DNA methylated status. This effect was also confirmed by a concomitant reduction DNMT1 expression level. The effect induced by caf1 was more evident not only with respect to untreated cells but also compared to H3CAF treated cells.

  14. Protein chemical synthesis in drug discovery.

    Science.gov (United States)

    Liu, Fa; Mayer, John P

    2015-01-01

    The discovery of novel therapeutics to combat human disease has traditionally been among the most important goals of research chemists. After a century of innovation, state-of-the-art chemical protein synthesis is now capable of efficiently assembling proteins of up to several hundred residues in length from individual amino acids. By virtue of its unique ability to incorporate non-native structural elements, chemical protein synthesis has been seminal in the recent development of several novel drug discovery technologies. In this chapter, we review the key advances in peptide and protein chemistry which have enabled our current synthetic capabilities. We also discuss the synthesis of D-proteins and their applications in mirror image phage-display and racemic protein crystallography, the synthesis of enzymes for structure-based drug discovery, and the direct synthesis of homogenous protein pharmaceuticals.

  15. Synthesis and Characterization of Multithiouracils

    Institute of Scientific and Technical Information of China (English)

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

    2003-01-01

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

  16. Methanol synthesis beyond chemical equilibrium

    NARCIS (Netherlands)

    van Bennekom, J. G.; Venderbosch, R. H.; Winkelman, J. G. M.; Wilbers, E.; Assink, D.; Lemmens, K. P. J.; Heeres, H. J.

    2013-01-01

    In commercial methanol production from syngas, the conversion is thermodynamically limited to 0.3-0.7 leading to large recycles of non-converted syngas. This problem can be overcome to a significant extent by in situ condensation of methanol during its synthesis which is possible nowadays due to the

  17. Chemical synthesis and characterization of J46 peptide, an atypical class IIa bacteriocin from Lactococcus lactis subsp. cremoris J46 Strain.

    Science.gov (United States)

    Lasta, Samar; Fajloun, Ziad; Darbon, Hervé; Mansuelle, Pascal; Andreotti, Nicolas; Sabatier, Jean-Marc; Boudabous, Abdellatif; Sampieri, François

    2008-02-01

    Bacteriocin J46 is a 27-residue polypeptide produced by Lactococcus lactis subsp. cremoris J46 in fermented milk. The natural form of J46 (nJ46) exhibits a broad antimicrobial spectrum. Herein, we produced the synthetic form of J46 (sJ46) by solid-phase chemical synthesis. The biochemical and physico-chemical properties of sJ46, as well as its antimicrobial activity, were found to be identical to those of its natural counterpart nJ46. It showed a potent antimicrobial activity against both lactic acid bacteria and other Gram-positive microorganisms. (1)H-NMR conformational analysis of sJ46 indicates that it adopts a flexible random coil structure.

  18. ALTERNATIVE FUELS AND CHEMICALS FROM SYNTHESIS GAS

    Energy Technology Data Exchange (ETDEWEB)

    Unknown

    1999-04-01

    The overall objectives of this program are to investigate potential technologies for the conversion of synthesis gas to oxygenated and hydrocarbon fuels and industrial chemicals, and to demonstrate the most promising technologies at DOE's LaPorte, Texas, Slurry Phase Alternative Fuels Development Unit (AFDU). The program will involve a continuation of the work performed under the Alternative Fuels from Coal-Derived Synthesis Gas Program and will draw upon information and technologies generated in parallel current and future DOE-funded contracts.

  19. Alternative Fuels and Chemicals from Synthesis Gas

    Energy Technology Data Exchange (ETDEWEB)

    None, None

    1998-12-02

    The overall objectives of this program are to investigate potential technologies for the conversion of synthesis gas to oxygenated and hydrocarbon fuels and industrial chemicals, and to demonstrate the most promising technologies at DOE's LaPorte, Texas, Slurry Phase Alternative Fuels Development Unit (AFDU). The program will involve a continuation of the work performed under the Alternative Fuels from Coal-Derived Synthesis Gas Program and will draw upon information and technologies generated in parallel current and future DOE-funded contracts.

  20. ALTERNATIVE FUELS AND CHEMICALS FROM SYNTHESIS GAS

    Energy Technology Data Exchange (ETDEWEB)

    Peter Tijrn

    2003-02-03

    The overall objectives of this program are to investigate potential technologies for the conversion of synthesis gas to oxygenated and hydrocarbon fuels and industrial chemicals, and to demonstrate the most promising technologies at DOE's LaPorte, Texas, Slurry Phase Alternative Fuels Development Unit (AFDU). The program will involve a continuation of the work performed under the Alternative Fuels from Coal-Derived Synthesis Gas Program and will draw upon information and technologies generated in parallel current and future DOE-funded contracts.

  1. Alternative fuels and chemicals from synthesis gas

    Energy Technology Data Exchange (ETDEWEB)

    Unknown

    1998-08-01

    The overall objectives of this program are to investigate potential technologies for the conversion of synthesis gas to oxygenated and hydrocarbon fuels and industrial chemicals, and to demonstrate the most promising technologies at DOE's LaPorte, Texas, Slurry Phase Alternative Fuels Development Unit (AFDU). The program will involve a continuation of the work performed under the Alternative Fuels from Coal-Derived Synthesis Gas Program and will draw upon information and technologies generated in parallel current and future DOE-funded contracts.

  2. New strategies in chemical synthesis and catalysis

    CERN Document Server

    Pignataro, Bruno

    2012-01-01

    Providing a comprehensive overview of the essential topics, this book covers the core areas of organic, inorganic, organometallic, biochemical synthesis and catalysis.The authors are among the rising stars in European chemistry, a selection of participants in the 2010 European Young Chemists Award competition, and their contributions deal with most of the frontier issues in chemical synthesis. They give an account of the latest research results in chemistry in Europe, as well as the state of the art in their field of research and the outlook for the future.

  3. Alternative Fuels and Chemicals from Synthesis Gas

    Energy Technology Data Exchange (ETDEWEB)

    Peter Tijrn

    2003-01-02

    The overall objectives of this program are to investigate potential technologies for the conversion of synthesis gas to oxygenated and hydrocarbon fuels and industrial chemicals, and to demonstrate the most promising technologies at DOE's LaPorte, Texas, Slurry Phase Alternative Fuels Development Unit (AFDU). The program will involve a continuation of the work performed under the Alternative Fuels from Coal-Derived Synthesis Gas Program and will draw upon information and technologies generated in parallel current and future DOE-funded contracts.

  4. ALTERNATIVE FUELS AND CHEMICALS FROM SYNTHESIS GAS

    Energy Technology Data Exchange (ETDEWEB)

    Unknown

    1999-01-01

    The overall objectives of this program are to investigate potential technologies for the conversion of synthesis gas to oxygenated and hydrocarbon fuels and industrial chemicals, and to demonstrate the most promising technologies at DOE's LaPorte, Texas, Slurry Phase Alternative Fuels Development Unit (AFDU). The program will involve a continuation of the work performed under the Alternative Fuels from Coal-Derived Synthesis Gas Program and will draw upon information and technologies generated in parallel current and future DOE-funded contracts.

  5. Alternative Fuels and Chemicals From Synthesis Gas

    Energy Technology Data Exchange (ETDEWEB)

    none

    1998-07-01

    The overall objectives of this program are to investigate potential technologies for the conversion of synthesis gas to oxygenated and hydrocarbon fuels and industrial chemicals, and to demonstrate the most promising technologies at DOE's LaPorte, Texas, Slurry Phase Alternative Fuels Development Unit (AFDU). The program will involve a continuation of the work performed under the Alternative Fuels from Coal-Derived Synthesis Gas Program and will draw upon information and technologies generated in parallel current and future DOE-funded contracts.

  6. Synthesis and characterization of M-type barium hexferrite by ultrasonic inter-dispersion of chemical precipitate; Sintese e caracterizacao de hexaferrita de bario tipo M por interdispersao ultrassonica de precipitado quimico

    Energy Technology Data Exchange (ETDEWEB)

    Garcia Junior, E.S.; Gomes Junior, G.G.; Ogasawara, T., E-mail: edil@metalmat.ufrj.b [Universidade Federal do Rio de Janeiro (COPPE/UFRJ), RJ (Brazil). Coordenacao dos Programas de Pos-Graduacao de Engenharia. Dept. de Eng. Metalurgica e Materiais

    2010-07-01

    This work is concerned with the study the synthesis and characterization of M-type barium hexaferrite powder by chemical precipitation type and ultrasonic interdispersion of precursor materials Fe(OH){sub 3} and Ba(OH){sub 2},separately and ultrasonic inter-dispersion, followed by drying and calcining. In order to guide the experimental work was carried out a preliminary thermodynamic analysis of the system Ba-Fe-H{sub 2}O at 25 deg C. The study shows that the phase formation of M-type barium hexaferrite is obtained at a calcination at 1000 deg C, characterized by X-ray diffraction, the grain growth of the final product of synthesis depending on the calcination temperature is visible by SEM. The synthesis method developed in this research is an option to achieve the results that would be obtained if the co-precipitation of ferric and barium hydroxide was thermodynamically possible, where you can get crystallization of barium hexaferrite in a calcination at 1000 deg C. (author)

  7. Synthesis and Characterization of Novel Quaternary Thioaluminogermanates

    KAUST Repository

    Al-Bloushi, Mohammed

    2013-05-01

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

  8. Speciality chemicals from synthesis gas

    Energy Technology Data Exchange (ETDEWEB)

    Lin, J.J.; Knifton, J.F. (Shell Development Company, Houston, TX (USA))

    1992-04-01

    Texaco has undertaken research to investigate the use of carbon monoxide and hydrogen as building blocks for the manufacture of amidocarbonylation products. The amidocarbonylation reaction offers a convenient method to construct two functionalities - amido and carboxylate - simultaneously. Texaco has extended this chemistry to make a variety of speciality chemicals by tailoring cobalt catalysts. Products which have been made including: surface active agents such as the C{sub 14} - C{sub 16} alkyl amidoacids; surfactants; intermediates for sweeteners like aspartame; food additives like glutamic acid; and chelating agents such as polyamidoacids. 20 refs., 10 figs., 1 tab.

  9. The Chemical Synthesis of Discodermolide

    Science.gov (United States)

    Paterson, I.; Florence, G. J.

    The marine sponge-derived polyketide discodermolide is a potent antimitotic agent that represents a promising natural product lead structure in the treatment of cancer. Discodermolide shares the same microtubule-stabilising mechanism of action as Taxol®, inhibits the growth of solid tumours in animal models and shows synergy with Taxol. The pronounced cytotoxicity of discodermolide, which is maintained against cancer cell lines that display resistance to Taxol and other drugs, combined with its scarce availability from its natural source, has fuelled significant academic and industrial interest in devising a practical total synthesis as a means of ensuring a sustainable supply for drug development. This chapter surveys the various total syntheses of discodermolide that have been completed over the period 1993-2007, focusing on the strategies employed for introduction of the multiple stereocentres and achieving control over the alkene geometry, along with the various methods used for realising the pivotal fragment couplings to assemble progressively the full carbon skeleton. This dedicated synthetic effort has triumphed in removing the supply problem for discodermolide, providing sufficient material for extensive biological studies and enabling its early stage clinical development, as well as facilitating SAR studies for lead optimisation.

  10. Synthesis, Characterization and Decomposition Studies of Tris(N,N-dibenzyldithiocarbamato) Indium(III): Chemical Spray Deposition of Polycrystalline CuInS2 on Copper Films

    Science.gov (United States)

    Hehemann, David G.; Lau, J. Eva; Harris, Jerry D.; Hoops, Michael D.; Duffy, Norman V.; Fanwick, Philip E.; Khan, Osman; Jin, Michael H.-C.; Hepp, Aloysius F.

    2005-01-01

    Tris(bis(phenylmethyl)carbamodithioato-S,S ), commonly referred to as tris(N,Ndibenzyldithiocarbamato) indium(III), In(S2CNBz2)3, was synthesized and characterized by single crystal X-ray crystallography. The compound crystallizes in the triclinic space group P1 bar with two molecules per unit cell. The material was further characterized using a novel analytical system employing the combined powers of thermogravimetric analysis, gas chromatography/mass spectrometry and Fourier-Transform infrared spectroscopy to investigate its potential use as a precursor for the chemical vapor deposition (CVD) of thin film materials for photovoltaic applications. Upon heating, the material thermally decomposes to release CS2 and benzyl moieties in to the gas phase, resulting in bulk In2S3. Preliminary spray CVD experiments indicate that In(S2CNBz2)3 decomposed on a Cu substrate reacts to produce stoichiometric CuInS2 films.

  11. Synthesis, characterization, and catalysis of metal nanoparticles

    Science.gov (United States)

    Mott, Derrick M.

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2013-07-15

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

  13. Synthesis of poly(D,L-lactide-co-glycolide) copolymers and its chemical characterization by NMR and FTIR; Sintese e caracterizacao quimica por RMN e FTIR do copolimero poli(D,L-lactideo-co-glicolideo)

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2011-07-01

    Poly(D,L-lactide-co-glycolide) copolymer is of great interest for medical applications. This interest is justified by the fact that it is bioreabsorbable, biocompatible and non-toxic, while its degradation kinetics can be modified by the copolymerization ratio of the monomers. In this study, copolymers were synthesized at 175 deg C by opening the rings of the cyclic dimers of the D,L-lactide and glycolide monomers in the presence of stannous octoate initiator and lauryl alcohol co-initiator. The efficient application of a vacuum to the reaction medium, coupled with adequate stirring, is fundamental for the success of the synthesis. The following analysis techniques were used to characterize the synthesized copolymers: Nuclear Magnetic Resonance Spectroscopy (NMR) and Fourier Transform Infrared Spectroscopy (FTIR). The chemical composition and the ratio of the monomers in the synthesized copolymer were determined. (author)

  14. Synthesis and physico-chemical characterization of CeO{sub 2}/ZrO{sub 2}-SO{sub 4}{sup 2-} mixed oxides

    Energy Technology Data Exchange (ETDEWEB)

    Hernandez E, J. M.; Silva R, R.; Garcia A, R. [Instituto Tecnologico de Ciudad Madero, Div. de Estudios de Posgrado e Investigacion, Juventino Rosas y Jesus Urueta s/n, Col. Los Mangos, 89440 Ciudad Madero, Tamaulipas (Mexico); Garcia S, L. A. [IPN, Centro Interdisciplinario de Investigaciones y de Estudios sobre Medio Ambiente y Desarrollo, 30 de Junio No. 1520, Barrio La Laguna Ticoman, 07340 Mexico D. F. (Mexico); Handy, B. E.; Cardenas G, G. [Universidad Autonoma de San Luis Potosi, CIEP, Facultad de Ciencias Quimicas, Av. Dr. Manuel Nava No. 6, Zona Universitaria, 78210 SLP, San Luis Potosi (Mexico); Cueto H, A. [Universidad Autonoma Metropolitana, Unidad Azcapotzalco, Av. San Pablo No. 180, Col. Reynosa Tamaulipas, 02200 Mexico D. F. (Mexico)

    2012-07-01

    Environmentally friendly solid-acid catalysts CeO{sub 2}/ZrO{sub 2}-SO{sub 4}{sup 2-} were prepared by the sol gel method varying CeO{sub 2} content (10, 20 and 30 wt %) and using sulfation in situ, maintaining the sulfate ions amount present in the materials at 20 wt %. ZrO{sub 2} and ZrO{sub 2}-SO{sub 4}{sup 2-} were also prepared for comparison proposes using the same synthesis method. The materials were characterized by X-ray diffraction, nitrogen physisorption, potentiometric titration with n-butylamine, decomposition of 2-propanol and n-pentane isomerization. The specific surface area of ZrO{sub 2}-SO{sub 4}{sup 2-} was high (160 m{sup 2}/g) compared with the unmodified ZrO{sub 2} (80 m{sup 2}/g), however this area decreased with increasing the CeO{sub 2} content (37-100 m{sup 2}/g). There was no significant effect of CeO{sub 2} on the tetragonal structure of ZrO{sub 2}-SO{sub 4}{sup 2-}. The variation of acid sites amount runs parallel to the change of specific surface area. The acid sites amount decreased with increasing cerium oxide content. The decomposition of 2-propanol results fundamentally in the formation of dehydration products such as propylene and diisopropyl ether, both involving acid sites. In addition, a good performance during the n-pentane isomerization was observed for these materials. The selectivity towards isopentane reaches 84% when the Pt/CeO{sub 2}/ZrO{sub 2}-SO{sub 4}{sup 2-} catalyst with the highest CeO{sub 2} content was used. (Author)

  15. Synthesis and characterization of mibolerone

    Institute of Scientific and Technical Information of China (English)

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

    2007-01-01

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

  16. A novel polyvinyl alcohol hydrogel functionalized with organic boundary lubricant for use as low-friction cartilage substitute: synthesis, physical/chemical, mechanical, and friction characterization.

    Science.gov (United States)

    Blum, Michelle M; Ovaert, Timothy C

    2012-10-01

    A novel material design was developed by functionalizing polyvinyl alcohol hydrogel with an organic low-friction boundary lubricant (molar ratios of 0.2, 0.5, and 1.0 moles of lauroyl chloride). The hydrogels were fabricated using two different techniques. First, the boundary lubricant was initially functionalized to the polymer, then the hydrogels were created by physically crosslinking the reacted polymer. Second, hydrogels were initially created by crosslinking pure polyvinyl alcohol, with the functionalization reaction performed on the fully formed gel. After the reaction, Fourier transform infrared spectroscopy and attenuated total reflectance spectra revealed a clear ester peak, the diminishment of the alcohol peak, and the amplification of the alkyl peaks, which confirmed attachment of the hydrocarbon chains to the polymer. Additional chemical characterization occurred through elemental analysis where an average increase of 22% carbon and 40% hydrogen provided further confirmation of attachment. Physical characterization of the boundary lubricant functionalized hydrogels was performed by water content and contact angle measurements. Water content dependency showed that method 1 had a direct relationship with boundary lubricant concentration, and method 2 displayed an inverse relationship. The contact angle increased as boundary lubricant concentration increased for the pure matrix material for both processing methods, suggesting that the hydrocarbons produced surface properties that mimic natural cartilage, and contact behavior of the biphasic system was dependent on processing method. Friction tests demonstrated a significant decrease in friction coefficient, with a maximum decrease of 70% and a minimum decrease of 24% for boundary lubricant functionalized hydrogels compared with nonfunctionalized polyvinyl alcohol hydrogels.

  17. Isomers of Poly Aminophenol: Chemical Synthesis, Characterization, and Its Corrosion Protection Aspect on Mild Steel in 1 M HCl

    Directory of Open Access Journals (Sweden)

    G. Thenmozhi

    2014-01-01

    Full Text Available The oxidative chemical polymerizations of three isomers of aminophenol, ortho, meta, and para (PoAP, PmAP, and PpAP, were performed in aqueous HCl using ammonium persulfate as an oxidant at 0–3°C. The synthesized polymers were characterized by employing elemental analysis, GPC, UV-VIS-NIR, FT-IR, XRD, and TGA. The corrosion inhibition effect of these three polymers on mild steel in 1 M HCl solution was studied by using electrochemical techniques such as potentiodynamic polarization and electrochemical impedance spectroscopy. These measurements reveal that the inhibition efficiency obtained by these polymers increased by increasing their concentration. The inhibition efficiency follows the order PpAP > PoAP > PmAP. The results further revealed that PpAP at a concentration of 250 mg/L furnishes maximum inhibition efficiency (96.5%. Polarization studies indicated that these three polymers act as the mixed type corrosion inhibitors.

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

    Science.gov (United States)

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

    2012-01-01

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

  19. Synthesis of Ethyl Salicylate Using Household Chemicals

    Science.gov (United States)

    Solomon, Sally; Hur, Chinhyu; Lee, Alan; Smith, Kurt

    1996-02-01

    Ethyl salicylate is synthesized, isolated, and characterized in a three-step process using simple equipment and household chemicals. First, acetylsalicylic acid is extracted from aspirin tablets with isopropyl alcohol, then hydrolyzed to salicylic acid with muriatic acid, and finally, the salicylic acid is esterified using ethanol and a boric acid catalyst. The experiment can be directed towards high school or university level students who have sufficient background in organic chemistry to recognize the structures and reactions that are involved.

  20. Osmium(III) analogues of KP1019: Electrochemical and chemical synthesis, spectroscopic characterization, x-ray crystallography, hydrolytic stability, and antiproliferative activity

    KAUST Repository

    Kuhn, Paul-Steffen

    2014-10-20

    A one-electron reduction of osmium(IV) complexes trans-[OsIVCl4(Hazole)2], where Hazole = 1H-pyrazole ([1]0), 2H-indazole ([2]0), 1H-imidazole ([3]0), and 1H-benzimidazole ([4]0), afforded a series of eight new complexes as osmium analogues of KP1019, a lead anticancer drug in clinical trials, with the general formula (cation)[trans-OsIIICl4(Hazole)2], where cation = H2pz+ (H2pz[1]), H2ind+ (H2ind[2]), H2im+ (H2im[3]), Ph4P+ (Ph4P[3]), nBu4N+ (nBu4N[3]), H2bzim+ (H2bzim[4]), Ph4P+ (Ph4P[4]), and nBu4N+ (nBu4N[4]). All complexes were characterized by elemental analysis, 1H NMR spectroscopy, electrospray ionization mass spectrometry, UV-vis spectroscopy, cyclic voltammetry, while H2pz[1], H2ind[2], and nBu4[3], in addition, by X-ray diffraction. The reduced species [1]- and [4]- are stable in aqueous media in the absence of air oxygen and do not react with small biomolecules such as amino acids and the nucleotide 5′-dGMP. Cell culture experiments in five different human cancer cell lines (HeLa, A549, FemX, MDA-MB-453, and LS-174) and one noncancerous cell line (MRC-5) were performed, and the results were discussed and compared to those for KP1019 and cisplatin. Benzannulation in complexes with similar structure enhances antitumor activity by several orders of magnitude, implicating different mechanisms of action of the tested compounds. In particular, complexes H2ind[2] and H2bzim[4] exhibited significant antiproliferative activity in vitro when compared to H2pz[1] and H2im[3]. (Chemical Equation Presented).

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

    Science.gov (United States)

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

    2016-08-10

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

  2. Chemically-enzymatic synthesis of photosensitive DNA.

    Science.gov (United States)

    Westphal, Kinga; Zdrowowicz, Magdalena; Zylicz-Stachula, Agnieszka; Rak, Janusz

    2017-02-01

    The sensitizing propensity of radio-/photosensitizing nucleoside depends on DNA sequence surrounding a sensitizer. Therefore, in order to compare sensitizers with regard to their ability to induce a DNA damage one has to study the sequence dependence of damage yield. However, chemical synthesis of oligonucleotides labeled with sensitizing nucleosides is hindered due to the fact that a limited number of such nucleoside phosphoramidites are accessible. Here, we report on a chemically-enzymatic method, employing a DNA polymerase and ligase, that enables a modified nucleoside, in the form of its 5'-triphosphate, to be incorporated into DNA fragment in a pre-determined site. Using such a protocol two double-stranded DNA fragments - a long one, 75 base pairs (bp), and a short one, 30bp in length - were pin-point labeled with 5-bromodeoxyuridine. Four DNA polymerases together with DHPLC for the inspection of reaction progress were used to optimize the process under consideration. As an ultimate test showing that the product possessing an assumed nucleotide sequence was actually obtained, we irradiated the synthesized oligonucleotide with UVB photons and analyzed its photoreactivity with the LC-MS method. Our results prove that a general approach enabling precise labeling of DNA with any nucleoside modification processed by DNA polymerase and ligase has been worked out.

  3. Ethyl coumarin-3-carboxylate: synthesis and chemical properties

    Directory of Open Access Journals (Sweden)

    Bakr F. Abdel-Wahab

    2014-03-01

    Full Text Available Ethyl coumarin-3-carboxylate occupies an important position in the organic synthesis and is used in production of biologically active compounds. Thus, the data published over the last few years on the methods of synthesis and chemical properties of ethyl coumarin-3-carboxylate are reviewed here for the first time. The reactions were classified as coumarin ring reactions and ester group reactions, and some of these reactions have been applied successfully to the synthesis of biologically and industrially important compounds.

  4. Aliphatic nitro alcohols. Synthesis, chemical transformations and applications

    Energy Technology Data Exchange (ETDEWEB)

    Shvekhgeimer, Mai-Genrikh A [A.N. Kosygin Moscow State Textile Academy, Moscow (Russian Federation)

    1998-01-31

    The data on the synthesis, chemical transformations and practical use of aliphatic nitro alcohols published over the last 25 years are described systematically and analysed. The bibliography includes 316 references.

  5. Trypsin inhibitors from the garden four o'clock (Mirabilis jalapa) and spinach (Spinacia oleracea) seeds: isolation, characterization and chemical synthesis.

    Science.gov (United States)

    Kowalska, Jolanta; Pszczoła, Katarzyna; Wilimowska-Pelc, Anna; Lorenc-Kubis, Irena; Zuziak, Ewa; Ługowski, Mateusz; Łegowska, Anna; Kwiatkowska, Anna; Sleszyńska, Małgorzata; Lesner, Adam; Walewska, Aleksandra; Zabłotna, Ewa; Rolka, Krzysztof; Wilusz, Tadeusz

    2007-06-01

    Five serine proteinase inhibitors (Mirabilis jalapa trypsin inhibitors, MJTI I and II and Spinacia oleracea trypsin inhibitors, SOTI I, II, and III) from the garden four-o'clock (M. jalapa) and spinach (S. oleracea) seeds were isolated. The purification procedures included affinity chromatography on immobilized methylchymotrypsin in the presence of 5M NaCl, ion exchange chromatography and/or preparative electrophoresis, and finally RP-HPLC on a C-18 column. The inhibitors, crosslinked by three disulfide bridges, are built of 35 to 37 amino-acid residues. Their primary structures differ from those of known trypsin inhibitors, but showed significant similarity to the antimicrobial peptides isolated from the seeds of M. jalapa (MJ-AMP1, MJ-AMP2), Mesembryanthemum crystallinum (AMP1), and Phytolacca americana (AMP-2 and PAFP-S) and from the hemolymph of Acrocinus longimanus (Alo-1, 2 and 3). The association equilibrium constants (K(a)) with bovine beta-trypsin for the inhibitors from M. jalapa (MJTI I and II) and S. oleracea (SOTI I-III) were found to be about 10(7)M(-1). Fully active MJTI I and SOTI I were obtained by solid-phase peptide synthesis. The disulfide bridge pattern in both inhibitors (Cys1-Cys4, Cys2-Cys5 and Cys3-Cys6) was established after their digestion with thermolysin and proteinase K followed by the MALDI-TOF analysis.

  6. Synthesis and characterization of polyethylene glycol (PEG) coated Fe3O4 nanoparticles by chemical co-precipitation method for biomedical applications.

    Science.gov (United States)

    Anbarasu, M; Anandan, M; Chinnasamy, E; Gopinath, V; Balamurugan, K

    2015-01-25

    Polyethylene glycol (PEG) coated Fe3O4 nanoparticles were synthesized by chemical co-precipitation method. With polyethylene glycol (PEG) as a stabilizer and dispersant. The X-ray diffraction and selected area electron diffraction (SAED) results show that the cubic inverse spinel structure of pure phase polycrystalline Fe3O4 was obtained. The scanning electron microscopy (SEM) and field emission transmission electron microscopy (FE-TEM) results exhibited that the resulted Fe3O4 nanoparticles were roughly spherical in shape with narrow size distribution and homogenous shape. Fourier transform infrared spectroscopy (FT-IR) results suggested that PEG indicated with Fe3O4 via its carbonyl groups. Results of vibrating sample magnetometer (VSM) indicated that the prepared Fe3O4 nanoparticles exhibit superparamagnetic behavior and high saturation magnetization at room temperature. Such Fe3O4 nanoparticles with favorable size and tunable magnetic properties are promising biomedical applications.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1993-10-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Smith, M.E.

    1993-10-01

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

  9. Fucoxanthin Derivatives: Synthesis and their Chemical Properties.

    Science.gov (United States)

    Komba, Shiro; Kotake-Nara, Eiichi; Machida, Sachiko

    2015-01-01

    Novel fucoxanthin derivatives that could change the size of mixed micelles were synthesized. The mixed micelles under consideration consist of a bile acid and some additives. To change the affinity against a bile acid, we designed the synthesis of a fucoxanthin-lithocholic acid complex. Lithocholic acid is one of the bile acids. The 3-OH on lithocholic acid was protected by a levulinyl group, and the protected lithocholic acid was selectively coupled via an ester linkage to the 3-OH on fucoxanthin to obtain levulinyl-protected lithocholyl fucoxanthin (LevLF). The levulinyl group was then selectively deprotected using hydrazine to obtain a lithocholyl fucoxanthin (LF). The average sizes of the micelles that contained these compounds (fucoxanthin, LevLF, and LF) with a bile acid (sodium taurocholate) were measured. The LevLF induced larger micelles than fucoxanthin or LF. Interestingly, the addition of 1-oleoyl-rac-glycerol induced a more efficient change in the micelle size. The large micelles grew larger, and the small micelles became smaller. Triple-mixed micelles with LevLF, sodium taurocholate, and 1-oleoyl-rac-glycerol formed the largest micelle with a diameter of 68 nm. On the other hand, triple-mixed micelles using LF, sodium taurocholate, and 1-oleoyl-rac-glycerol made the smallest micelles with diameters as low as 12 nm. We also investigated the hydrolysis of these compounds with enzymes (esterase from porcine liver, lipase from porcine pancreas, and cholesterol esterase from Pseudomonas sp.). The ester linkage between the lithocholic acid and fucoxanthin of LevLF was hydrolyzed with cholesterol esterase. In addition, the intestinal absorption was examined with Caco-2 cells, and no advantageous change in absorption efficiency was observed by chemically modifying the fucoxanthin unless different micelles sizes and increasing hydrophobicity are induced.

  10. Synthesis, physico-chemical characterization and biological activity of copper(ii and nickel(ii complexes with l-benzoyl-2-methylbenzimidazole derivatives

    Directory of Open Access Journals (Sweden)

    Podunavac-Kuzmanović Sanja O.

    2002-01-01

    Full Text Available Chlorides of copper(II and nickel(ll react with 1-benzoyl-2-methylbenzimidazole or 1-(4-chlorobenzoyl-2-methylbenzimidazole to give complexes of the type [M(LnCln(H20∙Cln (M = Cu or Ni; L = (1-benzoyl-2-methylbenzimidazole or 1-(4-chlorobenzoyl-2-methylbenzimidazole; n=O, 1 or 2. The complexes were synthesized and characterized by elemental analysis, molar conductivity magnetic susceptibility measurements and IR spectra. These studies suggest that all the complexes possess an octahedral stereochemistry. The antibacterial activity of (1-benzoyl-2-methylbenzimidazole or 1-(4-chlorobenzoyl-2-methylbenzimidazole and their complexes was evaluated against Escherichia coli and Bacillus sp.

  11. Synthesis, characterization, quantum chemical calculations and evaluation of antioxidant properties of 1,3,4-thiadiazole derivatives including 2- and 3-methoxy cinnamic acids

    Science.gov (United States)

    Gür, Mahmut; Muğlu, Halit; Çavuş, M. Serdar; Güder, Aytaç; Sayıner, Hakan S.; Kandemirli, Fatma

    2017-04-01

    A series of 1,3,4-thiadiazole derivatives including 2- and 3-methoxy cinnamic acids were synthesized, and their structures were elucidated by the UV, IR, 1H NMR, 13C NMR spectroscopies and elemental analysis. The UV and IR calculations of the molecules were performed by using B3LYP, HF and MP2 methods with selected 6-311++G(2d,2p), 6-311++G(3df,3pd) and cc-pvtz basis sets. Dipole moment, polarizability, chemical hardness/softness and electronegativity were also calculated and analyzed. Experimental FT-IR spectra and UV-Vis spectrum of the compounds were compared with theoretical data. Furthermore, antioxidant activities of the compounds were practised via different test methods such as 2,2-diphenyl-1-picryl-hydrazyl (DPPHrad), N,N-dimethyl-p-phenylenediamine (DMPDrad +), and 2,2‧-azino-bis(3-ethylbenzthiazoline-6-sulfonic acid) (ABTSrad +) scavenging activity assays. When compared with standards (BHA-Butylated hydroxyanisole, RUT-Rutin, and TRO-Trolox), it was observed that especially XIII and XIV which include methoxy groups at the o- and m-positions, respectively, had effective activities.

  12. Soft chemical synthesis of silicon nanosheets and their applications

    Science.gov (United States)

    Nakano, Hideyuki; Ikuno, Takashi

    2016-12-01

    Two-dimensional silicon nanomaterials are expected to show different properties from those of bulk silicon materials by virtue of surface functionalization and quantum size effects. Since facile fabrication processes of large area silicon nanosheets (SiNSs) are required for practical applications, a development of soft chemical synthesis route without using conventional vacuum processes is a challenging issue. We have recently succeeded to prepare SiNSs with sub-nanometer thicknesses by exfoliating layered silicon compounds, and they are found to be composed of crystalline single-atom-thick silicon layers. In this review, we present the synthesis and modification methods of SiNSs. These SiNSs have atomically flat and smooth surfaces due to dense coverage of organic moieties, and they are easily self-assembled in a concentrated state to form a regularly stacked structure. We have also characterized the electron transport properties and the electronic structures of SiNSs. Finally, the potential applications of these SiNSs and organic modified SiNSs are also reviewed.

  13. Synthesis and Characterization of High c-axis ZnO Thin Film by Plasma Enhanced Chemical Vapor Deposition System and its UV Photodetector Application.

    Science.gov (United States)

    Chao, Chung-Hua; Wei, Da-Hua

    2015-10-03

    In this study, zinc oxide (ZnO) thin films with high c-axis (0002) preferential orientation have been successfully and effectively synthesized onto silicon (Si) substrates via different synthesized temperatures by using plasma enhanced chemical vapor deposition (PECVD) system. The effects of different synthesized temperatures on the crystal structure, surface morphologies and optical properties have been investigated. The X-ray diffraction (XRD) patterns indicated that the intensity of (0002) diffraction peak became stronger with increasing synthesized temperature until 400 (o)C. The diffraction intensity of (0002) peak gradually became weaker accompanying with appearance of (10-10) diffraction peak as the synthesized temperature up to excess of 400 (o)C. The RT photoluminescence (PL) spectra exhibited a strong near-band-edge (NBE) emission observed at around 375 nm and a negligible deep-level (DL) emission located at around 575 nm under high c-axis ZnO thin films. Field emission scanning electron microscopy (FE-SEM) images revealed the homogeneous surface and with small grain size distribution. The ZnO thin films have also been synthesized onto glass substrates under the same parameters for measuring the transmittance. For the purpose of ultraviolet (UV) photodetector application, the interdigitated platinum (Pt) thin film (thickness ~100 nm) fabricated via conventional optical lithography process and radio frequency (RF) magnetron sputtering. In order to reach Ohmic contact, the device was annealed in argon circumstances at 450 (o)C by rapid thermal annealing (RTA) system for 10 min. After the systematic measurements, the current-voltage (I-V) curve of photo and dark current and time-dependent photocurrent response results exhibited a good responsivity and reliability, indicating that the high c-axis ZnO thin film is a suitable sensing layer for UV photodetector application.

  14. Synthesis and Characterization of Chemically Cross-Linked Acrylic Acid/Gelatin Hydrogels: Effect of pH and Composition on Swelling and Drug Release

    Directory of Open Access Journals (Sweden)

    Syed Majid Hanif Bukhari

    2015-01-01

    Full Text Available This present work was aimed at synthesizing pH-sensitive cross-linked AA/Gelatin hydrogels by free radical polymerization. Ammonium persulfate and ethylene glycol dimethacrylate (EGDMA were used as initiator and as cross-linking agent, respectively. Different feed ratios of acrylic acid, gelatin, and EGDMA were used to investigate the effect of monomer, polymer, and degree of cross-linking on swelling and release pattern of the model drug. The swelling behavior of the hydrogel samples was studied in 0.05 M USP phosphate buffer solutions of various pH values pH 1.2, pH 5.5, pH 6.5, and pH 7.5. The prepared samples were evaluated for porosity and sol-gel fraction analysis. Pheniramine maleate used for allergy treatment was loaded as model drug in selected samples. The release study of the drug was investigated in 0.05 M USP phosphate buffer of varying pH values (1.2, 5.5, and 7.5 for 12 hrs. The release data was fitted to various kinetic models to study the release mechanism. Hydrogels were characterized by Fourier transformed infrared (FTIR spectroscopy which confirmed formation of structure. Surface morphology of unloaded and loaded samples was studied by surface electron microscopy (SEM, which confirmed the distribution of model drug in the gel network.

  15. Synthesis and physico-chemical characterization of zinc(II, nickel(II and cobalt(II complexes with 2-phenyl-2-imidazoline

    Directory of Open Access Journals (Sweden)

    Podunavac-Kuzmanović Sanja O.

    2003-01-01

    Full Text Available Chlorides and nitrates of zinc(II, nickel(II and cobalt(II react with 2-phenyl-2-imidazoline to give complexes of the type [ML2X2]·nH2O (M=Zn, Ni or Co; L=2-phenyl-2-imidazoline; X=Cl or NO3; n=0, 1 or 2. The complexes were synthesized and characterized by elemental analysis of the metal molar conductivity, magnetic susceptibility measurements and IR spectra. The molar conductances of the zinc(II complexes in DMF solutions indicate that the complexes behave as non-electrolytes. The values of magnetic conductivity in the case of nickel(II complexes indicate that one of the coordinated anions (chloride or nitrate has been replaced by DMF molecule. The molar conductivity values of cobalt(II complexes indicate the partial substitution of coordinated anions with solvent molecules. The room temperature effective magnetic moments and IR data of the complexes suggest that all Zn(II, Ni(II and Co(II complexes have a tetrahedral configuration, which is realized by participation of the pyridine nitrogen of two organic ligand molecules, and two chloride or nitrate anions typical for these classes of organic ligands.

  16. Synthesis, characterization and chemical stability of silicon dichalcogenides, Si(SexS1₋x)2

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Chen; Zhang, Xiaotian; Krishna, Lakshmi; Kendrick, Chito; Shang, Shun-Li; Toberer, Eric; Liu, Zi-Kui; Tamboli, Adele; Redwing, Joan M.

    2016-10-01

    Silicon dichalcogenides have an intriguing crystal structure consisting of long tetrahedral chains held together by van der Waals forces but the electronic and optical properties have been less explored. In the present work, bulk SiSe2, SiS2, and Si(SexS1-x)2 were synthesized by the congruent melt growth method and characterized by Raman spectroscopy, X-ray Diffraction and UV/visible/IR transmission measurements supported by first-principles calculations. First-principles calculations reveal a nearly linear decrease of band gap energy in Si(SexS1-x)2 with increasing Se content, i.e., from SiS2 to SiSe2 which corresponds with a blue-shift in the transmission spectra from bulk SiSe2 to Si(Se0.6S0.4)2, and to SiS2. Air stability tests demonstrate the formation of toxic H2Se/H2S gas from sample oxidation at room temperature upon exposure to ambient air, and great care should be paid when handling these materials.

  17. Synthesis and characterization of a new material based on porous silica-Chemically immobilized C,N-pyridylpyrazole for heavy metals adsorption

    Energy Technology Data Exchange (ETDEWEB)

    Radi, Smaail [Laboratoire de Chimie Organique, Macromoleculaire et Produits Naturels, Departement de Chimie, Faculte des Sciences, Universite Mohamed 1er, BP 524, 60 000 Oujda (Morocco)], E-mail: radi_smaail@yahoo.fr; Attayibat, Ahmed [Laboratoire de Chimie Organique, Macromoleculaire et Produits Naturels, Departement de Chimie, Faculte des Sciences, Universite Mohamed 1er, BP 524, 60 000 Oujda (Morocco); Lekchiri, Yahya [Laboratoire de Biochimie, Departement de Biologie, Faculte des Sciences, Universite Mohamed 1er, BP 524, 60 000 Oujda (Morocco); Ramdani, Abdelkrim [Laboratoire de Chimie Organique, Macromoleculaire et Produits Naturels, Departement de Chimie, Faculte des Sciences, Universite Mohamed 1er, BP 524, 60 000 Oujda (Morocco); Bacquet, Maryse [Laboratoire de Chimie Macromoleculaire, Universite des Sciences et Technologies de Lille, 59655 Villeneuve d' Ascq (France)

    2008-10-15

    The immobilization of C,N-pyridylpyrazole on the surface of epoxy group containing silica gel phase for the formation of a newly synthesized material based on porous silica-bound C,N-pyridylpyrazole (SGPP) is described. The surface modification was characterized by {sup 13}C NMR of solid sample, elemental analysis and infrared spectra and was studied and evaluated by determination of the surface area using the BET equation, the adsorption and desorption capability using the isotherm of nitrogen and BJH pore sizes, respectively. The new material exhibits good thermal stability determined by thermogravimetry curves. The synthesized material was utilised in column and batch methods for separation and trace extraction of (Hg{sup 2+}, Cd{sup 2+}, Pb{sup 2+}, Cu{sup 2+}, Zn{sup 2+}, K{sup +}, Na{sup +} and Li{sup +}) and compared to results of classical liquid-liquid extraction with the unbound C,N-pyridylpyrazole compound. The grafting at the surface of silica does not affect complexing properties of the ligand and the material exhibits a high selectivity toward Hg(II)

  18. Osmium(III) analogues of KP1019: electrochemical and chemical synthesis, spectroscopic characterization, X-ray crystallography, hydrolytic stability, and antiproliferative activity.

    Science.gov (United States)

    Kuhn, Paul-Steffen; Büchel, Gabriel E; Jovanović, Katarina K; Filipović, Lana; Radulović, Siniša; Rapta, Peter; Arion, Vladimir B

    2014-10-20

    A one-electron reduction of osmium(IV) complexes trans-[Os(IV)Cl4(Hazole)2], where Hazole = 1H-pyrazole ([1](0)), 2H-indazole ([2](0)), 1H-imidazole ([3](0)), and 1H-benzimidazole ([4](0)), afforded a series of eight new complexes as osmium analogues of KP1019, a lead anticancer drug in clinical trials, with the general formula (cation)[trans-Os(III)Cl4(Hazole)2], where cation = H2pz(+) (H2pz[1]), H2ind(+) (H2ind[2]), H2im(+) (H2im[3]), Ph4P(+) (Ph4P[3]), nBu4N(+) (nBu4N[3]), H2bzim(+) (H2bzim[4]), Ph4P(+) (Ph4P[4]), and nBu4N(+) (nBu4N[4]). All complexes were characterized by elemental analysis, (1)H NMR spectroscopy, electrospray ionization mass spectrometry, UV-vis spectroscopy, cyclic voltammetry, while H2pz[1], H2ind[2], and nBu4[3], in addition, by X-ray diffraction. The reduced species [1](-) and [4](-) are stable in aqueous media in the absence of air oxygen and do not react with small biomolecules such as amino acids and the nucleotide 5'-dGMP. Cell culture experiments in five different human cancer cell lines (HeLa, A549, FemX, MDA-MB-453, and LS-174) and one noncancerous cell line (MRC-5) were performed, and the results were discussed and compared to those for KP1019 and cisplatin. Benzannulation in complexes with similar structure enhances antitumor activity by several orders of magnitude, implicating different mechanisms of action of the tested compounds. In particular, complexes H2ind[2] and H2bzim[4] exhibited significant antiproliferative activity in vitro when compared to H2pz[1] and H2im[3].

  19. Flow Chemistry for Designing Sustainable Chemical Synthesis (journal article)

    Science.gov (United States)

    An efficiently designed continuous flow chemical process can lead to significant advantages in developing a sustainable chemical synthesis or process. These advantages are the direct result of being able to impart a higher degree of control on several key reactor and reaction par...

  20. Synthesis and characterization of Bi-Te-Se thermoelectric materials

    Energy Technology Data Exchange (ETDEWEB)

    Tripathi, S. K., E-mail: surya.pu@ac.in [Department of Physics, Panjab University, Chandigarh, 160014 (India); Centre for Nanoscience & Nanotechnology, Panjab University, Chandigarh, 160014 (India); Kumari, Ankita [Centre for Nanoscience & Nanotechnology, Panjab University, Chandigarh, 160014 (India); Ridhi, R.; Kaur, Jagdish [Department of Physics, Panjab University, Chandigarh, 160014 (India)

    2015-08-28

    Bismuth Telluride (Bi{sub 2}Te{sub 3}) and its related alloys act as a promising thermoelectric material and preferred over other thermoelectric materials due to their high stability and efficiency under ambient conditions. In the present work, we have reported economical, environment friendly and low-temperature aqueous chemical method for the synthesis of Bi-Se-Te alloy. The prepared samples are characterized by X-Ray Diffraction to investigate the structural properties and UV-Visible spectroscopy for the spectroscopic analysis. The absorption spectrum reveals the sensitivity in the ultraviolet as well as in visible region.

  1. Synthesis, characterization and applications of graphene architectures

    Science.gov (United States)

    Thomas, Abhay Varghese

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

  2. Electrolytic Synthesis and Characterizations of Silver Nanopowder

    CERN Document Server

    Theivasanthi, T

    2011-01-01

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

  3. Synthesis and Characterization of Functionalized Metal-organic Frameworks

    Science.gov (United States)

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

    2014-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1997-06-24

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

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

    CERN Document Server

    bin M Yusoff, Abdul Rashid

    2014-01-01

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

  6. Analysis, synthesis and design of chemical processes

    Energy Technology Data Exchange (ETDEWEB)

    Turton, R. [West Virginia Univ., Morgantown, WV (United States); Bailie, R.C.; Whiting, W.B.

    1998-12-31

    The book illustrates key concepts through a running example from the real world: the manufacture of benzene; covers design, economic considerations, troubleshooting and health/environmental safety; and includes exclusive software for estimating chemical manufacturing equipment capital costs. This book will help chemical engineers optimize the efficiency of production processes, by providing both a philosophical framework and detailed information about chemical process design. Design is the focal point of the chemical engineering practice. This book helps engineers and senior-level students hone their design skills through process design rather than simply plant design. It introduces all the basics of process simulation. Learn how to size equipment, optimize flowsheets, evaluate the economics of projects, and plan the operation of processes. Learn how to use Process Flow Diagrams; choose the operating conditions for a process; and evaluate the performance of existing processes and equipment. Finally, understand how chemical process design impacts health, safety, the environment and the community.

  7. Characterizing Molecular Interactions in Chemical Systems.

    Science.gov (United States)

    Günther, David; Boto, Roberto A; Contreras-Garcia, Juila; Piquemal, Jean-Philip; Tierny, Julien

    2014-12-01

    Interactions between atoms have a major influence on the chemical properties of molecular systems. While covalent interactions impose the structural integrity of molecules, noncovalent interactions govern more subtle phenomena such as protein folding, bonding or self assembly. The understanding of these types of interactions is necessary for the interpretation of many biological processes and chemical design tasks. While traditionally the electron density is analyzed to interpret the quantum chemistry of a molecular system, noncovalent interactions are characterized by low electron densities and only slight variations of them--challenging their extraction and characterization. Recently, the signed electron density and the reduced gradient, two scalar fields derived from the electron density, have drawn much attention in quantum chemistry since they enable a qualitative visualization of these interactions even in complex molecular systems and experimental measurements. In this work, we present the first combinatorial algorithm for the automated extraction and characterization of covalent and noncovalent interactions in molecular systems. The proposed algorithm is based on a joint topological analysis of the signed electron density and the reduced gradient. Combining the connectivity information of the critical points of these two scalar fields enables to visualize, enumerate, classify and investigate molecular interactions in a robust manner. Experiments on a variety of molecular systems, from simple dimers to proteins or DNA, demonstrate the ability of our technique to robustly extract these interactions and to reveal their structural relations to the atoms and bonds forming the molecules. For simple systems, our analysis corroborates the observations made by the chemists while it provides new visual and quantitative insights on chemical interactions for larger molecular systems.

  8. 40 CFR 792.135 - Physical and chemical characterization studies.

    Science.gov (United States)

    2010-07-01

    ... 40 Protection of Environment 31 2010-07-01 2010-07-01 true Physical and chemical characterization... A Study § 792.135 Physical and chemical characterization studies. (a) All provisions of the GLPs shall apply to physical and chemical characterization studies designed to determine...

  9. Diversity-Oriented Synthesis as a Tool for Chemical Genetics

    Directory of Open Access Journals (Sweden)

    Elena Lenci

    2014-10-01

    Full Text Available Chemical genetics is an approach for identifying small molecules with the ability to induce a biological phenotype or to interact with a particular gene product, and it is an emerging tool for lead generation in drug discovery. Accordingly, there is a need for efficient and versatile synthetic processes capable of generating complex and diverse molecular libraries, and Diversity-Oriented Synthesis (DOS of small molecules is the concept of choice to give access to new chemotypes with high chemical diversity. In this review, the combination of chemical genetics and diversity-oriented synthesis to identify new chemotypes as hit compounds in chemical biology and drug discovery is reported, giving an overview of basic concepts and selected case studies.

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

    KAUST Repository

    Abulikemu, Mutalifu

    2014-11-05

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

  11. Synthesis and Characterization of Two Danazol Derivatives

    Directory of Open Access Journals (Sweden)

    Lauro Figueroa-Valverde

    2010-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2006-01-01

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

  13. His6 tag-assisted chemical protein synthesis

    Science.gov (United States)

    Bang, Duhee; Kent, Stephen B. H.

    2005-04-01

    To make more practical the total chemical synthesis of proteins by the ligation of unprotected peptide building blocks, we have developed a method to facilitate the isolation and handling of intermediate products. The synthetic technique makes use of a His6 tag at the C terminus of the target polypeptide chain, introduced during the synthesis of the C-terminal peptide segment building block. The presence of a His6 tag enables the isolation of peptide or protein products directly from ligation reaction mixtures by Ni-NTA affinity column purification. This simple approach enables facile buffer exchange to alternate reaction conditions and is compatible with direct analytical control by protein MS of the multiple ligation steps involved in protein synthesis. We used syntheses of crambin and a modular tetratricopeptide repeat protein of 17 kDa as models to examine the utility of this affinity purification approach. The results show that His6 tag-assisted chemical protein synthesis is a useful method that substantially reduces handling losses and provides for rapid chemical protein syntheses. affinity purification | native chemical ligation

  14. On the Plasma-Chemical Synthesis of Nanopowders

    Institute of Scientific and Technical Information of China (English)

    G. Vissokov; Iv. Grancharov; Tsv. Tsvetanov

    2003-01-01

    This paper presents an overview of nanopowders preparation using low-temperature plasma (LTP). LTP with its unique processing capabilities provides an attractive and chemically unspecific route for powder synthesis. Nanopowders such as oxides, nitrides, carbides, catalysts and other nanopowders have been successfully synthesized in LTP reactors based on high intensity arcs, plasma jets and radio-frequency (r. f.) inductively coupled discharges.

  15. Plant biopolyester cutin: a tough way to its chemical synthesis.

    Science.gov (United States)

    Benítez, José J; García-Segura, Rafael; Heredia, Antonio

    2004-09-06

    The chemical synthesis of an aliphatic biopolyester identical to the natural cutin which constitutes the major component of the cuticle of fruits and leaves of higher plants is for the first time achieved and reported. Potential applications of this new material is of great interest because its physical properties, non-toxicity, biodegradability, and availability of raw material.

  16. Recent advances in the chemical synthesis of RNA.

    Science.gov (United States)

    Beaucage, Serge L; Reese, Colin B

    2009-09-01

    As a consequence largely of recent developments in RNA interference (RNAi) research, the availability of rapid and efficient methods for the chemical synthesis of RNA sequences has become a matter of considerable urgency. This unit is concerned mainly with work that has been carried out, especially in the past decade, on the design of new and improved methods of RNA synthesis. The main criteria for the choice of protecting groups for the 2'-hydroxy functions of the ribonucleoside building blocks, which is arguably the most crucial strategic decision to be made, are discussed. A number of new ether-, acetal-, orthoester-, and ester-based 2'-protecting groups are described and their application, mainly in phosphoramidite-based solid-phase synthesis, is discussed in some detail. Brief consideration is also given to solution-phase RNA synthesis, which may well prove to be of great importance if a systemic drug is developed and multikilogram quantities of synthetic RNA sequences are required.

  17. Ultrasonic microspectroscopy characterization of chemically tempered glass

    Science.gov (United States)

    Arakawa, Mototaka; Kushibiki, Jun-ichi; Ohashi, Yuji

    2017-01-01

    We evaluated the elastic properties of the compressive stress (CS) layer of chemically tempered glass by ultrasonic microspectroscopy (UMS) in a very high frequency (VHF) range. Two commercial aluminosilicate glass specimens were prepared, and one of them was chemically tempered. Changes in elastic properties in the CS layer with the residual stress introduced by the exchange of Na+ ions for larger K+ ions were estimated by precisely measuring the densities and longitudinal and shear velocities for both the tempered and nontempered specimens. Using a single-layer model for the surface layer, we observed drastic increases in bulk-wave velocities and significant decreases in attenuation coefficients. We determined that the average elastic properties, namely, the elastic constants c 11 and c 44, and the density of the surface layer, were 9.6 and 7.1, and 1.2% larger than those of the nontempered specimen, respectively. We also estimated the distributions of the elastic properties according to the complementary error function (CEF) for the distribution of K+ ion concentration. Furthermore, using a line-focus-beam (LFB) system, we measured the frequency characteristics of the velocity (V LSAW) of leaky surface acoustic waves (LSAWs) on a water-loaded surface of the tempered specimen and clarified that the distributions of the elastic properties did not follow the CEF. The LFB system can be used for analyzing/determining details of the surface properties and is a promising tool for evaluating and characterizing chemically tempered glass and tempering process conditions.

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

    Science.gov (United States)

    Hughes, William L.

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

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

    Science.gov (United States)

    2014-01-09

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

  20. Nanostructured Mg-Al hydrotalcite as catalyst for fine chemical synthesis.

    Science.gov (United States)

    Basahel, Sulaiman N; Al-Thabaiti, Shaeel A; Narasimharao, Katabathini; Ahmed, Nesreen S; Mokhtar, Mohamed

    2014-02-01

    This paper reviews the recent research of nanostructured Mg-Al hydrotalcite (Mg-Al HT) and its application as an efficient solid base catalyst for the synthesis of fine chemicals. Mg-Al HT has many beneficial features, such as low cost, selectivity, catalytic properties, and wide range of preparation and modification methods. They hold promise for providing sought-after, environmentally friendly technologies for the 21st century. Replacement of currently used homogeneous alkaline bases for the synthesis of fine chemicals by a solid catalyst can result in catalyst re-use and waste stream reduction. We introduce briefly the structure, properties and characterization of the nanostructured Mg-Al HT. The efficacy and benign applications of Mg-Al HT as an alternative solid base to homogenous catalysts in the synthesis of fine chemicals are then reviewed. The challenges for the future applications of Mg-Al HT in the synthesis of fine chemicals in terms of green protocol processes are discussed.

  1. Synthesis, characterization and application of electrode materials

    Energy Technology Data Exchange (ETDEWEB)

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

    1995-07-07

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

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

    Directory of Open Access Journals (Sweden)

    Usman MS

    2013-11-01

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

  3. Microwave Technology--Applications in Chemical Synthesis

    Science.gov (United States)

    Microwave heating, being specific and instantaneous, is unique and has found a place for expeditious chemical syntheses. Specifically, the solvent-free reactions are convenient to perform and have advantages over the conventional heating protocols as summarized in the previous se...

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

    Science.gov (United States)

    Iyer, Aparna

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

  5. Green synthesis and characterization of graphene nanosheets

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-03-15

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

  6. Synthesis and characterization of some N-substituted amides of salicylic acid

    OpenAIRE

    Lupea Xenia Alfa; Padure Mirabela

    2003-01-01

    The synthesis of some N-substituted aromatic amides in the salicylic acid series was achieved, by direct reaction between primary amines and salicylic acid in inert organic solvent, in the presence of PCl3. The compounds that were obtained, partially not described in literature, were characterized by chemical-physical methods.

  7. Synthesis and characterization of some N-substituted amides of salicylic acid

    Directory of Open Access Journals (Sweden)

    Lupea Xenia Alfa

    2003-01-01

    Full Text Available The synthesis of some N-substituted aromatic amides in the salicylic acid series was achieved, by direct reaction between primary amines and salicylic acid in inert organic solvent, in the presence of PCl3. The compounds that were obtained, partially not described in literature, were characterized by chemical-physical methods.

  8. Zeolite from fly ash: synthesis and characterization

    Indian Academy of Sciences (India)

    Keka Ojha; Narayan C Pradhan; Amar Nath Samanta

    2004-12-01

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

  9. Metabolic design for cyanobacterial chemical synthesis.

    Science.gov (United States)

    Oliver, John W K; Atsumi, Shota

    2014-06-01

    Photosynthetic chemical production in cyanobacteria is a promising technology for renewable energy, CO2 mitigation, and fossil fuel replacement. Metabolic engineering has enabled a direct biosynthetic process from CO2 fixation to chemical feedstocks and biofuels, without requiring costly production, storage, and breakdown of cellulose or sugars. However, direct production technology is challenged by a need to achieve high-carbon partitioning to products in order to be competitive. This review discusses principles for the design of biosynthetic pathways in cyanobacteria and describes recent advances in relevant genetic tools. This field is at a critical juncture in assessing the strength and feasibility of carbon partitioning. To address this, we have included the stoichiometry of reducing equivalents and carbon conservation for heterologous pathways, and a method for calculating product yields against a theoretical maximum.

  10. Chemical synthesis and biochemical reactivity of bacteriophage lambda PR promoter.

    OpenAIRE

    1983-01-01

    By a combination of chemical and enzymatic methods, a 75 base pair DNA duplex containing the sequence of the lambda PR promoter including the OR1 and OR2 cI repressor binding sites was synthesized. The solid support phosphite triester procedure (Caruthers, M. H. et al., Cold Spring Harbor Symposia on Quantitative Biology XLVII, in press) was used for the synthesis of oligonucleotides comprising the sequence. We report here an adaptation of the method of DNA synthesis in test tubes. Assembly o...

  11. 40 CFR 160.135 - Physical and chemical characterization studies.

    Science.gov (United States)

    2010-07-01

    ... 40 Protection of Environment 23 2010-07-01 2010-07-01 false Physical and chemical characterization... and chemical characterization studies. (a) All provisions of the GLP standards shall apply to physical... physical and chemical characteristics of a test, control, or reference substance: § 160.31 (c), (d), and...

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-12-15

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

  13. Synthesis of magnetic tunnel junctions with full in situ atomic layer and chemical vapor deposition processes

    Energy Technology Data Exchange (ETDEWEB)

    Mantovan, R., E-mail: roberto.mantovan@mdm.imm.cnr.it [Laboratorio MDM, IMM-CNR, Via C. Olivetti 2, 20864 Agrate Brianza (Italy); Vangelista, S.; Kutrzeba-Kotowska, B.; Cocco, S.; Lamperti, A.; Tallarida, G. [Laboratorio MDM, IMM-CNR, Via C. Olivetti 2, 20864 Agrate Brianza (MB) (Italy); Mameli, D. [Laboratorio MDM, IMM-CNR, Via C. Olivetti 2, 20864 Agrate Brianza (Italy); Dipartimento di Scienze Chimiche, Universita di Cagliari, Cittadella Universitaria, 09042 Monserrato, Cagliari (Italy); Fanciulli, M. [Laboratorio MDM, IMM-CNR, Via C. Olivetti 2, 20864 Agrate Brianza (Italy); Dipartimento di Scienza dei Materiali, Universita degli studi Milano-Bicocca, Via R Cozzi 53, 20125 Milano (Italy)

    2012-05-01

    Magnetic tunnel junctions, i.e. the combination of two ferromagnetic electrodes separated by an ultrathin tunnel oxide barrier, are core elements in a large variety of spin-based devices. We report on the use of combined chemical vapor and atomic layer deposition processes for the synthesis of magnetic tunnel junctions with no vacuum break. Structural, chemical and morphological characterizations of selected ferromagnetic and oxide layers are reported, together with the evidence of tunnel magnetoresistance effect in patterned Fe/MgO/Co junctions.

  14. Chemical synthesis of Cd-free wide band gap materials for solar cells

    Energy Technology Data Exchange (ETDEWEB)

    Sankapal, B.R.; Sartale, S.D.; Ennaoui, A. [Hahn-Meitner-Institut, Berlin (Germany). Department of Solar Energy Research; Lokhande, C.D. [Shivaji University, Kolhapur (India). Department of Physics

    2004-07-01

    Chemical methods are nowadays very attractive, since they are relatively simple, low cost and convenient for larger area deposition of thin films. In this paper, we outline our work related to the synthesis and characterization of some wide band gap semiconducting material thin films prepared by using solution methods, namely, chemical bath deposition and successive ionic layer adsorption and reaction (SILAR). The optimum preparative parameters are given and respective structural, surface morphological, compositional, optical, and electrical properties are described. Some materials we used in solar cells as buffer layers and achieved remarkable results, which are summarized. (author)

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

    Science.gov (United States)

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

    2013-10-01

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

  16. Alternative fuels and chemicals from synthesis gas

    Energy Technology Data Exchange (ETDEWEB)

    Unknown

    1998-12-01

    A DOE/PETC funded study was conducted to examine the use of a liquid phase mixed alcohol synthesis (LPMAS) plant to produce gasoline blending ethers. The LPMAS plant was integrated into three utilization scenarios: a coal fed IGCC power plant, a petroleum refinery using coke as a gasification feedstock, and a standalone natural gas fed partial oxidation plant. The objective of the study was to establish targets for the development of catalysts for the LPMAS reaction. In the IGCC scenario, syngas conversions need only be moderate because unconverted syngas is utilized by the combined cycle system. A once through LPMAS plant achieving syngas conversions in the range of 38--49% was found to be suitable. At a gas hourly space velocity of 5,000 sL/Kg-hr and a methanol:isobutanol selectivity ratio of 1.03, the target catalyst productivity ranges from 370 to 460 g iBuOH/Kg-hr. In the petroleum refinery scenario, high conversions ({approximately}95%) are required to avoid overloading the refinery fuel system with low Btu content unconverted syngas. To achieve these high conversions with the low H{sub 2}/CO ratio syngas, a recycle system was required (because of the limit imposed by methanol equilibrium), steam was injected into the LPMAS reactor, and CO{sub 2} was removed from the recycle loop. At the most economical recycle ratio, the target catalyst productivity is 265 g iBuOH/Kg-hr. In the standalone LPMAS scenario, essentially complete conversions are required to achieve a fuel balanced plant. At the most economical recycle ratio, the target catalyst productivity is 285 g iBuOH/Kg-hr. The economics of this scenario are highly dependent on the cost of the natural gas feedstock and the location of the plant. For all three case scenarios, the economics of a LPMAS plant is marginal at current ether market prices. Large improvements over demonstrated catalyst productivity and alcohol selectivity are required.

  17. Meteorites - A petrologic-chemical synthesis

    Science.gov (United States)

    Dodd, Robert T.

    In this book, an attempt has been made to summarize current knowledge and understanding about meteorites in a manner comprehensible to both professional scientists and university students. Attention is given to the flux of meteoritic material, major meteorite types, sources of meteorites, the recovery of meteorites, meteorite nomenclature, and literature. The chemistry and classification of the chondrites is considered along with details regarding carbonaceous chondrites, ordinary chondrites, the enstatite chondrite-achondrite association, and questions regarding time and process in the evolution of chondrites. The eucrite association is discussed, taking into account eucrites, diogenites, howardites, mesosiderites, the radiometric ages of eucrites and their associates, and the chemical evolution of the eucrite association. Differentiated meteorites are considered along with source objects, and parent bodies.

  18. Synthesis, Characterization and Testing of Novel Anode and Cathode Materials for Li-Ion Batteries

    Energy Technology Data Exchange (ETDEWEB)

    White, Ralph E.; Popov, Branko N.

    2002-10-31

    During this program we have synthesized and characterized several novel cathode and anode materials for application in Li-ion batteries. Novel synthesis routes like chemical doping, electroless deposition and sol-gel method have been used and techniques like impedance, cyclic voltammetry and charge-discharge cycling have been used to characterize these materials. Mathematical models have also been developed to fit the experimental result, thus helping in understanding the mechanisms of these materials.

  19. N-TiO: Chemical Synthesis and Photocatalysis

    Directory of Open Access Journals (Sweden)

    Matias Factorovich

    2011-01-01

    Full Text Available The chemical synthesis of nitrogen-doped titanium dioxide (N-TiO2 is explored in an attempt to understand the mechanisms of doping. Urea is used as precursor in a sol gel synthesis of N-TiO2. Chemical and structural changes during thermal treatment of the precursors were followed by several techniques. The effect of doping on band gap, morphology, and microstructure was also determined. The byproducts produced during firing correspond to those obtained during urea thermal decomposition. Polynitrogenated colored compounds produced at temperatures below 400°C may act as sensitizer. Incorporation of N in the TiO2 structure is possible at higher temperatures. Degradation experiments of salicylic acid under UVA and visible light (>400 nm in the presence of TiO2 or N-TiO2 indicate that doping decreases the activity under UVA light, while stable byproducts are produced under visible light.

  20. Architectural self-construction in nature and chemical synthesis.

    Science.gov (United States)

    Sorensen, Erik J

    2003-07-31

    The chemistry of squalene oxide (1) exemplifies that architectural complexity can be encoded in the structures of relatively simple, polyunsaturated molecules. When the concept of architectural self-construction is an integral part of the design of a chemical synthesis, powerful strategies can be uncovered. this article addresses studies which showed that polyunsaturated, 19-membered ring carbocycle contains all of the molecular information that is required to give the stereochemically complex polycyclic architecture of the cytotoxic natural product FR182877.

  1. Synthesis and characterization of novel adsorbent fibers

    Science.gov (United States)

    Benak, Kelly Rene

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

  2. The impact of the chemical synthesis on the magnetic properties of intermetallic PdFe nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Castellanos-Rubio, I.; Insausti, M.; Muro, I. Gil de [Universidad del País Vasco, UPV/EHU, Dpto. de Química Inorgánica (Spain); Arias-Duque, D. Carolina; Hernández-Garrido, Juan Carlos [Universidad de Cadiz, Departamento de Ciencia de los Materiales e Ingeniería Metalúrgica y Química Inorgánica, Facultad de Ciencias (Spain); Rojo, T.; Lezama, L., E-mail: luis.lezama@ehu.es [Universidad del País Vasco, UPV/EHU, Dpto. de Química Inorgánica (Spain)

    2015-05-15

    Palladium-rich Iron nanoparticles in the 4–8 nm range have been produced by a combination of two methods: the thermal decomposition of organometallic precursors and the reduction of metallic salts by a polyol. Herein, it is shown how the details of the synthesis have a striking impact on the magnetic and morphological properties of the final products. In the synthesis of these bimetallic nanoparticles, the use of high reaction temperatures plays an essential role in attaining good chemical homogeneity, which has proved to have a key influence on the magnetic properties. Magnetic characterization has been performed by electron magnetic resonance and magnetization measurements, which have confirmed the superparamagnetic-like behavior at room temperature. No clear traces of magnetic polarization in palladium atoms have been detected. The combination of long-term stability and homogeneous chemical and magnetic properties makes these particles very suitable for a wide range of applications in nanotechnology.

  3. Nanotwinned gold nanowires obtained by chemical synthesis.

    Science.gov (United States)

    Bernardi, Marco; Raja, Shilpa N; Lim, Sung Keun

    2010-07-16

    We demonstrate a facile method for synthesizing and isolating Au nanowires with a high density of twin boundary defects normal to the growth axis. In this process, oleylamine conveniently plays the role of the solvent, the reducing agent and the ligand. The geometry of the twin boundaries in the nanowires is in sharp contrast with the pentagonal twinning commonly observed in metal nanowires, and is of particular interest for its ultrahigh tensile strength. The nanostructure geometry and twin-twin average spacing were characterized using high-resolution electron microscopy, and the tensile strength of the nanowires was estimated in solution using a Ti ultrasonication probe. We present a model for explaining the role of the bulky ligand oleylamine in the formation of the twin boundaries that could be extended to include elastic terms in the ligand shell. Our work demonstrates that the use of bulky, asymmetric ligands can induce extensive formation of twin boundary defects that in turn control the mechanical properties at the nanoscale.

  4. Microbial chemical factories: recent advances in pathway engineering for synthesis of value added chemicals.

    Science.gov (United States)

    Dhamankar, Himanshu; Prather, Kristala L J

    2011-08-01

    The dwindling nature of petroleum and other fossil reserves has provided impetus towards microbial synthesis of fuels and value added chemicals from biomass-derived sugars as a renewable resource. Microbes have naturally evolved enzymes and pathways that can convert biomass into hundreds of unique chemical structures, a property that can be effectively exploited for their engineering into Microbial Chemical Factories (MCFs). De novo pathway engineering facilitates expansion of the repertoire of microbially synthesized compounds beyond natural products. In this review, we visit some recent successes in such novel pathway engineering and optimization, with particular emphasis on the selection and engineering of pathway enzymes and balancing of their accessory cofactors.

  5. Synthesis and applications of 2-aminopyrimidine derivatives as key intermediates in chemical synthesis of biomolecules

    Energy Technology Data Exchange (ETDEWEB)

    Koroleva, Elena V; Gusak, K N; Ignatovich, Zh V [Institute of Chemistry of New Materials of the National Academy of Sciences of Belarus (Belarus)

    2010-10-19

    Published data on the main approaches to the formation of the heterocyclic 2-aminopyrimidine system, which is one of important pharmacophores responsible for the biological properties of its derivatives, are described systematically. Main chemical transformations of functionalized 2-aminopyrimidines and their application in the synthesis of modern pharmaceuticals are considered.

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

    Science.gov (United States)

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

    2012-12-01

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

  7. Synthesis and Characterization of Highly Intercalated Graphite Bisulfate

    Science.gov (United States)

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

    2017-03-01

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

  8. Synthesis, characterization and optical properties of nanoparticles

    Science.gov (United States)

    Li, Shoutian

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

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

    NARCIS (Netherlands)

    Hamdy M. Saad, M.S.

    2005-01-01

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

  10. Synthesis Technique and Characterizations of Silver Nanostructures

    Science.gov (United States)

    Rajawat, Shweta; Qureshi, M. S.

    2015-06-01

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

  11. Synthesis and characterization of novel nanothermometers

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-03-23

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

  12. Organic Ion Exchangers. Synthesis, Characterization and Applications

    Institute of Scientific and Technical Information of China (English)

    E. S. Dragan

    2005-01-01

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

  13. Chemical synthesis and modification of target phases of chalcogenide nanomaterials

    Science.gov (United States)

    Sines, Ian T.

    Inorganic nanoparticles have been at the forefront of materials research in recent years due to their utility in modern technological processes. Chalcogenide nanomaterials are of particular interest because of their wide range of desirable properties for semiconductors, magnetic devices, and energy industries. Primary factors that dictate the properties of the material are the elemental composition, crystal structure, stoichiometry, crystallite size, and particle morphology. One of the most common approaches to synthesize these materials is through solution mediated routes. This approach offers unique advantages in controlling the morphology and particle size that other methods lack. This dissertation describes our recent work on exploiting solution chemical routes to control the crystal structure and composition of chalcogenide nanomaterials. We will start by discussing solution chemistry routes to synthesize non-equilibrium phases of chaclogenide nanomaterials. By using low-temperature bottom-up techniques it is possible to trap kinetically stable phases that cannot be accessed using traditional high-temperature techniques. We used solution chemistry to synthesize and characterize, for the first time, wurtzite-type MnSe. Wurtzite-type MnSe is the end-member of the highly investigated ZnxMn1-xSe solid solution, a classic magnetic semiconductor system. We will then discuss PbO-type FeS, another non-equilibrium phase that is isostructural with the superconducting phase of FeSe. We synthesized phase-pure PbO-type FeS using a low-temperature solvothermal route. We will then discuss the post-synthetic modification of chalcogenides nanomaterials. By exploiting the solubility of Se and S in tri-n-octylphosphine we can selectively extract the chalcogen from preformed chalcogenide nanomaterials. This gives chemists a technique for purification and phase-targeting of particular chalcogenide phases. This method can be modified to facilitate anion exchange. When Te is

  14. SYNTHESIS OF PROTEINS BY NATIVE CHEMICAL LIGATION USING FMOC-BASED CHEMISTRY

    Energy Technology Data Exchange (ETDEWEB)

    Camarero, J A; Mitchell, A R

    2005-01-20

    C-terminal peptide {alpha}-thioesters are valuable intermediates in the synthesis/semisynthesis of proteins by native chemical ligation. They are prepared either by solid-phase peptide synthesis (SPPS) or biosynthetically by protein splicing techniques. The present paper reviews the different methods available for the chemical synthesis of peptide {alpha}-thioesters using Fmoc-based SPPS.

  15. Synthesis and Characterization of Bimodal Mesoporous Silica

    Institute of Scientific and Technical Information of China (English)

    ZHANG Xiaofang; GUO Cuili; WANG Xiaoli; WU Yuanyuan

    2012-01-01

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

  16. Synthesis and characterization of sodium alkoxides

    Indian Academy of Sciences (India)

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

    2006-04-01

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

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

    Indian Academy of Sciences (India)

    Babasaheeb P Bandgar; Pradip B Gujarathi

    2008-03-01

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

  18. Chemical synthesis of peptides within the insulin superfamily.

    Science.gov (United States)

    Liu, Fa; Zaykov, Alexander N; Levy, Jay J; DiMarchi, Richard D; Mayer, John P

    2016-05-01

    The synthesis of insulin has inspired fundamental advances in the art of peptide science while simultaneously revealing the structure-function relationship of this centrally important metabolic hormone. This review highlights milestones in the chemical synthesis of insulin that can be divided into two separate approaches: (i) disulfide bond formation driven by protein folding and (ii) chemical reactivity-directed sequential disulfide bond formation. Common to the two approaches are the persistent challenges presented by the hydrophobic nature of the individual A-chain and B-chain and the need for selective disulfide formation under mildly oxidative conditions. The extension and elaboration of these synthetic approaches have been ongoing within the broader insulin superfamily. These structurally similar peptides include the insulin-like growth factors and also the related peptides such as relaxin that signal through G-protein-coupled receptors. After a half-century of advances in insulin chemistry, we have reached a point where synthesis is no longer limiting structural and biological investigation within this family of peptide hormones. The future will increasingly focus on the refinement of structure to meet medicinal purposes that have long been pursued, such as the development of a glucose-sensitive insulin. Copyright © 2016 European Peptide Society and John Wiley & Sons, Ltd.

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

    Science.gov (United States)

    Kabbani, Ahmad; Kabbani, Mohamad; Safadi, Khadija

    2015-09-01

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

  20. Hydrothermal synthesis of pyrochlores and their characterization

    Science.gov (United States)

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

    2013-10-01

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

  1. Novel metallomesogenic polyurethanes: Synthesis, characterization and properties

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-12-01

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

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

    Science.gov (United States)

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

    2016-05-01

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

  3. Crystal chemical characterization of mullite-type aluminum borate compounds

    Science.gov (United States)

    Hoffmann, K.; Hooper, T. J. N.; Zhao, H.; Kolb, U.; Murshed, M. M.; Fischer, M.; Lührs, H.; Nénert, G.; Kudějová, P.; Senyshyn, A.; Schneider, H.; Hanna, J. V.; Gesing, Th. M.; Fischer, R. X.

    2017-03-01

    Al-rich aluminum borates were prepared by different synthesis routes using various Al/B ratios, characterized by diffraction methods, spectroscopy and prompt gamma activation analysis. The 11B NMR data show a small amount of BO4 species in all samples. The chemical analysis indicates a trend in the Al/B ratio instead of a fixed composition. Both methods indicate a solid solution Al5-xB1+xO9 where Al is substituted by B in the range of 1-3%. The structure of B-rich Al4B2O9 (C2/m, a=1488 pm, b=553 pm, c=1502 pm, ß=90.6°), was re-investigated by electron diffraction methods, showing that structural details vary within a crystallite. In most of the domains the atoms are orderly distributed, showing no signal for the postulated channel oxygen atom O5. The absence of O5 is supported by density functional theory calculations. Other domains show a probable disordered configuration of O5 and O10, indicated by diffuse scattering along the b direction.

  4. Chemical characterization of a marine conditioning film

    Digital Repository Service at National Institute of Oceanography (India)

    Garg, A.; Jain, A.; Bhosle, N.B.

    . 2. Materials and Methods 2.1. Chemicals and reagents Glass cover slips were purchased from Blue Star, India. Standard sugars and, myo- inositol were obtained from Sigma (St. Louis, MO, USA). Sodium carbonate, NaOH, HCl and methanol were of high... purity AR grades and were purchased from s.d. Fine Chemicals, Mumbai. Methanol was double distilled before use. Distilled water was purified using UV- Milli-Q water purification system (Millipore, Bangalore, India). 2.2. Preparation and deployment...

  5. Method for innovative synthesis-design of chemical process flowsheets

    DEFF Research Database (Denmark)

    Kumar Tula, Anjan; Gani, Rafiqul

    of chemical processes, where, chemical process flowsheets could be synthesized in the same way as atoms or groups of atoms are synthesized to form molecules in computer aided molecular design (CAMD) techniques [4]. That, from a library of building blocks (functional process-groups) and a set of rules to join......, the implementation of the computer-aided process-group based flowsheet synthesis-design framework is presented together with an extended library of flowsheet property models to predict the environmental impact, safety factors, product recovery and purity, which are employed to screen the generated alternatives. Also...... flowsheet (the well-known Hydrodealkylation of toluene process) and another for a biochemical process flowsheet (production of ethanol from lignocellulose). In both cases, not only the reported designs are found and matched, but also new innovative designs are found, which is possible because...

  6. In-situ preparation of polymer-coated alumina nanopowders by chemical vapor synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Schallehn, M.; Winterer, M.; Weirich, T.E.; Hahn, H. [Inst. of Materials Science, Darmstadt Univ. of Technology, Darmstadt (Germany); Keiderling, U. [Hahn-Meitner-Inst., Berlin (Germany)

    2003-01-01

    Nanocrystalline alumina particles coated with polyethylene have been prepared by a two-step chemical vapor synthesis (CVS) process using a hot-wall reactor to synthesize the nanocrystalline alumina core, and a RF plasma reactor for the subsequent polymer coating. The particle radius is about 4 nm, with the radius of the ceramic core being about 2.5 nm and the coating thickness about 1.5 nm. The powders have been characterized by Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET), small-angle neutron scattering (SANS), and high-resolution transmission electron microscopy (HRTEM). (orig.)

  7. Synthesis, characterization and study of magnetic, electrical and dielectric properties of La1-xDyxCo1-yFeyO3 nanoparticles prepared by wet chemical route

    Science.gov (United States)

    Choudhry, Qurshia; Azhar Khan, Muhammad; Nasar, Gulfam; Mahmood, Azhar; Shahid, Muhammad; Shakir, Imran; Farooq Warsi, Muhammad

    2015-11-01

    Dy3+ and Fe3+ co-doped LaCoO3 perovskite nanoparticles were prepared by chemical co-precipitation route. Structural elucidation was carried out by thermo gravimetric analysis (TGA), X-ray diffraction (XRD), scanning electron microscopy (SEM), and Fourier transform infrared (FTIR) spectroscopy. The data of all these characterization techniques confirmed the orthorhombic phase with particles size in the range of 20-60 nm. The magnetic parameters, DC-resistivity and dielectric properties were measured for La1-xDyxCo1-yFeyO3 nanoparticles. The purpose of all these application studies was to evaluate the prepared materials for practical applications. The substitution of Dy3+ and Fe3+ with La3+ and Co3+ respectively greatly influenced the magnetic, DC-resistivity and dielectric parameters.

  8. Synthesis, NMR spectroscopic characterization and structure of a divinyldisilazane-(triphenylphosphine)platinum(0) complex: observation of isotope-induced chemical shifts (1)Δ(12/13)C((195)Pt).

    Science.gov (United States)

    Wrackmeyer, Bernd; Klimkina, Elena V; Schmalz, Thomas; Milius, Wolfgang

    2013-05-01

    Tetramethyldivinyldisilazane-(triphenylphosphine)platinum(0) was prepared, characterized in solid state by X-ray crystallography and in solution by multinuclear magnetic resonance spectroscopy ((1)H, (13)C, (15)N, (29)Si, (31)P and (195)Pt NMR). Numerous signs of spin-spin coupling constants were determined by two-dimensional heteronuclear shift correlations (HETCOR) and two-dimensional (1)H/(1)H COSY experiments. Isotope-induced chemical shifts (1)Δ(12/13)C((195)Pt) were measured from (195)Pt NMR spectra of the title compound as well as of other Pt(0), Pt(II) and Pt(IV) compounds for comparison. In contrast to other heavy nuclei such as (199)Hg or (207)Pb, the "normal" shifts of the heavy isotopomers to low frequencies are found, covering a range of >500 ppb.

  9. Synthesis, crystal structure analysis, spectral characterization, quantum chemical calculations, antioxidant and antimicrobial activity of 3-(4-chlorophenyl)-3a,4,7,7a-tetrahydro-4,7-methanobenzo[d]isoxazole

    Science.gov (United States)

    Eryılmaz, Serpil; Gül, Melek; İnkaya, Ersin; İdil, Önder; Özdemir, Namık

    2016-10-01

    In this paper, 3-(4-chlorophenyl)-3a,4,7,7a-tetrahydro-4,7-methanobenzo[d]isoxazole was synthesized via 1,3 dipolar cycloaddition, characterized by spectroscopic analysis such as FT-IR, 1H NMR, 13C NMR, UV-Vis, LC-MS/MS, Elemental Analysis, and X-ray Single Crystal diffraction technique. The Density Functional Theory (DFT/B3LYP) method with 6-311G(d,p) basis set in the ground state was applied for quantum chemical calculations and molecular geometric parameters of the compound were compared with the X-ray analysis results. FT-IR, NMR and UV-Vis spectral analysis were analysed to determine the compliance with the vibrational frequencies, 1H NMR and 13C NMR chemical shifts and absorption wavelength values. The frontier molecular orbitals (FMOs), some global reactivity descriptors, molecular electrostatic potential (MEP), thermodynamic properties, non-linear optical (NLO) behaviour of the compound were examined with the same method in gas phase, theoretically. Moreover, antioxidant activity was determined with three different methods - DPPH radical scavenging, reducing and metal chelating, antimicrobial activity were carried out with Gram positive, Gram negative and Eukaryote for the title compound.

  10. Chemical synthesis of the lantibiotic lacticin 481 reveals the importance of lanthionine stereochemistry.

    Science.gov (United States)

    Knerr, Patrick J; van der Donk, Wilfred A

    2013-05-15

    Lantibiotics are a family of antibacterial peptide natural products characterized by the post-translational installation of the thioether-containing amino acids lanthionine and methyllanthionine. Until recently, only a single naturally occurring stereochemical configuration for each of these cross-links was known. The discovery of lantibiotics with alternative lanthionine and methyllanthionine stereochemistry has prompted an investigation of its importance to biological activity. Here, solid-supported chemical synthesis enabled the total synthesis of the lantibiotic lacticin 481 and analogues containing cross-links with non-native stereochemical configurations. Biological evaluation revealed that these alterations abolished the antibacterial activity in all of the analogues, revealing the critical importance of the enzymatically installed stereochemistry for the biological activity of lacticin 481.

  11. Controlled Synthesis of Atomically Layered Hexagonal Boron Nitride via Chemical Vapor Deposition

    Directory of Open Access Journals (Sweden)

    Juanjuan Liu

    2016-11-01

    Full Text Available Hexagonal boron nitrite (h-BN is an attractive material for many applications including electronics as a complement to graphene, anti-oxidation coatings, light emitters, etc. However, the synthesis of high-quality h-BN is still a great challenge. In this work, via controlled chemical vapor deposition, we demonstrate the synthesis of h-BN films with a controlled thickness down to atomic layers. The quality of as-grown h-BN is confirmed by complementary characterizations including high-resolution transition electron microscopy, atomic force microscopy, Raman spectroscopy and X-ray photo-electron spectroscopy. This work will pave the way for production of large-scale and high-quality h-BN and its applications as well.

  12. Green chemical synthesis of silver nanomaterials with maltodextrin.

    Energy Technology Data Exchange (ETDEWEB)

    Tallant, David Robert; Lu, Ping; Lambert, Timothy N.; Bell, Nelson Simmons

    2010-11-01

    Silver nanomaterials have significant application resulting from their optical properties related to surface enhanced Raman spectroscopy, high electrical conductivity, and anti-microbial impact. A 'green chemistry' synthetic approach for silver nanomaterials minimizes the environmental impact of silver synthesis, as well as lowers the toxicity of the reactive agents. Biopolymers have long been used for stabilization of silver nanomaterials during synthesis, and include gum Arabic, heparin, and common starch. Maltodextrin is a processed derivative of starch with lower molecular weight and an increase in the number of reactive reducing aldehyde groups, and serves as a suitable single reactant for the formation of metallic silver. Silver nanomaterials can be formed under either a thermal route at neutral pH in water or by reaction at room temperature under more alkaline conditions. Deposited silver materials are formed on substrates from near neutral pH solutions at low temperatures near 50 C. Experimental conditions based on material concentrations, pH and reaction time are investigated for development of deposited films. Deposit morphology and optical properties are characterized using SEM and UV-vis techniques. Silver nanoparticles are generated under alkaline conditions by a dissolution-reduction method from precipitated silver (II) oxide. Synthesis conditions were explored for the rapid development of stable silver nanoparticle dispersions. UV-vis absorption spectra, powder X-ray diffraction (PXRD), dynamic light scattering (DLS), and transmission electron microscopy (TEM) techniques were used to characterize the nanoparticle formation kinetics and the influence of reaction conditions. The adsorbed content of the maltodextrin was characterized using thermogravimetric analysis (TGA).

  13. Synthesis and Microstructural Characterization of SnO2:F Thin Films Deposited by AACVD

    OpenAIRE

    Chavarría-Castillo,Karen Alejandra; Amézaga-Madrid,Patricia; Esquivel-Pereyra,Oswaldo; Antúnez-Flores, Wilber; Pizá Ruiz, Pedro; Miki-Yoshida,Mario

    2016-01-01

    In this work, we report the synthesis and microstructural characterization of Tin oxide thin films doped with fluorine for applications such as transparent conductive oxides. Tin oxide doped with fluorine thin films were deposited by aerosol assisted chemical vapor deposition technique onto a borosilicate glass substrate, using a precursor solution of stannic chloride in ethanol and ammonium fluoride as the dopant. Deposition temperature was varied between 623-773 K. Also, other deposition pa...

  14. Synthesis, characterization and magnetic properties of room-temperature nanofluid ferromagnetic graphite

    OpenAIRE

    Souza, NS; Sergeenkov, S.; Speglich, C.; Rivera, VAG; Cardoso, CA; Pardo, H.; Mombru, AW; Rodrigues, AD; de Lima, OF; Araujo-Moreira, FM

    2009-01-01

    We report the chemical synthesis route, structural characterization, and physical properties of nanofluid magnetic graphite (NFMG) obtained from the previously synthesized bulk organic magnetic graphite (MG) by stabilizing the aqueous ferrofluid suspension with an addition of active cationic surfactant. The measured magnetization-field hysteresis curves along with the temperature dependence of magnetization confirmed room-temperature ferromagnetism in both MG and NFMG samples. (C) 2009 Americ...

  15. Synthesis and characterization of covalent diphenylalanine nanotube-folic acid conjugates

    DEFF Research Database (Denmark)

    León, John Jairo Castillo; Rindzevicius, Tomas; Wu, Kaiyu

    2014-01-01

    Herein, we describe the synthesis and characterization of a covalent nanoscale assembly formed between diphenylalanine micro/nanotubes (PNT) and folic acid (FA). The conjugate was obtained via chemical functionalization through coupling of amine groups of PNTs and carboxylic groups of FA. The sur...... for applications in the detection and diagnosis of cancer or tropical diseases such as leishmaniasis and as a carrier nanosystem delivering drugs to malignant tumors that overexpress folate receptors....

  16. Hydrothermal synthesis and characterization of zirconia based catalysts

    Energy Technology Data Exchange (ETDEWEB)

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

    2013-07-15

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

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

    OpenAIRE

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

    2014-01-01

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

  18. Nondestructive Method for Bulk Chemical Characterization of Barred Olivine Chondrules

    Science.gov (United States)

    Montoya-Perez, M. A.; Cervantes-de la Cruz, K. E.; Ruvalcaba-Sil, J. L.

    2017-02-01

    This work develops a bulk chemical characterization of barred olivine chondrules based on the XRF analysis using a portable equipment at the National Research and Conservation Science Laboratory of Cultural Heritage (LANCIC-IF) in Mexico City.

  19. Synthesis and chemical etching of Te/C nanocables

    Indian Academy of Sciences (India)

    Guang Sheng Cao; Yong Gang Liu; Wen Wu Yang; Chang Tan; Hui Li; Xiao Juan Zhang

    2011-10-01

    In this paper, Te/C nanocables were fabricated by a hydrothermal method in the presence of cetyltrimethylammonium bromide (CTAB). The products were characterized in detail by multiform techniques: transmission electron microscopy, X-ray diffraction, energy-dispersive X-ray analysis and Fourier transform infrared (FTIR) spectroscopy. The results showed that the products were nanocables with lengths of several microns, core about 20 nm in diameter, and a surrounding sheath of about 60–80 nm in thickness. Te/C nanocables were tailored freely by chemical etching. Carbonaceous nanotubes and Te/C nanocables with fragmentary Te core were obtained by adjusting time of chemical etching.

  20. SYNTHESIS AND CHARACTERIZATION OF A DERIVATIVE CYCLOHEXANONE CHALCONE-TYPE, AS AN INTEGRAL LABORATORY EXPERIENCE

    Directory of Open Access Journals (Sweden)

    Perla E. Hernández-González

    2015-03-01

    Full Text Available At present, chemistry teachers are searching new models that allow integrative laboratory experiences, converging interdisciplinary knowledge of the Chemistry field. With this framework of ideas, this work describes the synthesis and characterization of the (2E,6E-2,6-bis(4-methoxybenzylidenecyclohexanone compound as axis of knowledge in order to encourage the students to develop their cognitive skills, such as critical thinking and problem solving, and also interpretation and analysis of results. The compound was synthesized by a Claisen-Schmidt condensation reaction, involving an aromatic aldehyde and cyclohexanone. The compound was characterized spectroscopically by NMR, IR and UV-Vis. Melting point and solubility tests were also performed. The chemical structure was confirmed by single crystal X-Ray diffraction. In conclusion, this laboratory experience allows students to get involved with the techniques and procedures commonly used in the organic chemistry laboratory to the synthesis and characterization of organic compounds.

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

    Science.gov (United States)

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

    2016-12-10

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

  2. Synthesis and Characterization of Metal Phosphates for Photocatalytic Applications

    KAUST Repository

    Al-Sabban, Bedour

    2012-07-01

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

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

    Directory of Open Access Journals (Sweden)

    A. K. Singh

    2014-01-01

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

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

    Science.gov (United States)

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

    2014-01-01

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

  5. Synthesis, spectroscopic and X-ray structural characterization, quantum chemical studies and investigation of gama-irradiated effects of the novel hydrazone compound: [(E)-3-(2-nitrophenyl)-(E)-1-(2-phenylhydrazono)]-1-phenylallylidene

    Science.gov (United States)

    Yakalı, Gül; Çakıcı, Abban; Eke, Canel; Cin, Günseli Turgut; Aygün, Muhittin

    2017-04-01

    The novel hydrazone compound, [(E)-3-(2-nitrophenyl)-(E)-1-(2-phenylhydrazono)]-1-phenylallylidene (2), has been synthesized, characterized by FTIR, 1H NMR, 13C NMR techniques, elemental analysis, X-ray structure analysis and has been investigated gama-irradiated effect. Additionally, the molecular geometrical parameters, frontier molecular orbital energies (HOMO, LUMO), their energy gap (Δ E) , molecular electrostatic potential analysis of the compound have been calculated by using DFT/B3LYP with 6-311G (d, p) level. Also, IR frequencies, 1H and 13C NMR chemical shifts of the compound were calculated by using DFT calculations at the same level basis and changing in lattice parameters, unit cell volume and density of the compound are observed after gama irradiated at XRD data. Unirradiated state of the title compound (C21H17N3O2) crystallizes in the monoclinic space group P21/n with a = 9.1782(7) Å, b = 16.1359(12) Å, c = 11.9709(12) Å, β = 101.022(8)o, V = 1740.2(3) Å3, Dcalc = 1.3106 g/cm3 and Z = 4 while irradiated state of title compound showed significant changes in lattice parameters, crystal volume and density. In contrast, the crystal system is found to be the same at after and before irradiation. The calculated geometrical parameters, IR frequencies, 1H and 13C NMR chemical shifts of the compound were in good agreement with the observed single crystal- XRD data, IR, 1H and 13C NMR spectra.

  6. Recent Developments in Chemical Synthesis with Biocatalysts in Ionic Liquids.

    Science.gov (United States)

    Potdar, Mahesh K; Kelso, Geoffrey F; Schwarz, Lachlan; Zhang, Chunfang; Hearn, Milton T W

    2015-09-15

    Over the past decade, a variety of ionic liquids have emerged as greener solvents for use in the chemical manufacturing industries. Their unique properties have attracted the interest of chemists worldwide to employ them as replacement for conventional solvents in a diverse range of chemical transformations including biotransformations. Biocatalysts are often regarded as green catalysts compared to conventional chemical catalysts in organic synthesis owing to their properties of low toxicity, biodegradability, excellent selectivity and good catalytic performance under mild reaction conditions. Similarly, a selected number of specific ionic liquids can be considered as greener solvents superior to organic solvents owing to their negligible vapor pressure, low flammability, low toxicity and ability to dissolve a wide range of organic and biological substances, including proteins. A combination of biocatalysts and ionic liquids thus appears to be a logical and promising opportunity for industrial use as an alternative to conventional organic chemistry processes employing organic solvents. This article provides an overview of recent developments in this field with special emphasis on the application of more sustainable enzyme-catalyzed reactions and separation processes employing ionic liquids, driven by advances in fundamental knowledge, process optimization and industrial deployment.

  7. Recent Developments in Chemical Synthesis with Biocatalysts in Ionic Liquids

    Directory of Open Access Journals (Sweden)

    Mahesh K. Potdar

    2015-09-01

    Full Text Available Over the past decade, a variety of ionic liquids have emerged as greener solvents for use in the chemical manufacturing industries. Their unique properties have attracted the interest of chemists worldwide to employ them as replacement for conventional solvents in a diverse range of chemical transformations including biotransformations. Biocatalysts are often regarded as green catalysts compared to conventional chemical catalysts in organic synthesis owing to their properties of low toxicity, biodegradability, excellent selectivity and good catalytic performance under mild reaction conditions. Similarly, a selected number of specific ionic liquids can be considered as greener solvents superior to organic solvents owing to their negligible vapor pressure, low flammability, low toxicity and ability to dissolve a wide range of organic and biological substances, including proteins. A combination of biocatalysts and ionic liquids thus appears to be a logical and promising opportunity for industrial use as an alternative to conventional organic chemistry processes employing organic solvents. This article provides an overview of recent developments in this field with special emphasis on the application of more sustainable enzyme-catalyzed reactions and separation processes employing ionic liquids, driven by advances in fundamental knowledge, process optimization and industrial deployment.

  8. Synthesis and characterization of environmentally friendly fluorescent particle tracers

    Science.gov (United States)

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

    2013-04-01

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

  9. Synthesis, characterization, DNA binding and in vitro antimicrobial studies of a novel tetra-substituted N-isopropyl-N-(4-ferrocenylphenyl)-N‧-(2,6-diethylphenyl)-N″-benzoylguanidine: Crystallographic structure and quantum chemical computations

    Science.gov (United States)

    Rauf, Muhammad Khawar; Gul, Rukhsana; Rashid, Zahid; Badshah, Amin; Tahir, Muhammad Nawaz; Shahid, Muhammad; Khan, Azim

    2015-02-01

    A novel tetra-substituted guanidine, N-isopropyl-N-(4-ferrocenylphenyl)-N‧-(2,6-diethylphenyl)-N″-benzoylguanidine (1), [(CH3)2CH)(C5H5FeC5H4C6H4)NC(NHCOC6H5)(NHC6H3(CH2CH3)2] has been synthesized and characterized by elemental analysis, FT-IR, multinuclear (1H, 13C) NMR spectroscopy, single crystal X-rays diffraction analysis and density functional theory based quantum chemical calculations. The torsion angles indicating that the guanidine moiety and carbonyl group are almost co-planar, due to the pseudo hexagonal ring formed by intramolecular Nsbnd H⋯O hydrogen bonds. The DNA interaction studies performed by cyclic voltammetry and UV-visible spectroscopy are in close agreement with the binding constants (K) 1.4 × 104 and 1.2 × 104 respectively. The shift in peak potential, current and absorption maxima of the studied ferrocenyl guanidine in the presence of DNA discovered that CV coupled with UV-vis spectroscopy could provide an opportunity to elaborate DNA interaction mechanism, a prerequisite for the design of new drug like agents and understanding the molecular basis of their action. The synthesized compound (1) has also been screened for their antibacterial and antifungal.

  10. Modern catalysis in the synthesis of some pharmaceuticals and fine chemicals

    OpenAIRE

    Petrović Slobodan D.; Mišić-Vuković Milica M.; Mijin Dušan Ž.

    2002-01-01

    Catalysis in the synthesis of Pharmaceuticals and line chemicals nowadays becomes more and more important. Synthesis that minimizes wastes is important from the economical aspect, as well as from the environmental aspect. "Green chemistry" or "green technology" is an effort to protect the environment by increasing the efficiency of the overall synthetic processes in the chemical industry by minimizing or eliminating wasteful by-products. Modern catalytic methods in the synthesis of some Pharm...

  11. Effect of Microwave Radiation on Enzymatic and Chemical Peptide Bond Synthesis on Solid Phase

    Directory of Open Access Journals (Sweden)

    Alessandra Basso

    2009-01-01

    Full Text Available Peptide bond synthesis was performed on PEGA beads under microwave radiations. Classical chemical coupling as well as thermolysin catalyzed synthesis was studied, and the effect of microwave radiations on reaction kinetics, beads' integrity, and enzyme activity was assessed. Results demonstrate that microwave radiations can be profitably exploited to improve reaction kinetics in solid phase peptide synthesis when both chemical and biocatalytic strategies are used.

  12. Chemical Precipitation Synthesis and Thermoelectric Properties of Copper Sulfide

    Science.gov (United States)

    Wu, Sixin; Jiang, Jing; Liang, Yinglin; Yang, Ping; Niu, Yi; Chen, Yide; Xia, Junfeng; Wang, Chao

    2017-04-01

    Earth-abundant copper sulfide compounds have been intensively studied as potential thermoelectric materials due to their high dimensionless figure of merit ZT values. They have a unique phonon-liquid electron-crystal model that helps to achieve high thermoelectric performance. Many methods, such as melting and ball-milling, have been adopted to synthesize this copper sulfide compound, but they both use expensive starting materials with high purity. Here, we develop a simple chemical precipitation approach to synthesize copper sulfide materials through low-cost analytically pure compounds as the starting materials. A high ZT value of 0.93 at 800 K was obtained from the samples annealed at 1273 K. Its power factor is around 8.0 μW cm-1 K-2 that is comparable to the highest record reported by traditional methods. But, the synthesis here has been greatly simplified with reduced cost, which will be of great benefit to the potential mass production of thermoelectric devices. Furthermore, this method can be applied to the synthesis of other sulfur compound thermoelectric materials.

  13. An optimized chemical synthesis of human relaxin-2.

    Science.gov (United States)

    Barlos, Kostas K; Gatos, Dimitrios; Vasileiou, Zoe; Barlos, Kleomenis

    2010-04-01

    Human gene 2 relaxin (RLX) is a member of the insulin superfamily and is a multi-functional factor playing a vital role in pregnancy, aging, fibrosis, cardioprotection, vasodilation, inflammation, and angiogenesis. RLX is currently applied in clinical trials to cure among others acute heart failure, fibrosis, and preeclampsia. The synthesis of RLX by chemical methods is difficult because of the insolubility of its B-chain and the required laborious and low yielding site-directed combination of its A (RLXA) and B (RLXB) chains. We report here that oxidation of the Met(25) residue of RLXB improves its solubility, allowing its effective solid-phase synthesis and application in random interchain combination reactions with RLXA. Linear Met(O)(25)-RLX B-chain (RLXBO) reacts with a mixture of isomers of bicyclic A-chain (bcRLXA) giving exclusively the native interchain combination. Applying this method Met(O)(25)-RLX (RLXO) was obtained in 62% yield and was easily converted to RLX in 78% yield, by reduction with ammonium iodide.

  14. Thermodynamics principles characterizing physical and chemical processes

    CERN Document Server

    Honig, Jurgen M

    1999-01-01

    This book provides a concise overview of thermodynamics, and is written in a manner which makes the difficult subject matter understandable. Thermodynamics is systematic in its presentation and covers many subjects that are generally not dealt with in competing books such as: Carathéodory''s approach to the Second Law, the general theory of phase transitions, the origin of phase diagrams, the treatment of matter subjected to a variety of external fields, and the subject of irreversible thermodynamics.The book provides a first-principles, postulational, self-contained description of physical and chemical processes. Designed both as a textbook and as a monograph, the book stresses the fundamental principles, the logical development of the subject matter, and the applications in a variety of disciplines. This revised edition is based on teaching experience in the classroom, and incorporates many exercises in varying degrees of sophistication. The stress laid on a didactic, logical presentation, and on the relat...

  15. Frontiers and Approaches to Chemical Synthesis of Oligodeoxyribonucleotides

    OpenAIRE

    2013-01-01

    The advantages and disadvantages of existing approaches to the synthesis of oligodeoxyribonucleotides (ODN) are discussed focusing on large-scale methods. The liquid phase and solid supported synthesis and the synthesis on soluble polymers are discussed. Different problems concerning the methods and implementation of the ODN synthesis are outlined depending on goals of using target oligomers.

  16. The synthesis and characterization of the 'research chemical' N-(1-amino-3-methyl-1-oxobutan-2-yl)-1-(cyclohexylmethyl)-3-(4-fluorophenyl)-1H-pyrazole-5-carboxamide (3,5-AB-CHMFUPPYCA) and differentiation from its 5,3-regioisomer.

    Science.gov (United States)

    McLaughlin, Gavin; Morris, Noreen; Kavanagh, Pierce V; Power, John D; Twamley, Brendan; O'Brien, John; Talbot, Brian; Dowling, Geraldine; Brandt, Simon D

    2016-09-01

    This study presents the identification of N-(1-amino-3-methyl-1-oxobutan-2-yl)-1-(cyclohexylmethyl)-3-(4-fluorophenyl)-1H-pyrazole-5-carboxamide that was termed 3,5-AB-CHMFUPPYCA. This compound was obtained from a UK-based Internet vendor, who erroneously advertised this 'research chemical' as AZ-037 and which would have been associated with (S)-N-(1-amino-3-methyl-1-oxobutan-2-yl)-1-(5-fluoropentyl)-5-(4-fluorophenyl)-1H-pyrazole-3-carboxamide. The presence of the pyrazole core indicates a bioisosteric replacement of an indazole ring that is frequently associated with synthetic cannabinoids of the PINACA, FUBINACA, and CHMINACA series. The pyrazole ring system present in 3,5-AB-CHMFUPPYCA gives rise to the regioisomer N-(1-amino-3-methyl-1-oxobutan-2-yl)-1-(cyclohexylmethyl)-5-(4-fluorophenyl)-1H-pyrazole-3-carboxamide (named 5,3-AB-CHMFUPPYCA) and both isomers were synthesized using two specific routes which supported the correct identification of the 'research chemical' as 3,5-AB-CHMFUPPYCA. Both isomers could be conveniently differentiated. Interestingly, a route specific chlorine-containing by-product also was observed during the synthesis of 3,5-AB-CHMFUPPYCA and identified as N-(1-amino-3-methyl-1-oxobutan-2-yl)-4-chloro-1-(cyclohexylmethyl)-3-(4-fluorophenyl)-1H-pyrazole-5-carboxamide. An extensive analytical characterization included chromatographic, spectroscopic, mass spectrometric platforms as well as crystal structure analysis. The syntheses and analytical characterizations of both AB-CHMFUPPYCA isomers are reported for the first time and serves as a reminder that the possibility of mislabeling of 'research chemicals' cannot be excluded. The pharmacological activities of both AB-CHMFUPPYCA isomers remain to be explored. Copyright © 2015 John Wiley & Sons, Ltd.

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

    Institute of Scientific and Technical Information of China (English)

    Qi Fu; Bin Xiang

    2016-01-01

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

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

    NARCIS (Netherlands)

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

    2010-01-01

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

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

    Science.gov (United States)

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

    1973-01-01

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

  20. The synthesis and characterization of iron nanoparticles

    Science.gov (United States)

    Bennett, Tyler

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

  1. Molybdenum oxide nanocubes: Synthesis and characterizations

    Science.gov (United States)

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

    2015-06-01

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

  2. Molybdenum oxide nanocubes: Synthesis and characterizations

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-06-24

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

  3. Morphological and Chemical Characterization of Psidium Species

    Directory of Open Access Journals (Sweden)

    Anshu SHARMA

    2010-06-01

    Full Text Available The present study was conducted to estimate genetic relationship among 20 genotypes of Psidium guajava and two species viz., P friedrichsthalianum Ndz. and P. catleianum Sabine, by morphological characterization. Out of 16 morphological characters studied, only inflorescence type did not show any variation, while the remaining traits showed variability to considerable extent. Morphological data on different genotypes were used to calculate similarity matrix which ranged from 0.06 to 0.50.and based on this cluster analysis was done using UPGMA. The genetic variation among genotypes was high enough to divide them into two major clusters. Cluster I consisted of �Chakaiya Rehmannagar�, �Gutaniwala�, �Super Max Ruby�, and �Spear Acid�, whereas cluster II consisted of the rest of 18 genotypes.

  4. Synthesis and characterization of Li1.3Al0.3Ti1.7(PO4)3-coated LiMn2O4 by wet chemical route

    Institute of Scientific and Technical Information of China (English)

    WU Xianming; LI Runxiu; CHEN Shang; HE Zeqiang

    2009-01-01

    Li1.3Al0.3Ti1.7(PO4)3-coated LiMn2O4 was prepared by wet chemical route. The phase, surface morphology, and electrochemical properties of the prepared powders were characterized by X-ray diffraction, scanning electron micrograph, and galvanostatic charge-discharge experiments. Li1.3Al0.3Ti1.7(PO4)3-coated LiMn2O4 has similar X-ray diffraction patterns as LiMn2O4. The corner and border of Li1.3Al0.3Ti1.7(PO4)3-coated LiMn2O4 particles are not as clear as the uncoated one. The two powders show similar values of lithium-ion diffusion coefficient. When cy-cled at room temperature and 55℃ for 40 times at the charge-discharge rate of 0.2C, Li1.3Al0.3Ti1.7(PO4)3-coated LiMn2O4 shows the capacity retentions of 98.2% and 93.9%, respectively, which are considerably higher than the values of 85.4% and 79.1% for the uncoated one. Both the capacity retention differences between Li1.3Al0.3Ti1.7(PO4)3-coated LiMn2O4 and LiMn204 cycling at room temperature and 55℃ become larger with the increase of charge-discharge rate. When the charge-discharge rate reaches 2C, the capacity retention of LATP-coated LiMn2O4 becomes 8.4% higher than the uncoated LiMn2O4 for room temperature cycling, and it becomes 11.1% higher than the latter when cycled at 55℃.

  5. Synthesis and structure characterization of diethyldiallylammonium chloride

    Institute of Scientific and Technical Information of China (English)

    刘立华; 龚竹青; 郑雅杰

    2003-01-01

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

  6. Proficient magnesium nanoferrites: synthesis and characterization

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-01-15

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

  7. Synthesis and characterization of tantalum silsesquioxane complexes.

    Science.gov (United States)

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

    2013-02-14

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

  8. A Comparison between Chemical Synthesis Magnetite Nanoparticles and Biosynthesis Magnetite.

    Science.gov (United States)

    Kahani, Seyed Abolghasem; Yagini, Zahra

    2014-01-01

    The preparation of Fe3O4 from ferrous salt by air in alkaline aqueous solution at various temperatures was proposed. The synthetic magnetites have different particle size distributions. We studied the properties of the magnetite prepared by chemical methods compared with magnetotactic bacterial nanoparticles. The results show that crystallite size, morphology, and particle size distribution of chemically prepared magnetite at 293 K are similar to biosynthesis of magnetite. The new preparation of Fe3O4 helps to explain the mechanism of formation of magnetosomes in magnetotactic bacteria. The products are characterized by X-ray powder diffraction (XRD), infrared (IR) spectra, vibrating sample magnetometry (VSM), and scanning electron microscopy (SEM).

  9. Chemical synthesis of superconducting MgB{sub 2} nanopowder

    Energy Technology Data Exchange (ETDEWEB)

    Bansal, Narottam P., E-mail: Narottam.P.Bansal@nasa.gov [Materials and Structures Division, NASA Glenn Research Center, Cleveland, OH 44135 (United States); Goldsby, Jon C.; Rogers, Richard B. [Materials and Structures Division, NASA Glenn Research Center, Cleveland, OH 44135 (United States); Susner, Michael A.; Sumption, Michael D. [Center for Superconducting and Magnetic Materials, Department of Materials Science and Engineering, The Ohio State University, Columbus, OH 43210 (United States)

    2015-02-15

    Highlights: • MgB{sub 2} nanopowder has been synthesized by chemical method. • Powder characterized by XRD and SEM. • Superconducting behavior confirmed by susceptibility and magnetization measurements. • Nanopowder will facilitate the fabrication of small diameter MgB{sub 2} filaments. - Abstract: Superconducting MgB{sub 2} nanopowder has been synthesized through chemical reaction between lithium borohydride and magnesium hydride at relatively low temperatures. From quantitative Rietveld analysis, the average crystallite size of MgB{sub 2} powder was evaluated to be 33 nm. The superconducting transition temperature of the MgB{sub 2} nanopowder was found to be 38.8-38.9 K from magnetization and DC susceptibility measurements. Powder morphology has been evaluated by scanning electron microscopy.

  10. NEW ROOM TEMPERATURE LIQUIDS: SYNTHESIS AND CHARACTERIZATION

    Directory of Open Access Journals (Sweden)

    Macaev Fliur

    2007-06-01

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

  11. Towards consensus in chemical characterization modeling for LCA:

    DEFF Research Database (Denmark)

    Rosenbaum, Ralf; Hauschild, Michael Zwicky; Bachmann, Till;

    2006-01-01

    A comprehensive LCIA characterization model comparison is being undertaken in the UNEP/SETAC Life Cycle Initiative, focusing on toxicity impacts and directly involving the developers of all models included. The main objective is to identify where differences come from, what indispensable model...... components are and if there can be a consensus model built from them, leading towards recommended practice in chemical characterization for LCIA. The models were selected in an open process inviting all models identified to be capable of characterizing a chemical in terms of environmental fate, human...... exposure, human toxicity and ecotoxicity. The invitation was accepted by the developers of CalTOX, IMPACT 2002, USES-LCA, EDIP, WATSON, and EcoSense. A consistent chemical test set comprising 66 organic (generic, amphiphilic and dissociating) and inorganic (metals, salts) compounds was selected...

  12. Synthesis and Characterization of Polymer-Templated Magnetic Nanoparticles

    Science.gov (United States)

    Tamakloe, Beatrice

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

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

    Directory of Open Access Journals (Sweden)

    Jingfei Luan

    2011-05-01

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

  14. Gaseous detonation synthesis and characterization of nano-oxide

    Science.gov (United States)

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

    2015-07-01

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

  15. Anisotropic Gold Nanocrystals:. Synthesis and Characterization

    Science.gov (United States)

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

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

  16. Enzymatic Synthesis of Rhamnose Containing Chemicals by Reverse Hydrolysis.

    Directory of Open Access Journals (Sweden)

    Lili Lu

    Full Text Available Rhamnose containing chemicals (RCCs are widely occurred in plants and bacteria and are known to possess important bioactivities. However, few of them were available using the enzymatic synthesis method because of the scarcity of the α-L-rhamnosidases with wide acceptor specificity. In this work, an α-L-rhamnosidase from Alternaria sp. L1 was expressed in Pichia pastroris strain GS115. The recombinant enzyme was purified and used to synthesize novel RCCs through reverse hydrolysis in the presence of rhamnose as donor and mannitol, fructose or esculin as acceptors. The effects of initial substrate concentrations, reaction time, and temperature on RCC yields were investigated in detail when using mannitol as the acceptor. The mannitol derivative achieved a maximal yield of 36.1% by incubation of the enzyme with 0.4 M L-rhamnose and 0.2 M mannitol in pH 6.5 buffers at 55°C for 48 h. In identical conditions except for the initial acceptor concentrations, the maximal yields of fructose and esculin derivatives reached 11.9% and 17.9% respectively. The structures of the three derivatives were identified to be α-L-rhamnopyranosyl-(1→6'-D-mannitol, α-L-rhamnopyranosyl-(1→1'-β-D-fructopyranose, and 6,7-dihydroxycoumarin α-L-rhamnopyranosyl-(1→6'-β-D-glucopyranoside by ESI-MS and NMR spectroscopy. The high glycosylation efficiency as well as the broad acceptor specificity of this enzyme makes it a powerful tool for the synthesis of novel rhamnosyl glycosides.

  17. Synthesis and Characterizations of Some New Diacylhydrazones

    Institute of Scientific and Technical Information of China (English)

    WANG,Shu-Xiang; WANG,Wei; LI,Ji-Tai; LI,Tong-Shuang

    2004-01-01

    @@ Acylhydrazine and hydrazine are highly reactive chemicals that have a wide spectrum of uses such as in the chemical and pharmaceutical industries and as a fuel and propellant in aircraft, rockets and satellites. And they can react with microelement in the organism, so they were reported to possess different biological and pharmacological activities, such as antiphthistic, antitumour and so on. But, acylhydrazine and hydrazine have free group of NH2, so they usually have some toxicity to the organism. Hydrazones were investigated in view of the possibility of their being less toxic than the parent hydrazides, because of the blocking of the free NH2 group. In order to reduce the toxicity to the organism, people have been interested in the hydrazones compounds in recent years. In this work, 2,6-dimethylpyridine-3,5-diacylhydrazones were synthesized.

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

    Science.gov (United States)

    Xiong, Guangyong

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

  19. Synthesis, characterization and functionalization of vertically aligned carbon nanotube arrays

    OpenAIRE

    2012-01-01

    Ankara : The Materials Science and Nanotechnology Program of the Graduate School of Engineering and Sciences of Bilkent University, 2012. Thesis (Ph. D.) -- Bilkent University, 2012. Includes bibliographical refences. In the last decade, there has been an increased interest on carbon nanotubes (CNTs) for various applications due to their unique structural, electronic, mechanical and chemical properties. Synthesis of CNTs is no more a challenge with the enhancements and diver...

  20. Characterization and synthesis of carbon aggregates in high temperature environment

    OpenAIRE

    2013-01-01

    Carbon materials in all its forms, from the natural carbon solid materials, as coal and graphite, to the synthesized carbon materials, as carbon black, pitch fibers, fullerenes, carbon nanotubes, etc,. have been object of many studies regarding their characteristics and behaviour due to their importance in the energy and industrial sectors. Recently, most of the research efforts have been focused on the synthesis of new carbon materials and in particular on their physico-chemical propertie...

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

    Science.gov (United States)

    Haders, Daniel Joseph, II

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

  2. Controlled oxidation of iron nanoparticles in chemical vapour synthesis

    Science.gov (United States)

    Ruusunen, Jarno; Ihalainen, Mika; Koponen, Tarmo; Torvela, Tiina; Tenho, Mikko; Salonen, Jarno; Sippula, Olli; Joutsensaari, Jorma; Jokiniemi, Jorma; Lähde, Anna

    2014-02-01

    In the present study, iron oxide nanoparticles (primary particle size of 80-90 nm) with controlled oxidation state were prepared via an atmospheric pressure chemical vapour synthesis (APCVS) method. Iron pentacarbonyl [Fe(CO)5], a precursor material, was thermally decomposed to iron in the APCVS reactor. Subsequently, the iron was oxidized with controlled amount of oxygen in the reactor to produce nearly pure magnetite or haematite particles depending on the oxygen concentration. Size, morphology and crystal structure of the synthesized nanoparticles were studied with scanning mobility particle sizer (SMPS), transmission electron microscopy (TEM) and X-ray diffraction (XRD). In addition, thermodynamic equilibrium calculations and computational fluid dynamics model were used to predict the oxidation state of the iron oxides and the reaction conditions during mixing. Aggregates of crystalline particles were formed, determined as magnetite at the oxygen volumetric fraction of 0.1 % and haematite at volumetric fraction of 0.5 %, according to the XRD. The geometric mean electrical mobility diameter of the aggregates increased from 110 to 155 nm when the volumetric fraction of oxygen increased from 0.1 to 0.5 %, determined using the SMPS. The aggregates were highly sintered based on TEM analyses. As a conclusion, APCVS method can be used to produce nearly pure crystalline magnetite or haematite nanoparticles with controlled oxidation in a continuous one-stage gas-phase process.

  3. 3D printing of versatile reactionware for chemical synthesis.

    Science.gov (United States)

    Kitson, Philip J; Glatzel, Stefan; Chen, Wei; Lin, Chang-Gen; Song, Yu-Fei; Cronin, Leroy

    2016-05-01

    In recent decades, 3D printing (also known as additive manufacturing) techniques have moved beyond their traditional applications in the fields of industrial manufacturing and prototyping to increasingly find roles in scientific research contexts, such as synthetic chemistry. We present a general approach for the production of bespoke chemical reactors, termed reactionware, using two different approaches to extrusion-based 3D printing. This protocol describes the printing of an inert polypropylene (PP) architecture with the concurrent printing of soft material catalyst composites, using two different 3D printer setups. The steps of the PROCEDURE describe the design and preparation of a 3D digital model of the desired reactionware device and the preparation of this model for use with fused deposition modeling (FDM) type 3D printers. The protocol then further describes the preparation of composite catalyst-silicone materials for incorporation into the 3D-printed device and the steps required to fabricate a reactionware device. This combined approach allows versatility in the design and use of reactionware based on the specific needs of the experimental user. To illustrate this, we present a detailed procedure for the production of one such reactionware device that will result in the production of a sealed reactor capable of effecting a multistep organic synthesis. Depending on the design time of the 3D model, and including time for curing and drying of materials, this procedure can be completed in ∼3 d.

  4. Chemical Synthesis of Proanthocyanidins in Vitro and Their Reactions in Aging Wines

    Directory of Open Access Journals (Sweden)

    Qiu-Hong Pan

    2008-12-01

    Full Text Available Proanthocyanidins are present in many fruits and plant products like grapes and wine, and contribute to their taste and health benefits. In the past decades of years, substantial progresses has been achieved in the identification of composition and structure of proanthocyanidins, but the debate concerning the existence of an enzymatic or nonenzymatic mechanism for proanthocyanidin condensation still goes on. Substantial attention has been paid to elucidating the potential mechanism of formation by means of biomimetic and chemical synthesis in vitro. The present paper aims at summarizing the research status on chemical synthesis of proanthocyanidins, including non-enzymatic synthesis of proanthocyanidin precursors, chemical synthesis of proanthocyanidins with direct condensation of flavanols and stereoselective synthesis of proanthocyanidins. Proanthocyanidin-involved reactions in aging wines are also reviewed such as direct and indirect reactions among proanthocyanidins, flavanols and anthocyanins. Topics for future research in this field are also put forward in this paper.

  5. DEVELOPMENT OF ALTERNATIVE FUELS AND CHEMICALS FROM SYNTHESIS GAS

    Energy Technology Data Exchange (ETDEWEB)

    Peter J. Tijrn

    2003-05-31

    This Final Report for Cooperative Agreement No. DE-FC22-95PC93052, the ''Development of Alternative Fuels and Chemicals from Synthesis Gas,'' was prepared by Air Products and Chemicals, Inc. (Air Products), and covers activities from 29 December 1994 through 31 July 2002. The overall objectives of this program were to investigate potential technologies for the conversion of synthesis gas (syngas), a mixture primarily of hydrogen (H{sub 2}) and carbon monoxide (CO), to oxygenated and hydrocarbon fuels and industrial chemicals, and to demonstrate the most promising technologies at the LaPorte, Texas Alternative Fuels Development Unit (AFDU). Laboratory work was performed by Air Products and a variety of subcontractors, and focused on the study of the kinetics of production of methanol and dimethyl ether (DME) from syngas, the production of DME using the Liquid Phase Dimethyl Ether (LPDME{trademark}) Process, the conversion of DME to fuels and chemicals, and the production of other higher value products from syngas. Four operating campaigns were performed at the AFDU during the performance period. Tests of the Liquid Phase Methanol (LPMEOH{trademark}) Process and the LPDME{trademark} Process were made to confirm results from the laboratory program and to allow for the study of the hydrodynamics of the slurry bubble column reactor (SBCR) at a significant engineering scale. Two campaigns demonstrated the conversion of syngas to hydrocarbon products via the slurry-phase Fischer-Tropsch (F-T) process. Other topics that were studied within this program include the economics of production of methyl tert-butyl ether (MTBE), the identification of trace components in coal-derived syngas and the means to economically remove these species, and the study of systems for separation of wax from catalyst in the F-T process. The work performed under this Cooperative Agreement has continued to promote the development of technologies that use clean syngas produced

  6. DEVELOPMENT OF ALTERNATIVE FUELS AND CHEMICALS FROM SYNTHESIS GAS

    Energy Technology Data Exchange (ETDEWEB)

    Peter J. Tijrn

    2003-05-31

    This Final Report for Cooperative Agreement No. DE-FC22-95PC93052, the ''Development of Alternative Fuels and Chemicals from Synthesis Gas,'' was prepared by Air Products and Chemicals, Inc. (Air Products), and covers activities from 29 December 1994 through 31 July 2002. The overall objectives of this program were to investigate potential technologies for the conversion of synthesis gas (syngas), a mixture primarily of hydrogen (H{sub 2}) and carbon monoxide (CO), to oxygenated and hydrocarbon fuels and industrial chemicals, and to demonstrate the most promising technologies at the LaPorte, Texas Alternative Fuels Development Unit (AFDU). Laboratory work was performed by Air Products and a variety of subcontractors, and focused on the study of the kinetics of production of methanol and dimethyl ether (DME) from syngas, the production of DME using the Liquid Phase Dimethyl Ether (LPDME{trademark}) Process, the conversion of DME to fuels and chemicals, and the production of other higher value products from syngas. Four operating campaigns were performed at the AFDU during the performance period. Tests of the Liquid Phase Methanol (LPMEOH{trademark}) Process and the LPDME{trademark} Process were made to confirm results from the laboratory program and to allow for the study of the hydrodynamics of the slurry bubble column reactor (SBCR) at a significant engineering scale. Two campaigns demonstrated the conversion of syngas to hydrocarbon products via the slurry-phase Fischer-Tropsch (F-T) process. Other topics that were studied within this program include the economics of production of methyl tert-butyl ether (MTBE), the identification of trace components in coal-derived syngas and the means to economically remove these species, and the study of systems for separation of wax from catalyst in the F-T process. The work performed under this Cooperative Agreement has continued to promote the development of technologies that use clean syngas produced

  7. SYNTHESIS AND CHARACTERIZATION OF FULLY SOLUBLE POLYPHENYLENEVINYLENE

    Institute of Scientific and Technical Information of China (English)

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

    2000-01-01

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

  8. Synthesis and Characterization of Electrodeposited Nanocrystalline Nickel

    Institute of Scientific and Technical Information of China (English)

    DAI Pin-qiang; YU Hui, LI Qiang

    2004-01-01

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

  9. Synthesis and Characterization of Glassy Carbon Nanowires

    Directory of Open Access Journals (Sweden)

    C. M. Lentz

    2011-01-01

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

  10. PLLA-HA composites: Synthesis and characterization

    Science.gov (United States)

    Gonzalez, Gema; Albano, Carmen; Palacios, Jordana

    2012-07-01

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

  11. Synthesis and Characterization of Electrodeposited Nanocrystalline Nickel

    Institute of Scientific and Technical Information of China (English)

    DAIPin-qiang; YUHui; LIQiang

    2004-01-01

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

  12. Physical and chemical characterization of particles in producer gas

    DEFF Research Database (Denmark)

    Hindsgaul, Claus; Henriksen, Ulrik B.; Bentzen, Jens Dall;

    2000-01-01

    Particles in the gas from a two-stage (separate pyrolysis and gasification) down-draft biomass gasifier were collected and characterized. Their concentration, geometries and chemical compositions were investigated. Special attention was given to features suspected to harm internal combustion (IC...

  13. On the chemical characterization of colloid cyst contents

    NARCIS (Netherlands)

    Veerman, ECI; Go, KG; Molenaar, WM; Amerongen, AVN; Vissink, A

    1998-01-01

    Colloid cysts of the third ventricle have been investigated by chemical characterization of the cyst contents using ELISA with monoclonal antibodies for certain carbohydrate epitopes as well as a polyclonal antiserum against peptide domains, and immunohistochemistry on the cyst wall using the same a

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

    Science.gov (United States)

    Chu, Jin

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

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

    Science.gov (United States)

    Rami, Soukaina

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

  16. Synthesis and electrochemical characterization of substituted indolizine carboxylates

    Directory of Open Access Journals (Sweden)

    Soare Maria-Laura

    2013-01-01

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

  17. A Chemical Synthesis of Ferromagnetic Zn0.99Co0.01O Nano-Needles

    Institute of Scientific and Technical Information of China (English)

    BI Hong; CHEN Qian-Wang; YOU Feng-Yong; ZHOU Xiao-Li

    2006-01-01

    @@ Zn0.99Co0.01 O nano-needles are synthesized by using pure ZnO powder as the starting material via chemical reactions in ammonia aqueous solution. The nano-needles show the room-temperature ferromagnetism (RTFM) characterized by using a superconducting quantum interference device. Non-reductive chemical synthesis steps ensure to prevent forming Co-metal nanoclusters within the doped sample. All the results of thermal gravimetric analysis, Fourier transform infrared spectroscopy, x-ray diffraction and ultraviolet spectroscopy demonstrate that Co ions have doped into ZnO lattices and occupied some Zn sites without changing the wurtzite structure of ZnO lattices, and no potential second phase except for the doped Co ions substituting the Zn sites in ZnO lattice can account for the observed RTFM behaviour. Moreover, the synthesis process is of high reproducibility over 80% which is higher than that of commonly-used sol-gel method.

  18. Wet chemical synthesis of chitosan hydrogel-hydroxyapatite composite membranes for tissue engineering applications.

    Science.gov (United States)

    Madhumathi, K; Shalumon, K T; Rani, V V Divya; Tamura, H; Furuike, T; Selvamurugan, N; Nair, S V; Jayakumar, R

    2009-07-01

    Chitosan, a deacetylated derivative of chitin is a commonly studied biomaterial for tissue-engineering applications due to its biocompatibility, biodegradability, low toxicity, antibacterial activity, wound healing ability and haemostatic properties. However, chitosan has poor mechanical strength due to which its applications in orthopedics are limited. Hydroxyapatite (HAp) is a natural inorganic component of bone and teeth and has mechanical strength and osteoconductive property. In this work, HAp was deposited on the surface of chitosan hydrogel membranes by a wet chemical synthesis method by alternatively soaking the membranes in CaCl(2) (pH 7.4) and Na(2)HPO(4) solutions for different time intervals. These chitosan hydrogel-HAp membranes were characterized using SEM, AFM, EDS, FT-IR and XRD analyses. MTT assay was done to evaluate the biocompatibility of these membranes using MG-63 osteosarcoma cells. The biocompatibility studies suggest that chitosan hydrogel-HAp composite membranes can be useful for tissue-engineering applications.

  19. Chemical Synthesis and Functionalization of Cobalt Ferrite Nanoparticles with Oleic Acid and Citric Acid Encapsulation

    Directory of Open Access Journals (Sweden)

    Watawe Shrikant C.

    2015-01-01

    Full Text Available The functionalized nanoparticles have now a prime importance because of their wide ranging biomedical applications. The particles having size range 30nm-150nm are useful for cell wall interaction specifically the pinocytosis which takes place in all types of cells. The Cobalt ferrite nanoparticles have been synthesized using chemical co- precipitation route and the pH and temperature of the synthesis is controlled to obtain the optimum sized particles. The coating of Sodium Oleate and Citric acid was carried out in aqueous medium at room temperature. The characterization of coated and uncoated particles has been carried out using XRD and IR which confirm the ferrite structure formation. The TGA-DTA analysis shows the coating of magnetic particles. The SEM micrographs reveal the particle size, before and after coating to be in the range of 45 to 90 nm. The saturation magnetization is found to be 16.8 emu/gm.

  20. Synthesis and Electroluminescence Characterization of Cadmium Complex

    Directory of Open Access Journals (Sweden)

    Rahulkumar

    2011-01-01

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

  1. SYNTHESIS, CHARACTERIZATION AND BIOLOGICAL ACTIVITY OF POLYKETONES

    Institute of Scientific and Technical Information of China (English)

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

    2013-01-01

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

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

    CERN Document Server

    Torres, Tomas

    2013-01-01

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

  3. Synthesis and characterization of tetraethylammonium tetrachlorocobaltate crystals

    Indian Academy of Sciences (India)

    M A Kandhaswamy; V Srinivasan

    2002-02-01

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

  4. Synthesis and characterization of mesoporous hydrocracking catalysts

    Science.gov (United States)

    Munir, D.; Usman, M. R.

    2016-08-01

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

  5. Synthesis and characterization of magnetic nanoparticles

    Institute of Scientific and Technical Information of China (English)

    邱星屏

    2000-01-01

    Magnetic nanoparticles with average diameter in the range of 6.4-8.3 nm have been synthesized by a chemical co-precipi-tation of Fe(Ⅱ) and Fe(Ⅲ) salts in 1.5 M NH4OH solution.The size of the magenetic particles is dependent on both temperature and the ionic strength of the iron ion solutions. The magnetic particles formed at higher temperature or lower ionic strength were slightly larger than those formed at lower temperature or higher ionic strength respectively. In spite of the different reaction co nditions, all the resultant nanopar ticles are nearly spherical and have a similar crystalline structure. At300 K, such prepared nanoparticles are superparamagnetic. The saturation magnetizations for 7.8 and 6.4 nm particles are 71 and 63 emu/g respectively, which are only -20-30% less than the saturation magnetization (90 emu/g) of bulk Fe3O4. Our results indicated that a control of the reaction conditions could be used to tailor the size of magnetic nanoparticles in free precipita tion.

  6. SYNTHESIS AND CHARACTERIZATION OF PROTON CONDUCTORS

    Energy Technology Data Exchange (ETDEWEB)

    Brinkman, K.

    2010-02-18

    The morphological and electrical properties of yttrium (Y) and indium (In) doped barium cerate perovskites of the form BaIn{sub 0.3-x}Y{sub x}Ce{sub 0.7}O{sub 3-{delta}} (with x=0-0.3) prepared by a modified Pechini method were investigated as potential high temperature proton conductors with improved chemical stability. The sinterability increased with the increase of In-doping, and the perovskite phase was found in the BaIn{sub 0.3-x}Y{sub x}Ce{sub 0.7}O{sub 3-{delta}} solid solutions over the range 0 {le} x {le} 0.3. The conductivities decreased (from x to x, insert quantitative values) while the tolerance to wet CO{sub 2} improved for BaIn{sub 0.3-x}Y{sub x}Ce{sub 0.7}O{sub 3-{delta}} samples with an increase of In-doping.

  7. Synthesis of carbon nanotubes using the cobalt nanocatalyst by thermal chemical vapor deposition technique

    Energy Technology Data Exchange (ETDEWEB)

    Madani, S.S. [Department of Chemistry, Science and Research Branch, Islamic Azad University, Tehran (Iran, Islamic Republic of); Zare, K. [Department of Chemistry, Science and Research Branch, Islamic Azad University, Tehran (Iran, Islamic Republic of); Department of Chemistry, Shahid Beheshti University, Tehran (Iran, Islamic Republic of); Ghoranneviss, M. [Plasma Physics Research Center, Science and Research Branch, Islamic Azad University, Tehran (Iran, Islamic Republic of); Salar Elahi, A., E-mail: Salari_phy@yahoo.com [Plasma Physics Research Center, Science and Research Branch, Islamic Azad University, Tehran (Iran, Islamic Republic of)

    2015-11-05

    The three main synthesis methods of Carbon nanotubes (CNTs) are the arc discharge, the laser ablation and the chemical vapour deposition (CVD) with a special regard to the latter one. CNTs were produced on a silicon wafer by Thermal Chemical Vapor Deposition (TCVD) using acetylene as a carbon source, cobalt as a catalyst and ammonia as a reactive gas. The DC-sputtering system was used to prepare cobalt thin films on Si substrates. A series of experiments was carried out to investigate the effects of reaction temperature and deposition time on the synthesis of the nanotubes. The deposition time was selected as 15 and 25 min for all growth temperatures. Energy Dispersive X-ray (EDX) measurements were used to investigate the elemental composition of the Co nanocatalyst deposited on Si substrates. Atomic Force Microscopy (AFM) was used to characterize the surface topography of the Co nanocatalyst deposited on Si substrates. The as-grown CNTs were characterized under Field Emission Scanning Electron Microscopy (FESEM) to study the morphological properties of CNTs. Also, the grown CNTs have been investigated by High Resolution Transmission Electron Microscopy (HRTEM) and Raman spectroscopy. The results demonstrated that increasing the temperature leads to increasing the diameter of CNTs. The ideal reaction temperature was 850 °C and the deposition time was 15 min. - Graphical abstract: FESEM images of CNTs grown on the cobalt catalyst at growth temperatures of (a) 850 °C, (b) 900 °C, (c) 950 °C and (d) 1000 °C during the deposition time of 15 min. - Highlights: • Carbon nanotubes (CNTs) were produced on a silicon wafer by TCVD technique. • EDX and AFM were used to investigate the elemental composition and surface topography. • FESEM was used to study the morphological properties of CNTs. • The grown CNTs have been investigated by HRTEM and Raman spectroscopy.

  8. Synthesis and characterization of thermoplastic polyphenoxyquinoxalines

    Science.gov (United States)

    Erdem, Haci Bayram

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

  9. Synthesis and characterization of hematite nanopowders

    Science.gov (United States)

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

    2016-10-01

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

  10. Polypeptide Grafted Hyaluronan: Synthesis and Characterization

    Energy Technology Data Exchange (ETDEWEB)

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

    2010-01-01

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

  11. Synthesis and characterization of organosoluble aromatic copolyimids

    Institute of Scientific and Technical Information of China (English)

    YANG Jintian; HUANG Wei; ZHOU Yongfeng; YAN Deyue

    2007-01-01

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

  12. Synthesis of multiferroic Er-Fe-O thin films by atomic layer and chemical vapor deposition

    Energy Technology Data Exchange (ETDEWEB)

    Mantovan, R., E-mail: roberto.mantovan@mdm.imm.cnr.it; Vangelista, S.; Wiemer, C.; Lamperti, A.; Tallarida, G. [Laboratorio MDM IMM-CNR, I-20864 Agrate Brianza (MB) (Italy); Chikoidze, E.; Dumont, Y. [GEMaC, Université de Versailles St. Quentin en Yvelines-CNRS, Versailles (France); Fanciulli, M. [Laboratorio MDM IMM-CNR, I-20864 Agrate Brianza (MB) (Italy); Dipartimento di Scienza dei Materiali, Università di Milano Bicocca, Milano (Italy)

    2014-05-07

    R-Fe-O (R = rare earth) compounds have recently attracted high interest as potential new multiferroic materials. Here, we report a method based on the solid-state reaction between Er{sub 2}O{sub 3} and Fe layers, respectively grown by atomic layer deposition and chemical vapor deposition, to synthesize Er-Fe-O thin films. The reaction is induced by thermal annealing and evolution of the formed phases is followed by in situ grazing incidence X-ray diffraction. Dominant ErFeO{sub 3} and ErFe{sub 2}O{sub 4} phases develop following subsequent thermal annealing processes at 850 °C in air and N{sub 2}. Structural, chemical, and morphological characterization of the layers are conducted through X-ray diffraction and reflectivity, time-of-flight secondary ion-mass spectrometry, and atomic force microscopy. Magnetic properties are evaluated by magnetic force microscopy, conversion electron Mössbauer spectroscopy, and vibrating sample magnetometer, being consistent with the presence of the phases identified by X-ray diffraction. Our results constitute a first step toward the use of cost-effective chemical methods for the synthesis of this class of multiferroic thin films.

  13. Synthesis of multiferroic Er-Fe-O thin films by atomic layer and chemical vapor deposition

    Science.gov (United States)

    Mantovan, R.; Vangelista, S.; Wiemer, C.; Lamperti, A.; Tallarida, G.; Chikoidze, E.; Dumont, Y.; Fanciulli, M.

    2014-05-01

    R-Fe-O (R = rare earth) compounds have recently attracted high interest as potential new multiferroic materials. Here, we report a method based on the solid-state reaction between Er2O3 and Fe layers, respectively grown by atomic layer deposition and chemical vapor deposition, to synthesize Er-Fe-O thin films. The reaction is induced by thermal annealing and evolution of the formed phases is followed by in situ grazing incidence X-ray diffraction. Dominant ErFeO3 and ErFe2O4 phases develop following subsequent thermal annealing processes at 850 °C in air and N2. Structural, chemical, and morphological characterization of the layers are conducted through X-ray diffraction and reflectivity, time-of-flight secondary ion-mass spectrometry, and atomic force microscopy. Magnetic properties are evaluated by magnetic force microscopy, conversion electron Mössbauer spectroscopy, and vibrating sample magnetometer, being consistent with the presence of the phases identified by X-ray diffraction. Our results constitute a first step toward the use of cost-effective chemical methods for the synthesis of this class of multiferroic thin films.

  14. Synthesis and characterization of luminescence magnetic nanocomposite

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-01-01

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

  15. Facile Synthesis and Characterization of Two Dimensional Layered Tin Disulfide Nanowalls

    Science.gov (United States)

    Mutlu, Zafer; Shahrezaei, Sina; Temiz, Selcuk; Ozkan, Mihrimah; Ozkan, Cengiz S.

    2016-04-01

    Two dimensional layered metal chalcogenides, especially tin sulfides, have recently received great interest due to their enticing physical and chemical properties and hold promise for various applications. We report on synthesis of phase-pure two dimensional tin disulfide nanowalls by a facile vapor-phase synthesis method on insulator substrates such as silicon dioxide and magnesium oxide using tin dioxide and sulfur powders as precursors. The synthesized tin disulfide nanowalls have been characterized to study their fundamental properties by using various techniques such as scanning electron microscopy, x-ray diffraction, Raman spectroscopy, x-ray photoelectron spectroscopy, and ultraviolet photoelectron spectroscopy. The synthesized films have an open network structure constituted of very uniform interconnected nanowalls with high crystallinity.

  16. Zinc acetylacetonate hydrate adducted with nitrogen donor ligands: Synthesis, spectroscopic characterization, and thermal analysis

    Science.gov (United States)

    Brahma, Sanjaya; Shivashankar, S. A.

    2015-12-01

    We report synthesis, spectroscopic characterization, and thermal analysis of zinc acetylacetonate complex adducted by nitrogen donor ligands, such as pyridine, bipyridine, and phenanthroline. The pyridine adducted complex crystallizes to monoclinic crystal structure, whereas other two adducted complexes have orthorhombic structure. Addition of nitrogen donor ligands enhances the thermal property of these complexes as that with parent metal-organic complex. Zinc acetylacetonate adducted with pyridine shows much higher volatility (106 °C), decomposition temperature (202 °C) as that with zinc acetylacetonate (136 °C, 220 °C), and other adducted complexes. All the adducted complexes are thermally stable, highly volatile and are considered to be suitable precursors for metal organic chemical vapor deposition. The formation of these complexes is confirmed by powder X-ray diffraction, Fourier transform infrared spectroscopy, mass spectroscopy, and elemental analysis. The complexes are widely used as starting precursor materials for the synthesis of ZnO nanostructures by microwave irradiation assisted coating process.

  17. A new chalcone structure of (E)-1-(4-Bromophenyl)-3-(napthalen-2-yl)prop-2-en-1-one: Synthesis, structural characterizations, quantum chemical investigations and biological evaluations.

    Science.gov (United States)

    Thanigaimani, Kaliyaperumal; Arshad, Suhana; Khalib, Nuridayanti Che; Razak, Ibrahim Abdul; Arunagiri, C; Subashini, A; Sulaiman, Shaida Fariza; Hashim, Nurul Shafiqah; Ooi, Kheng Leong

    2015-01-01

    The structure of (E)-1-(4-Bromophenyl)-3-(napthalen-2-yl)prop-2-en-1-one (C19H13BrO) crystallized in the triclinic system of P-1 space group. The unit cell dimensions are: a=5.8944 (9)Å, b=7.8190 (12)Å, c=16.320 (2)Å, α=102.4364 (19)°, β=95.943 (2)°, γ=96.274 (2)° and Z=2. The physical properties of this compound was determined by the spectroscopic methods (FTIR and (1)H and (13)C NMR). Quantum chemical investigations have been employed to investigate the structural and spectral properties. The molecular structure, vibrational assignments, (1)H and (13)C NMR chemical shift values, non-linear optical (NLO) effect, HOMO-LUMO analysis and natural bonding orbital (NBO) analysis were calculated using HF and DFT/B3LYP methods with 6-311++G(d,p) basis set in the ground state. The results show that the theoretical calculation of the geometrical parameters, vibrational frequencies and chemical shifts are comparable with the experimental data. The crystal structure is influenced and stabilized by weak C-H⋯π interactions connecting the molecules into infinite supramolecular one dimensional ladder-like arrangement. Additionally, this compound is evaluated for their antibacterial activities against gram positive and gram negative strains using a micro dilution procedure and shows activities against a panel of microorganisms.

  18. Synthesis and characterization of LiFePO4 cathode preparation by low temperature method

    Science.gov (United States)

    Rajesh, Desapogu; Srinivas Naik, V.; Sunandana, C. S.

    2015-05-01

    We review in detail the physics and technology of the novel material LiFePO4, a potential cathode material for Li-ion batteries. In the present work, nano crystalline LiFePO4 film has been synthesized in both powder and thin film forms from a non-aqueous sol-gel synthesis route based on oxalates of Li and Fe (II). Ferrous oxalate has been synthesized indigenously using a ferrous sulphate based chemical reaction and characterized. Nano powders and thin films of LiFePO4 have been fabricated and coated on stainless steel substrates with the aim of device development in future. The material has been characterized extensively by XRD for crystal structure, FESEM for microstructure, EDS for elemental analysis and FTIR for the internal modes of phosphate ion. Fe3+ impurity characterization has been done by using ESR.

  19. Targeting deubiquitinases enabled by chemical synthesis of proteins.

    Science.gov (United States)

    Ohayon, Shimrit; Spasser, Liat; Aharoni, Amir; Brik, Ashraf

    2012-02-15

    Ubiquitination/ubiquitylation is involved in a wide range of cellular processes in eukaryotes, such as protein degradation and DNA repair. Ubiquitination is a reversible post-translational modification, with the removal of the ubiquitin (Ub) protein being catalyzed by a family of enzymes known as deubiquitinases (DUBs). Approximately 100 DUBs are encoded in the human genome and are involved in a variety of regulatory processes, such as cell-cycle progression, tissue development, and differentiation. DUBs were, moreover, found to be associated with several diseases and as such are emerging as potential therapeutic targets. Several directions have been pursued in the search for lead anti-DUB compounds. However, none of these strategies have delivered inhibitors reaching advanced clinical stages due to several challenges in the discovery process, such as the absence of a highly sensitive and practically available high-throughput screening assay. In this study, we report on the design and preparation of a FRET-based assay for DUBs based on the application of our recent chemical method for the synthesis of Ub bioconjugates. In the assay, the ubiquitinated peptide was specifically labeled with a pair of FRET labels and used to screen a library comprising 1000 compounds against UCH-L3. Such analysis identified a novel and potent inhibitor able to inhibit this DUB in time-dependent manner with k(inact) = 0.065 min(-1) and K(i) = 0.8 μM. Our assay, which was also found suitable for the UCH-L1 enzyme, should assist in the ongoing efforts targeting the various components of the ubiquitin system and studying the role of DUBs in health and disease.

  20. Exploring experimental fitness landscapes for chemical synthesis and property optimization.

    Science.gov (United States)

    Tibbetts, Katharine Moore; Feng, Xiao-Jiang; Rabitz, Herschel

    2017-02-08

    Optimization is a central goal in the chemical sciences, encompassing diverse objectives including synthesis yield, catalytic activity of a material, and binding efficiency of a molecule to a target protein. Considering the enormous size of chemical space and the expected large numbers of experiments necessary to search through it in any particular application, optimization in chemistry is surprisingly efficient. This good fortune has recently been explained by analysis of the fitness landscape, i.e., the functional relationship between a target objective J (e.g., percent yield, catalytic activity) and a suitable set of variables (e.g., resources such as reactant concentrations and processing conditions). Mathematical analysis has demonstrated that, upon satisfaction of reasonable physical assumptions, the fitness landscape contains no local sub-optimal "traps" that preclude identification of the globally best value of J, in a development called the "OptiChem" theorem. One of the key assumptions behind the theorem is that sufficient resources are available to achieve the posed optimization goal. This work assesses the validity of this assumption underlying the OptiChem theorem through examination of experimental data from the recent literature. In order to explore fitness landscapes in high dimensions where the landscape cannot be visualized, a high dimensional model representation (HDMR) of experimental data is used to construct a model landscape amenable to topology assessment via gradient algorithm search. This method is shown to correctly capture the trap-free topology of a four-dimensional landscape where the objective is to optimize the composition of a solid state material (subject to an elemental mole-fraction constraint) for catalytic activity towards the oxygen evolution reaction. Analysis of a six-dimensional landscape for the objective of maximizing the photoluminescence of rare-earth solid state materials subject to two elemental mole

  1. A Comprehensive Approach for Pectin Chemical and Functional Characterization

    DEFF Research Database (Denmark)

    de Sousa, António Felipe Gomes Teixeira

    In this work, a comprehensive approach for the chemical and functional analysis of pectin was used in order to relate the different extraction conditions used to the polymer structure and the final functional (mainly gelling) properties. A wide range of methods were utilized including chemical...... and chromatographic characterization methods (HPAEC and HPSEC), rheological measurements of elasticity, and biological epitopes detection using carbohydrate microarrays. The end product of this study is expected to contribute to the knowledge of pectin polymeric conformation and structure-function properties as well...

  2. Synthesis, characterization, and applications of nanocomposite membranes

    Science.gov (United States)

    Kizilel, Riza

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

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

    Science.gov (United States)

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

    2015-11-21

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

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

    Science.gov (United States)

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

    2017-04-01

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

  5. Flame synthesis and characterization of nanocrystalline titania powders

    Directory of Open Access Journals (Sweden)

    Bhaskaran Manjith Kumar

    2012-09-01

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

  6. Nepenthes khasiana mediated synthesis of stabilized gold nanoparticles: Characterization and biocompatibility studies.

    Science.gov (United States)

    Dhamecha, Dinesh; Jalalpure, Sunil; Jadhav, Kiran

    2016-01-01

    The current study summarizes a unique green process for the synthesis of gold nanoparticles by simple treatment of gold salts with aqueous extract of Nepenthes khasiana (NK)--a red listed medicinal plant and its characterization. Study on the effect of different process parameters like temperature, pH and stirring on surface and stability characteristics has been demonstrated. Formation of GNPs was visually observed by change in color from colorless to wine red and characterized by UV-Visible spectroscopy, FT-IR spectroscopy, Zetasizer, X-RD, ICP-AES, SEM-EDAX, AFM and TEM. In vitro stability studies of gold colloidal dispersion in various blood components suggest that, NK mediated GNPs exhibit remarkable in vitro stability in 2% bovine serum albumin, 2% human serum albumin (HSA), 0.2M histidine, and 0.2M cysteine but unstable in 5% NaCl solution and acidic pH. Biocompatibility of NK stabilized GNPs against normal mouse fibroblasts (L929) cell lines revealed nontoxic nature of GNPs and thus provides exceptional opportunities for their uses as nanomedicine for diagnosis and drug therapy. The role of antioxidant phytochemicals (flavonoids and polyphenols) of NK extract in synthesis of biocompatible and stabilized GNPs was demonstrated by estimating total flavonoid content, total phenolic content and total antioxidant capacity of extract before and after formation of GNPs. Fast and easy synthesis of biocompatible GNPs possesses unique physical and chemical features which serve as an advantage for its use in various biomedical applications. The overall approach designated in the present research investigation for the synthesis of GNPs is based on all 12 principles of green chemistry, in which no man-made chemical other than the gold chloride was used.

  7. Nanoscale Synthesis and Characterization Laboratory Annual Report 2007

    Energy Technology Data Exchange (ETDEWEB)

    Hamza, A V

    2008-04-07

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-09-25

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

  9. Material Synthesis and Characterization on Low-Dimensional Cobaltates

    Science.gov (United States)

    Sha, Hao

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

  10. Herbal Plant Synthesis of Antibacterial Silver Nanoparticles by Solanum trilobatum and Its Characterization

    Directory of Open Access Journals (Sweden)

    M. Vanaja

    2014-01-01

    Full Text Available Green synthesis method of nanomaterials is rapidly growing in the nanotechnology field; it replaces the use of toxic chemicals and time consumption. In this present investigation we report the green synthesis of silver nanoparticles (AgNPs by using the leaf extract of medicinally valuable plant Solanum trilobatum. The influence of physical and chemical parameters on the silver nanoparticle fabrication such as incubation time, silver nitrate concentration, pH, and temperature is also studied in this present context. The green synthesized silver nanoparticles were characterized by UV-vis spectroscopy, X-ray diffraction (XRD, scanning electron microscope (SEM, energy dispersive X-ray (EDX, and transmission electron microscope (TEM. The SEM and TEM confirm the synthesis of spherical shape of nanocrystalline particles with the size range of 2–10 nm. FTIR reveals that the carboxyl and amine groups may be involved in the reduction of silver ions to silver nanoparticles. Antibacterial activity of synthesized silver nanoparticles was done by agar well diffusion method against different pathogenic bacteria. The green synthesized silver nanoparticles can be used in the field of medicine, due to their high antibacterial activity.

  11. New Synthesis of TATB. Scaleup and Product Characterization

    Energy Technology Data Exchange (ETDEWEB)

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

    2000-03-15

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

  12. Synthesis and characterization of MWCNT/CdS nanocomposite

    Directory of Open Access Journals (Sweden)

    M R Khanlary

    2014-12-01

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

  13. Physical and chemical characterization of cerium(IV) oxide nanoparticles.

    Science.gov (United States)

    Cepriá, Gemma; Córdova, Walvin R; Céspedes, Oscar; Sánchez-García, Laura; Ferrer, Pilar; Gianolio, Diego; Castillo, Juan R

    2016-09-01

    Chemical composition, size and structure of the nanoparticle are required to describe nanoceria. Nanoparticles of similar size and Ce(III) content might exhibit different chemical behaviour due to their differences in structure. A simple and direct procedure based on affordable techniques for all the laboratories is presented in this paper. The combination of Raman and UV-vis spectroscopy and particle impact coulometry (PIC) allows the characterization of nanoceria of small size from 4 to 65 nm at a concentration from micromolar to nanomolar, a concentration range suitable for the analysis of lab-prepared or commercial nanoparticle suspensions, but too high for most analytical purposes aimed at nanoparticle monitoring. While the PIC limits of size detection are too high to observe small nanoparticles unless catalytic amplification is used, the method provides a simple means to study aggregation of nanoparticles in the media they are needed to be dispersed for each application. Raman spectroscopy provided information about structure of the nanoparticle, and UV-vis about their chemical behaviour against some common reducing and oxidizing agents. Graphical Abstract To characterize nanoceria it is necessary to provide information about the shape, size and structure of the nanoparticles as well as the chemical composition.

  14. Chemical characterization and genetic relationships among Ocimum basilicum L. cultivars.

    Science.gov (United States)

    Liber, Zlatko; Carović-Stanko, Klaudija; Politeo, Olivera; Strikić, Frane; Kolak, Ivan; Milos, Mladen; Satovic, Zlatko

    2011-11-01

    Twenty-seven Ocimum basilicum cultivars were subjected to a chemical characterization of essential oil components by gas chromatography/mass spectrometry (GC/MS) and a genetic characterization using the amplified fragment-length polymorphism (AFLP) technique. Since the same 27 accessions had previously been classified into six morphotypes, these analyses allowed us to make detailed comparisons of chemistry, genetics, and morphology. The chemical composition and morphology of the studied cultivars appeared to have a strong genetic component. The AFLP analysis revealed a distinction between the green and purple morphotypes. The green morphotypes predominantly utilized the terpene biosynthetic pathway, while most purple morphotypes primarily utilized the phenylpropene biosynthetic pathway. The GC/MS analysis led to identification of 87 volatiles. Among the 27 cultivars, five chemotypes were identified. A detailed characterization of the essential oil constituents indicated the existence of both specific combinations of compounds and 'private' compounds with the potential to be used in many aspects of human life. The established relationship between a genetic profile, chemical composition, and morphology represents an important step in future breeding programs and in the cultivation of this species.

  15. Physical and chemical characterization of bioaerosols - Implications for nucleation processes

    Science.gov (United States)

    Ariya, P. A.; Sun, J.; Eltouny, N. A.; Hudson, E. D.; Hayes, C. T.; Kos, G.

    The importance of organic compounds in the oxidative capacity of the atmosphere, and as cloud condensation and ice-forming nuclei, has been recognized for several decades. Organic compounds comprise a significant fraction of the suspended matter mass, leading to local (e.g. toxicity, health hazards) and global (e.g. climate change) impacts. The state of knowledge of the physical chemistry of organic aerosols has increased during the last few decades. However, due to their complex chemistry and the multifaceted processes in which they are involved, the importance of organic aerosols, particularly bioaerosols, in driving physical and chemical atmospheric processes is still very uncertain and poorly understood. Factors such as solubility, surface tension, chemical impurities, volatility, morphology, contact angle, deliquescence, wettability, and the oxidation process are pivotal in the understanding of the activation processes of cloud droplets, and their chemical structures, solubilities and even the molecular configuration of the microbial outer membrane, all impact ice and cloud nucleation processes in the atmosphere. The aim of this review paper is to assess the current state of knowledge regarding chemical and physical characterization of bioaerosols with a focus on those properties important in nucleation processes. We herein discuss the potential importance (or lack thereof) of physical and chemical properties of bioaerosols and illustrate how the knowledge of these properties can be employed to study nucleation processes using a modeling exercise. We also outline a list of major uncertainties due to a lack of understanding of the processes involved or lack of available data. We will also discuss key issues of atmospheric significance deserving future physical chemistry research in the fields of bioaerosol characterization and microphysics, as well as bioaerosol modeling. These fundamental questions are to be addressed prior to any definite conclusions on the

  16. Synthesis and characterization of Nd2O3 nanoparticles in a radiofrequency thermal plasma reactor

    Science.gov (United States)

    Dhamale, G. D.; Mathe, V. L.; Bhoraskar, S. V.; Sahasrabudhe, S. N.; Dhole, S. D.; Ghorui, S.

    2016-02-01

    The synthesis of nanocrystalline Nd2O3 through an inductively coupled radiofrequency thermal plasma route is reported. Unlike in conventional synthesis processes, plasma-synthesized nanoparticles are directly obtained in a stable hexagonal crystal structure with a faceted morphology. The synthesized nanoparticles are highly uniform with an average size around 20 nm. The nanoparticles are characterized in terms of phase formation, crystallinity, morphology, size distribution, nature of chemical bonds and post-synthesis environmental effects using standard characterization techniques. X-ray diffraction, transmission electron microscopy, and scanning electron microscopy are used for structural and morphological studies. The thermo-gravimetric technique, using a differential scanning calorimeter, is used to investigate the purity of phase. Fourier transform infrared spectroscopy is used to investigate the nature of existing bonds. The optical response of the nanoparticles is investigated through the electronic transition of Nd3+ ions in its crystalline structure via UV-visible spectroscopy. The presence of defect states and corresponding activation energies in the nanocrystalline Nd2O3 compared to those of the precursors are studied using thermoluminescence.

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

    Directory of Open Access Journals (Sweden)

    Aparecida M. Kawamoto

    2009-01-01

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

  18. Procafd: Computer Aided Tool for Synthesis-Design & Analysis of Chemical Process Flowsheets

    DEFF Research Database (Denmark)

    Kumar Tula, Anjan; Eden, Mario R.; Gani, Rafiqul

    2015-01-01

    In practice, chemical process synthesis-design involves identification of the processing route to reach a desired product from a specified set of raw materials, design of the operations involved in the processing route, the calculations of utility requirements, the calculations of waste...... are synthesized to form molecules in computer-aided molecular design (CAMD) techniques [4]. The main idea here was to apply the principle of group-contribution approach from chemical property estimation to the synthesis and design of chemical process flowsheets. That is, use process-groups representing different...... of mathematical programming techniques, (c) hybrid approach which combine two or more approaches. D’Anterroches [3] proposed a group contribution based hybrid approach to solve the synthesis-design problem where, chemical process flowsheets could be synthesized in the same way as atoms or groups of atoms...

  19. An efficient chemical synthesis of nicotinamide riboside (NAR) and analogues.

    Science.gov (United States)

    Tanimori, Shinji; Ohta, Takeshi; Kirihata, Mitsunori

    2002-04-22

    A simple and efficient synthesis of nicotinamide riboside (NAR) 1 and derivatives 4 and 5 via trimethylsilyl trifluoromethanesulfonate (TMSOTf)-mediated N-glycosilation followed by spontaneous deacetylation by treating with methanol is reported.

  20. Synthesis and characterization of aminated perfluoro polymer electrolytes

    Science.gov (United States)

    Page-Belknap, Zachary Stephan Glenn

    Polymer electrolytes have been developed for use in anion exchange membrane fuel cells for years. However, due to the highly corrosive environment within these fuel cells, poor chemical stability of the polymers and low ion conductivity have led to high development costs and thus prevention from widespread commercialization. The work in this study aims to provide a solution to these problems through the synthesis and characterization of a novel polymer electrolyte. The 800 EW 3M PFSA sulfonyl fluoride precursor was aminated with 3-(dimethylamino)-1-propylamine to yield a functional polymer electrolyte following quaternization, referred to in this work as PFSa-PTMa. 1 M solutions of LiPF6, HCL, KOH, NaOH, CsOH, NaHCO3 and Na2CO3 were used to exchange the polymer to alternate counterion forms. Chemical structure analysis was performed using both FT and ATR infrared spectroscopy to confirm sulfonyl fluoride replacement and the absence of sulfonic acid sites. Mechanical testing of the polymer, following counterion exchange with KOH, at saturated conditions and 60 ºC exhibited a tensile strength of 13 +/- 2.0 MPa, a Young's modulus of 87 +/- 16 MPa and a degree of elongation reaching 75% +/- 9.1%, which indicated no mechanical degradation following exposure to a highly basic environment. Conductivities of the polymer in the Cl- and OH- counterion forms at saturated conditions and 90 ºC were observed at 26 +/- 8.0 mS cm-1 and 1.1 +/- 0.1 mS cm-1, respectively. OH- conductivities were slightly above those observed for CO32- and HCO 3- counterions at the same conditions, 0.63 +/- 0.18 and 0.66 +/- 0.21 mS cm-1 respectively. The ion exchange capacity (IEC) of the polymer in the Cl- counterion form was measured via titration at 0.57 meq g-1 which correlated to 11.2 +/- 0.10 water molecules per ion site when at 60ºC and 95% relative humidity. The IEC of the polymer in the OH- counterion form following titration expressed nearly negligible charge density, less than 0.01 meq

  1. Synthesis and characterization of metal oxide nanorod brushes

    Indian Academy of Sciences (India)

    Kalyan Raidongia; M Eswaramoorthy

    2008-02-01

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

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

    Institute of Scientific and Technical Information of China (English)

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

    2005-01-01

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

  3. Controllable synthesis and characterization of alumina/MWNT nanocomposites

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-11-15

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

  4. Synthesis and characterization of the polyaniline dopant Schiff base

    Directory of Open Access Journals (Sweden)

    Mirian Y. Matsumoto

    2012-06-01

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

  5. SYNTHESIS AND CHARACTERIZATION OF HETEROAROMATIC POLYMERS CONTAINING PYRIDINE MOIETIES

    Institute of Scientific and Technical Information of China (English)

    LI Yanfeng; WANG Xiaolong; ZHANG Shujiang

    2006-01-01

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

  6. Schiff base functionalized Organopropylsilatranes: Synthesis and structural characterization

    Indian Academy of Sciences (India)

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

    2016-02-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1981-09-01

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

  8. Synthesis and characterization of boron nitrides nanotubes; Sintese e caracterizacao de nanotubos de nitreto de boro

    Energy Technology Data Exchange (ETDEWEB)

    Ferreira, T.H.; Sousa, E.M.B. [Centro de Desenvolvimento da Tecnologia Nuclear (CDTN/CNEN-MG), Belo Horizonte, MG (Brazil). Servico de Nanotecnologia

    2010-07-01

    This paper presents a new synthesis for the production of boron nitride nanotubes (BNNT) from boron powder, ammonium nitrate and hematite tube furnace CVD method. The samples were subjected to some characterization techniques as infrared spectroscopy, thermal analysis, X-ray diffraction and scanning electron microscopy and transmission. By analyzing the results can explain the chemical reactions involved in the process and confirm the formation of BNNT with several layers and about 30 nanometers in diameter. Due to excellent mechanical properties and its chemical and thermal stability this material is promising for various applications. However, BNNT has received much less attention than carbon nanotubes, it is because of great difficulty to synthesize appreciable quantities from the techniques currently known, and this is one of the main reasons this work.(author)

  9. Metal-organic frameworks: structure, properties, methods of synthesis and characterization

    Science.gov (United States)

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

    2016-03-01

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

  10. Synthesis and characterization of ZnO/ZnS/MoS2 core-shell nanowires

    Science.gov (United States)

    Butanovs, Edgars; Kuzmin, Alexei; Butikova, Jelena; Vlassov, Sergei; Polyakov, Boris

    2017-02-01

    Hybrid nanostructures composed of layered materials have recently attracted a lot of attention due to their promising electronic and catalytic properties. In this study, we describe a novel synthesis strategy of ZnO/ZnS/MoS2 core-shell nanowire growth using a three-step route. First, ZnO nanowire array was grown on a silicon wafer. Second, the sample was immersed in ammonium molybdate solution and dried. At the third step, the sample was annealed in a sulfur atmosphere at 700 °C. Two solid state chemical reactions occur simultaneously during the annealing and result in a formation of ZnS and MoS2 phases. Produced ZnO/ZnS/MoS2 core-shell nanowires were characterized by scanning and transmission electron microscopy, whereas their chemical composition was confirmed by selected area electron diffraction and micro-Raman spectroscopy.

  11. Synthesis and structural characterization of hexacoordinate silicon, germanium, and titanium complexes of the E. coli siderophore enterobactin.

    Science.gov (United States)

    Baramov, Todor; Keijzer, Karlijn; Irran, Elisabeth; Mösker, Eva; Baik, Mu-Hyun; Süssmuth, Roderich

    2013-08-01

    The E. coli siderophore enterobactin, one of the strongest Fe(III) chelators known to date, is also capable of binding Si(IV) under physiological conditions. We report on the synthesis and structural characterization of the tris(catecholate) Si(IV) -enterobactin complex and its Ge(IV) and Ti(IV) analogues. Comparative structural analysis, supported by quantum-chemical calculations, reveals the correlation between the ionic radius and the structural changes in enterobactin upon complexation.

  12. Chemical synthesis of Fe{sub 2}O{sub 3} thin films for supercapacitor application

    Energy Technology Data Exchange (ETDEWEB)

    Kulal, P.M.; Dubal, D.P.; Lokhande, C.D. [Holography and Material Research Laboratory, Department of Physics, Shivaji University, Kolhapur 416004, M.S. (India); Fulari, V.J., E-mail: vijayfulari@gmail.com [Holography and Material Research Laboratory, Department of Physics, Shivaji University, Kolhapur 416004, M.S. (India)

    2011-02-03

    Research highlights: > Simple chemical synthesis of Fe{sub 2}O{sub 3}. > Formation of amorphous and hydrous Fe{sub 2}O{sub 3}. > Potential candidate for supercapacitors. - Abstract: Fe{sub 2}O{sub 3} thin films have been prepared by novel chemical successive ionic layer adsorption and reaction (SILAR) method. Further these films were characterized for their structural, morphological and optical properties by means of X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectrum, scanning electron microscopy (SEM), wettability test and optical absorption studies. The XRD pattern showed that the Fe{sub 2}O{sub 3} films exhibit amorphous in nature. Formation of iron oxide compound was confirmed from FTIR studies. The optical absorption showed existence of direct optical band gap of energy 2.2 eV. Fe{sub 2}O{sub 3} film surface showed superhydrophilic nature with water contact angle less than 10{sup o}. The supercapacitive properties of Fe{sub 2}O{sub 3} thin film investigated in 1 M NaOH electrolyte showed supercapacitance of 178 F g{sup -1} at scan rate 5 mV/s.

  13. Keto-enol tautomerism of (E)-2-[(3,4-dimethylphenylimino)methyl]-4-nitrophenol: Synthesis, X-ray, FT-IR, UV-Vis, NMR and quantum chemical characterizations

    Science.gov (United States)

    Özek Yıldırım, Arzu; Yıldırım, M. Hakkı; Albayrak Kaştaş, Çiǧdem

    2017-01-01

    (E)-2-((3,4-dimethylphenylimino)methyl)-4-nitrophenol, which is a new Schiff base compound, was synthesized and characterized by experimental and computational methods. Molecular geometry, harmonic oscillator model of aromaticity (HOMA) indices, intra- and inter-molecular interactions in the crystal structure were determined by using single crystal X-ray diffraction technique. The optimized structures, which are obtained by Gaussian and Slater type orbitals, were compared to experimental structures to determine how much correlation is found between the experimental and the calculated properties. Intramolecular and hyperconjugative interactions of bonds have been found by Natural Bond Orbital analysis. The experimental infrared spectrum of the compound has been analyzed in detail by the calculated infrared spectra and Potential Energy Distribution analysis. To find out about the correlation between the solvent polarity and the enol-keto equilibrium, experimental UV-Visible spectra of the compound were obtained in benzene, CHCl3, EtOH and DMSO solvents. In these solvents, the UV-Vis spectra and relaxed potential energy surface scan (PES) calculations have been performed to get more insight into the equilibrium dynamics. Solvent effects in UV-Vis and PES calculations have been taken into account by using Polarizable Continuum Modelling method. 1H and 13C NMR spectra of the compound (in DMSO) were analyzed. The computational study of nonlinear optical properties shows that the compound can be used for the development of nonlinear optical materials.

  14. Synthesis, vapor growth, polymerization, and characterization of thin films of novel diacetylene derivatives of pyrrole. The use of computer modeling to predict chemical and optical properties of these diacetylenes and poly(diacetylenes)

    Science.gov (United States)

    Paley, M. S.; Frazier, D. O.; Abeledeyem, H.; Mcmanus, S. P.; Zutaut, S. E.

    1992-01-01

    In the present work two diacetylene derivatives of pyrrole which are predicted by semiempirical AM1 calculations to have very different properties, are synthesized; the polymerizability of these diacetylenes in the solid state is determined, and the results are compared to the computer predictions. Diacetylene 1 is novel in that the monomer is a liquid at room temperature; this may allow for the possibility of polymerization in the liquid state as well as the solid state. Thin poly(diacetylene) films are obtained from compound 1 by growing films of the monomer using vapor deposition and polymerizing with UV light; these films are then characterized. Interestingly, while the poly(diacetylene) from 1 does not possess good nonlinear optical properties, the monomer exhibits very good third-order effects (phase conjugation) in solution. Dilute acetone solutions of the monomer 1 give intensity-dependent refractive indices on the order of 10 exp -6 esu; these are 10 exp 6 times better than for CS2.

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

    Science.gov (United States)

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

    2015-04-01

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

  16. Mineralogical, chemical and toxicological characterization of urban air particles.

    Science.gov (United States)

    Čupr, Pavel; Flegrová, Zuzana; Franců, Juraj; Landlová, Linda; Klánová, Jana

    2013-04-01

    Systematic characterization of morphological, mineralogical, chemical and toxicological properties of various size fractions of the atmospheric particulate matter was a main focus of this study together with an assessment of the human health risks they pose. Even though near-ground atmospheric aerosols have been a subject of intensive research in recent years, data integrating chemical composition of particles and health risks are still scarce and the particle size aspect has not been properly addressed yet. Filling this gap, however, is necessary for reliable risk assessment. A high volume ambient air sampler equipped with a multi-stage cascade impactor was used for size specific particle collection, and all 6 fractions were a subject of detailed characterization of chemical (PAHs) and mineralogical composition of the particles, their mass size distribution and genotoxic potential of organic extracts. Finally, the risk level for inhalation exposure associated to the carcinogenic character of the studied PAHs has been assessed. The finest fraction (<0.45 μm) exhibited the highest mass, highest active surface, highest amount of associated PAHs and also highest direct and indirect genotoxic potentials in our model air sample. Risk assessment of inhalation scenario indicates the significant cancer risk values in PM 1.5 size fraction. This presented new approach proved to be a useful tool for human health risk assessment in the areas with significant levels of air dust concentration.

  17. 铝纳米粒子的液相化学还原法制备与表征%Solution Phase Chemical Reduction Synthesis and Characterization of Aluminum Nanoparticles

    Institute of Scientific and Technical Information of China (English)

    梁晓蕾; 刘才林; 任先艳; 杨海君; 王绵; 王用; 冉卷平

    2013-01-01

    分别以聚乙二醇(PEG)、聚乙二醇二甲醚(NHD)作为分散稳定剂,均三甲苯作溶剂,通过氢化铝锂还原氯化铝,用液相化学还原法制备铝纳米粒子(AINPs).采用激光粒度分析(LPSA)、透射电镜(TEM)、X射线能谱(EDS)、X射线衍射(XRD)、傅里叶红外光谱(FT-IR)、热重(TG)研究了AlNPs的粒度、形貌、尺寸、成分、结构特点及活性等.结果表明:PEG作分散稳定剂制备的PEG/AlNPs平均粒径可达67.7 nm,但分散性较差;当NHD与AlNPs的质量比为1.1∶1时,制得的NHD/AlNPs平均粒径为23.4 nm;AlNPs属立方晶系,表面包覆有分散稳定剂.%Alumnium nanoparticles (AlNPs) were synthesized via reduction of aluminium chloride anhydrous by lithium aluminium hydride with the solution-phase chemical reduction method,using polyethylene glycol (PEG) or polyethylene glycol dimethyl ether (NHD) as a dispersion stabilizer and mesitylene as solvent.The granularity,distribution,morphology,size,component,structure and activity of AlNPs were studied by laser particle size analyzer (LPSA),transmission electron microscopy (TEM),X-ray photoelectron spectroscopy (EDS),X-ray diffraction (XRD),Fourier transform infrared spectrum (FT-IR) and thermogravimetry (TG),respectively.Results show that the average particle size of PEG/AlNPs prepared by PEG as a dispersion stabilizer is 67.7 nm.The average particle size of NHD/AlNPs prepared by NHD/ AlNPs =1.1/1 (mass ratio) is 23.4 nm.AlNPs belong to cubic crystal system,and their surface are coated with dispersion stabilizer.

  18. Hydrothermal synthesis, structural and physico-chemical characterizations of two Nasicon phosphates: M{sub 0.50}{sup II}Ti{sub 2}(PO{sub 4}){sub 3} (M = Mn, Co)

    Energy Technology Data Exchange (ETDEWEB)

    Essehli, Rachid, E-mail: essehli_rachid@yahoo.fr [Laboratory of Mineral Solid and Analytical Chemistry ' LMSAC' , Department of Chemistry, Faculty of Sciences, University Mohamed I, Po. Box 717, 60000 Oujda (Morocco); Bali, Brahim El [Laboratory of Mineral Solid and Analytical Chemistry ' LMSAC' , Department of Chemistry, Faculty of Sciences, University Mohamed I, Po. Box 717, 60000 Oujda (Morocco); Benmokhtar, S. [Laboratoire de Chimie des Materiaux Solides (LCMS) Universite HassanII-Mohammedia, Faculte des Sciences Ben M' Sik, Departement de Chimie, Casablanca (Morocco); Fejfarova, Karla; Dusek, Michal [Institute of Physics, Na Slovance 2, 182 21 Praha 8 (Czech Republic)

    2009-07-01

    The family of titanium Nasicon-phosphates of generic formula M{sub 0.5}{sup II}Ti{sub 2}(PO{sub 4}){sub 3} has been revisited using hydrothermal techniques. Two phases have been synthesized: Mn{sub 0.5}{sup II}Ti{sub 2}(PO{sub 4}){sub 3} (MnTiP) and Co{sub 0.5}{sup II}Ti{sub 2}(PO{sub 4}){sub 3} (CoTiP). Single crystal diffraction studies show that they exhibit two different structural types. Mn{sub 0.5}{sup II}Ti{sub 2}(PO{sub 4}){sub 3} phosphate crystallizes in the R-3 space group, with the cell parameters a = 8.51300(10) A and c = 21.0083(3) A (V = 1318.52(3) A{sup 3} and Z = 6). The Co{sub 0.5}{sup II}Ti{sub 2}(PO{sub 4}){sub 3} phosphate crystallizes in the R-3c space group, with a = 8.4608(9) A and c = 21.174(2) A (V = 1312.7(2) A{sup 3} and Z = 6). These two compounds are clearly related to the parent Nasicon-type rhombohedral structure, which can be described using [Ti{sub 2}(PO{sub 4}){sub 3}] framework composed of two [TiO{sub 6}] octahedral interlinked via three [PO{sub 4}] tetrahedra. {sup 31}P magic-angle spinning nuclear magnetic resonance (MAS-NMR) data are presented as supporting data. Curie-Weiss-type behavior is observed in the magnetic susceptibility. The phases are also characterized by IR spectroscopy and UV-visible.

  19. Curdlan microspheres. Synthesis, characterization and interaction with proteins (enzymes, vaccines).

    Science.gov (United States)

    Mocanu, Georgeta; Mihai, Doina; Moscovici, Misu; Picton, Luc; LeCerf, Didier

    2009-04-01

    Microparticles of curdlan, synthesized through crosslinking with epichlorohydrin in organic suspension media, were chemically modified with the aim of introducing strongly and/or weakly acidic anionic and palmitoyl hydrophobic groups. Microparticles of both curdlan and curdlan derivatives were physico-chemically characterized. Study of the interaction with enzymes, such as lysozyme, and vaccines, such as tetanus anatoxin, showed a co-operative protein retention effect, induced by electrostatic and hydrophobic forces. The results of the in vitro release studies on support-protein complexes recommend them as potential controlled release systems.

  20. Synthesis, Spectral Characterization, and Antibacterial and Antifungal Studies of PANI/V2O5 Nanocomposites

    Directory of Open Access Journals (Sweden)

    Chakradhar Sridhar

    2016-01-01

    Full Text Available The present study deals with the synthesis and characterization of nanocrystalline vanadium pentoxide (V2O5 nanoparticles and their antibacterial and antifungal activity on Staphylococcus aureus and Aspergillus niger, respectively, by agar diffusion method. The metal oxide has been synthesized by employing the sol-gel method, polyaniline (PANI has been synthesized by chemical oxidation, and PANI/V2O5 composites have been synthesized by in situ polymerization method with different ratios (10, 20, 30, 40, and 50 weight% of V2O5 in PANI. The newly prepared composites were characterized by FTIR and powder X-ray diffraction (P-XRD techniques and are found to be formed of PANI/V2O5 nanocomposites, and also the compounds showed moderate antibacterial and antifungal activity.

  1. Synthesis and characterization of surfactant assisted Mn2+ doped ZnO nanocrystals

    Directory of Open Access Journals (Sweden)

    N. Shanmugam

    2016-09-01

    Full Text Available We report the synthesis and characterization of Mn doped ZnO nanocrystals, both in the free standing and PVP capped particle forms. The nanocrystals size could be controlled by capping them with polyvinylpyrollidone and was estimated by X-ray diffraction and transmission electron microscopy. The chemical compositions of the products were characterized by FT-IR spectroscopy. UV–Vis absorption spectroscopy measurements reveal that the capping of ZnO leads to blue shift due to quantum confinement effect. The morphology of the particles was evaluated by Scanning Electron Microscopy (SEM and Transmission Electron Microscopy (TEM. Both the Thermo Gravimetric Analysis (TGA and Differential Thermal Analysis (DTA curves of the ZnO show no further weight loss and thermal effect at a temperature above 510 °C.

  2. Eco-friendly green synthesis of silver nanoparticles using salmalia malabarica: synthesis, characterization, antimicrobial, and catalytic activity studies

    Science.gov (United States)

    Murali Krishna, I.; Bhagavanth Reddy, G.; Veerabhadram, G.; Madhusudhan, A.

    2016-06-01

    An economically viable and "green" process has been developed for the synthesis of silver nanoparticles (AgNPs) with an average size of 7 nm using non-toxic and renewable salmalia malabarica gum (SMG) as reducing and capping agent without using any chemical reducing agent. The effect of various parameters such as concentration of SMG and silver nitrate and reaction time for the synthesis of AgNPs was studied. The synthesized AgNPs are systematically characterized by UV/Vis spectroscopy, Fourier transform infrared spectroscopy, X-ray diffraction and Transmission electron microscopy. The resultant SMG-capped AgNPs are highly stable and had significant antibacterial action on both Escherichia coli ( E. coli) and Staphylococcus aureus ( S. aureus). The catalytic action of the SMG-capped AgNPs to initiate the reduction of 4-nitrophenol (4-NP) in the presence of NaBH4 has also been reported. The kinetics of the reaction was found to be of pseudo-first-order with respect to the 4-NP.

  3. Síntese de zeólitas a partir de cinza volante de caldeiras: caracterização física, química e mineralógica Synthesis of zeolites from boiler fly ash: physical, chemical and mineralogical characterization

    Directory of Open Access Journals (Sweden)

    C. A. F. Rocha Junior

    2012-03-01

    chemical, physical and mineralogical characterization methods were carried out: X-ray diffractometry, X-ray fluorescence, scanning electron microscopy, granulometric analysis, differential thermal and thermogravimetric analysis (DTA-TG. The analyses were carried out at the following conditions: 60, 100, 150 and 190 °C, Na2O/Al2O3 molar ratio of 5 and Si/Al molar ratio ranging from 2.12 to 15, and reaction time of 24 h. The results of the fly characterization demonstrate its enormous potential as raw material for the zeolite synthesis. SiO2 and Al2O3 represent more than 50% of its composition, mineralogical phases defined, low humidity content, low particle size (d90 < 10 µm, among others. Mineralogical analyses of the synthesized products showed the formation of some zeolite types, as follow: analcime, phillipsite, sodalite, zeolite P and tobermorite. The results show that the mixture fly ash-microsilica in these reaction conditions point to a promising material for zeolite synthesis.

  4. Synthesis and characterization of novel cellulose ether sulfates.

    Science.gov (United States)

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

    2016-05-20

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

  5. Chemical, Electrical and Thermal Characterization of Nanoceramic Silicon Carbide

    Science.gov (United States)

    Martin, Hervie; Abunaemeh, Malek; Smith, Cydale; Muntele, Claudiu; Budak, Satilmish; Ila, Daryush

    2009-03-01

    Silicon carbide (SiC) is a lightweight high bandgap semiconductor material that can maintain dimensional and chemical stability in adverse environments and very high temperatures. These properties make it suitable for high temperature thermoelectric converters. At the Center for Irradiaton of Materials (CIM) we design, manufacture and fabricate nanoceramic SiC, and perform electrical, thermal and chemical characterization of the material using particle induced X-ray emission (PIXE), Rutherford backscattering spectroscopy (RBS), Seebeck coefficient, electrical conductivity, and thermal conductivity measurements to calculate its efficiency as a thermoelectric generator. We are looking to compare the electrical and thermal properties of SiC ceramics with some other materials used for the same purposes.

  6. Characterization of iron-phosphate-silicate chemical garden structures.

    Science.gov (United States)

    Barge, Laura M; Doloboff, Ivria J; White, Lauren M; Stucky, Galen D; Russell, Michael J; Kanik, Isik

    2012-02-28

    Chemical gardens form when ferrous chloride hydrate seed crystals are added or concentrated solutions are injected into solutions of sodium silicate and potassium phosphate. Various precipitation morphologies are observed depending on silicate and phosphate concentrations, including hollow plumes, bulbs, and tubes. The growth of precipitates is controlled by the internal osmotic pressure, fluid buoyancy, and membrane strength. Additionally, rapid bubble-led growth is observed when silicate concentrations are high. ESEM/EDX analysis confirms compositional gradients within the membranes, and voltage measurements across the membranes during growth show a final potential of around 150-200 mV, indicating that electrochemical gradients are maintained across the membranes as growth proceeds. The characterization of chemical gardens formed with iron, silicate, and phosphate, three important components of an early earth prebiotic hydrothermal system, can help us understand the properties of analogous structures that likely formed at submarine alkaline hydrothermal vents in the Hadean-structures offering themselves as the hatchery of life.

  7. Chemical characterization of fingerprints from adults and children

    Energy Technology Data Exchange (ETDEWEB)

    Buchanan, M.V.; Asano, K. [Oak Ridge National Lab., TN (United States); Bohanon, A. [Knoxville Police Dept., TN (United States)

    1996-12-31

    Observation that children`s fingerprints disappear from surfaces more quickly than adults`, initiated a study to characterize the chemical components in fingerprints. Samples were obtained from about 50 individuals ranging in age from 3 to 64 by extracting chemicals from the fingertips using rubbing alcohol. Using combined gas chromatography/mass spectrometry, a wide range of compounds were identified. Samples from children contained higher levels of relatively volatile free fatty acids, while those from adults had higher levels of less volatile long chain esters of fatty acids. These esters are thought to originate from sebaceous glands located on the face and levels of these compounds increase substantially after puberty. Also, other compounds were observed that could be used to develop improved methods for fingerprint detection at a crime scene. Further, observation of specific compounds raises the possibility of being able to identify personal traits (gender, habits, diseases, etc. ) via analysis of components in fingerprints and/or skin.

  8. Chemical and Physicochemical Characterization of Winter Squash (Cucurbita moschata D.

    Directory of Open Access Journals (Sweden)

    Noelia JACOBO-VALENZUELA

    2011-05-01

    Full Text Available Winter squash cv ‘Cehualca’ (Cucurbita moschata Duchense is a seasonal crop that has been used as food and animal feed. The objective of the present study was to characterize physical, chemical and physicochemical properties of the winter squash cv ‘Cehualca’. Morphological, chemical and physicochemical analyses were performed, including fiber, carotenoids, phenolic and mineral contents in the winter squash. The morphological analysis showed that the squash ‘Cehualca’ did not have a homogeneous morphology. Data about their physical and physicochemical characteristics showed large variability. Also, high content of carotenoids and dietary fiber was observed in squash. The oil and total phenolic content was low in comparison with other fruits. The mineral content exceeded the values recommended to meet the nutritional needs of consumers, except for sodium (both in pulp and shell, potassium and magnesium in the shell.

  9. The chemical synthesis of porphobilinogen an important intermediate of the biosynthesis of the "pigments of life"

    OpenAIRE

    Bobal, Pavel; Neier, Reinhard

    2007-01-01

    Porphobilinogen is the second dedicated intermediate in the biosynthesis of «pigments of life». Only very few alkylpyrroles have been isolated from natural sources so far. The absence of stabilising substituents confers to porphobilinogen a high reactivity. The chemical synthesis of porphobilinogen had to take its sensitivity into account. The published synthesis of this unusual pyrrole are reviewed. The synthetic strategies used are analysed and compared with the biosynthesis.

  10. Physico-chemical characterizations of Cr doped persistent luminescence nanoparticles

    Science.gov (United States)

    Lecuyer, T.; Teston, E.; Maldiney, T.; Scherman, D.; Richard, C.

    2016-03-01

    Persistent luminescence nanoparticles have recently been proposed as innovative optical probes for small animal in vivo imaging. The main advantage of such probes is their ability to emit light for a long time after the end of their excitation, allowing in vivo imaging with low background. This work reports new information on the physico-chemical characterizations of Cr doped ZnGa2O4 nanoprobes in terms of synthetic procedure, luminescence properties as well as colloidal stabilities in different aqueous media and over the time.

  11. Metal oxide and mercuric sulfide nanoparticles synthesis and characterization

    Science.gov (United States)

    Xu, Xin

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

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

    Science.gov (United States)

    Asha, Goyal, Sneh Lata; Kishore, Nawal

    2016-05-01

    Polyaniline (PANI) and PANI /cobalt chloride composites were synthesized by in situ chemical oxidative polymerization of aniline with CoCl2.6H2O using ammonium peroxidisulphate as an oxidant. These composites were characterized by X-ray diffraction (XRD) and Scanning electron microscopy (SEM). The XRD study reveals that both PANI and composites are amorphous. The XRD and SEM results confirm the presence of cobalt chloride in the composites.

  13. Total synthesis approaches to natural product derivatives based on the combination of chemical synthesis and metabolic engineering.

    Science.gov (United States)

    Kirschning, Andreas; Taft, Florian; Knobloch, Tobias

    2007-10-21

    Secondary metabolites are an extremely diverse and important group of natural products with industrial and biomedical implications. Advances in metabolic engineering of both native and heterologous secondary metabolite producing organisms have allowed the directed synthesis of desired novel products by exploiting their biosynthetic potentials. Metabolic engineering utilises knowledge of cellular metabolism to alter biosynthetic pathways. An important technique that combines chemical synthesis with metabolic engineering is mutasynthesis (mutational biosynthesis; MBS), which advanced from precursor-directed biosynthesis (PDB). Both techniques are based on the cellular uptake of modified biosynthetic intermediates and their incorporation into complex secondary metabolites. Mutasynthesis utilises genetically engineered organisms in conjunction with feeding of chemically modified intermediates. From a synthetic chemist's point of view the concept of mutasynthesis is highly attractive, as the method combines chemical expertise with Nature's synthetic machinery and thus can be exploited to rapidly create small libraries of secondary metabolites. However, in each case, the method has to be critically compared with semi- and total synthesis in terms of practicability and efficiency. Recent developments in metabolic engineering promise to further broaden the scope of outsourcing chemically demanding steps to biological systems.

  14. Direct synthesis of nanocrystalline oxide powders by wet-chemical techniques

    Directory of Open Access Journals (Sweden)

    Vladimir V. Srdić

    2010-09-01

    Full Text Available In a recent period there is a great need for increasing the knowledge of tailoring the innovative procedures for the synthesis of electroceramic nanopowders and materials with improved quality for specific application. In order to produce electroceramics with desirable microstructure and properties, synthesis of stoichiometric, ultra-fine and agglomerate free powders with narrow size distributions is one of the most important steps. Within this scope, in the present paper we summarize our recent results on direct synthesis of some important perovskites and ferrites nanopowders by wet-chemical techniques.

  15. Solution-phase synthesis of inorganic nanostructures by chemical transformation from reactive templates

    Institute of Scientific and Technical Information of China (English)

    2010-01-01

    The solution-phase synthesis by chemical transformation from reactive templates has proved to be very effective in morphology-controlled synthesis of inorganic nanostructures. This review paper summarizes the recent progress in solution-phase synthesis of one-dimensional and hollow inorganic nanostructures via reactive templates, focusing on the approaches developed in our lab. The formation mechanisms based on reactive templates are discussed in depth to show the general concepts for the preparation processes. An outlook on the future development in this area is also presented.

  16. Molecular design, synthesis and evaluation of chemical biology tools

    NARCIS (Netherlands)

    Hoogenboom, Jorin

    2017-01-01

    Chapter 1 provides a perspective of synthetic organic chemistry as a discipline involved in the design, synthesis and evaluation of complex molecules. The reader is introduced with a brief history of synthetic organic chemistry, all the while dealing with different aspects of synthe

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

    Institute of Scientific and Technical Information of China (English)

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

    2006-01-01

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

  18. Advances in acrylic-alkyd hybrid synthesis and characterization

    Science.gov (United States)

    Dziczkowski, Jamie

    2008-10-01

    performance. Reversible-addition fragmentation polymerization techniques were employed to create a new class of acrylic-alkyd hybrid materials. Medium and long oil alkyds made from the monoglyceride process using soybean oil, glycerol, and phthalic anhydride were modified with a RAFT chain transfer agent. The alkyd macro-RAFT agents were reached by end-capping a medium oil soya-based alkyd with a carboxy-functional trithiocarbonate. The alkyd macro-RAFT agents were then used to create acrylic-alkyd block structures by polymerizing different acrylic monomers, including both acrylates and methacrylates in the presence of the macro-RAFT agent and 2, 2'-azobisisobutyronitrile (AIBN). Co-acrylic segments were reached by complete polymerization of one monomer followed by the addition of a second monomer and additional free radical initiator. The alkyds, macro-RAFT agents and, acrylic-alkyd blocks were characterized by size-exclusion chromatography (SEC), FTIR, and 1H-NMR. Pseudo-first-order kinetics behavior and conversion vs. molecular weight plots show that the RAFT-mediated reaction afforded a more controlled process for the synthesis of acrylated-alkyd materials. Preliminary coatings tests showed that material properties of acrylated-alkyds achieved by RAFT polymerization exhibit good overall coatings properties including adhesion, gloss, hardness, and impact resistance.

  19. Synthesis and Characterization of New Heterocyclic Liquid Crystals

    Directory of Open Access Journals (Sweden)

    D. Srividhya

    2009-01-01

    Full Text Available This investigation enumerates the synthesis and mesomorphic properties of 1,2,3-triazole containing azobenzene liquid crystals. In these liquid crystals the methylene chain length at non polar end was varied from six to ten carbons to investigate the association properties of non polar chain on the melt. The compound was designed to have a polar ether chain at the other side of the molecule adjacent to the triazole ring and synthesized to enhance the dipolar interactions. These alterations in chemical structure produce two series of new liquid crystalline compounds with each series containing five variations in the methylene chain. The structure of the target compounds and the intermediates were confirmed by the 1H NMR, 13C NMR and IR spectral techniques. Polarized microscopic studies revealed that all the compounds in the series exhibited enantiotropic liquid crystalline properties. This was further confirmed using differential scanning calorimetric experiments. The energy minimized structure supports the mesogenic behavior of the structure.

  20. Synthesis and characterization of a nanocrystalline diamond aerogel.

    Science.gov (United States)

    Pauzauskie, Peter J; Crowhurst, Jonathan C; Worsley, Marcus A; Laurence, Ted A; Kilcoyne, A L David; Wang, Yinmin; Willey, Trevor M; Visbeck, Kenneth S; Fakra, Sirine C; Evans, William J; Zaug, Joseph M; Satcher, Joe H

    2011-05-24

    Aerogel materials have myriad scientific and technological applications due to their large intrinsic surface areas and ultralow densities. However, creating a nanodiamond aerogel matrix has remained an outstanding and intriguing challenge. Here we report the high-pressure, high-temperature synthesis of a diamond aerogel from an amorphous carbon aerogel precursor using a laser-heated diamond anvil cell. Neon is used as a chemically inert, near-hydrostatic pressure medium that prevents collapse of the aerogel under pressure by conformally filling the aerogel's void volume. Electron and X-ray spectromicroscopy confirm the aerogel morphology and composition of the nanodiamond matrix. Time-resolved photoluminescence measurements of recovered material reveal the formation of both nitrogen- and silicon- vacancy point-defects, suggesting a broad range of applications for this nanocrystalline diamond aerogel.

  1. Synthesis and characterization of a nanocrystalline diamond aerogel

    Energy Technology Data Exchange (ETDEWEB)

    Pauzauskie, Peter J.; Crowhurst, Jonathan C.; Worsley, Marcus A.; Laurence, Ted A.; Kilcoyne, A. L. David; Wang, Yinmin; Willey, Trevor M.; Visbeck, Kenneth S.; Fakra, Sirine C.; Evans, William J.; Zaug, Joseph M.; Satcher, Jr., Joe H.

    2011-07-06

    Aerogel materials have myriad scientific and technological applications due to their large intrinsic surface areas and ultralow densities. However, creating a nanodiamond aerogel matrix has remained an outstanding and intriguing challenge. Here we report the high-pressure, high-temperature synthesis of a diamond aerogel from an amorphous carbon aerogel precursor using a laser-heated diamond anvil cell. Neon is used as a chemically inert, near-hydrostatic pressure medium that prevents collapse of the aerogel under pressure by conformally filling the aerogel's void volume. Electron and X-ray spectromicroscopy confirm the aerogel morphology and composition of the nanodiamond matrix. Time-resolved photoluminescence measurements of recovered material reveal the formation of both nitrogen- and silicon- vacancy point-defects, suggesting a broad range of applications for this nanocrystalline diamond aerogel.

  2. Synthesis and characterization of vanadiumoxidecatalysts supported on copper orthophosphates

    Science.gov (United States)

    Ouchabi, M.; Baalala, M.; Elaissi, A.; Loulidi, I.; Bensitel, M.

    2017-03-01

    Synthesis of a pure copper orthophosphate (CuP) prepared by Coprecipitation, and CuP modified by impregnation of vanadium (2-12 wt % of V2O5) have been carried out. The solids obtained were investigated as synthesized or after calcination by various physico-chemical techniques such as X-Ray Diffraction (XRD), Infrared Spectroscopy (IR), Thermogravimetric analysis (TGA), and differential thermal analysis (DTA). The results revealed that the solids V/CuP consisted of copper orthophosphate Cu3(PO4)2 as major phases, together with V2O5 as minor phase. The diffraction lines of V2O5 increase by increasing the vanadium content.

  3. Synthesis and characterization of mixed melilite-type oxides

    Science.gov (United States)

    Granata, V.; Ubaldini, A.; Fittipaldi, R.; Rocco, L.; Pace, S.; Vecchione, A.

    2017-01-01

    The melilite-type oxides are potential targets for exploring interesting magnetic and electronic properties as well as multiferroicity and magnetoelectric effects. Polycrystalline samples of Ba2Cu1-xMnxGe2O7 have been synthesized by solid state reaction method. The morphology and chemical composition of the samples have been investigated by scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS). By using powder X-ray diffraction, the phase composition of the synthesized compounds and the evolution of their crystallographic axes as a function of the doping have been systematically studied. The synthesis of the polycrystalline compounds reported in this work is a prerequisite for the growth of high quality single crystals of mixed melilite-type oxides essential for the investigations of the complex magnetic phase diagram of these non-centrosymmetric systems.

  4. Total Chemical Synthesis,Assembly of Human Torque Teno Virus Genome

    Institute of Scientific and Technical Information of China (English)

    Zheng Hou; Gengfu Xiao

    2011-01-01

    Torque teno virus(TTV)is a nonenveloped virus containing a single-stranded,circular DNA genome of approximately 3.8kb.We completely synthesized the 3808 nucleotides of the TTV(SANBAN isolate)genome,which contains a hairpin structure and a GC-rich region.More than 100 overlapping oligonucleotides were chemically synthesized and assembled by polymerise chain assembly reaction(PCA),and the synthesis was completed with splicing by overlap extension(SOEing).This study establishes the methodological basis of the chemical synthesis of a viral genome for use as a live attenuated vaccine or gene therapy vector.

  5. Review on palladium-containing perovskites: synthesis, physico-chemical properties and applications in catalysis.

    Science.gov (United States)

    Essoumhi, Abdellatif; El Kazzouli, Saïd; Bousmina, Mosto

    2014-02-01

    This review reports on the recent advances in the synthesis and physico-chemical properties of palladium-containing perovskites. Initially, the perovskite structure is briefly reviewed, then palladium-containing perovskites synthesis and physico-chemical properties are detailed. The applications of palladium-containing perovskites in catalysis; namely, NO reduction, methane combustion, methanol as well as ethanol oxidation, are briefly highlighted. The involvement and the important contribution of palladium-containing perovskites in cross-coupling reactions, especially Suzuki-Miyaura, Sonogashira, Ulmann and Grignard, are discussed.

  6. Studies on solid phase synthesis,characterization and fluorescent property of the new rare earth complexes

    Directory of Open Access Journals (Sweden)

    Jianwei SHI

    2015-04-01

    Full Text Available Rare earth-β-diketone ligand complex luminescent material has stable chemical properties and excellent luminous property. Using europium oxide and (γ-NTA as raw materials, novel rare earth-β-dione complexes are synthesized by solid state coordination chemistry. The synthesis temperature and milling time are discussed for optimization. Experimental results show that the suitable reaction situation is at 50 ℃ and 20 h for solid-phase synthesis. The compositions and structures of the complexes are characterized by means of elemental analysis, UV-Vis and FTIR methods, and the phase stability of the complex is determined by using TG-DTA technique. It is proved that preparation of waterless binary rare earth complexes by the solid phase reaction method results in a higher product yield. The fluorescence spectra show that between Eu (Ⅲ and γ-NTA, there exists efficient energy transfer, and the rare earth complexes synthesis is an excellent red bright light-emitting material with excellent UV excited luminescence properties.

  7. Green Synthesis and Characterization of Palladium Nanoparticles Using Origanum vulgare L. Extract and Their Catalytic Activity

    Directory of Open Access Journals (Sweden)

    Mohammed Rafi Shaik

    2017-01-01

    Full Text Available The synthesis of Palladium (Pd nanoparticles by green methods has attracted remarkable attention in recent years because of its superiority above chemical approaches, owing to its low cost and ecological compatibility. In this present work, we describe a facile and environmentally friendly synthesis of Pd nanoparticles (Pd NPs using an aqueous extract of aerial parts of Origanum vulgare L. (OV as a bioreductant. This plant is available in many parts of the world as well as in Saudi Arabia and is known to be a rich source of phenolic components, a feature we fruitfully utilized in the synthesis of Pd NPs, using various concentrations of plant extracts. Moreover, the OV extract phytomolecules are not only accountable for the reduction and progression of nanoparticles, but they also act as stabilizing agents, which was confirmed by several characterization methods. The as-synthesized Pd nanoparticles (Pd NPs were analyzed using ultraviolet-visible spectroscopy (UV-Vis, Fourier-transform infrared spectroscopy (FT-IR, X-ray diffraction (XRD, transmission electron microscopy (TEM, energy-dispersive X-ray spectroscopy (EDX, and thermal gravimetric analysis (TGA. Further, FT-IR study has proven that the OV not merely represents a bioreductant but also functionalizes the nanoparticles. Furthermore, the green synthesized metallic Pd NPs were successfully applied as catalysts for selective oxidation of alcohols.

  8. AB-stacked multilayer graphene synthesized via chemical vapor deposition: a characterization by hot carrier transport.

    Science.gov (United States)

    Diaz-Pinto, Carlos; De, Debtanu; Hadjiev, Viktor G; Peng, Haibing

    2012-02-28

    We report the synthesis of AB-stacked multilayer graphene via ambient pressure chemical vapor deposition on Cu foils and demonstrate a method to construct suspended multilayer graphene devices. In four-terminal geometry, such devices were characterized by hot carrier transport at temperatures down to 240 mK and in magnetic fields up to 14 T. The differential conductance (dI/dV) shows a characteristic dip at longitudinal voltage bias V = 0 at low temperatures, indicating the presence of hot electron effect due to a weak electron-phonon coupling. Under magnetic fields, the magnitude of the dI/dV dip diminishes through the enhanced intra-Landau level cyclotron phonon scattering. Our results provide new perspectives in obtaining and understanding AB-stacked multilayer graphene, important for future graphene-based applications.

  9. Characterization of members to stellar kinematic groups using chemical tagging

    Science.gov (United States)

    Tabernero, H. M.

    2014-10-01

    In this thesis we have characterized more than one thousand late-type stars. For this characterization we have been making use of high resolution spectroscopy (R > 40,000) taken in different spectrographs, HERMES at the Mercator telescope in La Palma, FOCES in the 2.2m telescope at Calar Alto, the Coudé-Echelle spectrograph at 2 m-the Alfred- Jensch-Teleskop in Tautenburg, and UVES at the Very Large Telescope in La Silla. Stellar spectroscopy, in particular at high-resolution, is a modern tool that allows us to extract a lot of information of a given star. In particular, we have obtained their atmospheric parameters, namely: effective temperature (Teff), surface gravity (log g), microturbulent velocity (ξ), and iron abundance ([Fe/H], used as a metallicity proxy). An automatic code (StePar) has been developed. This code allows to derive stellar atmospheric parameters (Teff , log g, ξ, and [Fe/H]) only in a few minutes. Also, with these parameters at hand we have derived chemical abundances for 20 different chemical elements: Na, Mg, Al, Si, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Y, Zr, Ba, Ce, and Nd, which offer many or at least some isolated transitions in the wavelength range of the spectra taken with these spectrographs. This work comprises two publications in Astronomy & Astrophysics. The first one is about chemical tagging applied to the Hyades SC (see Chapter 2 or Tabernero et al. 2012). The second paper is a in-depth study of the chemical composition of candidate members to the Ursa Major MG (see Chapter 3 or Tabernero et al. 2015). Additionally there is another chapter that comprises the analysis of Galactic stars within the GAIA ESO Survey stars (GES, Gilmore et al. 2012; Randich & Gilmore 2013) whose data have contributed to the publication of some release (Lanzafame et al. 2014; Smiljanic et al. 2014) and science papers (Jofre et al. 2014; Sousa et al. 2014; Spina et al. 2014a,b) that made use the survey results. The two papers included in

  10. Catalytic synthesis of sulfated polysaccharides I: Characterization of chemical structure.

    Science.gov (United States)

    Wang, Junlong; Yang, Wen; Yang, Ting; Zhang, Xiaonuo; Zuo, Yuan; Tian, Jia; Yao, Jian; Zhang, Ji; Lei, Ziqiang

    2015-03-01

    In the present study, sulfated derivatives of Artemisia sphaerocephala polysaccharide (SASP) with high degree of substitution (DS) were synthesized by using 4-dimethylaminopyridine (DMAP)/dimethylcyclohexylcarbodiimide (DCC) as catalyst in homogeneous conditions. It was found that DMAP/DCC showed marked improvement in DS of sulfated samples. Compared to sulfated derivatives without catalyst, the DS of SASP increased from 0.91 to 1.28 with an increment in dosage of DMAP from 0 to 10 mg. The influence of DMAP/DCC on the DS of sulfated derivatives was depended on the content of DMAP. The effect of DMAP might be due to its strong coordination to the hydroxy group. The results of FT-IR and X-ray photoelectron spectroscopy (XPS) indicated that SO3- group (S6+, binding energy of 172.3 eV) was widely present in sulfated polysaccharide molecules. 13C NMR results indicated that C-6 substitution was predominant for sulfated polysaccharide when compared with other positions. In the sulfation reaction, a sharp decrease in MW was observed. DMAP/DCC was an effective catalyst system in sulfated modification of polysaccharide.

  11. Recent Applications of Alkene Metathesis in Fine Chemical Synthesis

    Science.gov (United States)

    Bicchielli, Dario; Borguet, Yannick; Delaude, Lionel; Demonceau, Albert; Dragutan, Ileana; Dragutan, Valerian; Jossifov, Christo; Kalinova, Radostina; Nicks, François; Sauvage, Xavier

    During the last decade or so, the emergence of the metathesis reaction in organic synthesis has revolutionised the strategies used for the construction of complex molecular structures. Olefin metathesis is indeed particularly suited for the construction of small open-chain molecules and macrocycles using crossmetathesis and ring-closing metathesis, respectively. These reactions serve, inter alia, as key steps in the synthesis of various agrochemicals and pharmaceuticals such as macrocyclic peptides, cyclic sulfonamides, novel macrolides, or insect pheromones. The present chapter is aiming at illustrating the great synthetic potential of metathesis reactions. Shortcomings, such as the control of olefin geometry and the unpredictable effect of substituents on the reacting olefins, will also be addressed. Examples to be presented include epothilones, amphidinolides, spirofungin A, and archazolid. Synthetic approaches involving silicon-tethered ring-closing metathesis, relay ring-closing metathesis, sequential reactions, domino as well as tandem metathesis reactions will also be illustrated.

  12. A new antiproliferative noscapine analogue: chemical synthesis and biological evaluation

    OpenAIRE

    Ghaly, Peter E.; Abou El-Magd, Rabab M.; Churchill, Cassandra D. M.; Tuszynski, Jack A.; West, F. G.

    2016-01-01

    Noscapine, a naturally occurring opium alkaloid, is a widely used antitussive medication. Noscapine has low toxicity and recently it was also found to possess cytotoxic activity which led to the development of many noscapine analogues. In this paper we report on the synthesis and testing of a novel noscapine analogue. Cytotoxicity was assessed by MTT colorimetric assay using SKBR-3 and paclitaxel-resistant SKBR-3 breast cancer cell lines using different concentrations for both noscapine and t...

  13. Technology Evaluation Workshop Report for Tank Waste Chemical Characterization

    Energy Technology Data Exchange (ETDEWEB)

    Eberlein, S.J.

    1994-04-01

    A Tank Waste Chemical Characterization Technology Evaluation Workshop was held August 24--26, 1993. The workshop was intended to identify and evaluate technologies appropriate for the in situ and hot cell characterization of the chemical composition of Hanford waste tank materials. The participants were asked to identify technologies that show applicability to the needs and good prospects for deployment in the hot cell or tanks. They were also asked to identify the tasks required to pursue the development of specific technologies to deployment readiness. This report describes the findings of the workshop. Three focus areas were identified for detailed discussion: (1) elemental analysis, (2) molecular analysis, and (3) gas analysis. The technologies were restricted to those which do not require sample preparation. Attachment 1 contains the final workshop agenda and a complete list of attendees. An information package (Attachment 2) was provided to all participants in advance to provide information about the Hanford tank environment, needs, current characterization practices, potential deployment approaches, and the evaluation procedure. The participants also received a summary of potential technologies (Attachment 3). The workshop opened with a plenary session, describing the background and issues in more detail. Copies of these presentations are contained in Attachments 4, 5 and 6. This session was followed by breakout sessions in each of the three focus areas. The workshop closed with a plenary session where each focus group presented its findings. This report summarizes the findings of each of the focus groups. The evaluation criteria and information about specific technologies are tabulated at the end of each section in the report. The detailed notes from each focus group are contained in Attachments 7, 8 and 9.

  14. Nanomechanical characterization of chemical interaction between gold nanoparticles and chemical functional groups

    Science.gov (United States)

    Lee, Gyudo; Lee, Hyungbeen; Nam, Kihwan; Han, Jae-Hee; Yang, Jaemoon; Lee, Sang Woo; Yoon, Dae Sung; Eom, Kilho; Kwon, Taeyun

    2012-10-01

    We report on how to quantify the binding affinity between a nanoparticle and chemical functional group using various experimental methods such as cantilever assay, PeakForce quantitative nanomechanical property mapping, and lateral force microscopy. For the immobilization of Au nanoparticles (AuNPs) onto a microscale silicon substrate, we have considered two different chemical functional molecules of amine and catecholamine (here, dopamine was used). It is found that catecholamine-modified surface is more effective for the functionalization of AuNPs onto the surface than the amine-modified surface, which has been shown from our various experiments. The dimensionless parameter (i.e., ratio of binding affinity) introduced in this work from such experiments is useful in quantitatively depicting such binding affinity, indicating that the binding affinity and stability between AuNPs and catecholamine is approximately 1.5 times stronger than that between amine and AuNPs. Our study sheds light on the experiment-based quantitative characterization of the binding affinity between nanomaterial and chemical groups, which will eventually provide an insight into how to effectively design the functional material using chemical groups.

  15. Nanomechanical characterization of chemical interaction between gold nanoparticles and chemical functional groups.

    Science.gov (United States)

    Lee, Gyudo; Lee, Hyungbeen; Nam, Kihwan; Han, Jae-Hee; Yang, Jaemoon; Lee, Sang Woo; Yoon, Dae Sung; Eom, Kilho; Kwon, Taeyun

    2012-10-31

    We report on how to quantify the binding affinity between a nanoparticle and chemical functional group using various experimental methods such as cantilever assay, PeakForce quantitative nanomechanical property mapping, and lateral force microscopy. For the immobilization of Au nanoparticles (AuNPs) onto a microscale silicon substrate, we have considered two different chemical functional molecules of amine and catecholamine (here, dopamine was used). It is found that catecholamine-modified surface is more effective for the functionalization of AuNPs onto the surface than the amine-modified surface, which has been shown from our various experiments. The dimensionless parameter (i.e., ratio of binding affinity) introduced in this work from such experiments is useful in quantitatively depicting such binding affinity, indicating that the binding affinity and stability between AuNPs and catecholamine is approximately 1.5 times stronger than that between amine and AuNPs. Our study sheds light on the experiment-based quantitative characterization of the binding affinity between nanomaterial and chemical groups, which will eventually provide an insight into how to effectively design the functional material using chemical groups.

  16. Synthesis of nanostructured framework of novel ZnBaO2 nanopowder via wet chemical approach and hepatocytotoxicity response

    Science.gov (United States)

    Athar, Taimur; Vishwakarma, Sandeep Kumar; Alabass, Razzaq; Alqaralosy, Ahmed; Khan, Aleem Ahmed

    2016-08-01

    Wet synthetic process is an effective and facile method at low cost, environmentally benign process for easy scaling-up and then used for fabrication of multi-utility devices. Self-assembling of nanobrick leads to architecture framework with new functional properties which help to make its vast applications as nanodevices with their intrinsic shape, size and functional properties. The bimetallic oxide nanostructure with phase structure was characterized by FTIR, UV-visible electronic absorption, XRD, thermal studies, SEM, TEM, DLS and fluorescence. Nanocrystalline ZnBaO2 powder can be used due to its chemical stability and excellent transmission in the visible region. It was observed that the annealing rate plays an important role to redefine the structural and other physicochemical properties which finally help to change gel into crystalline functional properties with porosity. Wet chemical approach can be used for the synthesis of other metal oxide nanopowders which can be easily scale up for production level. Along with synthesis and characterization, we also assessed biological responses of human hepatocytes exposed to ZnBaO2 nanopowder. Cell membrane permeability and ammonia detoxification were investigated against various concentrations of nanoparticles on in vitro cultured hepatocytes. Our results suggest that low concentrations (<40 μg/ml) of ZnBaO2 nanopowder have no cytotoxic effect on hepatocytes viability, proliferation and detoxification, whereas concentrations above 40 μg/ml depict significant toxicity on cells.

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

    Science.gov (United States)

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

    2016-03-01

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

  18. Synthesis, Characterization, and Secondary Structure Determination of a Silk-Inspired, Self-Assembling Peptide: A Laboratory Exercise for Organic and Biochemistry Courses

    Science.gov (United States)

    Albin, Tyler J.; Fry, Melany M.; Murphy, Amanda R.

    2014-01-01

    This laboratory experiment gives upper-division organic or biochemistry undergraduate students a comprehensive look at the synthesis, chemical characterization, self-assembly, and secondary structure determination of small, N-acylated peptides inspired by the protein structure of silkworm silk. All experiments can be completed in one 4 h lab…

  19. “Miswak” Based Green Synthesis of Silver Nanoparticles: Evaluation and Comparison of Their Microbicidal Activities with the Chemical Synthesis

    Directory of Open Access Journals (Sweden)

    Mohammed Rafi Shaik

    2016-11-01

    Full Text Available Microbicidal potential of silver nanoparticles (Ag-NPs can be drastically improved by improving their solubility or wettability in the aqueous medium. In the present study, we report the synthesis of both green and chemical synthesis of Ag-NPs, and evaluate the effect of the dispersion qualities of as-prepared Ag-NPs from both methods on their antimicrobial activities. The green synthesis of Ag-NPs is carried out by using an aqueous solution of readily available Salvadora persica L. root extract (RE as a bioreductant. The formation of highly crystalline Ag-NPs was established by various analytical and microscopic techniques. The rich phenolic contents of S. persica L. RE (Miswak not only promoted the reduction and formation of NPs but they also facilitated the stabilization of the Ag-NPs, which was established by Fourier transform infrared spectroscopy (FT-IR analysis. Furthermore, the influence of the volume of the RE on the size and the dispersion qualities of the NPs was also evaluated. It was revealed that with increasing the volume of RE the size of the NPs was deteriorated, whereas at lower concentrations of RE smaller size and less aggregated NPs were obtained. During this study, the antimicrobial activities of both chemically and green synthesized Ag-NPs, along with the aqueous RE of S. persica L., were evaluated against various microorganisms. It was observed that the green synthesized Ag-NPs exhibit comparable or slightly higher antibacterial activities than the chemically obtained Ag-NPs.

  20. Synthesis and Characterization of Plant based Polythiophene Copolymers for Light Harvesting Applications

    Science.gov (United States)

    Kodithuwakku, Udari; Malavi Arachchi, Prashantha; Ratnaweera, Dilru

    Polythiophenes became more attractive in diverse applications due to some of their inherent properties including thermal and environmental stability as well as optical and electronic conductive properties. Commonly thiophene monomers are obtained from byproducts of crude oils. The current study discuss for the first time the synthesis and characterization of light harvesting polythiophenes copolymers from thiophene derivatives extracted from Tagetes species. There were mainly two thiophenes derivatives, 5-(3-buten-1-ynyl)-2, 2-bithienyl and 2, 2', 5, 2''-terthienyl (terthiophene), in the roots of the plant. Chemical oxidative radical polymerization was followed during the synthesis of copolymers with various block compositions of plant based terthiophenes and 3-hexyl terthiophenes. Structural characterization of the synthetic products was done using FTIR, NMR, Uv-vis, XRD and DSC techniques. Polythiophene homopolymers obtained from plant based terthiophenes have limited processability of solar cells due to poor solubility in common organic solvents. A significant solubility improvement was observed with copolymers having minor contributions of 3-hexylthiophenes. Research Grants, University of Sri Jayewardenepura, Sri Lanka.

  1. Nanoscale zero-valent metals: a review of synthesis, characterization, and applications to environmental remediation.

    Science.gov (United States)

    Li, Lingyun; Hu, Jiwei; Shi, Xuedan; Fan, Mingyi; Luo, Jin; Wei, Xionghui

    2016-09-01

    Engineered nanoscale zero-valent metals (NZVMs) representing the forefront of technologies have been considered as promising materials for environmental remediation and antimicrobial effect, due to their high reducibility and strong adsorption capability. This review is focused on the methodology for synthesis of bare NZVMs, supported NZVMs, modified NZVMs, and bimetallic systems with both traditional and green methods. Recent studies have demonstrated that self-assembly methods can play an important role for obtaining ordered, controllable, and tunable NZVMs. In addition to common characterization methods, the state-of-the-art methods have been developed to obtain the properties of NZVMs (e.g., granularity, size distribution, specific surface area, shape, crystal form, and chemical bond) with the resolution down to subnanometer scale. These methods include spherical aberration corrected scanning transmission electron microscopy (Cs-corrected STEM), electron energy-loss spectroscopy (EELS), and near edge X-ray absorption fine structure (NEXAFS). A growing body of experimental data has proven that nanoscale zero-valent iron (NZVI) is highly effective and versatile. This article discusses the applications of NZVMs to treatment of heavy metals, halogenated organic compounds, polycyclic aromatic hydrocarbons, nutrients, radioelements, and microorganisms, using both ex situ and in situ methods. Furthermore, this paper briefly describes the ecotoxicological effects for NZVMs and the research prospects related to their synthesis, modification, characterization, and applications.

  2. A Comparison between Chemical Synthesis Magnetite Nanoparticles and Biosynthesis Magnetite

    OpenAIRE

    2014-01-01

    The preparation of Fe3O4 from ferrous salt by air in alkaline aqueous solution at various temperatures was proposed. The synthetic magnetites have different particle size distributions. We studied the properties of the magnetite prepared by chemical methods compared with magnetotactic bacterial nanoparticles. The results show that crystallite size, morphology, and particle size distribution of chemically prepared magnetite at 293 K are similar to biosynthesis of magnetite. The new preparation...

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

    Directory of Open Access Journals (Sweden)

    Selinay Y. Erişkin

    2014-01-01

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

  4. Nanoscale Synthesis and Characterization Laboratory Annual Report 2005

    Energy Technology Data Exchange (ETDEWEB)

    Hamza, A V; Lesuer, D R

    2006-01-03

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

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

    Directory of Open Access Journals (Sweden)

    Magdalena Zarzecka-Napierala

    2007-12-01

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

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

    Institute of Scientific and Technical Information of China (English)

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

    2000-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Antonio L. Doadrio

    2002-07-01

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

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

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

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

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

    Institute of Scientific and Technical Information of China (English)

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

    2002-01-01

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

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

    Institute of Scientific and Technical Information of China (English)

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

    2007-01-01

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

  11. Synthesis and characterization of carbon cryogel/zeolite composites

    Directory of Open Access Journals (Sweden)

    Biljana Babić

    2011-06-01

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

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

    Science.gov (United States)

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

    2017-01-17

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

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

    Science.gov (United States)

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

    2012-10-15

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

  14. Phosphorus-containing cyclodextrins. Characteristics of the synthesis and chemical behaviour

    Science.gov (United States)

    Grachev, M. K.

    2013-11-01

    Published data on the preparation of phosphorus-containing cyclodextrins are summarized. It is demonstrated that some significant features of their synthesis and chemical behaviour are caused by specific supramolecular interactions involving the inner chiral cavity of cyclodextrins capable of incorporating various guests, which often leads to alteration of customary routes of chemical transformations. The possibilities of practical applications of phosphorus-containing cyclodextrins are briefly analyzed. The bibliography includes 89 references.

  15. Synthesis mechanism of sono-chemically prepared mesoporous ZnS nanoparticles

    Science.gov (United States)

    Motejadded Emrooz, H. B.; Jalaly, M.

    2017-03-01

    The mechanism of sono-chemically synthesized mesoporous ZnS nanoparticles has been investigated. ZnS nanoparticles were synthesized with a facile and quick method. The sonication process was carried out for several times up to 60 min. The synthesized particles have been characterized with scanning electron microscopy, transmission electron microscopy, high resolution x-ray diffraction, UV–visible technique, diffuse reflectance spectroscopy, Brunauer–Emmett–Teller and Fourier transformation infrared spectroscopy. Based on x-ray diffraction patterns, crystallite size and lattice strain increase with sonication time. Adsorption–desorption results showed that applying the sono-chemistry synthesizing method in the aqueous atmosphere will cause a mesoporous structure. The obtained specific surface area of the synthesized mesoporous ZnS nanoparticles varied from 53 to 58 m2 · g‑1. Also the surface areas created from the porosity of the particles varied from 27 to 29 m2 · g‑1. Regarding these results, the mechanism of porosity formation during synthesis of nanoparticles has been explained. Photocatalytic behavior of the synthesized particles has been investigated for degradation of methylene blue from aqueous solution. Factors affecting this behavior have been discussed and it was found that interaction between opposing factors caused the specimen synthesized with 40 min sonication time has the best methylene blue degradation efficiency.

  16. Synthesis of mono and multidomain YIG particles by chemical coprecipitation or ceramic procedure

    Energy Technology Data Exchange (ETDEWEB)

    Fernandez-Garcia, L. [Departamento de Materiales Nanoestructurados, Centro de Investigacion en Nanomateriales y Nanotecnologia (CINN), Principado de Asturias - Consejo superior de Investigaciones Cientificas (CSIC) - Universidad de Oviedo - UO, Parque Tecnologico de Asturias, 33428 Llanera, Asturias (Spain); Suarez, M., E-mail: m.suarez@cinn.e [Departamento de Materiales Nanoestructurados, Centro de Investigacion en Nanomateriales y Nanotecnologia (CINN), Principado de Asturias - Consejo superior de Investigaciones Cientificas (CSIC) - Universidad de Oviedo - UO, Parque Tecnologico de Asturias, 33428 Llanera, Asturias (Spain); Menendez, J.L. [Departamento de Materiales Nanoestructurados, Centro de Investigacion en Nanomateriales y Nanotecnologia (CINN), Principado de Asturias - Consejo superior de Investigaciones Cientificas (CSIC) - Universidad de Oviedo -UO, Parque Tecnologico de Asturias, 33428 Llanera, Asturias (Spain)

    2010-04-09

    Yttrium iron garnet powders have been synthesized by chemical coprecipitation using two different precursors, nitrates and chlorides, and by an oxides mixture route. It is shown that depending on the precursors and synthesis conditions used pure yttrium iron garnet powders can be obtained with a mono or multidomain magnetic behaviour. The yttrium iron garnet crystalline structure, as studied by Raman spectroscopy, was already formed after calcination at temperatures as low as 800 {sup o}C when the nitrate precursors were used. However, calcination temperatures of up to 1100 {sup o}C were required to obtain yttrium iron garnet powders when the precursors were chlorides or when the oxides mixture route was chosen. The saturation magnetization of the powders correlates well with the structural characterization: when nitrate precursors were used, the saturation magnetization was already close to the bulk value, 26.8 emu/cm{sup 3}, after calcination at 800 {sup o}C. However, the saturation magnetization of the powders obtained by the chlorides and oxides mixture routes was close to zero up to calcination temperatures of 1100 {sup o}C. Finally, both the chlorides and the oxides mixture routes yield multidomain micron sized yttrium iron garnet powders, whereas the nitrates route led to monodomain submicron sized powders.

  17. Synthesis of monolayer hexagonal boron nitride on Cu foil using chemical vapor deposition.

    Science.gov (United States)

    Kim, Ki Kang; Hsu, Allen; Jia, Xiaoting; Kim, Soo Min; Shi, Yumeng; Hofmann, Mario; Nezich, Daniel; Rodriguez-Nieva, Joaquin F; Dresselhaus, Mildred; Palacios, Tomas; Kong, Jing

    2012-01-11

    Hexagonal boron nitride (h-BN) is very attractive for many applications, particularly, as protective coating, dielectric layer/substrate, transparent membrane, or deep ultraviolet emitter. In this work, we carried out a detailed investigation of h-BN synthesis on Cu substrate using chemical vapor deposition (CVD) with two heating zones under low pressure (LP). Previous atmospheric pressure (AP) CVD syntheses were only able to obtain few layer h-BN without a good control on the number of layers. In contrast, under LPCVD growth, monolayer h-BN was synthesized and time-dependent growth was investigated. It was also observed that the morphology of the Cu surface affects the location and density of the h-BN nucleation. Ammonia borane is used as a BN precursor, which is easily accessible and more stable under ambient conditions than borazine. The h-BN films are characterized by atomic force microscopy, transmission electron microscopy, and electron energy loss spectroscopy analyses. Our results suggest that the growth here occurs via surface-mediated growth, which is similar to graphene growth on Cu under low pressure. These atomically thin layers are particularly attractive for use as atomic membranes or dielectric layers/substrates for graphene devices.

  18. Physico-Chemical and In-vitro Microbial Studies of Newly Synthesis Organometallic Complexes

    Directory of Open Access Journals (Sweden)

    Isam Hussain Al-Karkhi

    2014-05-01

    Full Text Available Drugs normally synthesized to use as medication to treat diseases like cancer and microbial infections, these synthesized drugs were interested more than naturally-derived drugs which have been shows low activity or not as efficient against diseases. A new ligand 3-methylbenzyl (2Z-2-[1-(pyridin-4-ylethylidene]hydrazine carbodithioate (PE3MBC and its Cd(II, Cu(II, Co(II and Zn(II metal complexes. The new ligand and metal complexes were characterized via various physico-chemical and spectroscopic techniques. Cd(II complex show more activity against microbes and against cancer cell line MCF-7, while other complexes does not shows activity like cadmium complex, all the complexes does not shows any activity against MDAMB-231 cell line. The fatal of the cancer and the microbes cell was due to inhibition of DNA synthesis which was probably due to chelating with metals complexes, or could be referred to lipophilicity, presence of hydrophobic moiety in the complex molecule, also could be due to steric effects and electronic effects.

  19. Synthesis of advanced chemically bonded ceramics for solidification of radioactive wastes

    Energy Technology Data Exchange (ETDEWEB)

    Seneda, Jose A.; Dellamano, Jose C.; Queiroz, Carlos A.S.; Genova, Luis A.; Rocha, Soraya M.R. da; Vicente, Roberto, E-mail: jaseneda@ipen.b, E-mail: jcdellam@ipen.b, E-mail: cqueiroz@ipen.b, E-mail: lgenova@ipen.b, E-mail: smrrocha@ipen.b, E-mail: rvicente@ipen.b [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

    2011-07-01

    This paper presents the results of a preliminary study on the synthesis of advanced chemically bounded ceramics for use to immobilize radioactive wastes. A monolithic, crystalline, ceramic-like material, in the form of MgKPO{sub 4}.6H{sub 2}O, is obtained by reaction of magnesium oxide with potassium monophosphate, at room temperature. The thermodynamics of the reaction indicates the need of a previous treatment of the MgO above 1200 deg C to avoid the formation of magnesium phosphate salts, as revealed by thermogravimetric analysis and X-ray diffraction. The different crystalline phases and microstructure of reaction products are analyzed by X-ray diffraction and scanning electron microscopy, indicating that the material has the characteristics of a matrix for immobilization of radioactive waste. Results obtained thus far indicate the possibility of using this material to replace Portland cement in waste immobilization, offsetting the higher cost of raw material input with a larger fraction of waste in the waste form. More research on characterization of the waste form with mechanical strength tests of specimens incorporating varying waste compositions, and on the leaching potential of the material for a series of radioactive as well hazardous industrial wastes is being planned. (author)

  20. Synthesis of Copper Nanoparticles in Ethylene Glycol by Chemical Reduction with Vanadium (+2 Salts

    Directory of Open Access Journals (Sweden)

    Andrea Pietro Reverberi

    2016-09-01

    Full Text Available Copper nanoparticles have been synthesized in ethylene glycol (EG using copper sulphate as a precursor and vanadium sulfate as an atypical reductant being active at room temperature. We have described a technique for a relatively simple preparation of such a reagent, which has been electrolytically produced without using standard procedures requiring an inert atmosphere and a mercury cathode. Several stabilizing agents have been tested and cationic capping agents have been discarded owing to the formation of complex compounds with copper ions leading to insoluble phases contaminating the metallic nanoparticles. The elemental copper nanoparticles, stabilized with polyvinylpyrrolidone (PVP and sodium dodecyl sulphate (SDS, have been characterized for composition by energy dispersive X-ray spectroscopy (EDS, and for size by dynamic light scattering (DLS, and transmission electron microscopy (TEM, giving a size distribution in the range of 40–50 nm for both stabilizing agents. From a methodological point of view, the process described here may represent an alternative to other wet-chemical techniques for metal nanoparticle synthesis in non-aqueous media based on conventional organic or inorganic reductants.

  1. Interdisciplinary Learning for Chemical Engineering Students from Organic Chemistry Synthesis Lab to Reactor Design to Separation

    Science.gov (United States)

    Armstrong, Matt; Comitz, Richard L.; Biaglow, Andrew; Lachance, Russ; Sloop, Joseph

    2008-01-01

    A novel approach to the Chemical Engineering curriculum sequence of courses at West Point enabled our students to experience a much more realistic design process, which more closely replicated a real world scenario. Students conduct the synthesis in the organic chemistry lab, then conduct computer modeling of the reaction with ChemCad and…

  2. A wet-chemical approach to perovskite and fluorite-type nanoceramics: synthesis and processing

    NARCIS (Netherlands)

    Veldhuis, Sjoerd Antonius

    2015-01-01

    In thesis the low-temperature, wet-chemical approach to various functional inorganic oxide materials is described. The main focus of this research is to control the material’s synthesis from liquid precursor to metal oxide powder or thin film; while understanding its formation mechanism. In addition

  3. Modeling and Experimental Studies on Phase and Chemical Equilibria in High-Pressure Methanol Synthesis

    NARCIS (Netherlands)

    van Bennekom, Joost G.; Winkelman, Jozef G. M.; Venderbosch, Robertus H.; Nieland, Sebastiaan D. G. B.; Heeres, Hero J.

    2012-01-01

    A solution method was developed to calculate the simultaneous phase and chemical equilibria in high-pressure methanol synthesis (P = 20 MPa, 463

  4. Synthesis of chemicals and polymers: towards cleaner processes and atom economy, session 5

    Energy Technology Data Exchange (ETDEWEB)

    Razavi, A.; Thivolle-Cazat, J.; Hutchings, G.; Murata, K.; Leininger, S.; Sorokin, A.; Angelis, A. de; Apesteguia, C.I.; Mayoral, J.A.; Hardacre, C.; Jeon, J.; Tominaga, K.; Plasseraud, L.; Kervennal, J.; Souza, R.F. de; Ciardelli, F.; Dominguez, J.M.

    2004-07-01

    The abstracts of all the presentations (1 plenary session, 2 keynotes, 16 oral communications, 151 posters) of the thematic session 5 'synthesis of chemicals and polymers: towards cleaner processes and atom economy' are gathered in the CD-Rom of the conference. (O.M.)

  5. The Use of Aryl Hydrazide Linkers for the Solid Phase Synthesis of Chemically Modified Peptides

    Energy Technology Data Exchange (ETDEWEB)

    Woo, Y; Mitchell, A R; Camarero, J A

    2006-11-03

    Since Merrifield introduced the concept of solid phase synthesis in 1963 for the rapid preparation of peptides, a large variety of different supports and resin-linkers have been developed that improve the efficiency of peptide assembly and expand the myriad of synthetically feasible peptides. The aryl hydrazide is one of the most useful resin-linkers for the synthesis of chemically modified peptides. This linker is completely stable during Boc- and Fmoc-based solid phase synthesis and yet it can be cleaved under very mild oxidative conditions. The present article reviews the use of this valuable linker for the rapid and efficient synthesis of C-terminal modified peptides, head-to-tail cyclic peptides and lipidated peptides.

  6. Synthesis and characterization of powders calcium phosphate for biomedical applications

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira, D.M.P. de; Prants, W.T.; Camargo, N.H.A.; Gemelli, E., E-mail: daniellapinheiro@gmail.com, E-mail: w_prants@hotmail.com, E-mail: dem2nhac@joinville.udesc.br, E-mail: dma2ec@joinville.udesc.br [Universidade do Estado de Santa Catarina (UDESC), Joinville, SC (Brazil). Centro de Ciencias Tecnologicas

    2009-07-01

    Scientists of different areas research the bioceramics as new materials to substitute parts of the human body. The bioceramics of the calcium phosphate have the advantage present similar chemical composition to the structure of the bony apatite of the human skeleton. In this study, calcium phosphate powder was synthesized chemically using the solution of phosphorus pentoxide (P{sub 2}O{sub 5}) and calcium oxide (CaO) necessary for molar Ca/P =1.67. These works aim the study of different thermal treatments, physics and of the microstructure properties. For characterization the bony matrix were used the techniques of: X-ray diffraction (DRX); Scanning Electronic Microscopy (SEM) and Differential Scanning Calorimetry (DSC). (author)

  7. Temperature buffer test. Hydro-mechanical and chemical/ mineralogical characterizations

    Energy Technology Data Exchange (ETDEWEB)

    Aakesson, Mattias; Olsson, Siv; Dueck, Ann; Nilsson, Ulf; Karnland, Ola [Clay Technology AB, Lund (Sweden); Kiviranta, Leena; Kumpulainen, Sirpa [BandTech Oy, Helsinki (Finland); Linden, Johan [Aabo Akademi, Aabo (Finland)

    2012-01-15

    The Temperature Buffer Test (TBT) is a joint project between SKB/ANDRA and supported by ENRESA (modeling) and DBE (instrumentation), which aims at improving the understanding and to model the thermo-hydro-mechanical behavior of buffers made of swelling clay submitted to high temperatures (over 100 deg C) during the water saturation process. The test has been carried out in a KBS-3 deposition hole at Aspo HRL. It was installed during the spring of 2003. Two steel heaters (3 m long, 0.6 m diameter) and two buffer arrangements have been investigated: the lower heater was surrounded by rings of compacted Wyoming bentonite only, whereas the upper heater was surrounded by a composite barrier, with a sand shield between the heater and the bentonite. The test was dismantled and sampled during the winter of 2009/2010. This report presents the hydro-mechanical and chemical/mineralogical characterization program which was launched subsequent to the dismantling operation. The main goal has been to investigate if any significant differences could be observed between material from the field experiment and the reference material. The field samples were mainly taken from Ring 4 (located at the mid-section around the lower heater), in which the temperature in the innermost part reached 155 deg C. The following hydro-mechanical properties have been determined for the material (test technique within brackets): hydraulic conductivity (swelling pressure device), swelling pressure (swelling pressure device), unconfined compression strength (mechanical press), shear strength (triaxial cell) and retention properties (jar method). The following chemical/mineralogical properties (methods within brackets) were determined: anion analysis of water leachates (IC), chemical composition (ICP/AES+MS, EGA), cation exchange capacity (CEC, Cu-trien method) and exchangeable cations (exchange with NH4, ICPAES), mineralogical composition (XRD and FTIR), element distribution and microstructure (SEM and

  8. STM CONTROL OF CHEMICAL REACTIONS: Single-Molecule Synthesis

    Science.gov (United States)

    Hla, Saw-Wai; Rieder, Karl-Heinz

    2003-10-01

    The fascinating advances in single atom/molecule manipulation with a scanning tunneling microscope (STM) tip allow scientists to fabricate atomic-scale structures or to probe chemical and physical properties of matters at an atomic level. Owing to these advances, it has become possible for the basic chemical reaction steps, such as dissociation, diffusion, adsorption, readsorption, and bond-formation processes, to be performed by using the STM tip. Complete sequences of chemical reactions are able to induce at a single-molecule level. New molecules can be constructed from the basic molecular building blocks on a one-molecule-at-a-time basis by using a variety of STM manipulation schemes in a systematic step-by-step manner. These achievements open up entirely new opportunities in nanochemistry and nanochemical technology. In this review, various STM manipulation techniques useful in the single-molecule reaction process are reviewed, and their impact on the future of nanoscience and technology are discussed.

  9. Trophic magnification of organic chemicals: A global synthesis

    Science.gov (United States)

    Walters, David; Jardine, T.D.; Cade, Brian S.; Kidd, K.A.; Muir, D.C.G.; Leipzig-Scott, Peter C.

    2016-01-01

    Production of organic chemicals (OCs) is increasing exponentially, and some OCs biomagnify through food webs to potentially toxic levels. Biomagnification under field conditions is best described by trophic magnification factors (TMFs; per trophic level change in log-concentration of a chemical) which have been measured for more than two decades. Syntheses of TMF behavior relative to chemical traits and ecosystem properties are lacking. We analyzed >1500 TMFs to identify OCs predisposed to biomagnify and to assess ecosystem vulnerability. The highest TMFs were for OCs that are slowly metabolized by animals (metabolic rate kM  0.2 day–1). This probabilistic model provides a new global tool for screening existing and new OCs for their biomagnification potential.

  10. Synthesis and characterization of lanthanum doped zinc oxide nanoparticles

    Science.gov (United States)

    Kumar, Vinod; Sonia, Suman, Kumar, Sacheen; Kumar, Dinesh

    2016-05-01

    La doped ZnO (Zn1-xLaxO, x = 0, 3, 6 and 9) were prepared via chemical co-precipitation method using Zinc Acetate, Lanthanum Acetate and Sodium Hydroxide at 50°C. Hydrate nanoparticles were annealed in air at 300°C for 3 hours. The synthesized samples have been characterized by powder X-ray diffraction and UV-Visiblespectrophotometer. The XRD measurement revealsthat the prepared nanoparticles have different microstructure without changing a hexagonal wurtzite structure. The result shows the change in nanoparticles size with the increment of lanthanum concentration for lower concentration for x = 0 to 6 and decreases at x = 9.

  11. Synthesis and Characterization of Nanostructured Fe-Ni Alloy Whisker

    Institute of Scientific and Technical Information of China (English)

    DONG Guo-jun; WANG Gui-xiang; ZHANG Mi-lin; LI Ru-Min; WANG Jun

    2002-01-01

    The nanocrystalline γ-(Fe,Ni) alloy whiskers have been prepared by chemical reduction of Fe2+ and Ni2+ ions with potassium borohydride under the function of a dispersant agent PE followed by heat treatment at 600℃ under the protection of nitrogen.Conditions, such as quantity of NaOH, concentration of salts, and species of surfactants, of preparation of Fe-Ni alloy have been discussed. X-ray diffraction(XRD), transmission electron microscopy(TEM) and vibrating sample magnetometer(VSM) characterized the synthesized Fe-Ni alloy. Character, capability and use of the materials have been summarized.

  12. Synthesis and characterization of MCM-41-supported nano zirconia catalysts

    Directory of Open Access Journals (Sweden)

    Mohamed S. Abdel Salam

    2015-03-01

    Full Text Available Series of MCM-41 supported sulfated Zirconia (SZ catalysts with different loadings (2.5–7.5% wt. were prepared using direct impregnation method. The acquired solid catalysts were characterized structurally and chemically using X-RD, HRTEM, BET, FT-IR, Raman spectroscopy and TPD analysis. The acidity of the solid catalysts was investigated through cumene cracking and isopropanol dehydration at different temperatures. As the SZ loading increases, the surface acidity of the mesoporous catalysts was enhanced, this was reflected by the higher catalytic activity toward cumene cracking and isopropanol dehydration.

  13. Synthesis and Characterization of the TAPO-5 Molecular Sieve

    Directory of Open Access Journals (Sweden)

    Sarah P.O. Rios

    2002-09-01

    Full Text Available Aluminophosphate sieves with AFI structure substituted by Ti (denominated TAPO-5 have been synthesized hydrothermally. These materials were characterized by X-ray diffraction (XRD, chemical analysis (ICP, scanning electronic microscopy (SEM, ultraviolet diffuse reflectance spectroscopy (DRS-UV and thermogravimetric analysis (TGA. XRD results showed the materials have good TAPO-5 crystallinity, although DRS-UV spectra indicated anatase phase as contamination. TGA analysis showed mass loss in the range of high temperatures, which can be attributed to protonated template decomposition. This indicates the existence of structural charge as a consequence of Ti incorporation into AFI structure

  14. Synthesis and Characterization of High Aluminum Zeolite X from Technical Grade Materials

    Directory of Open Access Journals (Sweden)

    Seyed Kamal Masoudian

    2013-06-01

    Full Text Available Zeolites are widely used as ion exchangers, adsorbents, separation materials and catalyst due to their well-tailored and highly-reproducible structures; therefore, the synthesis of zeolite from low grade resources can be interested. In the present work, high aluminum zeolite X was prepared from mixing technical grade sodium aluminate and sodium silicate solutions at temperatures between 70°C and 100°C. The synthesized zeolite X was characterized by SEM and X-ray methods according to ASTM standard procedures. The results showed that aging of the synthesis medium at the room temperature considerably increased the selectivity of zeolite X formation. On the other hand, high temperature of reaction mixture during crystallization formed zeolite A in the product; therefore, it decreased the purity of zeolite X. In addition, it was found that increasing H2O/Na2O and decreasing Na2O/SiO2 molar ratios in the reaction mixture resulted product with higher purity. © 2013 BCREC UNDIP. All rights reservedReceived: 7th January 2013; Revised: 7th April 2013; Accepted: 19th April 2013[How to Cite: Masoudian, S. K., Sadighi, S., Abbasi, A. (2013. Synthesis and Characterization of High Alu-minum Zeolite X from Technical Grade Materials. Bulletin of Chemical Reaction Engineering & Catalysis, 8 (1: 54-60. (doi:10.9767/bcrec.8.1.4321.54-60][Permalink/DOI: http://dx.doi.org/10.9767/bcrec.8.1.4321.54-60] | View in  |

  15. Physico-chemical characterization of sesame oil derivatives.

    Science.gov (United States)

    Zanardi, Iacopo; Travagli, Valter; Gabbrielli, Alessandro; Chiasserini, Luisa; Bocci, Velio

    2008-09-01

    Ozone treatment of commercially available vegetable oils gives rise to the formation of chemical species that are responsible for the therapeutic properties of ozonated oil derivatives in dermatological diseases. In the last years, these products have been successfully used as a topical disinfectant in a number of serious skin affections. The medical application of empirically prepared ozonated oil has yielded striking improvements with unexpected and rapid healing, compelling us to begin a long-range study aiming first to define the main characteristics of the most common ozonated vegetable oils, about which there is usually no medical consensus because of the lack of standardization of their technological parameters. Sesame oil was selected because of its great amount of polyunsaturated acyl groups, as well as natural antioxidants. Moreover, we have determined the kinetics and optimal conditions of ozonation (e.g., ozone concentrations, time of exposure, temperature) for obtaining an ozonated oil characterized by well-established technological and physico-chemical properties, namely an accurate peroxide value determination. On the basis of the results, we have gained an understanding of the modifications of the vegetable oils during the ozonation process.

  16. Interfacial characterization and analytical applications of chemically-modified surfaces

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Jianhong [Iowa State Univ., Ames, IA (United States)

    1998-02-23

    The goal of this work is to explore several new strategies and approaches to the surface modification and the microscopic characterization of interfaces in the areas mainly targeting sensor technologies that are of interest to environmental control or monitoring, and scanning probe microscopies techniques that can monitor interfacial chemical reactions in real time. Centered on the main theme, four specific topics are presented as four chapters in this dissertation following the general introduction. Chapter 1 describes the development of two immobilization schemes for covalently immobilizing fluoresceinamine at cellulose acetate and its application as a pH sensing film. Chapter 2 investigates the applicability of SFM to following the base-hydrolysis of a dithio-bis(succinimidylundecanoate) monolayer at gold in situ. Chapter 3 studies the mechanism for the accelerated rate of hydrolysis of the dithio-bis(succinimidylundecanoate) monolayer at Au(111) surface. Chapter 4 focuses on the development of an electrochemical approach to the elimination of chloride interference in Chemical Oxygen Demand (COD) analysis of waste water. The procedures, results and conclusions are described in each chapter. This report contains the introduction, references, and general conclusions. Chapters have been processed separately for inclusion on the data base. 95 refs.

  17. Synthesis and characterization of hydrogel bonded with rare earth

    Institute of Scientific and Technical Information of China (English)

    YAN Changhao; JIAO Lianlian; GUO Chunfang; ZHANG Ming; QIU Guanming

    2008-01-01

    Chitosan-poly(acrylic acid) hydrogel bonded with Eu3+ was prepared by radical solution polymerization. Biodegradable chitosan,N,N'-methylen-diacrylamide, and potassium persulphate were used as the basic material, cross-linking agent, and initiator, respectively. The structure and thermal property of hydrogel were characterized by infrared spectrometry, X-ray diffraction, scanning electron microscopy, and differential scanning calorimetry. The swollen property and fluorescent performance were also characterized. The results showed that the rare earth presented unique distribution in the hydrogel due to the formation of chemical bonds after polymerization. The glass transition tem-perature of the hydrogel decreased remarkably, which might broaden the range of its elastic application considerably. Moreover, the charac-teristic fluorescent emission of Eu3+ was observed in the hydrogel, which was indicative of the excellent luminescent performance.

  18. Physico-Chemical Characterization Of Maluku Nutmeg Oil

    Directory of Open Access Journals (Sweden)

    Ilyas Marzuki

    2014-05-01

    Full Text Available The essential oil of Banda nutmeg was extracted using hydro-distillation method to characterize their essential oil and volatile components.  Banda, Ambon, and Luhu nutmegs were chosen as sample ecotypes. Nutmeg oils were subjected to physico-chemical and GC-MC analyses.  Results indicated that nutmeg from the three ecotypes produced uncolored oils with the contents in mature seed were 11.69, 11.92, and 9.99%, respectively. Meanwhile those of immature seeds contained 13.32, 11.99, and 11.03% respectively.  Furthermore, the physico-chemical of the oil are specific gravity 0.897 to 0.909 g/ml; refraction index, 1.489 to 1.491; and optical rotation, +11.40 to +16,30.GC-MS analysis suggested that essential oils Maluku nutmegs composed of 28 to 31 components and also showed that nutmeg from Banda comprised 52.8% monoterpene hydrocarbon (MH, 21.11% oxygenated monoterpene (OM, and 18,04% aromatic compound (AC; Ambon’s 45.12% MH, 24.51% OM, and 16.97% AC; and Luhu’s 56.06% MH, 27.34% OM, and 13.62% AC.  Further analysis indicated that there were four important volatile oils fractions in nutmegs i.e. myristicin, elemicin, safrole, and eugenol. Maluku nutmeg contain 5.57 to 13.76% myristicin and 0.97 to 2.46% safrole. In conclusion, nutmeg oil shows a high stability in all physico-chemical properties.  Nutmeg from Banda ecotype has the highest content in myristicin.

  19. Synthesis and structural characterization of manganese olivine lithium phosphate

    Energy Technology Data Exchange (ETDEWEB)

    Herrera Robles, Joel O. [Basic Science Department, IIT, Universidad Autónoma de Ciudad Juárez, Av. del Charro 460 norte Cd. Juárez, Chih. C.P. 32310 (Mexico); Fuentes Cobas, Luis E. [Centro de Investigación en Materiales Avanzados CIMAV, Complejo Industrial, M. Cervantes 120, Chihuahua C.P. 31109 (Mexico); Díaz de la Torre, Sebastián [Instituto Politécnico Nacional, Centro de Investigación e Innovación Tecnológica CIITEC, Azcapotzalco, México, D.F. C.P. 02250 (Mexico); Camacho Montes, Héctor, E-mail: hcamacho@uacj.mx [Basic Science Department, IIT, Universidad Autónoma de Ciudad Juárez, Av. del Charro 460 norte Cd. Juárez, Chih. C.P. 32310 (Mexico); Elizalde Galindo, José T.; García Casillas, Perla E.; Rodríguez González, Claudia A. [Basic Science Department, IIT, Universidad Autónoma de Ciudad Juárez, Av. del Charro 460 norte Cd. Juárez, Chih. C.P. 32310 (Mexico); Álvarez Contreras, Lorena [Centro de Investigación en Materiales Avanzados CIMAV, Complejo Industrial, M. Cervantes 120, Chihuahua C.P. 31109 (Mexico)

    2015-09-15

    Highlights: • LiMnPO{sub 4} was obtained by sol gel method and crystallization in reducing atmosphere. • Magnetic and electric properties are reported for LiMnPO{sub 4}. • Electrochemical properties are also found and enhanced by adding carbon. • SEM and HRTEM show the submicron powder nature. • The multifunctional behavior of LiMnPO{sub 4} is experimentally demonstrated. - Abstract: The manganese olivine lithium phosphate is a multifunctional material. If carbon is added to form a composite LiMnPO{sub 4}–C, electrochemical properties can be enhanced, making this material a good candidate for battery cathode. High magnetic susceptibility is reported for this compound at room temperature. In this work, the magnetic response was measured through a Field Cooling/Zero Field Cooling technique at temperature below 100 K. Weak ferroelectric properties at room temperature were measured. Even though, the promising applications and the interesting properties of this system, the attention received in the literature is relatively low. The synthesis of this material is difficult because of the rapid manganese oxidation and the need of a reducing atmosphere. In fact, only few authors report the synthesis of the pure phase. In the present work, nanostructured LiMnPO{sub 4} is obtained by sol gel chemical method and according to X-ray diffraction patterns, pure LiMnPO{sub 4} is obtained after calcination in a reducing atmosphere (10% H{sub 2} – 90% Ar). Nanostructured LiMnPO{sub 4} is a material with very interesting properties that deserves attentions.

  20. Novel aldehyde and thiosemicarbazone derivatives: Synthesis, spectroscopic characterization, structural studies and molecular docking studies

    Science.gov (United States)

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

    2016-12-01

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

  1. Green synthesis, Characterization and anti microbial activity of silver nano particles –Review Paper

    Directory of Open Access Journals (Sweden)

    Seeram. Hariprasad

    2015-10-01

    Full Text Available The exploitation of various plant materials for the biosynthesis of silver nano particles is considered a green technology. Because it does not involve any harmful chemicals. Nanotechnology field is one of the most attractive researches. The field of nanotechnology is applied to bio materials. This review focuses on the green synthesis of silver nanoparticles using various plant sources. A detailed study on the reduction of silver ions to silver nanoparticles from medical plant leaves extract were demonstrated with a brief experimental procedure. Characterization of the synthesized nanoparticles performed through UV spectroscopy, Fourier Transform Infra Red spectroscopy analysis, X-Ray Diffraction analysis, Scanning Electron Microscopy and Transmission Electron Microscopy. This review mainly focus on anti microbial activities of synthesized silver nano particles.

  2. Facile Synthesis and Characterization of Au Nanoclusters-Silica Fluorescent Composite Nanospheres

    Directory of Open Access Journals (Sweden)

    Huiping Wang

    2013-01-01

    Full Text Available We developed a novel method for the synthesis of Au nanoclusters (NCs silica fluorescent composite nanospheres by mixing the as-prepared bovine serum albumin (BSA protected Au NCs with amino-modified silica spheres in acetate buffer solution. The products were characterized by high-resolution transmission electron microscopy (HRTEM, X-ray photoelectron spectroscopy (XPS, fluorescent microscope imaging (FLMI, and dynamic light scattering (DLS measurements. The proposed method was simple, efficient, and inexpensive. In addition, the composite nanospheres exhibited favorable water-dispersible, stable, and fluorescent properties, potentially leading to further applications in chemical and biological sensors. A reasonable mechanism was also proposed for the formation of composite nanospheres.

  3. Novel acridone-modified MCM-41 type silica: Synthesis, characterization and fluorescence tuning

    Directory of Open Access Journals (Sweden)

    Maximilian Hemgesberg

    2011-06-01

    Full Text Available A Mobil Composition of Matter (MCM-41 type mesoporous silica material containing N-propylacridone groups has been successfully prepared by co-condensation of an appropriate organic precursor with tetraethyl orthosilicate (TEOS under alkaline sol–gel conditions. The resulting material was fully characterized by means of X-ray diffraction (XRD, N2-adsorption–desorption, transmission electron microscopy (TEM, IR and UV–vis spectroscopy, as well as 29Si and 13C CP-MAS NMR techniques. The material features a high inner surface area and a highly ordered two-dimensional hexagonal pore structure. The fluorescence properties of the organic chromophore can be tuned via complexation of its carbonyl group with scandium triflate, which makes the material a good candidate for solid state sensors and optics. The successful synthesis of highly ordered MCM materials through co-condensation was found to be dependent on the chemical interaction of the different precursors.

  4. Synthesis and Characterization of Magnetic Metal-encapsulated Multi-walled Carbon Nanobeads

    Directory of Open Access Journals (Sweden)

    Leela Mohana Reddy A

    2008-01-01

    Full Text Available AbstractA novel, cost-effective, easy and single-step process for the synthesis of large quantities of magnetic metal-encapsulated multi-walled carbon nanobeads (MWNB and multi-walled carbon nanotubes (MWNT using catalytic chemical vapour deposition of methane over Mischmetal-based AB3alloy hydride catalyst is presented. The growth mechanism of metal-encapsulated MWNB and MWNT has been discussed based on the catalytically controlled root-growth mode. These carbon nanostructures have been characterized using scanning electron microscopy (SEM, transmission electron microscopy (TEM and HRTEM, energy dispersive analysis of X-ray (EDAX and thermogravimetric analysis (TGA. Magnetic properties of metal-filled nanobeads have been studied using PAR vibrating sample magnetometer up to a magnetic field of 10 kOe, and the results have been compared with those of metal-filled MWNT.

  5. Modified Polyacrylic Acid-Zinc Composites: Synthesis, Characterization and Biological Activity

    Directory of Open Access Journals (Sweden)

    Mohammed Rafi Shaik

    2016-02-01

    Full Text Available Polyacrylic acid (PAA is an important industrial chemical, which has been extensively applied in various fields, including for several biomedical purposes. In this study, we report the synthesis and modification of this polymer with various phenol imides, such as succinimide, phthalimide and 1,8-naphthalimide. The as-synthesized derivatives were used to prepare polymer metal composites by the reaction with Zn+2. These composites were characterized by using various techniques, including NMR, FT-IR, TGA, SEM and DSC. The as-prepared PAA-based composites were further evaluated for their anti-microbial properties against various pathogens, which include both Gram-positive and Gram-negative bacteria and different fungal strains. The synthesized composites have displayed considerable biocidal properties, ranging from mild to moderate activities against different strains tested.

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

    Science.gov (United States)

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

    2014-02-01

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

  7. Synthesis and characterization of porous hydroxyapatite and hydroxyapatite coatings

    Energy Technology Data Exchange (ETDEWEB)

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

    2000-10-25

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

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

    Science.gov (United States)

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

    2015-03-16

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-01-01

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

  10. Synthesis and characterization of thermoplastic polyurethane/nanoclay composites

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-03-01

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

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

    Science.gov (United States)

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

    2017-01-01

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

  12. Palm Olein as Renewable Raw Materials for Industrial and Pharmaceutical Products Applications: Chemical Characterization and Physicochemical Properties Studies

    Directory of Open Access Journals (Sweden)

    Darfizzi Derawi

    2014-01-01

    Full Text Available Palm olein (POo is widely produced as edible oil in tropical countries. POo is considered as renewable raw material for the new industrial and pharmaceutical products synthesis based on its characterization. Palm olein was good on its viscosity index, oxidative stability, and flash and fire point. POo contained unsaturated triacylglycerols (TAGs: POO (33.3%; POP (29.6% which plays an important role in chemical modification process to produce new industrial products. The double bond was detected on 1H-NMR (5.3 ppm and 13C-NMR (130 ppm spectra. The chemical compositions of POo were tested by using high performance liquid chromatography (HPLC and gas chromatography (GC techniques. This unsaturated oil is potentially to be used as renewable raw materials in chemical modification process to synthesise polyols, polyurethane, and biolubricant for industrial and pharmaceutical products application.

  13. Chemical characterization of tomato juice fermented with bifidobacteria.

    Science.gov (United States)

    Koh, Jong-Ho; Kim, Youngshik; Oh, Jun-Hyun

    2010-06-01

    The objective of this research was to characterize the chemical properties of tomato juice fermented with bifidobacterial species. Tomato juice was prepared from fresh tomatoes and heated at 100 degrees C prior to fermentation. Bifidobacterium breve, Bifidobacterium longum, and Bifidobacterium infantis were inoculated in tomato juice and kept at 35 to 37 degrees C for up to 6 h. Fructooligosaccharide (FOS) was added to tomato juice prior to fermentation. The analyses for brix, total titratable acidity (TTA), pH, color, and lycopene content were conducted to characterize tomato juices fermented with bifidobacterial species. Heat treatment of tomato juice did not cause any significant changes in brix, pH, and TTA. Only the redness of tomato juice was significantly increased, as the heating time increased to 30 min. The tomato juices fermented with B. breve and B. longum exhibited significant decreases in pH (3.51 and 3.80, respectively) and significant increases in TTA (13.50 and 12.50, respectively) (P tomato juice. The addition of FOS further improved the fermentation of tomato juice by bifidobacterial species. The lycopene contents of tomato juice were significantly increased from 88 to 113 microg/g by heat treatment at 100 degrees C (P < 0.05), however did not exhibit any significant change after fermentation with bifidobacterial species.

  14. Physical and chemical characterization of asphalt (bitumen) paving exposures.

    Science.gov (United States)

    Herrick, Robert F; McClean, Michael D; Meeker, John D; Zwack, Leonard; Hanley, Kevin

    2007-01-01

    The purpose of this research was to characterize the physical and chemical properties of asphalt (bitumen) fume and vapor in hot mix asphalt roadway paving operations. Area and personal air samples were taken using real-time equipment and extractive sampling and analytical methods to determine worker asphalt exposure, as well as to characterize the properties of the particulate and vapor phase components. Analysis of personal inhalation and dermal samples by gas chromatography/mass spectroscopy showed that the polycyclic aromatic hydrocarbon profile is dominated by compounds with molecular weights below 228, and that substituted and heterocyclic polycyclic aromatic hydrocarbons comprised approximately 71% of the detectable mass concentration (vapor and particulate combined). Principal components analysis shows that the polycyclic aromatic hydrocarbons with molecular weights greater than 190 are the driving force behind the polycyclic aromatic compound exposures measured for the dermal and particulate phases; there was no clear trend for the vapor phase Most of the aerosol particles are fine (mass median aerodynamic diameter 1.02 microm; count median diameter 0.24 microm).

  15. Synthesis of chemical vapor deposition graphene on tantalum wire for supercapacitor applications

    Energy Technology Data Exchange (ETDEWEB)

    Li, Mingji, E-mail: limingji@163.com [Tianjin Key Laboratory of Film Electronic and Communicate Devices, School of Electronics Information Engineering, Tianjin University of Technology, Tianjin 300384 (China); Guo, Wenlong [Tianjin Key Laboratory of Film Electronic and Communicate Devices, School of Electronics Information Engineering, Tianjin University of Technology, Tianjin 300384 (China); Li, Hongji, E-mail: hongjili@yeah.net [Tianjin Key Laboratory of Organic Solar Cells and Photochemical Conversion, School of Chemistry and Chemical Engineering, Tianjin University of Technology, Tianjin 300384 (China); Xu, Sheng [School of Precision Instrument and Optoelectronics Engineering, Tianjin University, Tianjin 300072 (China); Qu, Changqing; Yang, Baohe [Tianjin Key Laboratory of Film Electronic and Communicate Devices, School of Electronics Information Engineering, Tianjin University of Technology, Tianjin 300384 (China)

    2014-10-30

    Highlights: • The capacitance of graphene/tantalum (Ta) wire electrodes is firstly reported. • Graphene was grown on the Ta surface by hot-filament chemical vapor deposition. • Graphene/Ta wire structure is favorable for fast ion and electron transfer. • The graphene/Ta wire electrode shows high capacitive properties. - Abstract: This paper studies the synthesis and electrochemical characterization of graphene/tantalum (Ta) wires as high-performance electrode material for supercapacitors. Graphene on Ta wires is prepared by the thermal decomposition of methane under various conditions. The graphene nanosheets on the Ta wire surface have an average thickness of 1.3–3.4 nm and consist typically of a few graphene monolayers, and TaC buffer layers form between the graphene and Ta wire. A capacitor structure is fabricated using graphene/Ta wire with a length of 10 mm and a diameter of 0.6 mm as the anode and Pt wire of the same size as the cathode. The electrochemical behavior of the graphene/Ta wires as supercapacitor electrodes is characterized by cyclic voltammetry, galvanostatic charge/discharge, and electrochemical impedance spectroscopy in 1 M Na{sub 2}SO{sub 4} aqueous electrolyte. The as-prepared graphene/Ta electrode has highest capacitance of 345.5 F g{sup −1} at current density of 0.5 A g{sup −1}. The capacitance remains at about 84% after 1000 cycles at 10 A g{sup −1}. The good electrochemical performance of the graphene/Ta wire electrode is attributed to the unique nanostructural configuration, high electrical conductivity, and large specific surface area of the graphene layer. This suggests that graphene/Ta wire electrode materials have potential applications in high-performance energy storage devices.

  16. Synthesis of Gold and Silver Nanoparticles and Characterization of Structural, Optical, and Electronic Properties

    Science.gov (United States)

    2011-09-01

    of alloy quantum dots could serve to absorb and emit energy on a wide range of wavelengths and therefore increase electronic efficiency. Synthesis ...Society 2006, 128, 7756–7757. 14. Chen, Y.; Rosenzweig, Z. Luminescent CdSe Quantum Dot Doped Stabilized Micelles. American Chemical Society 2002, 2... Synthesis and Functionalization of Highly Fluorescent Gold Quantum Dots . American Chemical Society, 2008, 112, 10778–10783 18. Hasobe, T.; Imahori, H

  17. Chemical synthesis of erythropoietin glycoforms for insights into the relationship between glycosylation pattern and bioactivity.

    Science.gov (United States)

    Murakami, Masumi; Kiuchi, Tatsuto; Nishihara, Mika; Tezuka, Katsunari; Okamoto, Ryo; Izumi, Masayuki; Kajihara, Yasuhiro

    2016-01-01

    The role of sialyloligosaccharides on the surface of secreted glycoproteins is still unclear because of the difficulty in the preparation of sialylglycoproteins in a homogeneous form. We selected erythropoietin (EPO) as a target molecule and designed an efficient synthetic strategy for the chemical synthesis of a homogeneous form of five EPO glycoforms varying in glycosylation position and the number of human-type biantennary sialyloligosaccharides. A segment coupling strategy performed by native chemical ligation using six peptide segments including glycopeptides yielded homogeneous EPO glycopeptides, and folding experiments of these glycopeptides afforded the correctly folded EPO glycoforms. In an in vivo erythropoiesis assay in mice, all of the EPO glycoforms displayed biological activity, in particular the EPO bearing three sialyloligosaccharides, which exhibited the highest activity. Furthermore, we observed that the hydrophilicity and biological activity of the EPO glycoforms varied depending on the glycosylation pattern. This knowledge will pave the way for the development of homogeneous biologics by chemical synthesis.

  18. Chemical synthesis of erythropoietin glycoforms for insights into the relationship between glycosylation pattern and bioactivity

    Science.gov (United States)

    Murakami, Masumi; Kiuchi, Tatsuto; Nishihara, Mika; Tezuka, Katsunari; Okamoto, Ryo; Izumi, Masayuki; Kajihara, Yasuhiro

    2016-01-01

    The role of sialyloligosaccharides on the surface of secreted glycoproteins is still unclear because of the difficulty in the preparation of sialylglycoproteins in a homogeneous form. We selected erythropoietin (EPO) as a target molecule and designed an efficient synthetic strategy for the chemical synthesis of a homogeneous form of five EPO glycoforms varying in glycosylation position and the number of human-type biantennary sialyloligosaccharides. A segment coupling strategy performed by native chemical ligation using six peptide segments including glycopeptides yielded homogeneous EPO glycopeptides, and folding experiments of these glycopeptides afforded the correctly folded EPO glycoforms. In an in vivo erythropoiesis assay in mice, all of the EPO glycoforms displayed biological activity, in particular the EPO bearing three sialyloligosaccharides, which exhibited the highest activity. Furthermore, we observed that the hydrophilicity and biological activity of the EPO glycoforms varied depending on the glycosylation pattern. This knowledge will pave the way for the development of homogeneous biologics by chemical synthesis. PMID:26824070

  19. Capturing Biological Activity in Natural Product Fragments by Chemical Synthesis.

    Science.gov (United States)

    Crane, Erika A; Gademann, Karl

    2016-03-14

    Natural products have had an immense influence on science and have directly led to the introduction of many drugs. Organic chemistry, and its unique ability to tailor natural products through synthesis, provides an extraordinary approach to unlock the full potential of natural products. In this Review, an approach based on natural product derived fragments is presented that can successfully address some of the current challenges in drug discovery. These fragments often display significantly reduced molecular weights, reduced structural complexity, a reduced number of synthetic steps, while retaining or even improving key biological parameters such as potency or selectivity. Examples from various stages of the drug development process up to the clinic are presented. In addition, this process can be leveraged by recent developments such as genome mining, antibody-drug conjugates, and computational approaches. All these concepts have the potential to identify the next generation of drug candidates inspired by natural products.

  20. Synthesis and characterization of carbon nanotube from coconut shells activated carbon

    Science.gov (United States)

    Melati, A.; Hidayati, E.

    2016-03-01

    Carbon nanotubes (CNTs) have been explored in almost every single cancer treatment modality, including drug delivery, lymphatic targeted chemotherapy, photodynamic therapy, and gene therapy. They are considered as one of the most promising nanomaterial with the capability of both detecting the cancerous cells and delivering drugs or small therapeutic molecules to the cells. CNTs have unique physical and chemical properties such as high aspect ratio, ultralight weight, high mechanical strength, high electrical conductivity, and high thermal conductivity. Coconut Shell was researched as active carbon source on 500 - 600°C. These activated carbon was synthesized becomes carbon nanotube and have been proposed as a promising tool for detecting the expression of indicative biological molecules at early stage of cancer. Clinically, biomarkers cancer can be detected by CNT Biosensor. We are using pyrolysis methods combined with CVD process or Wet Chemical Process on 600°C. Our team has successfully obtained high purity, and aligned MWCNT (Multi Wall Nanotube) bundles on synthesis CNT based on coconut shells raw materials. CNTs can be used to cross the mammalian cell membrane by endocytosis or other mechanisms. SEM characterization of these materials have 179 nm bundles on phase 83° and their materials compound known by using FTIR characterization.

  1. Synthesis and characterization of nanostructured CaSiO3 biomaterial

    Science.gov (United States)

    Jagadale, Pramod N.; Kulal, Shivaji R.; Joshi, Meghanath G.; Jagtap, Pramod P.; Khetre, Sanjay M.; Bamane, Sambhaji R.

    2013-04-01

    Here we report a successful preparation of nanostructured calcium silicate by wet chemical approach. The synthesized sample was characterized by various physico-chemical methods. Thermal stability was investigated using thermo-gravimetric and differential thermal analysis (TG-DTA). Structural characterization of the sample was carried out by the X-ray diffraction technique (XRD) which confirmed its single phase hexagonal structure. Transmission electron microscopy (TEM) was used to study the nanostructure of the ceramics while homogeneous grain distribution was revealed by scanning electron microscopy studies (SEM). The elemental analysis data obtained from energy dispersive X-ray spectroscopy (EDAX) were in close agreement with the starting composition used for the synthesis. Superhydrophilic nature of CaSiO3 was investigated at room temperature by sessile drop technique. Effect of porous nanosized CaSiO3 on early adhesion and proliferation of human bone marrow mesenchymal stem cells (BMMSCs) and cord blood mesenchymal stem (CBMSCs) cells was measured in vitro. MTT cytotoxicity test and cell adhesion test showed that the material had good biocompatibility and promoted cell viability and cell proliferation. It has been stated that the cell viability and proliferation are significantly affected by time and concentration of CaSiO3. These findings indicate that the CaSiO3 ceramics has good biocompatibility and that it is promising as a biomaterial.

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

    Indian Academy of Sciences (India)

    MUSTAFA BARIS; TUNCAY SIMSEK; ADNAN AKKURT

    2016-08-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2007-05-16

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

  4. Synthesis, characterization and evaluation of antimicrobial activity of zinc oxide nanoparticles

    Directory of Open Access Journals (Sweden)

    Jeeva Lakshmi Venkataraju

    2012-08-01

    Full Text Available The study involved synthesis of Zinc Oxide nanoparticles using biological and  chemical reducing agents. The aim was to compare the yield, nature and antimicrobial activity of nanoparticles synthesized by the two methods. In biological method, hot and cold Aloe vera leaf extract; and in chemical method, sodium hydroxide was used as reducing agents. Nanoparticles synthesized by the two methods were characterized by XRD and SEM. It was evident from SEM images that particles obtained by biological method were rod-shaped and those synthesized by chemical method were spherical. Antibacterial study was carried out on gram-positive and gram-negative bacterial strains by agar-well diffusion method and their MIC values were determined. ZnO-AC showed almost consistent activity on all the strains, whereas ZnO-AH and ZnO-C showed greater activity on some strains compared to others. ZnO-AH showed least overall activity on all strains as compared to ZnO- AC and ZnO-C.Keywords: Zinc Oxide nanoparticles, biological method, XRD, SEM, antibacterial study, agar diffusion method.

  5. Synthesis and characterization of cobalt-manganese oxides

    Energy Technology Data Exchange (ETDEWEB)

    Valencia, J. [Laboratorio de Magnetismo y Materiales Avanzados, Facultad de Ciencias Exactas y Naturales, Universidad Nacional de Colombia, Sede Manizales, Manizales (Colombia); Department of Aerospace Engineering and Mechanics, University of Minnesota, Minneapolis 55455-0153 (United States); Arias, N.P. [Laboratorio de Materiales Nanoestructurados y Funcionales, Facultad de Ciencias Exactas y Naturales, Universidad Nacional de Colombia, Sede Manizales, Manizales (Colombia); Departamento de Ingenieria Electrica, Electronica y Computacion, Facultad de Ingenieria y Arquitectura, Universidad Nacional de Colombia, Sede Manizales, Manizales (Colombia); Giraldo, O. [Laboratorio de Materiales Nanoestructurados y Funcionales, Facultad de Ciencias Exactas y Naturales, Universidad Nacional de Colombia, Sede Manizales, Manizales (Colombia); Rosales-Rivera, A., E-mail: arosalesr@unal.edu.co [Laboratorio de Magnetismo y Materiales Avanzados, Facultad de Ciencias Exactas y Naturales, Universidad Nacional de Colombia, Sede Manizales, Manizales (Colombia)

    2012-08-15

    Cobalt doped/un-doped manganese oxides materials were synthesized at various doping rates by soft chemical reactions, oxidation-reduction method, which allows generating a metal-mixed oxide. The synthesized materials were characterized using several techniques including chemical analysis, X-rays diffraction (XRD), scanning electron microscopy (SEM), thermogravimetric analysis (TGA), and vibrating sample magnetometer (VSM). The chemical analysis confirmed the presence of cobalt in the samples. XRD patterns reveal mainly a spinel-like structure and SEM micrographs exhibited morphology with fine aggregate of particles. TGA profiles showed weight loss due to loss of water in a first step, followed by a loss of oxygen from the lattice associated with partial reduction of Mn{sup 4+} to Mn{sup 3+}. VSM was used to measure the magnetization as a function of the applied magnetic field at temperatures T=50 and 300 K. Different magnetic behaviors were observed when cobalt percentage changed in the samples. These behaviors are considered to be related to the size of the particles and composition of the materials. Higher coercive field and lesser magnetization were observed for the sample with higher cobalt content.

  6. Plasma-chemical Synthesis and Regeneration of Catalysts for CH4 Steam Conversion

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    We carried out experimental studies concerning the plasma-chemical synthesis(PCS) of a catalyst for CH4 steam conversion and designed and built the equipment for PCS and/ or regeneration of spent catalyst for CH4 steam conversion. Under the conditions of an electric-arc low-temperature plasma (LTP), we studied the Ni-O-Al system and performed a comprehensive physicochemical analysis of the ultradispersed product obtained. It's the first time worldwide when the conditions of plasma-chemical synthesis and/ or regeneration of CH4 steam conversion catalysts under the conditions of electric-arc LTP are investigated depending on the plasma-chemical process (PCP) parameters and the plasma-chemical reactor (PCP) type (with CW-"cold walls" Tw = 500 K or WW-"warm walls" Tw = 1500 K), samples with a specific surface of 120 m2/g are obtained. Plasma-chemically synthesized and/ or regenerated samples have a homogenous chemical composition similar to that the Girdller (USA) conventional industrial catalyst. It is empirically established that the optimal temperature range in PCR for synthesis of samples with maximum dispersity is (2000 ~ 3000) K. Results from investigation on dynamics and kinetics of plasma-chemically synthesized and / or regenerated catalysts for CH4 steam conversion show that under LTP conditions premises for the formation of catalyst compositions are established. They are reduced 3 to 4 times faster than their industrial analogues. High specific surface of the samples, homogenous composition, high rate of active chemical surface formed by reduction, faulty crystal lattice of catalytically active phases and mostly high catalytic activity make them a potential competitor with their industrial analogues for their probable production in catalyst shops.

  7. Synthesis, chemical modification, and surface assembly of carbon nanowires

    Energy Technology Data Exchange (ETDEWEB)

    Amma, A.; St. Angelo, S.K.; Mallouk, T.E. [Department of Chemistry, The Pennsylvania State University, University Park, PA 16802 (United States); Razavi, B.; Mayer, T.S. [Electrical Engineering, The Pennsylvania State University, University Park, PA 16802 (United States)

    2003-05-01

    Carbon nanotubules and nanowires were synthesized by pyrolysis of polymer precursors in the pores of alumina membranes. The nanowires were released by dissolving the membranes, and were then made hydrophobic or hydrophilic by chemical surface derivatization. These nanowires could be placed into lithographically defined wells on surfaces by means of electrostatic interactions with monolayers at the bottoms of the wells. (Abstract Copyright [2003], Wiley Periodicals, Inc.)

  8. Nanostructured conjugated polymers in chemical sensors: synthesis, properties and applications.

    Science.gov (United States)

    Correa, D S; Medeiros, E S; Oliveira, J E; Paterno, L G; Mattoso, Luiz C

    2014-09-01

    Conjugated polymers are organic materials endowed with a π-electron conjugation along the polymer backbone that present appealing electrical and optical properties for technological applications. By using conjugated polymeric materials in the nanoscale, such properties can be further enhanced. In addition, the use of nanostructured materials makes possible miniaturize devices at the micro/nano scale. The applications of conjugated nanostructured polymers include sensors, actuators, flexible displays, discrete electronic devices, and smart fabric, to name a few. In particular, the use of conjugated polymers in chemical and biological sensors is made feasible owning to their sensitivity to the physicochemical conditions of its surrounding environment, such as chemical composition, pH, dielectric constant, humidity or even temperature. Subtle changes in these conditions bring about variations on the electrical (resistivity and capacitance), optical (absorptivity, luminescence, etc.), and mechanical properties of the conjugated polymer, which can be precisely measured by different experimental methods and ultimately associated with a specific analyte and its concentration. The present review article highlights the main features of conjugated polymers that make them suitable for chemical sensors. An especial emphasis is given to nanostructured sensors systems, which present high sensitivity and selectivity, and find application in beverage and food quality control, pharmaceutical industries, medical diagnosis, environmental monitoring, and homeland security, and other applications as discussed throughout this review.

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

    Science.gov (United States)

    Kanniah, Vinod

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

  10. Chemical Synthesis, Computational Modeling, and Surface Reactions of Silicon Nanotube Anodes and Silicate Cathodes for Lithium Ion Batteries

    Science.gov (United States)

    Hinkle, Christopher

    2014-03-01

    Nanostructured materials show significant promise in enhancing the performance and safety of Li-ion batteries at greatly reduced cost. We highlight certain classes of materials for next generation anodes, cathodes, and solid electrolytes in addition to interface reactions and show how advanced chemical spectroscopy and first principles modeling can be utilized to improve battery performance and stability. In this work, we utilize advanced materials characterization techniques (in-situ XPS and FTIR, Raman, AFM, XRD) to elucidate the chemical bonding, nanostructure, and electrochemical properties that lead to improved storage capabilities in these materials. We describe the recent progress in chemical synthesis methods of fabricating hydrogenated amorphous-Si nanotube anodes and tetrahedral transition metal silicate cathodes (Li2MSiO4) , which may be well-suited for future technologies. Additionally, insight into the redox potentials and ionic and electronic conductivities has been investigated using first-principles modeling. Our findings suggest that high-voltage, multi-component Li2MSiO4 cathodes (M = Fe, Mn, Ni) with high Mn content are strong candidates for future Li-ion batteries. Inorganic solid electrolytes are also discussed highlighting their potential for improved safety, increased ionic conductivities, and stability against adverse reactions with the electrodes. Finally, we illustrate the complexity of interfacial chemistry in these new materials and the need for advanced spectroscopic characterization to make progress on all aspects of electrode and electrolyte development.

  11. ALTERNATIVE FUELS AND CHEMICALS FROM SYNTHESIS GAS. FINAL QUARTERLY STATUS REPORT NO. 10

    Energy Technology Data Exchange (ETDEWEB)

    None

    1998-11-01

    The overall objectives of this program are to investigate potential technologies for the conversion of synthesis gas to oxygenated and hydrocarbon fuels and industrial chemicals, and to demonstrate the most promising technologies at DOE's LaPorte, Texas, Slurry Phase Alternative Fuels Development Unit (AFDU). The program will involve a continuation of the work performed under the Alternative Fuels from Coal-Derived Synthesis Gas Program and will draw upon information and technologies generated in parallel current and future DOE-funded contracts.

  12. Alternative fuels and chemicals from synthesis gas. Fourth quarterly report, 1994

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    1997-10-01

    The overall objectives of this program are to investigate potential technologies for the conversion of synthesis gas to oxygenated and hydrocarbon fuels and industrial chemicals, and to demonstrate the most promising technologies at DOE`s LaPorte, Texas, Slurry Phase Alternative Fuels Development Unit (AFDU). The program will involve a continuation of the work performed under the Alternative Fuels from Coal-Derived Synthesis Gas Program and will draw upon information and technologies generated in parallel current and future DOE-funded contracts.

  13. ALTERNATIVE FUELS AND CHEMICALS FROM SYNTHESIS GAS. FINAL QUARTERLY STATUS REPORT

    Energy Technology Data Exchange (ETDEWEB)

    None

    1999-04-01

    The overall objectives of this program are to investigate potential technologies for the conversion of synthesis gas to oxygenated and hydrocarbon fuels and industrial chemicals, and to demonstrate the most promising technologies at DOE's LaPorte, Texas, Slurry Phase Alternative Fuels Development Unit (AFDU). The program will involve a continuation of the work performed under the Alternative Fuels from Coal-Derived Synthesis Gas Program and will draw upon information and technologies generated in parallel current and future DOE-funded contracts.

  14. Synthesis and Characterization of Gold Nanoparticles by Tryptophane

    Directory of Open Access Journals (Sweden)

    Azim Akbarzadeh

    2009-01-01

    Full Text Available Problem statement: Preparation and synthesis of gold nanoparticles with small size and suitable stability is very important and applicable particularly in medicine. In this study, we have prepared gold nanoparticles by chemical reduction method employing L-Tryptophane as a reducing agent for ionic gold. Approach: The gold nanoparticles are the most employed amongst the different metallic nanoparticles in the fields of nanomedicine and nanobiotechnology. Therefore, the employed method should provide suitable particle size, shape and particle distribution in order to obtain nanoparticles of high activity and efficiency indicating the importance of the technique. In this study, HAuCl4 .3H2O, L-Tryptophane and polyethyleneglycol (PEG were used to produce AuCl-4 ions. They were acted as pre-material, reducing and stabilizing agents respectively. Results: The size, distribution and formation of gold nanoparticles were confirmed by Transmission Electron Microscopy (TEM indicating the diameter of gold nanoparticles at the range of 10-25 nm and UV spectroscopy. The formed nanoparticles showed the highest absorption at 518 nm. Conclusion: The gold nanoparticles were stable in PEG1000. Since these nanoparticles have suitable size distribution they can be considered as a suitable candidate to be employed in nanomedicine and nanobiotechnology.

  15. MOCVD of zirconium oxide thin films: Synthesis and characterization

    Science.gov (United States)

    Torres-Huerta, A. M.; Domínguez-Crespo, M. A.; Ramírez-Meneses, E.; Vargas-García, J. R.

    2009-02-01

    The synthesis of thin films of zirconia often produces tetragonal or cubic phases, which are stable at high temperatures, but that can be transformed into the monoclinic form by cooling. In the present study, we report the deposition of thin zirconium dioxide films by metalorganic chemical vapor deposition using zirconium (IV)-acetylacetonate as precursor. Colorless, porous, homogeneous and well adherent ZrO 2 thin films in the cubic phase were obtained within the temperature range going from 873 to 973 K. The deposits presented a preferential orientation towards the (1 1 1) and (2 2 0) planes as the substrate temperature was increased, and a crystal size ranging between 20 and 25 nm. The kinetics is believed to result from film growth involving the deposition and aggregation of nanosized primary particles produced during the CVD process. A mismatch between the experimental results obtained here and the thermodynamic prediction was found, which can be associated with the intrinsic nature of the nanostructured materials, which present a high density of interfaces.

  16. MOCVD of zirconium oxide thin films: Synthesis and characterization

    Energy Technology Data Exchange (ETDEWEB)

    Torres-Huerta, A.M., E-mail: atohuer@hotmail.com [Centro de Investigacion en Ciencia Aplicada y Tecnologia Avanzada, Unidad Altamira, Instituto Politecnico Nacional, Km. 14.5 Carr. Tampico-Puerto Industrial, C.P. 89600, Altamira, Tamaulipas (Mexico); Dominguez-Crespo, M.A.; Ramirez-Meneses, E. [Centro de Investigacion en Ciencia Aplicada y Tecnologia Avanzada, Unidad Altamira, Instituto Politecnico Nacional, Km. 14.5 Carr. Tampico-Puerto Industrial, C.P. 89600, Altamira, Tamaulipas (Mexico); Vargas-Garcia, J.R. [ESIQIE, Departamento de Metalurgia y Materiales, Instituto Politecnico Nacional. A.P. 75-876, 07300 Mexico, D.F. (Mexico)

    2009-02-15

    The synthesis of thin films of zirconia often produces tetragonal or cubic phases, which are stable at high temperatures, but that can be transformed into the monoclinic form by cooling. In the present study, we report the deposition of thin zirconium dioxide films by metalorganic chemical vapor deposition using zirconium (IV)-acetylacetonate as precursor. Colorless, porous, homogeneous and well adherent ZrO{sub 2} thin films in the cubic phase were obtained within the temperature range going from 873 to 973 K. The deposits presented a preferential orientation towards the (1 1 1) and (2 2 0) planes as the substrate temperature was increased, and a crystal size ranging between 20 and 25 nm. The kinetics is believed to result from film growth involving the deposition and aggregation of nanosized primary particles produced during the CVD process. A mismatch between the experimental results obtained here and the thermodynamic prediction was found, which can be associated with the intrinsic nature of the nanostructured materials, which present a high density of interfaces.

  17. Synthesis, characterization and optical properties of nanocrystalline lead molybdate

    Energy Technology Data Exchange (ETDEWEB)

    Anandakumar, V.M. [Department of Physics University of Kerala, Thiruvananthapuram (India); Department of Physics, Mahatma Gandhi College, Thiruvananthapuram (India); Khadar, M.A. [Department of Physics University of Kerala, Thiruvananthapuram (India); Centre for Nanosciences and Nanotechnology, University of Kerala, Thiruvananthapuram (India)

    2008-11-15

    Lead molybdate (PbMoO{sub 4}) finds wide practical application due to its acousto-optic and luminescent properties. In the present study, nanoparticles of PbMoO{sub 4} of different grain sizes were synthesized through chemical precipitation technique. Precipitation reactions carried out in non-aqueous media below room temperature were used for the synthesis of samples of two lower grain sizes. The crystal structure and grain size of the samples were determined using X-ray diffraction and transmission electron microscopy. UV-Visible absorption spectra showed a broad absorption peak for the sample with average grain size of 52 nm which is blue shifted considerably as the average grain size was reduced to 14 nm. The fundamental absorption follows an exponential edge indicating Urbach-like behaviour. The temperature dependence of Urbach parameter is also determined. The micro-Raman spectra and FT Raman spectra of the samples were recorded and the features in the Raman spectra are discussed. (copyright 2008 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  18. Cobalt-based Magnetic Nanoparticles: Design, Synthesis and Characterization

    Science.gov (United States)

    Zamanpour, Mehdi

    The ever-increasing desire for more energy attainable from a smaller volume of matter has driven researchers to explore advanced materials at the molecular or even atomic size scale. Magnetic materials at the nanometer size scale have been the subject of enormous research effort worldwide for more than half a century. Different magnetic nanoparticles have shown different behavior in the absence and presence of an external magnetic field, which has led them to be categorized as soft (easy to demagnetize) or hard (resistive against demagnetization) magnets. Applications range from medical and biomedical devices to magnetic recording media and magnetic sensing have emphasized the importance of this class of materials. Soft magnetic phases have found application in power generation and magnetic targeted drug delivery, while hard magnets have been subject of extensive research for application as energy storage media. Discovery of the exchange-coupling phenomenon between the spins of two adjacent hard and soft magnetic phases which means taking advantage of both high magnetic moment of the soft phase as well as high coercivity of the hard phase has attracted scientists to develop advanced materials for energy storage with no usage of fossil fuels: clean energy. In this Dissertation, synthesis of pure phase, soft FeCo nanoparticles with high magnetic moment and hard phase CoxC nanoparticles possessing high coercivity is reported. The polyol method (chemical co-precipitating at polyhydric alcohol as reducing agent) is used to make FeCo and Co xC nanoparticles and the effects of important reaction kinetics parameters on the structure and magnetic properties of the products are studied. Careful analysis of correlations between these parameters and the properties of the magnetic particles has made synthesis of FeCo and CoxC nanoparticles with desired properties possible. Fabrication of MnAlC-FeCo heterostructures as a rare earth-free alternative for high-performance permanent

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

    Science.gov (United States)

    Franus, Wojciech; Wdowin, Magdalena; Franus, Małgorzata

    2014-09-01

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

  20. One-Dimensional Perovskite Manganite Oxide Nanostructures: Recent Developments in Synthesis, Characterization, Transport Properties, and Applications.

    Science.gov (United States)

    Li, Lei; Liang, Lizhi; Wu, Heng; Zhu, Xinhua

    2016-12-01

    One-dimensional nanostructures, including nanowires, nanorods, nanotubes, nanofibers, and nanobelts, have promising applications in mesoscopic physics and nanoscale devices. In contrast to other nanostructures, one-dimensional nanostructures can provide unique advantages in investigating the size and dimensionality dependence of the materials' physical properties, such as electrical, thermal, and mechanical performances, and in constructing nanoscale electronic and optoelectronic devices. Among the one-dimensional nanostructures, one-dimensional perovskite manganite nanostructures have been received much attention due to their unusual electron transport and magnetic properties, which are indispensable for the applications in microelectronic, magnetic, and spintronic devices. In the past two decades, much effort has been made to synthesize and characterize one-dimensional perovskite manganite nanostructures in the forms of nanorods, nanowires, nanotubes, and nanobelts. Various physical and chemical deposition techniques and growth mechanisms are explored and developed to control the morphology, identical shape, uniform size, crystalline structure, defects, and homogenous stoichiometry of the one-dimensional perovskite manganite nanostructures. This article provides a comprehensive review of the state-of-the-art research activities that focus on the rational synthesis, structural characterization, fundamental properties, and unique applications of one-dimensional perovskite manganite nanostructures in nanotechnology. It begins with the rational synthesis of one-dimensional perovskite manganite nanostructures and then summarizes their structural characterizations. Fundamental physical properties of one-dimensional perovskite manganite nanostructures are also highlighted, and a range of unique applications in information storages, field-effect transistors, and spintronic devices are discussed. Finally, we conclude this review with some perspectives/outlook and future

  1. A novel and easy chemical-clock synthesis of nanocrystalline iron-cobalt bearing layered double hydroxides.

    Science.gov (United States)

    Hadi, Jebril; Grangeon, Sylvain; Warmont, Fabienne; Seron, Alain; Greneche, Jean-Marc

    2014-11-15

    A novel synthesis of cobalt-iron layered double hydroxide (LDH) with interlayer chlorides was investigated. The method consists in mixing concentrated solutions of hexaamminecobalt(III) trichloride with ferrous chloride at room temperature and in anoxic conditions. Four initial Fe/Co atomic ratios have been tried out (0.12, 0.6, 1.2 and 1.8). Neither heating nor addition of alkali was employed for adjusting the pH and precipitating the metal hydroxides. Still, each mixture led to the spontaneous precipitation of a LDH-rich solid having a crystal-chemistry that depended on the initial solution Fe/Co. These LDHs phases were carefully characterized by mean of X-ray diffraction, (57)Fe Mössbauer spectrometry, transmission electron microscopy and chemical analysis (total dissolution and phenanthroline method). Solution Eh and pH were also monitored during the synthesis. Increasing initial Fe/Co ratio impacted the dynamic of the observed stepwise reaction and the composition of the resulting product. Once the two solutions are mixed, a spontaneous and abrupt color change occurs after an induction time which depends on the starting Fe/Co ratio. This makes the overall process acting as a chemical clock. This spontaneous generation of CoFe-LDH arises from the interplay between redox chemistries of iron and cobalt-ammonium complexes.

  2. Synthesis of Lead Sulfide Nanoparticles by Chemical Precipitation Method

    Science.gov (United States)

    Chongad, L. S.; Sharma, A.; Banerjee, M.; Jain, A.

    2016-10-01

    Lead sulfide (PbS) nanoparticles were prepared by chemical precipitation method (CPM) with the assistance of H2S gas. The microstructure and morphology of the synthesized nanoparticles have been investigated using X-ray diffraction (XRD) and transmission electron microscopy (TEM). The XRD patterns of the PbS nanoparticles reveal formation of cubic phase. To investigate the quality of prepared nanoparticles, the particles size, lattice constant, strain, dislocation density etc. have been determined using XRD. TEM images reveal formation of cubic nanoparticles and the particle size determined from TEM images agree well with those from XRD.

  3. A new antiproliferative noscapine analogue: chemical synthesis and biological evaluation.

    Science.gov (United States)

    Ghaly, Peter E; Abou El-Magd, Rabab M; Churchill, Cassandra D M; Tuszynski, Jack A; West, F G

    2016-06-28

    Noscapine, a naturally occurring opium alkaloid, is a widely used antitussive medication. Noscapine has low toxicity and recently it was also found to possess cytotoxic activity which led to the development of many noscapine analogues. In this paper we report on the synthesis and testing of a novel noscapine analogue. Cytotoxicity was assessed by MTT colorimetric assay using SKBR-3 and paclitaxel-resistant SKBR-3 breast cancer cell lines using different concentrations for both noscapine and the novel compound. Microtubule polymerization assay was used to determine the effect of the new compound on microtubules. To compare the binding affinity of noscapine and the novel compound to tubulin, we have done a fluorescence quenching assay. Finally, in silico methods using docking calculations were used to illustrate the binding mode of the new compound to α,β-tubulin. Our cytotoxicity results show that the new compound is more cytotoxic than noscapine on both SKBR-3 cell lines. This was confirmed by the stronger binding affinity of the new compound, compared to noscapine, to tubulin. Surprisingly, our new compound was found to have strong microtubule-destabilizing properties, while noscapine is shown to slightly stabilize microtubules. Our calculation indicated that the new compound has more binding affinity to the colchicine-binding site than to the noscapine site. This novel compound has a more potent cytotoxic effect on cancer cell lines than its parent, noscapine, and hence should be of interest as a potential anti-cancer drug.

  4. Temperature buffer test. Hydro-mechanical and chemical/ mineralogical characterizations

    Energy Technology Data Exchange (ETDEWEB)

    Aakesson, Mattias; Olsson, Siv; Dueck, Ann; Nilsson, Ulf; Karnland, Ola [Clay Technology AB, Lund (Sweden); Kiviranta, Leena; Kumpulainen, Sirpa [BandTech Oy, Helsinki (Finland); Linden, Johan [Aabo Akademi, Aabo (Finland)

    2012-01-15

    The Temperature Buffer Test (TBT) is a joint project between SKB/ANDRA and supported by ENRESA (modeling) and DBE (instrumentation), which aims at improving the understanding and to model the thermo-hydro-mechanical behavior of buffers made of swelling clay submitted to high temperatures (over 100 deg C) during the water saturation process. The test has been carried out in a KBS-3 deposition hole at Aspo HRL. It was installed during the spring of 2003. Two steel heaters (3 m long, 0.6 m diameter) and two buffer arrangements have been investigated: the lower heater was surrounded by rings of compacted Wyoming bentonite only, whereas the upper heater was surrounded by a composite barrier, with a sand shield between the heater and the bentonite. The test was dismantled and sampled during the winter of 2009/2010. This report presents the hydro-mechanical and chemical/mineralogical characterization program which was launched subsequent to the dismantling operation. The main goal has been to investigate if any significant differences could be observed between material from the field experiment and the reference material. The field samples were mainly taken from Ring 4 (located at the mid-section around the lower heater), in which the temperature in the innermost part reached 155 deg C. The following hydro-mechanical properties have been determined for the material (test technique within brackets): hydraulic conductivity (swelling pressure device), swelling pressure (swelling pressure device), unconfined compression strength (mechanical press), shear strength (triaxial cell) and retention properties (jar method). The following chemical/mineralogical properties (methods within brackets) were determined: anion analysis of water leachates (IC), chemical composition (ICP/AES+MS, EGA), cation exchange capacity (CEC, Cu-trien method) and exchangeable cations (exchange with NH4, ICPAES), mineralogical composition (XRD and FTIR), element distribution and microstructure (SEM and

  5. Use of Modern Chemical Protein Synthesis and Advanced Fluorescent Assay Techniques to Experimentally Validate the Functional Annotation of Microbial Genomes

    Energy Technology Data Exchange (ETDEWEB)

    Kent, Stephen [University of Chicago

    2012-07-20

    The objective of this research program was to prototype methods for the chemical synthesis of predicted protein molecules in annotated microbial genomes. High throughput chemical methods were to be used to make large numbers of predicted proteins and protein domains, based on microbial genome sequences. Microscale chemical synthesis methods for the parallel preparation of peptide-thioester building blocks were developed; these peptide segments are used for the parallel chemical synthesis of proteins and protein domains. Ultimately, it is envisaged that these synthetic molecules would be ‘printed’ in spatially addressable arrays. The unique ability of total synthesis to precision label protein molecules with dyes and with chemical or biochemical ‘tags’ can be used to facilitate novel assay technologies adapted from state-of-the art single molecule fluorescence detection techniques. In the future, in conjunction with modern laboratory automation this integrated set of techniques will enable high throughput experimental validation of the functional annotation of microbial genomes.

  6. The synthesis of polystyrene with a new chemical approach

    OpenAIRE

    Naima Bensaada; Moulkheir Ayat; Rachid Meghabar; Mohammed Belbachir

    2015-01-01

    The bulk room-temperature polymerization of styrene initiated by environmentally friendly catalysts Maghnite-Na+ is investigated. The catalyst removed from the reaction mixture simply by filtration could be regenerated and reused. The effect of the Maghnite-Na+ catalyst loading on degree of polymerization had been studied and state their inverse relation. The catalyst was characterized by X-ray diffraction and FTIR spectroscopy.

  7. The synthesis of polystyrene with a new chemical approach

    Directory of Open Access Journals (Sweden)

    Naima Bensaada

    2015-03-01

    Full Text Available The bulk room-temperature polymerization of styrene initiated by environmentally friendly catalysts Maghnite-Na+ is investigated. The catalyst removed from the reaction mixture simply by filtration could be regenerated and reused. The effect of the Maghnite-Na+ catalyst loading on degree of polymerization had been studied and state their inverse relation. The catalyst was characterized by X-ray diffraction and FTIR spectroscopy.

  8. Microwave-irradiation-assisted hybrid chemical approach for titanium dioxide nanoparticle synthesis: microbial and cytotoxicological evaluation.

    Science.gov (United States)

    Ranjan, Shivendu; Dasgupta, Nandita; Rajendran, Bhavapriya; Avadhani, Ganesh S; Ramalingam, Chidambaram; Kumar, Ashutosh

    2016-06-01

    Titanium dioxide nanoparticles (TNPs) are widely used in the pharmaceutical and cosmetics industries. It is used for protection against UV exposure due to its light-scattering properties and high refractive index. Though TNPs are increasingly used, the synthesis of TNPs is tedious and time consuming; therefore, in the present study, microwave-assisted hybrid chemical approach was used for TNP synthesis. In the present study, we demonstrated that TNPs can be synthesized only in 2.5 h; however, the commonly used chemical approach using muffle furnace takes 5 h. The activity of TNP depends on the synthetic protocol; therefore, the present study also determined the effect of microwave-assisted hybrid chemical approach synthetic protocol on microbial and cytotoxicity. The results showed that TNP has the best antibacterial activity in decreasing order from Escherichia coli, Bacillus subtilis, and Staphylococcus aureus. The IC50 values of TNP for HCT116 and A549 were found to be 6.43 and 6.04 ppm, respectively. Cell death was also confirmed from trypan blue exclusion assay and membrane integrity loss was observed. Therefore, the study determines that the microwave-assisted hybrid chemical approach is time-saving; hence, this technique can be upgraded from lab scale to industrial scale via pilot plant scale. Moreover, it is necessary to find the mechanism of action at the molecular level to establish the reason for greater bacterial and cytotoxicological toxicity. Graphical abstract A graphical representation of TNP synthesis.

  9. Synthesis and characterization of MgO nanocrystals for biosensing applications

    Energy Technology Data Exchange (ETDEWEB)

    Li, Hongji [Tianjin Key Laboratory of Organic Solar Cells and Photochemical Conversion, School of Chemistry & Chemical Engineering, Tianjin University of Technology, Tianjin 300384 (China); Li, Mingji, E-mail: limingji@163.com [Tianjin Key Laboratory of Film Electronic and Communication Devices, School of Electronics Information Engineering, Tianjin University of Technology, Tianjin 300384 (China); Qiu, Guojun [Tianjin Key Laboratory of Organic Solar Cells and Photochemical Conversion, School of Chemistry & Chemical Engineering, Tianjin University of Technology, Tianjin 300384 (China); Li, Cuiping; Qu, Changqing; Yang, Baohe [Tianjin Key Laboratory of Film Electronic and Communication Devices, School of Electronics Information Engineering, Tianjin University of Technology, Tianjin 300384 (China)

    2015-05-25

    Highlights: • MgO nanocrystals were prepared using DC arc plasma jet CVD method. • The growth time does not exceed 10 min in process of the synthesis. • The samples were found to consist of cubic MgO nanobelts and nanosheets. • Nanocrystals contain contacts, rough edges, vacancies, and doping defects. • The samples exhibited excellent electrochemical biosensing properties. - Abstract: MgO nanocrystals were prepared using a simple direct current arc plasma jet chemical vapor deposition method. Magnesium nitrate was used as source material and Mo film was used as a substrate and catalyst. The high-temperature plasma produced ensured rapid synthesis of the MgO nanocrystals. The as-prepared nanocrystals were characterized by field-emission scanning electron microscopy, high-resolution transmission electron microscopy, X-ray diffraction, energy-dispersive spectroscopy, Fourier transform infrared spectrometry, ultraviolet–visible spectrophotometry, and photoluminescence measurements. The as-synthesized samples were found to consist of cubic MgO nanobelts and nanosheets with large surface areas and low coordination oxide ions, and contained numerous contacts, rough edges, vacancies, and doping defects. The nanostructures exhibited excellent electrochemical sensing properties with high-sensing sensitivity toward ascorbic acid. Their high electrocatalytic activity was attributed to the effect of defects and the surface electron transfer ability of the one-dimensional MgO nanobelts.

  10. Novel LLM series high density energy materials: Synthesis, characterization, and thermal stability

    Science.gov (United States)

    Pagoria, Philip; Zhang, Maoxi; Tsyshevskiy, Roman; Kuklja, Maija

    Novel high density energy materials must satisfy specific requirements, such as an increased performance, reliably high stability to external stimuli, cost-efficiency and ease of synthesis, be environmentally benign, and be safe for handling and transportation. During the last decade, the attention of researchers has drifted from widely used nitroester-, nitramine-, and nitroaromatic-based explosives to nitrogen-rich heterocyclic compounds. Good thermal stability, the low melting point, high density, and moderate sensitivity make heterocycle materials attractive candidates for use as oxidizers in rocket propellants and fuels, secondary explosives, and possibly as melt-castable ingredients of high explosive formulations. In this report, the synthesis, characterization, and results of quantum-chemical DFT study of thermal stability of LLM-191, LLM-192 and LLM-200 high density energy materials are presented. Work performed under the auspices of the DOE by the LLNL (Contract DE-AC52-07NA27344). This research is supported in part by ONR (Grant N00014-12-1-0529) and NSF. We used NSF XSEDE (Grant DMR-130077) and DOE NERSC (Contract DE-AC02-05CH11231) resources.

  11. Synthesis and characterization of covalent diphenylalanine nanotube-folic acid conjugates

    Science.gov (United States)

    Castillo, John J.; Rindzevicius, Tomas; Wu, Kaiyu; Schmidt, Michael S.; Janik, Katarzyna A.; Boisen, Anja; Svendsen, Winnie; Rozlosnik, Noemi; Castillo-León, Jaime

    2014-07-01

    Herein, we describe the synthesis and characterization of a covalent nanoscale assembly formed between diphenylalanine micro/nanotubes (PNT) and folic acid (FA). The conjugate was obtained via chemical functionalization through coupling of amine groups of PNTs and carboxylic groups of FA. The surface analysis of PNT-FA indicated the presence of FA aggregates on the surface of PNTs. The covalent interaction between FA and self-assembled PNTs was further investigated using fluorescence microscopy, Raman and surface-enhanced Raman scattering (SERS) spectroscopies. The SERS experiments were performed on a large area silver-capped (diameter of 62 nm) silicon nanopillars with an approximate height of 400 nm and a width of 200 nm. The results showed that the PNT-FA synthesis procedure preserves the molecular structure of FA. The PNT-FA conjugate presented in this study is a promising candidate for applications in the detection and diagnosis of cancer or tropical diseases such as leishmaniasis and as a carrier nanosystem delivering drugs to malignant tumors that overexpress folate receptors.

  12. Synthesis, isolation and characterization of methyl levulinate from cellulose catalyzed by extremely low concentration acid

    Institute of Scientific and Technical Information of China (English)

    Hui; Li; Lincai; Peng; Lu; Lin; Keli; Chen; Heng; Zhang

    2013-01-01

    A direct synthesis of methyl levulinate from cellulose alcoholysis in methanol medium under mild condition(180 210 C)catalyzed by extremely low concentration sulfuric acid(0.01 mol/L)and the product isolation were developed in this study.Effects of different process variables towards the catalytic performance were performed as a function of reaction time.The results indicated that sulfuric acid concentration,temperature and initial cellulose concentration had significant effects on the synthesis of methyl levulinate.An optimized yield of around 50%was achieved at 210 C for 120 min with sulfuric acid concentration of 0.01 mol/L and initial cellulose concentration below 100 g/L.The resulting product mixture was isolated by a distillation technique that combines an atmospheric distillation with a vacuum distillation where n-dodecane was added to help distill the heavy fraction.The light fraction including mainly methanol could be reused as the reaction medium without any substantial change in the yield of methyl levulinate.The chemical composition and structural of lower heavy fraction were characterized by GC/MS,FTIR,1H-NMR and13C-NMR techniques.Methyl levulinate was found to be a major ingredient of lower heavy fraction with the content over 96%.This pathway is efficient,environmentally benign and economical for the production of pure levulinate esters from cellulose.

  13. Novel magnetic nanomaterials: Synthesis, characterization and study of their catalytic application

    Energy Technology Data Exchange (ETDEWEB)

    Judy Azar, Amir Reza; Mohebbi, Sajjad, E-mail: smohebbi@uok.ac.ir

    2015-11-15

    A simple chemical process has been successfully developed to synthesize some N{sub 2}O{sub 2} Schiff base metal complexes as an organic shell on an inorganic support. Schiff base complexes of Ni(II), Cu(II), Co(II) and Zn(II) were immobilized on modified magnetic support. The magnetic support was modified using tetraethylorthosilicate (TEOS) and then functionalized with Schiff base complexes of transition metals ions. The synthesized nanocatalysts show high catalytic activity and selectivity in the oxidation of sulfide compounds to corresponding sulfoxides. The hybrid nanomaterials were fully characterized with different physicochemical techniques including Fourier transform Infrared, X-ray diffraction analysis, thermal gravimeter, scanning electron microscopy and transmission electron microscopy. Also, magnetic properties of hybrid nanomaterials were measured by Alternative Gradient Field Magnetometer. Magnetic measurements showed that the coating of nanomaterials reduces the magnetization indicating modification of NPs with Schiff base complexes. - Highlights: • Designing an easy procedure for synthesis of magnetic heterogeneous catalysts. • Anchoring of variety of Lewis acids on magnetic support. • Synthesis of materials as environmentally friendly systems for catalytic reaction. • Novel high-yield and selective catalysts for oxidation reaction. • Recyclable catalysts with excellent reusability.

  14. Synthesis and Characterization of Core-shell ZrO2/PAAEM/PS Nanoparticles

    Directory of Open Access Journals (Sweden)

    Jiang XC

    2008-01-01

    Full Text Available Abstract This work demonstrates the synthesis of core-shell ZrO2/PAAEM/PS nanoparticles through a combination of sol–gel method and emulsifier-free emulsion polymerizaiton. By this method, the modified nanometer ZrO2cores were prepared by chemical modification at a molecular level of zirconium propoxide with monomer of acetoacetoxyethylmethacrylate (AAEM, and then copolymerized with vinyl monomer to form uniform-size hybrid nanoparticles with diameter of around 250 nm. The morphology, composition, and thermal stability of the core-shell particles were characterized by various techniques including transmission electron microscopy (TEM, X-ray diffractometer (XRD, Fourier transform infrared spectroscopy (FTIR, X-ray photoelectron spectroscopy (XPS, and thermal-gravimetry analyzer (TGA. The results indicate that the inorganic–organic nanocomposites exhibit good thermal stability with the maximum decomposition temperature of ~447 °C. This approach would be useful for the synthesis of other inorganic–organic nanocomposites with desired functionalities.

  15. Chemical synthesis and stabilization of magnesium substituted brushite

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Donghyun [Department of Biomedical Engineering, Chung-Ang University, 221 Heukseok-Dong, Dongjak-Gu, Seoul 156-756 (Korea, Republic of); Kumta, Prashant N., E-mail: pkumta@pitt.edu [Department of Bioengineering, University of Pittsburgh, Pittsburgh, PA 15260 (United States); Department of Mechanical Engineering and Materials Sceince, University of Pittsburgh, Pittsburgh, PA 15260 (United States); Department of Chemical and Petroleum Engineering, University of Pittsburgh, Pittsburgh, PA 15260 (United States)

    2010-08-30

    Hydroxyapatite (Ca{sub 10}(PO{sub 4}){sub 6}(OH){sub 2}) is the most ubiquitous calcium phosphate phase used in implant coatings and more recently in gene/drug delivery applications due to its chemical stability under normal physiological conditions (37 deg. C, pH {approx} 7.5, 1 atm.). However, different calcium phosphate phases, such as brushite (CaH(PO{sub 4}){center_dot}2(H{sub 2}O)) and tricalcium phosphate (Ca{sub 3}(PO{sub 4}){sub 2}) which are thermodynamically unstable under physiological conditions are also being explored for biomedical applications. One way of stabilizing these phases under physiological conditions is to introduce magnesium to substitute for calcium in the brushite lattice. The role of magnesium as a stabilizing agent for synthesizing brushite under physiological conditions at room temperature has been studied. Chemical analysis, Fourier transform infrared spectroscopy and X-ray diffraction have also been conducted to validate the formation of magnesium substituted brushite under physiological conditions.

  16. Cu(II AND Zn(II COMPLEX COMPOUNDS WITH BIGUANIDES AROMATIC DERIVATIVES. SYNTHESIS, CHARACTERIZATION, BIOLOGICAL ACTIVITY

    Directory of Open Access Journals (Sweden)

    Ticuţa Negreanu-Pîrjol

    2011-05-01

    Full Text Available In this paper we report the synthesis, physical-chemical characterization and antimicrobial activity of some new complex compounds of hetero-aromatic biguanides ligands, chlorhexidine base (CHX and chlorhexidine diacetate (CHXac2 with metallic ions Cu(II and Zn(II, in different molar ratio. The synthesized complexes were characterized by elemental chemical analysis and differential thermal analysis. The stereochemistry of the metallic ions was determined by infrared spectra, UV-Vis, EPR spectroscopy and magnetic susceptibility in the aim to establish the complexes structures. The biological activity of the new complex compounds was identified in solid technique by measuring minimum inhibition diameter of bacterial and fungal culture, against three standard pathogen strains, Escherichia coli ATCC 25922, Staphilococcus aureus ATCC 25923 and Candida albicans ATCC 10231. The results show an increased specific antimicrobial activity for the complexes chlorhexidine:Cu(II 1:1 and 1:2 compared with the one of the Zn(II complexes.

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

    Science.gov (United States)

    1983-11-04

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

  18. Nanostructured Thin Film Synthesis by Aerosol Chemical Vapor Deposition for Energy Storage Applications

    Science.gov (United States)

    Chadha, Tandeep S.

    Renewable energy sources offer a viable solution to the growing energy demand while mitigating concerns for greenhouse gas emissions and climate change. This has led to a tremendous momentum towards solar and wind-based energy harvesting technologies driving efficiencies higher and costs lower. However, the intermittent nature of these energy sources necessitates energy storage technologies, which remain the Achilles heel in meeting the renewable energy goals. This dissertation focusses on two approaches for addressing the needs of energy storage: first, targeting direct solar to fuel conversion via photoelectrochemical water-splitting and second, improving the performance of current rechargeable batteries by developing new electrode architectures and synthesis processes. The aerosol chemical vapor deposition (ACVD) process has emerged as a promising single-step approach for nanostructured thin film synthesis directly on substrates. The relationship between the morphology and the operating parameters in the process is complex. In this work, a simulation based approach has been developed to understand the relationship and acquire the ability of predicting the morphology. These controlled nanostructured morphologies of TiO2 , compounded with gold nanoparticles of various shapes, are used for solar water-splitting applications. Tuning of light absorption in the visible-light range along with reduced electron-hole recombination in the composite structures has been demonstrated. The ACVD process is further extended to a novel single-step synthesis of nanostructured TiO2 electrodes directly on the current collector for applications as anodes in lithium-ion batteries, mainly for electric vehicles and hybrid electric vehicles. The effect of morphology of the nanostructures has been investigated via experimental studies and electrochemical transport modelling. Results demonstrate the exceptional performance of the single crystal one-dimensional nanostructures over granular

  19. Synthesis of multi-walled carbon nanotubes using CoMnMgO catalysts through catalytic chemical vapor deposition

    Science.gov (United States)

    Yang, Wen; Feng, Yan-Yan; Jiang, Cheng-Fa; Chu, Wei

    2014-12-01

    The CoMgO and CoMnMgO catalysts are prepared by a co-precipitation method and used as the catalysts for the synthesis of carbon nanotubes (CNTs) through the catalytic chemical vapor deposition (CCVD). The effects of Mn addition on the carbon yield and structure are investigated. The catalysts are characterized by temperature programmed reduction (TPR) and X-ray diffraction (XRD) techniques, and the synthesized carbon materials are characterized by transmission electron microscopy (TEM) and thermo gravimetric analysis (TG). TEM measurement indicates that the catalyst CoMgO enclosed completely in the produced graphite layer results in the deactivation of the catalyst. TG results suggest that the CoMnMgO catalyst has a higher selectivity for CNTs than CoMgO. Meanwhile, different diameters of CNTs are synthesized by CoMnMgO catalysts with various amounts of Co content, and the results show that the addition of Mn avoids forming the enclosed catalyst, prevents the formation of amorphous carbon, subsequently promotes the growth of CNTs, and the catalyst with decreased Co content is favorable for the synthesis of CNTs with a narrow diameter distribution. The CoMnMgO catalyst with 40% Co content has superior catalytic activity for the growth of carbon nanotubes.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2003-11-18

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

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

    Directory of Open Access Journals (Sweden)

    NITIN G. GHODILE

    2012-07-01

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

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

    Directory of Open Access Journals (Sweden)

    S. V. Prabhakar Vattikuti

    2015-01-01

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

  3. Synthesis and characterization of MoS2 nanosheets.

    Science.gov (United States)

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

    2016-02-19

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

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

    Directory of Open Access Journals (Sweden)

    Jumbad H. Tomma

    2014-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2010-10-01

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

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

    Indian Academy of Sciences (India)

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

    2016-10-01

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

  7. Synthesis and characterization of furazan energetics ADAAF and DOATF

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-01-01

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

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

    Science.gov (United States)

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

    2016-11-01

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

  9. Synthesis and characterization of phosphorescent platinum complexes containing phenylpyridazine

    Energy Technology Data Exchange (ETDEWEB)

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

    2004-01-05

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

  10. Synthesis and characterization of molybdenum incorporated mesoporous aluminophosphate

    Science.gov (United States)

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

    2006-07-01

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

  11. NOVEL PREPARATION AND MAGNETO CHEMICAL CHARACTERIZATION OF NANOPARTICLE MIXED ALCOHOL CATALYSTS

    Energy Technology Data Exchange (ETDEWEB)

    Seetala V. Naidu; Upali Siriwardane

    2005-05-24

    introducing a novel method of nanoparticle metal oxide co-entrapped sol-gel that gave the highest metal loading with precise control and reproducibility, and greater mechanical strength of granules than the metal nitrate solution co-entrapping and wet impregnation methods. Both, slurry-phase-batch and gas-phase-continuous-flow, reactors were used for syngas conversion reactions. Our investigations of Co and Fe thin film deposited micro-reactors showed higher CO/H{sub 2} conversion for Fe compared to Co. The catalytic activity for CO/H{sub 2} conversion was observed in the increasing order for the nanocatalysts Cu, Co, Fe, Co/Fe, Cu/Co and Cu/Fe in alumina sol-gel support, and Co/Fe showed the highest yield for methane. The optimization of CO/H{sub 2} ratio indicated that 1:1 ratio gave more alkanes distribution in F-T process with Co/Fe (6% each) impregnated on alumina. We could estimate the activity of catalysts (involving Co, Fe) during hydrogenation and after catalytic reaction using magnetization studies. In summary our accomplishments are: (1) Novel chemical methods for the synthesis of (5 nm) Fe, Co, Cu nanoparticles with narrow size distribution. (2) Developing a method of metal oxide nanoparticles addition to alumina/silica sol-gel to control metal loading of pure and mixed metal catalysts compositions in high yields. (3) A low-cost GC-TCD system to analyze wide spectrum of alkanes (F-T reaction products). (4) Fe/Co mixed metal alumina/silica mesoporous catalysts with higher FT activity. (5) Characterizing nanoparticle catalysts and supports for detail understanding of FT-process.

  12. Characterization of biomass burning particles: chemical composition and processing

    Science.gov (United States)

    Hudson, P. K.; Murphy, D. M.; Cziczo, D. J.; Thomson, D. S.; Degouw, J.; Warneke, C.

    2003-12-01

    During the Intercontinental Transport and Chemical Transformation (ITCT) mission in April and May of 2002, a forest fire plume was intercepted over Utah on May 19. Gas phase species acetonitrile (CH3CN) (a biomass burning tracer) and carbon monoxide (CO) measured greater than five fold enhancements over background concentrations during this plume crossing. In the 100 sec plume crossing, the Particle Analysis by Laser Mass Spectrometry (PALMS) instrument acquired 202 positive mass spectra of biomass burning particles. Many of these particles contained potassium in addition to organics, carbon, and NO+ (which is a signature for any nitrogen containing compound such as ammonium or nitrate). From characterization of the particle mass spectra obtained during the plume crossing, a qualitative signature has been determined for identifying biomass burning particles. By applying this analysis to the entire ITCT mission, several transport events of smoke plumes have been identified and were confirmed by gas phase measurements. Additional species, such as sulfate, found in the mass spectra of the transported particles indicated processing or aging of the biomass burning particles that had taken place. The analysis has been extended to other field missions (Crystal-Face, ACCENT, and WAM) to identify biomass burning particles without the added benefit of gas phase measurements.

  13. Chemical and Biological Characterization of Oleanane Triterpenoids from Soy

    Directory of Open Access Journals (Sweden)

    David G. Popovich

    2009-08-01

    Full Text Available Soyasaponins are a group of complex and structural diverse oleanane triterpenoids found in soy (Glycine max and other legumes. They are primarily classified into two main groups − group A and B − based on the attachment of sugar moieties at positions C-3 and C-22 of the ring structures. Group A soyasaponins are bidesmosidic, while group B soyasaponins are monodesmosidic. Group B soyasaponins are further classified into two subcategories known as 2,3-dihydro-2,5-dihydroxy-6 -methyl-4H-pyran-4-one (DDMP and non-DDMP conjugated molecules. The preparation and purification of soyasaponin molecules is complicated by the presence of bioactive soy isoflavones, which often overlap with soyasaponin in polarity and must removed from extracts before biological assessment. Soyasaponin extracts, aglycones of group A and B and individual group B soyasaponins such as soyasaponin I have been reported to posses specific bioactive properties, such as in vitro anti-cancer properties by modulating the cell cycle and inducing apoptosis. The isolation, chemical characterization and detection strategies by HPLC and HPLC-MS are reviewed, along with the reported bioactive effects of soyasaponin extracts and individual molecules in cultured cancer cell experiments.

  14. Chemical and biological characterization of sclerosin, an antifungal lipopeptide.

    Science.gov (United States)

    Berry, Chrystal L; Brassinga, Ann Karen C; Donald, Lynda J; Fernando, W G Dilantha; Loewen, Peter C; de Kievit, Teresa R

    2012-08-01

    Pseudomonas sp. strain DF41 produces a lipopeptide, called sclerosin that inhibits the fungal pathogen Sclerotinia sclerotiorum . The aim of the current study was to deduce the chemical structure of this lipopeptide and further characterize its bioactivity. Mass spectrometry analysis determined the structure of sclerosin to be CH(3)-(CH(2))(6)-CH(OH)-CH(2)-CO-Dhb-Pro-Ala-Leu/Ile-Ala-Val-Val-Dhb-Thr-Val-Leu/Ile-Dhp-Ala-Ala-Ala-Val-Dhb-Dhb-Ala-Dab-Ser-Val-OH, similar to corpeptins A and B of the tolaasin group, differing by only 3 amino acids in the peptide chain. Subjecting sclerosin to various ring opening procedures revealed no new ions, suggesting that this molecule is linear. As such, sclerosin represents a new member of the tolaasin lipopeptide group. Incubation of S. sclerotinia ascospores and sclerotia in the presence of sclerosin inhibited the germination of both cell types. Sclerosin also exhibited antimicrobial activity against Bacillus species. Conversely, this lipopeptide demonstrated no zoosporicidal activity against the oomycete pathogen Phytophthora infestans . Next, we assessed the effect of DF41 and a lipopeptide-deficient mutant on the growth and development of Caenorhabditis elegans larvae. We discovered that sclerosin did not protect DF41 from ingestion by and degradation in the C. elegans digestive tract. However, another metabolite produced by this bacterium appeared to shorten the life-span of the nematode compared to C. elegans growing on Escherichia coli OP50.

  15. The chemical characterization of the gene: vicissitudes of evidential assessment.

    Science.gov (United States)

    Stegenga, Jacob

    2011-01-01

    The chemical characterization of the substance responsible for the phenomenon of "transformation" of pneumococci was presented in the now famous 1944 paper by Avery, MacLeod, and McCarty. Reception of this work was mixed. Although interpreting their results as evidence that deoxyribonucleic acid (DNA) is the molecule responsible for genetic changes was, at the time, controversial, this paper has been retrospectively celebrated as providing such evidence. The mixed and changing assessment of the evidence presented in the paper was due to the work's interpretive flexibility--the evidence was interpreted in various ways, and such interpretations were justified given the neophytic state of molecular biology and methodological limitations of Avery's transformation studies. I argue that the changing context in which the evidence presented by Avery's group was interpreted partly explains the vicissitudes of the assessments of the evidence. Two less compelling explanations of the reception are a myth-making account and an appeal to the wartime historical context of its publication.

  16. Chemical surface modification of porous silicon with palladium and characterizations

    Energy Technology Data Exchange (ETDEWEB)

    Kanungo, J.; Maji, S.; Saha, H. [IC Design and Fabrication Centre, Department of Electronics and Telecommunication Engineering, Jadavpur University, Kolkata 700032 (India); Basu, S., E-mail: sukumar_basu@yahoo.co.u [IC Design and Fabrication Centre, Department of Electronics and Telecommunication Engineering, Jadavpur University, Kolkata 700032 (India)

    2010-03-15

    Porous silicon (PS) was formed on p-type crystalline silicon of (1 0 0) orientation and 2-5 OMEGA cm resistivity by the electrochemical anodization method using HF and ethanol as the electrolyte. Adjusting the current density and the HF concentration in the electrolyte the porosity of the samples were varied from 40% to 60%. The porous silicon surface was modified with PdCl{sub 2} solution by a low cost chemical method. Both the unmodified and the modified PS were thoroughly characterized by the EDAX analysis, the digital X-ray image mapping and the XPS study. Electrical characteristics were performed by the I-V measurements for both the lateral and the sandwich structures using Al metal contact. The I-V characteristics of the modified PS for all the porosity were more reproducible compared to the unmodified PS surfaces. It was further observed that the conductivity increased with the increasing porosity for the Pd-modified surfaces whereas it decreased for the unmodified PS.

  17. Wet Chemical Synthesis and Screening of Thick Porous Oxide Films for Resistive Gas Sensing Applications

    Directory of Open Access Journals (Sweden)

    Wilhelm F. Maier

    2006-11-01

    Full Text Available A method of wet chemical synthesis suitable for high throughput and combinatorial applications has been developed for the synthesis of porous resistive thick-film gas sensors. This method is based on the robot-controlled application of unstable metal oxide suspensions on an array of 64 inter-digital electrodes positioned on an Al2O3 substrate. SnO2, WO3, ZrO2, TiO2, CeO2, In2O3 and Bi2O3 were chosen as base oxides, and were optimised by doping or mixed oxide formation. The parallel synthesis of mixed oxide sensors is illustrated by representative examples. The electrical characteristics and the sensor performance of the films were measured by high-throughput impedance spectroscopy while supplying various test gases (H2, CO, NO, NO2, propene. Data collection, data mining techniques applied and the best potential sensor materials discovered are presented.

  18. Systematic methods for synthesis and design of sustainable chemical and biochemical processes

    DEFF Research Database (Denmark)

    Gani, Rafiqul

    , biomass, coal, natural gas, rock, etc., that are usually extracted), to a bigger set of basic chemical products (such as, ethylene, benzene sulfuric acid, ammonia, etc., that are produced in large quantities), to an even bigger set of intermediates (such as, methanol, urea, succinic acid, ethylene glycol...... from the renewable resources, the sustainability of the product and therefore the process can be improved. Also, the number of alternatives that exist provide opportunities and challenges to find the best synthesis routes, for example, for process intensification or a multi-product processing complex...... like a biorefinery. The process synthesis design problem can be formulated as one where first a synthesis-design target (a process with desired qualities) is defined and then design alternatives (process flowsheets for different raw material-product connection) that match the target are identified...

  19. Alternative fuels and chemicals from synthesis gas. Quarterly report, April 1--June 30, 1995

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    1995-12-31

    The overall objectives of this program are to investigate potential technologies for the conversion of synthesis gas to oxygenated and hydrocarbon fuels and industrial chemicals, and to demonstrate the most promising technologies at DOE`s LaPorte, Texas, Slurry Phase Alternative Fuels Development Unit (AFDU). The program will involve a continuation of the work performed under the Alternative Fuels from Coal-Derived Synthesis Gas Program and will draw upon information and technologies generated in parallel current and future DOE-funded contracts. The paper reports the progress on the following tasks: engineering and modifications: AFDU shakedown, operations, deactivation and disposal; and research and development on new processes for DME, chemistry and catalyst development, and oxygenates via synthesis gas.

  20. Wet-chemical synthesis and characteristics of Au nanoshell

    Institute of Scientific and Technical Information of China (English)

    LIU Zhongxin; SONG Hongwei; YU Lixin; YANG Linmei; PAN Guohui

    2005-01-01

    Gold nanoshells were prepared by an easy wet-chemical method, with Ag nanoparticles used as the templates. Transmission electron microscopy (TEM) indicated that the shells were sphere in shape, the size was homogenous, being about 20 nm, and no hard agglomerates were observed. The plasma resonance absorption of gold was tuned from visible to near-infrared (NIR) with the increased volume of HAuCl4. The temperature grads (ΔT) of the gold nanoshell hydrosol under the exposure of an 808-nm optical fiber laser with different power densities were measured. The highest ΔT was 30℃ (5 W/cm2, irradiation area was 2 cm2). This kind of gold nanoshell hydrosol is a promising material to be used in biomedicine such as photothermal cancer therapy, and its special photothermal convert property will photothermally trigger drug release.

  1. Accelerated Chemical Reactions and Organic Synthesis in Leidenfrost Droplets.

    Science.gov (United States)

    Bain, Ryan M; Pulliam, Christopher J; Thery, Fabien; Cooks, R Graham

    2016-08-22

    Leidenfrost levitated droplets can be used to accelerate chemical reactions in processes that appear similar to reaction acceleration in charged microdroplets produced by electrospray ionization. Reaction acceleration in Leidenfrost droplets is demonstrated for a base-catalyzed Claisen-Schmidt condensation, hydrazone formation from precharged and neutral ketones, and for the Katritzky pyrylium into pyridinium conversion under various reaction conditions. Comparisons with bulk reactions gave intermediate acceleration factors (2-50). By keeping the volume of the Leidenfrost droplets constant, it was shown that interfacial effects contribute to acceleration; this was confirmed by decreased reaction rates in the presence of a surfactant. The ability to multiplex Leidenfrost microreactors, to extract product into an immiscible solvent during reaction, and to use Leidenfrost droplets as reaction vessels to synthesize milligram quantities of product is also demonstrated.

  2. Synthesis of Aligned Carbon Nanotubes by Thermal Chemical Vapor Deposition

    Institute of Scientific and Technical Information of China (English)

    LI Gang; ZHOU Ming; MA Weiwei; CAI Lan

    2009-01-01

    Single crystal silicon was found to be very beneficial to the growth of aligned carbon nanotubes by chemical vapor deposition with C2H2 as carbon source. A thin film of Ni served as catalyst was deposited on the Si substrate by the K575X Peltier Cooled High Resolution Sputter Coater before growth. The growth properties of carbon nanotubes were studied as a function of the Ni catalyst layer thickness. The diameter, growth rate and areal density of the carbon nanotubes were controlled by the initial thickness of the catalyst layer. Steric hindrance between nanotubes forces them to grow in well-aligned manner at an initial stage of growth. Transmission electron microscope analysis revealed that nanotubes grew by a tip growth mechanism.

  3. Chemical vapor deposition synthesis of tunable unsubstituted polythiophene.

    Science.gov (United States)

    Nejati, Siamak; Lau, Kenneth K S

    2011-12-20

    Despite having exceptional electroactive properties, applications of unsubstituted polythiophene (PTh) have been limited due to its insolubility. To overcome this challenge, we have employed oxidative chemical vapor deposition (oCVD) as a unique liquid-free technique to enable the oxidative polymerization of PTh using thiophene as the starting monomer and vanadium oxytrichloride as an effective vaporizable oxidant initiator. Vibrational and phototelectron spectroscopy indicated the formation of unsubstituted polythiophene. Cyclic voltammetry revealed its electrochromic behavior in solution. Significantly, polymer conjugation length and electrical conductivity can be tuned by controlling oCVD process variables. Polymerization is found to be adsorption-limited, so by providing sufficient monomer and limiting the amount of initiator at the growth surface, PTh is believed to be formed through α-α thiophene linkages.

  4. Synthesis of mullite coatings by chemical vapor deposition

    Energy Technology Data Exchange (ETDEWEB)

    Mulpuri, R.P.; Auger, M.; Sarin, V.K. [Boston Univ., MA (United States)

    1996-08-01

    Formation of mullite on ceramic substrates via chemical vapor deposition was investigated. Mullite is a solid solution of Al{sub 2}O{sub 3} and SiO{sub 2} with a composition of 3Al{sub 2}O{sub 3}{circ}2SiO{sub 2}. Thermodynamic calculations performed on the AlCl{sub 3}-SiCl{sub 4}-CO{sub 2}-H{sub 2} system were used to construct equilibrium CVD phase diagrams. With the aid of these diagrams and consideration of kinetic rate limiting factors, initial process parameters were determined. Through process optimization, crystalline CVD mullite coatings have been successfully grown on SiC and Si{sub 3}N{sub 4} substrates. Results from the thermodynamic analysis, process optimization, and effect of various process parameters on deposition rate and coating morphology are discussed.

  5. Calcium, Strontium and Barium Homogeneous Catalysts for Fine Chemicals Synthesis.

    Science.gov (United States)

    Sarazin, Yann; Carpentier, Jean-François

    2016-12-01

    The large alkaline earths (Ae), calcium, strontium and barium, have in the past 15 years yielded a brand new generation of heteroleptic molecular catalysts for the production of fine chemicals. However, the integrity of these complexes is often plagued by ligand redistribution equilibria in solution. This personal account retraces the paths followed in our research group towards the design of stable heteroleptic alkalino-earth complexes, including the use of intramolecular noncovalent Ae···H-Si and Ae···F-C interactions. Their implementation as homogenous precatalysts for reactions such as the intramolecular and intermolecular hydroamination and hydrophosphination of activated alkenes, the hydrophosphonylation of ketones, and the dehydrogenative coupling of amines and hydrosilanes that enable the efficient and controlled formations of CP, CN, or SiN σ-bonds, is presented in a synthetic perspective that highlights their overall outstanding catalytic performance.

  6. Chemoenzymatic Synthesis and Chemical Recycling of Poly(ester-urethanes

    Directory of Open Access Journals (Sweden)

    Hiroto Hayashi

    2011-08-01

    Full Text Available Novel poly(ester-urethanes were prepared by a synthetic route using a lipase that avoids the use of hazardous diisocyanate. The urethane linkage was formed by the reaction of phenyl carbonate with amino acids and amino alcohols that produced urethane-containing diacids and hydroxy acids, respectively. The urethane diacid underwent polymerization with polyethylene glycol and a,w-alkanediols and also the urethane-containing hydroxy acid monomer was polymerized by the lipase to produce high-molecular-weight poly(ester-urethanes. The periodic introduction of ester linkages into the polyurethane chain by the lipase-catalyzed polymerization afforded chemically recyclable points. They were readily depolymerized in the presence of lipase into cyclic oligomers, which were readily repolymerized in the presence of the same enzyme. Due to the symmetrical structure of the polymers, poly(ester-urethanes synthesized in this study showed higher Tm, Young’s modulus and tensile strength values.

  7. SYNTHESIS, CHARACTERIZATION AND BIOLOGICAL EVALUATION OF SOME NOVEL THIAZOLIDINONES DERIVATIVES

    Directory of Open Access Journals (Sweden)

    S. Chandramohan et al.

    2012-05-01

    Full Text Available The main objective of the medicinal chemistry is to synthesize the compounds that show promising activity and therapeutic agents with lower toxicity. Thiazolidinone are very useful compound with well known biological activities. Notable among these are antibacterial, antiviral, analgesic, anti-inflammatory, antitubercular and anticonvulsant. In the current research work, three novel substituted thiazolidin-4-one derivatives were prepared from the corresponding Schiff bases and 2-mercapto acetic acid in benzene using Stark and Dean Apparatus. The identification and characterization of synthesized compounds were carried out by Elemental analysis, FT-IR and NMR data to ascertain that all synthesized compounds were of different chemical nature than the respective parent compound. The synthesized compounds showed good antibacterial activity against Escherichia Coli, Staphylococcus, Pseudomonas aeruginosa and Salmonella typhi.

  8. Low temperature synthesis and characterization of carbonated hydroxyapatite nanocrystals

    Science.gov (United States)

    Anwar, Aneela; Asghar, Muhammad Nadeem; Kanwal, Qudsia; Kazmi, Mohsin; Sadiqa, Ayesha

    2016-08-01

    Carbonate substituted hydroxyapatite (CHA) nanorods were synthesized via coprecipitation method from aqueous solution of calcium nitrate tetrahydrate and diammonium hydrogen phosphate (with urea as carbonate ion source) in the presence of ammonium hydroxide solution at 70 °C at the conditions of pH 11. The obtained powders were physically characterized using transmission electron microscopy (TEM), X-ray powder diffraction analysis (XRD), and FTIR and Raman spectroscopy. The particle size was evaluated by Dynamic light scattering (DLS). The chemical structural analysis of as prepared sample was performed using X-ray photoelectron spectroscopy (XPS). After ageing for 12 h, and heat treatment at 1000 °C for 1 h, the product was obtained as highly crystalline nanorods of CHA.

  9. Synthesis and characterization of stable aqueous dispersions of graphene

    Indian Academy of Sciences (India)

    Ujjal Kumar Sur; Abhijit Saha; Aparna Datta; Balaprasad Ankamwar; Farah Surti; Sannak Dutta Roy; Debasish Roy

    2016-02-01

    A stable aqueous dispersion (5 mg ml$^{−1}$) of graphene was synthesized by a simple protocol based on three-step reduction of graphene oxide (GO) dispersion synthesized using the modified version of Hummers and Offeman method. Reduction of GO was carried out using sodium borohydride, hydrazine hydrate and dimethyl hydrazine as reducing agents. The chemically synthesized graphene was characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), UV–visible absorption spectroscopy, Fourier transform infrared (FTIR) and Raman spectroscopy, thermogravimetric analysis (TGA), optical microscopy. The stability of aqueous dispersions of graphene was confirmed through zeta potential measurements and the negative zeta potentials of 55–60 mV were obtained indicating the high stability of aqueous graphene dispersions.

  10. Carbon nanotube catalysts: recent advances in synthesis, characterization and applications.

    Science.gov (United States)

    Yan, Yibo; Miao, Jianwei; Yang, Zhihong; Xiao, Fang-Xing; Yang, Hong Bin; Liu, Bin; Yang, Yanhui

    2015-05-21

    Carbon nanotubes are promising materials for various applications. In recent years, progress in manufacturing and functionalizing carbon nanotubes has been made to achieve the control of bulk and surface properties including the wettability, acid-base properties, adsorption, electric conductivity and capacitance. In order to gain the optimal benefit of carbon nanotubes, comprehensive understanding on manufacturing and functionalizing carbon nanotubes ought to be systematically developed. This review summarizes methodologies of manufacturing carbon nanotubes via arc discharge, laser ablation and chemical vapor deposition and functionalizing carbon nanotubes through surface oxidation and activation, doping of heteroatoms, halogenation, sulfonation, grafting, polymer coating, noncovalent functionalization and nanoparticle attachment. The characterization techniques detecting the bulk nature and surface properties as well as the effects of various functionalization approaches on modifying the surface properties for specific applications in catalysis including heterogeneous catalysis, photocatalysis, photoelectrocatalysis and electrocatalysis are highlighted.

  11. Synthesis and characterization of single-crystalline alumina nanowires

    Institute of Scientific and Technical Information of China (English)

    ZHAO Qing; XU Xiang-yu; ZHANG Hong-zhou; CHEN Yao-feng; XU Jun; YU Da-peng

    2005-01-01

    Alumina nanowires were synthesized on large-area silicon substrate via simple thermal evaporation method of heating a mixture of aluminum and alumina powders without using any catalyst or template. The phase structure and the surface morphology of the as-grown sample were analyzed by X-ray diffractometry(XRD) and scanning electron microscopy (SEM), respectively. The chemical composition and the microstructure of the as-grown alumina nanowires were characterized using transmission electron microscope(TEM). The nanowires are usually straight and the single crystalline has average diameter of 40 nm and length of 3 - 5 μm. The growth direction is along the [002] direction. Well aligned alumina nanowire arrays were observed on the surface of many large particles. The catalyst-free growth of the alumina nanowires was explained under the framework of a vapor-solid(VS)growth mechanism. This as-synthesized alumina nanowires could find potential applications in the fabrication of nanodevices.

  12. Synthesis, characterization and vibrational properties of p-fluorosulfinylaniline.

    Science.gov (United States)

    Páez Jerez, Ana L; Flores Antognini, Andrea; Cutin, Edgardo H; Robles, Norma L

    2015-02-25

    The reaction of p-fluoroaniline and SOCl2 rendered p-fluorosulfinylaniline in good yield. The obtained dark yellowish liquid compound was characterized by NMR, UV-visible, FT-IR and Raman spectroscopies. The observed features were consistent with the existence of only one conformer, belonging to the CS symmetry group. A tentative assignment of the vibrational modes was performed on the basis of experimental spectra and quantum chemical calculations at different levels of theory (B3LYP and MP2 with 6-31+G(d), 6-311+G(d) and 6-311+G(df) basis sets). The conformational and vibrational properties of p-fluorosulfinylaniline were in good agreement with experimental data reported for other substituted sulfinylanilines and p-halogenanilines.

  13. Synthesis and characterization of polyaniline coated gold nanocomposites

    Energy Technology Data Exchange (ETDEWEB)

    Zuber, Siti Nurzulaiha Mohd; Kamarun, Dzaraini; Zaki, Hamizah; Kamarudin, Mohamad Shukri [Faculty of Applied Sciences, Universiti Teknologi MARA (UiTM), Shah Alam, 40450 Selangor Darul Ehsan (Malaysia); Thomas, Sabu; Kalarikkal, Nandakumar [International and Inter University Centre of Nanoscience and Nanotechnoogy, Mahatma Ghandi University, Priyadarsini Hills Kottayam, Kerala India-686560 (India)

    2015-08-28

    Considerable attention has been drawn during the last two decades to prepare nanocomposites consists of conducting polymer and noble metal due to their potential ability to generate a new class of material with novel optical, chemical, electronic or mechanical properties for various applications. In this work, an attempt has been made to synthesize nanocomposite of polyaniline (PANI) coated with gold nanoparticles (AuNPs) chemically with various types of surfactants such as polyvinylpyrrolidone (PVP), and sodium dodecyl sulphate (SDS) which act as stabilizing agents to help in stabilization of the PANI/Gold nanocomposites system. The synthesized nanocomposites were characterized by UV-Visible, field emission scanning electron microscope (FESEM) and particle size analyzer (PSA). The formation of finger like structure can be seen in the FESEM images when the AuNPs were incorporated into the polymer matrix. The EDX data showed that 18.66% and 12.67% of AuNPs atoms were present in the composite system thus proved the incorporation of AuNPs into the polymer matrix. A small red shift of the absorption peak in the UV-Vis of both PANI/AuNPs composites system may be due to the incorporation of AuNPs in the PANI matrix.

  14. Synthesis, characterization and gas sensing property of hydroxyapatite ceramic

    Indian Academy of Sciences (India)

    M P Mahabole; R C Aiyer; C V Ramakrishna; B Sreedhar; R S Khairnar

    2005-10-01

    Hydroxyapatite (HAp) biomaterial ceramic was synthesized by three different processing routes viz. wet chemical process, microwave irradiation process, and hydrothermal technique. The synthesized ceramic powders were characterized by SEM, XRD, FTIR and XPS techniques. The dielectric measurements were carried out as a function of frequency at room temperature and the preliminary study on CO gas sensing property of hydroxyapatite was investigated. The XRD pattern of the hydroxyapatite biomaterial revealed that hydroxyapatite ceramic has hexagonal structure. The average crystallite size was found to be in the range 31–54 nm. Absorption bands corresponding to phosphate and hydroxyl functional groups, which are characteristic of hydroxyapatite, were confirmed by FTIR. The dielectric constant was found to vary in the range 9–13 at room temperature. Hydroxyapatite can be used as CO gas sensor at an optimum temperature near 125°C. X-ray photoelectron spectroscopic studies showed the Ca/P ratio of 1.63 for the HAp sample prepared by chemical process. The microwave irradiation technique yielded calcium rich HAp whereas calcium deficient HAp was obtained by hydrothermal method.

  15. Amidated pectin based hydrogels: synthesis, characterization and cytocompatibility study.

    Science.gov (United States)

    Mishra, R K; Singhal, J P; Datt, M; Banthia, A K

    2007-01-01

    The design and development of pectin-based hydrogels were attempted through the chemical modification of pectin with diethanolamine (DA). Diethanolamine modified pectin (DAMP) was synthesized by the chemical modification of pectin with varying concentrations of DA (1:1,1:2,1:3 and 1:4) at 5 oC in methanol. The modified product was used for the preparation of the hydrogel with glutaraldehyde (GA) reagent. The prepared hydrogels were characterized by Fourier transform infrared (FTIR) spectroscopy; organic elemental analysis, and X-ray diffraction (XRD), and swelling, hemocompatibility and cytocompatibility studies of the prepared hydrogels were also done. FTIR spectroscopy indicated the presence of primary and secondary amide absorption bands. The XRD pattern of the DAMP hydrogel clearly indicated that there was a considerable increase in crystallinity as compared to parent pectin. The degree of amidation (DA) and molar and mass reaction yields (Ym and Yn) was calculated based on the results of organic elemental analysis. Drug release studies from the hydrogel membranes were also evaluated in a Franz's diffusion cell. The hydrogels demonstrated good water holding properties and were found to be compatible with B-16 melanoma cells and human blood.

  16. Synthesis and characterization of polyaniline-hexaferrite composites

    Energy Technology Data Exchange (ETDEWEB)

    Khursheed, Tooba [Department of Physics, Bahauddin Zakariya University, Multan 60800 (Pakistan); Islam, M.U., E-mail: dr.misbahulislam@bzu.edu.pk [Department of Physics, Bahauddin Zakariya University, Multan 60800 (Pakistan); Asif Iqbal, M. [Department of Physics, Bahauddin Zakariya University, Multan 60800 (Pakistan); College of E & ME, National University of Science and Technology, Islamabad (Pakistan); Ali, Irshad, E-mail: irshadalibzu@gmail.com [Department of Physics, Bahauddin Zakariya University, Multan 60800 (Pakistan); Shakoor, Abdul [Department of Physics, Bahauddin Zakariya University, Multan 60800 (Pakistan); Awan, M.S. [Center for Micro and Nano Devices Department of Physics, COMSATS Institute of Information Technology, Islamabad (Pakistan); Iftikhar, Aisha [Department of Physics, Bahauddin Zakariya University, Multan 60800 (Pakistan); Azhar Khan, Muhammad [Department of Physics, The Islamia University of Bahawalpur, Bahawalpur 63100 (Pakistan); Naeem Ashiq, Muhammad [Institute of Chemical Science, Bahauddin Zakariya University, Multan 60800 (Pakistan)

    2015-11-01

    Polyaniline was synthesized by chemical polymerization using aniline as monomer, and Y-type hexaferrite with composition (Co{sub 2}Mn{sub 2}Sr{sub 1.66}Nd{sub 0.4}Fe{sub 10}O{sub 22}) was prepared by co-precipitation assisted by surfactant. Three composites of Polyaniline with different ferrite ratios were prepared by mechanical blending. The synthesized samples were characterized by X-Ray diffraction, Scanning electron microscopy and electrical measurements. The XRD analysis reveals that no second phase was observed in Y-type hexagonal ferrite. In PANI-Ferrite composites, significant changes in resistivity, real and imaginary part of complex permittivity were observed with the increase of ferrite in the polyaniline matrix. At low frequencies the magnitude of dielectric constant and complex permittivity is high with few relaxation peaks. AC conductivity of PANI-Ferrite composites increase with the increase of frequency following Jonscher law. The resistivity and activation energy were found to show similar behavior. - Highlights: • Co{sub 2}Mn{sub 2}Sr{sub 1.66}Nd{sub 0.4}Fe{sub 10}O{sub 22} was prepared by co-precipitation. • Polyaniline was synthesized by chemical polymerization. • AC conductivity increase with the increase of frequency. • The resistivity and activation energy were found to show similar behavior.

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

    Science.gov (United States)

    2016-03-31

    AFRL-AFOSR-VA-TR-2016-0168 Design, Synthesis, and Characterization of High Performance Polymer Electrolytes for Printed Electronics and Energy ...Sep 2015 4. TITLE AND SUBTITLE Design, Synthesis, and Characterization of High Performance Polymer Electrolytes for Printed Electronics and Energy ... energy storage. This project produced 11 peer reviewed papers and results in the training of 3 graduate students and two postdoctoral fellows. The

  18. Solution phase synthesis of aluminum-doped silicon nanoparticles via room-temperature, solvent based chemical reduction of silicon tetrachloride

    Science.gov (United States)

    Mowbray, Andrew James

    We present a method of wet chemical synthesis of aluminum-doped silicon nanoparticles (Al-doped Si NPs), encompassing the solution-phase co-reduction of silicon tetrachloride (SiCl4) and aluminum chloride (AlCl 3) by sodium naphthalide (Na[NAP]) in 1,2-dimethoxyethane (DME). The development of this method was inspired by the work of Baldwin et al. at the University of California, Davis, and was adapted for our research through some noteworthy procedural modifications. Centrifugation and solvent-based extraction techniques were used throughout various stages of the synthesis procedure to achieve efficient and well-controlled separation of the Si NP product from the reaction media. In addition, the development of a non-aqueous, formamide-based wash solution facilitated simultaneous removal of the NaCl byproduct and Si NP surface passivation via attachment of 1-octanol to the particle surface. As synthesized, the Si NPs were typically 3-15 nm in diameter, and were mainly amorphous, as opposed to crystalline, as concluded from SAED and XRD diffraction pattern analysis. Aluminum doping at various concentrations was accomplished via the inclusion of aluminum chloride (AlCl3); which was in small quantities dissolved into the synthesis solution to be reduced alongside the SiCl4 precursor. The introduction of Al into the chemically-reduced Si NP precipitate was not found to adversely affect the formation of the Si NPs, but was found to influence aspects such as particle stability and dispersibility throughout various stages of the procedure. Analytical techniques including transmission electron microscopy (TEM), FTIR spectroscopy, and ICP-optical emission spectroscopy were used to comprehensively characterize the product NPs. These methods confirm both the presence of Al and surface-bound 1-octanol in the newly formed Si NPs.

  19. Molecular self-assembly and nanochemistry: A chemical strategy for the synthesis of nanostructures

    Science.gov (United States)

    Whitesides, George M.; Mathias, John P.; Seto, Christopher T.

    1991-12-01

    Molecular self assembly is the spontaneous association of molecules under equilibrium conditions into stable, structurally well-defined aggregates joined by non-covalent bonds. Molecular self-assembly is ubiquitous in biological systems, and underlies the formation of a wide variety of complex biological structures. Understanding self-assembly and the associated non-covalent interactions that connect complementary interacting molecular surfaces in biological aggregates is a central concern in structural biochemistry. Self-assembly is also emerging as a new strategy in chemical synthesis, with the potential of generating non-biological structures having dimensions of 1-10(exp 2) nanometers. Structures in the upper part of this range of sizes are presently inaccessible through chemical synthesis, and the ability to prepare them would open a route to structures comparable in size (and perhaps complementary in function) to those that can be prepared by microlithography and other techniques of microfabrication.

  20. Synthesis of bioactive β-TCP coatings with tailored physico-chemical properties on zirconia bioceramics.

    Science.gov (United States)

    Stefanic, Martin; Milacic, Radmila; Drazic, Goran; Škarabot, Miha; Budič, Bojan; Krnel, Kristoffer; Kosmač, Tomaž

    2014-10-01

    The objective of this work was to develop a synthesis procedure for the deposition of β-TCP coatings with tailored physico-chemical properties on zirconia bioceramics. The synthesis procedure involved two steps: (i) a rapid wet-chemical deposition of a biomimetic CaP coating and (ii) a subsequent post-deposition processing of the biomimetic CaP coating, which included a heat treatment between 800 and 1200 °C, followed by a short sonication in a water bath. By regulating the heating temperature the topography of the β-TCP coatings could be controlled. The average surface roughness (Ra) ranged from 42 nm for the coating that was heated at 900 °C (TCP-900) to 630 nm for the TCP-1200 coating. Moreover, the heating temperature also affected the dissolution rate of the coatings in a physiological solution, their protein-adsorption capacity and their bioactivity in a simulated body fluid.