WorldWideScience

Sample records for chemical synthesis characterization

  1. Facile chemical synthesis and structure characterization of copper molybdate nanoparticles

    Science.gov (United States)

    Rahimi-Nasrabadi, Mehdi; Pourmortazavi, Seied Mahdi; Khalilian-Shalamzari, Morteza

    2015-03-01

    Experimental parameters of a synthesis route were optimized by Taguchi robust design for the facile and controllable synthesis of copper molybdate nanoparticles. CuMoO4 nanoparticles were synthesized by chemical precipitation followed by hydrothermal process. Effects of different parameters of synthesis procedure, i.e. concentrations of both reagents, copper feeding flow rate and temperature of reactor on the particle size of prepared copper molybdate nanoparticles were investigated. The results of statistical optimization revealed that the size of copper molybdate particles is dependent on the procedure variables involving copper concentrations, flow rate and temperature of the reactor; while, molybdate concentration has a no considerable role in determining the size of CuMoO4 particles. Based on the results obtained by statistical optimization process, the nanoparticles of copper molybdate were prepared and then their structure and chemical composition were characterized by various techniques, i.e. SEM, TEM, XRD, EDX, FT-IR, UV-Vis and photoluminescence spectroscopy.

  2. 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

  3. Synthesis, characterization and sintering of nanocrystalline titania powders produced by chemical vapour synthesis

    International Nuclear Information System (INIS)

    The chemical vapour synthesis (CVS) route is a versatile process that can be used for the synthesis of nanocrystalline ceramics with very small crystallite sizes having a narrow particle size distribution. In this study, a CVS technique was used to prepare nanocrystalline titania from tetraisopropyl orthotitanate at a processing temperature of 1273 K (1000 deg, C). High resolution transmission electron microscopy, x-ray diffraction and nitrogen adsorption techniques were used for the characterization of the as-synthesized powders. Green bodies were produced by a combination of uniaxial and cold isostatic pressing, which were then sintered. A simple pressureless sintering route was established that led to the production of a dense titania ceramic with a uniform microstructure and an average grain size well in the nanophase regime

  4. A simple wet chemical synthesis and characterization of hydroxyapatite nanorods

    International Nuclear Information System (INIS)

    Calcium hydroxyapatite (Ca5(PO4)3(OH):HAP) nanorods have been synthesized successfully via wet chemical technique at low temperature in the presence of suitable surfactant. The as-made nanorods have a diameter of 50-80 nm and a length of 0.5-1.2 μm. The microstructures and composition are characterized via X-ray diffraction (XRD), transmission electron microscopy (TEM), and Fourier transform infrared spectrometer (FT-IR). The formation mechanism of HAP nanorod is discussed in detail. It has been found that nanorods are pure, there is no HAP carbonated HAP. The growth mechanism of HAP nanorods could be explained by a soft template

  5. Chemically functionalized gold nanoparticles: Synthesis, characterization, and applications

    Science.gov (United States)

    Daniel, Weston Lewis

    This thesis focuses on the development and application of gold nanoparticle based detection systems and biomimetic structures. Each class of modified nanoparticle has properties that are defined by its chemical moieties that interface with solution and the gold nanoparticle core. In Chapter 2, a comparison of the biomolecular composition and binding properties of various preparations of antibody oligonucleotide gold nanoparticle conjugates is presented. These constructs differed significantly in terms of their structure and binding properties. Chapter 3 reports the use of electroless gold deposition as a light scattering signal enhancer in a multiplexed, microarray-based scanometric immunoassay using the gold nanoparticle probes evaluated in Chapter 2. The use of gold development results in greater signal enhancement than the typical silver development, and multiple rounds of metal development were found to increase the resulting signal compared to one development. Chapter 4 describes an amplified scanometric detection method for human telomerase activity. Gold nanoparticles functionalized with specific oligonucleotide sequences can efficiently capture telomerase enzymes and subsequently be elongated. Both the elongated and unmodified oligonucleotide sequences are simultaneously measured. At low telomerase concentrations, elongated strands cannot be detected, but the unmodified sequences, which come from the same probe particles, can be detected because their concentration is higher, providing a novel form of amplification. Chapter 5 reports the development of a novel colorimetric nitrite and nitrate ion assay based upon gold nanoparticle probes functionalized with Griess reaction reagents. This assay takes advantage of the distance-dependent plasmonic properties of the gold nanoparticles and the ability of nitrite ion to facilitate the cross coupling of novel nanoparticle probes. The assay works on the concept of a kinetic end point and can be triggered at the EPA

  6. 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

  7. 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.

  8. 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.

  9. Synthesis and characterization of chemically functionalized shape memory nanofoams for unattended sensing applications

    Science.gov (United States)

    Soliani, Anna Paola

    The work in this dissertation is devoted to the synthesis and characterization of novel materials for off-line unattended sensing: shape-memory grafted nanofoams. The fabrication process and characterization of highly efficient, polymeric nanosensor element with the ability to selectively detect analytes and retain memory of specific exposure events is reported. These shape memory nanofoams could potentially act as efficient and highly sensitive coatings for evanescent waveguide-based optical monitoring systems. On exposure to specific analytes, the polymeric coatings locally change their internal structure irreversibly at the nanolevel, affecting the local optical properties such as refractive index. Currently, enrichment polymer layers (EPLs) are currently being used to detect of chemical vapors. EPLs are thin polymer films that can increase signal of an analyte through absorption. These films are designed to interact with analytes via chemical interactions while this analyte is present in the environment. Once the analyte is removed from the environment surrounding the EPL, these EPLs have no residual memory of the interaction(s). This dissertation will address this limitation in the field of chemical unattended sensing through the use of functionalized polymeric films that possess ability to retain memory of analyte exposure. Specifically, we will use chemically cross-linked gradient nanofoam as a material with built-in analyte-specific sensing properties. A novel method has been created to fabricate chemically functionalized shape memory nanofoams. First, a polymer film containing epoxy groups is deposited onto a substrate. Then, the film is cross-linked via reaction of the epoxy groups to create a non-soluble, yet swellable coating. This film is then treated with specific chemical substances capable of reacting with the epoxy functionalities. This procedure is necessary to convert the epoxy groups into various functional moieties. This process generates a

  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 hydroxyapatite nanofiber by chemical precipitation method using surfactants

    Energy Technology Data Exchange (ETDEWEB)

    Gao, Shan, E-mail: coralgao@hotmail.com [Key Laboratory for Liquid-Solid Structure Evolution and Processing of Materials (Ministry of Education), Shandong University, Jinan 250061 (China); Engineering Ceramics Key Laboratory of Shandong Province, Shandong University, Jinan 250061 (China); Sun, Kangning, E-mail: sunkangning@sdu.edu.cn [Key Laboratory for Liquid-Solid Structure Evolution and Processing of Materials (Ministry of Education), Shandong University, Jinan 250061 (China); Engineering Ceramics Key Laboratory of Shandong Province, Shandong University, Jinan 250061 (China); Li, Aimin; Wang, Hongyou [Key Laboratory for Liquid-Solid Structure Evolution and Processing of Materials (Ministry of Education), Shandong University, Jinan 250061 (China); Engineering Ceramics Key Laboratory of Shandong Province, Shandong University, Jinan 250061 (China)

    2013-03-15

    Highlights: ► We succeeded in synthesizing hydroxyapatite nano fibers by a chemical method. ► The reaction temperature is only 90 °C. ► The synthetic hydroxyapatite nano fiber is single crystal. - Abstract: We report a novel chemical precipitation route for the synthesis of hydroxyapatite (Ca{sub 10}(PO{sub 4}){sub 6}(OH){sub 2}, HA) fibers using surfactants as templates. Fourier transform infrared spectroscopy (FTIR) and powder X-ray diffraction (PXRD) reveal the characteristic peaks of HA. Transmission electron microscope (TEM) and high-resolution TEM revealed the nano structure, crystallinity and morphology of the HA fibers. The morphology of the HA fibers after calcinations were characterized by scanning electron microscope (SEM). Br{sup −} ions were quickly replaced by the excess PO{sub 4}{sup 3−} ions in the solution after the addition of cetyltrime-thylammonium bromide (CTAB). Meanwhile, CTAB formed a rod-like micelles. Precursors reacted with PO{sub 4}{sup 3−} at the surface of CTAB micelles and finally formed the nanofiber structure.

  12. Synthesis and characterization of hydroxyapatite nanofiber by chemical precipitation method using surfactants

    International Nuclear Information System (INIS)

    Highlights: ► We succeeded in synthesizing hydroxyapatite nano fibers by a chemical method. ► The reaction temperature is only 90 °C. ► The synthetic hydroxyapatite nano fiber is single crystal. - Abstract: We report a novel chemical precipitation route for the synthesis of hydroxyapatite (Ca10(PO4)6(OH)2, HA) fibers using surfactants as templates. Fourier transform infrared spectroscopy (FTIR) and powder X-ray diffraction (PXRD) reveal the characteristic peaks of HA. Transmission electron microscope (TEM) and high-resolution TEM revealed the nano structure, crystallinity and morphology of the HA fibers. The morphology of the HA fibers after calcinations were characterized by scanning electron microscope (SEM). Br− ions were quickly replaced by the excess PO43− ions in the solution after the addition of cetyltrime-thylammonium bromide (CTAB). Meanwhile, CTAB formed a rod-like micelles. Precursors reacted with PO43− at the surface of CTAB micelles and finally formed the nanofiber structure

  13. Ethics of Chemical Synthesis

    OpenAIRE

    Joachim Schummer

    2001-01-01

    Unlike other branches of science, the scientific products of synthetic chemistry are not only ideas but also new substances that change our material world, for the benefit or harm of living beings. This paper provides for the first time a systematical analysis of moral issues arising from chemical synthesis, based on concepts of responsibility and general morality. Topics include the questioning of moral neutrality of chemical synthesis as an end in itself, chemical weapons research, moral ob...

  14. Synthesis Characterization and Decomposition Studies of tris[N-N-dibenzyidithocarbaso)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.

    2005-01-01

    This paper presents the results of the synthesis characterization and decomposition studies of tris[N-N-dibenzyidithocarbaso)Indium (III) with chemical spray deposition of polycrystalline CuInS2 on Copper Films.

  15. Synthesis of silver nanoparticles by chemical reduction at various fraction of MSA and their structure characterization

    Energy Technology Data Exchange (ETDEWEB)

    Diantoro, Markus, E-mail: m-diantoror@yahoo.com; Fitrianingsih, Rina, E-mail: m-diantoror@yahoo.com; Mufti, Nandang, E-mail: m-diantoror@yahoo.com; Fuad, Abdulloh, E-mail: m-diantoror@yahoo.com [Department of Physics, Faculty of Mathematics and Natural Sciences, Universitas Negeri Malang (UM), Jl. Semarang No. 5 Malang 65145 (Indonesia)

    2014-03-24

    Nanosilver is currently one of the most common engineered nanomaterials and is used in many applications that lead to the release of silver nanoparticles and silver ions into aqueous systems. Nanosilver also possesses enhanced antimicrobial activity and bioavailability that may less environmental risk compared with other manufactured nanomaterials. Described in this research are the synthesis of silver nanoparticle produced by chemical reduction from silver nitrate (AgNO{sub 3}) solution. As a reducing agent, Sodium Borohydride (NaBH{sub 4}) was used and mercaptosuccinic Acid (MSA) as stabilizer to prevent the nanoparticle from aglomerating. It was also used two kinds of solvent, they are water and methanol. In typical experiment MSA was dissolve in methanol with a number of variation of molarity i.e. 0,03 M, 0,06 M, 0,12 M, 0,15 M, and the mixture was kept under vigorous stirring in an ice bath. A solution of silver nitrate of 340 mg in 6,792 ml water was added. A freshly prepared aqueous solution of sodium borohydride (756,6 mL in 100 mL of water) was added drop wisely. The solution was kept for half an hour for stirring and were allowed to settle down in methanol. The obtained samples then characterized by means of x-ray diffractometer, and scanning electron microscopy, as well as transmission electron microscopy to obtain their structures of silver nanoparticles, morphology, and sizes. It is shown that diameter of silver nanoparticle sized about 24.3 nm (Ag@MSA 0.03 M), 20.4 nm (Ag@MSA 0.06 M), 16.8 nm (Ag@MSA 0.12 M), 16.9 nm (Ag@MSA 0.15 M) which was calculated by Scherrer formula by taking the FWHM from fitting to Gaussian. The phases and lattice parameter showed that there is no significant change in its volume by increasing molarity of stabilizer. In contrast, the size of particles is decreasing.

  16. Synthesis of silver nanoparticles by chemical reduction at various fraction of MSA and their structure characterization

    International Nuclear Information System (INIS)

    Nanosilver is currently one of the most common engineered nanomaterials and is used in many applications that lead to the release of silver nanoparticles and silver ions into aqueous systems. Nanosilver also possesses enhanced antimicrobial activity and bioavailability that may less environmental risk compared with other manufactured nanomaterials. Described in this research are the synthesis of silver nanoparticle produced by chemical reduction from silver nitrate (AgNO3) solution. As a reducing agent, Sodium Borohydride (NaBH4) was used and mercaptosuccinic Acid (MSA) as stabilizer to prevent the nanoparticle from aglomerating. It was also used two kinds of solvent, they are water and methanol. In typical experiment MSA was dissolve in methanol with a number of variation of molarity i.e. 0,03 M, 0,06 M, 0,12 M, 0,15 M, and the mixture was kept under vigorous stirring in an ice bath. A solution of silver nitrate of 340 mg in 6,792 ml water was added. A freshly prepared aqueous solution of sodium borohydride (756,6 mL in 100 mL of water) was added drop wisely. The solution was kept for half an hour for stirring and were allowed to settle down in methanol. The obtained samples then characterized by means of x-ray diffractometer, and scanning electron microscopy, as well as transmission electron microscopy to obtain their structures of silver nanoparticles, morphology, and sizes. It is shown that diameter of silver nanoparticle sized about 24.3 nm (Ag@MSA 0.03 M), 20.4 nm (Ag@MSA 0.06 M), 16.8 nm (Ag@MSA 0.12 M), 16.9 nm (Ag@MSA 0.15 M) which was calculated by Scherrer formula by taking the FWHM from fitting to Gaussian. The phases and lattice parameter showed that there is no significant change in its volume by increasing molarity of stabilizer. In contrast, the size of particles is decreasing

  17. 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.

  18. Synthesis and Characterization of Carbon nanofibers on Co and Cu Catalysts by Chemical Vapor Deposition

    Energy Technology Data Exchange (ETDEWEB)

    Park, Eunsil; Kim, Jongwon; Lee, Changseop [Keimyung Univ., Daegu (Korea, Republic of)

    2014-06-15

    This study reports on the synthesis of carbon nanofibers via chemical vapor deposition using Co and Cu as catalysts. In order to investigate the suitability of their catalytic activity for the growth of nanofibers, we prepared catalysts for the synthesis of carbon nanofibers with Cobalt nitrate and Copper nitrate, and found the optimum concentration of each respective catalyst. Then we made them react with Aluminum nitrate and Ammonium Molybdate to form precipitates. The precipitates were dried at a temperature of 110 .deg. C in order to be prepared into catalyst powder. The catalyst was sparsely and thinly spread on a quartz tube boat to grow carbon nanofibers via thermal chemical vapor deposition. The characteristics of the synthesized carbon nanofibers were analyzed through SEM, EDS, XRD, Raman, XPS, and TG/DTA, and the specific surface area was measured via BET. Consequently, the characteristics of the synthesized carbon nanofibers were greatly influenced by the concentration ratio of metal catalysts. In particular, uniform carbon nanofibers of 27 nm in diameter grew when the concentration ratio of Co and Cu was 6:4 at 700 .deg. C of calcination temperature; carbon nanofibers synthesized under such conditions showed the best crystallizability, compared to carbon nanofibers synthesized with metal catalysts under different concentration ratios, and revealed 1.26 high amorphicity as well as 292 m{sup 2}g{sup -1} high specific surface area.

  19. Synthesis of zeolites from boiler fly ash: physical, chemical and mineralogical characterization

    International Nuclear Information System (INIS)

    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 2O/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-micro silica in these reaction conditions point to a promising material for zeolite synthesis (author)

  20. Chemical synthesis and characterization of elastin-like polypeptides (ELPs) with variable guest residues.

    Science.gov (United States)

    Aladini, Firouzeh; Araman, Can; Becker, Christian F W

    2016-05-01

    The properties of elastin-like polypeptides (ELPs), specifically the fact that they are soluble in aqueous buffers below and aggregate reversibly above a well-defined transition temperature, are extensively used for protein purification, enzyme recycling, and more recently, for in vivo applications such as drug delivery and tissue engineering. ELPs are artificial but biocompatible polypeptides composed of pentameric repeats (Val-Pro-Gly-Xaa-Gly) containing different guest residues Xaa, derived from mammalian elastin. The temperature-dependent aggregation and desaggregation of ELPs is controlled by composition of the pentameric repeats as well as the number of repetitive units within the ELP. External parameters such as ELP concentration, pH, and most importantly, salt effects heavily influence the transition temperature. Here, we explore the chemical synthesis of a series of 51mer peptides consisting of 10 pentameric ELP repeats with hydrophobic as well as charged guest residues such as isoleucine, leucine, alanine, lysine, and/or glutamate all prepared by Boc-based solid phase peptide synthesis. These guest residues expand the available toolbox of synthetic ELPs and provide ELPs that can be chemically modified and tuned to specific environments. An N-terminal cysteine is added allowing disulfide-based crosslinking of ELPs and to link synthetic ELPs to a recombinantly produced protein using native chemical ligation. Transition temperatures of all synthetic ELPs and the fusion construct were determined by measuring turbidity in solution and spanned a large temperature range between 25 and 70 °C, providing synthetically accessible ELPs with transition temperatures suitable for in vitro and in vivo applications. Cycling between their soluble and aggregate state has been observed at least 6 times without significant loss of material for all synthetic ELPs. Copyright © 2016 European Peptide Society and John Wiley & Sons, Ltd. PMID:27005861

  1. Synthesis and Characterization of Graphene Thin Films by Chemical Reduction of Exfoliated and Intercalated Graphite Oxide

    OpenAIRE

    Thema, F. T.; M. J. Moloto; E. D. Dikio; Nyangiwe, N. N.; L. Kotsedi; Maaza, M.; Khenfouch, M.

    2013-01-01

    Commercial flakes of graphite were prepared into functionalized graphene oxide (GO) by chemical treatment. After the exfoliation and intercalation of graphene into functionalized graphene oxide that formed stable colloidal dispersion in polar aprotic solvent, the reduction process was undertaken by continuous stirring with hydrazine hydrate. The reduced material was characterized by X-ray diffraction (XRD), attenuated total reflectance (ATR) FT-IR, ultraviolet visible (UV-vis), atomic force m...

  2. Ethics of Chemical Synthesis

    Directory of Open Access Journals (Sweden)

    Joachim Schummer

    2001-10-01

    Full Text Available Unlike other branches of science, the scientific products of synthetic chemistry are not only ideas but also new substances that change our material world, for the benefit or harm of living beings. This paper provides for the first time a systematical analysis of moral issues arising from chemical synthesis, based on concepts of responsibility and general morality. Topics include the questioning of moral neutrality of chemical synthesis as an end in itself, chemical weapons research, moral objections against improving material conditions of life by chemical means, and freedom of research. The paper aims at providing both a sound basis for moral judgements of chemistry in a public discourse and a framework for chemists to reflect on the moral relevance of their activity.

  3. Synthesis and characterization of M-type barium hexferrite by ultrasonic inter-dispersion of chemical precipitate

    International Nuclear Information System (INIS)

    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)3 and Ba(OH)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-H2O 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)

  4. Synthesis, structural characterization and quantum chemical studies of silicon-containing benzoic acid derivatives

    Science.gov (United States)

    Zaltariov, Mirela-Fernanda; Cojocaru, Corneliu; Shova, Sergiu; Sacarescu, Liviu; Cazacu, Maria

    2016-09-01

    The present paper is concerned with the synthesis and molecular structure investigation of two new benzoic acid derivatives having trimethylsilyl tails, 4-((trimethylsilyl)methoxy) and 4-(3-(trimethylsilyl)propoxy)benzoic acids. The structures of the novel compounds have been confirmed by X-ray crystallography, Fourier-transform infrared spectroscopy (FTIR) and nuclear magnetic resonance (1H and 13C NMR). The theoretical studies of molecules were conducted by using the quantum chemical methods, such as Density Functional Theory (DFT B3LYP/6-31 + G**), Hartree-Fock (HF/6-31 + G**) and semiempirical computations (PM3, PM6 and PM7). The optimized molecular geometries have been found to be in good agreement with experimental structures resulted from the X-ray diffraction. The maximum electronic absorption bands observed at 272-287 nm (UV-vis spectra) have been assigned to π → π* transitions, which were in reasonable agreement with the time dependent density functional theory (TD-DFT) calculations. The computed vibrational frequencies by DFT method were assigned and compared with the experimental FTIR spectra. The mapped electrostatic potentials revealed the reactive sites, which corroborated the observation of the dimer supramolecular structures formed in the crystals by hydrogen-bonding. The energies of frontier molecular orbitals (HOMO and LUMO), energy gap, dipole moment and molecular descriptors for the new compounds were calculated and discussed.

  5. Physico-chemical characterization of lignins from different sources for use in phenol-formaldehyde resin synthesis.

    Science.gov (United States)

    Tejado, A; Peña, C; Labidi, J; Echeverria, J M; Mondragon, I

    2007-05-01

    During the last decades lignin has been investigated as a promising natural alternative to petrochemicals in phenol-formaldehyde (PF) resin production, due to their structural similarity. Physico-chemical characterization of three types of lignin, namely kraft pine lignin (L1), soda-anthraquinone flax lignin (L2), and ethanol-water wild tamarind lignin (L3) has been evaluated to determine which one is the most suitable chemical structure for above purpose. Characterization has been performed using Fourier transform infrared spectroscopy (FT-IR) and proton nuclear magnetic resonance spectrometry ((1)H NMR) to analyse the chemical structure, gel permeation chromatography (GPC) for determining molecular weight (MW) and molecular weight distribution (MWD), differential scanning calorimetry (DSC) to measure the glass transition temperature and thermogravimetric analysis (TGA) to follow the thermal degradation. Both structural and thermal characteristics suggest that kraft pine lignin (L1) would be a better phenol (P) substitute in the synthesis of lignin-phenol-formaldehyde (LPF) resins, as it presents higher amounts of activated free ring positions, higher MW and higher thermal decomposition temperature. PMID:16843657

  6. A novel chemical synthesis and characterization of Mn3O4 thin films for supercapacitor application

    International Nuclear Information System (INIS)

    Mn3O4 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 Mn3O4 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. Mn3O4 film surface showed hydrophilic nature with water contact angle of 55o. The supercapacitive properties of Mn3O4 thin film investigated in 1 M Na2SO4 electrolyte showed maximum supercapacitance of 314 F g-1 at scan rate 5 mV s-1.

  7. 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.

  8. 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.

  9. 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.

  10. Synthesis and spectroscopic characterization of gold nanobipyramids prepared by a chemical reduction method

    Science.gov (United States)

    Thanh Ngo, Vo Ke; Phat Huynh, Trong; Giang Nguyen, Dang; Phuong Uyen Nguyen, Hoang; Lam, Quang Vinh; Dat Huynh, Thanh

    2015-12-01

    Gold nanobipyramids (NBPs) have attracted much attention because they have potential for applications in smart sensing devices, such as medical diagnostic equippments. This is due to the fact that they show more advantageous plasmonic properties than other gold nanostructures. We describe a chemical reduction method for synthesizing NBPs using conventional heating with ascorbic acid reduction and cetyltrimethylamonium bromide (CTAB) + AgNO3 as capping agents. The product was characterized by ultraviolet-visible spectroscopy (UV-vis), Fourier transmission infrared spectroscopy (FTIR), transmission electron microscopy (TEM), x-ray powder diffraction (XRD). The results showed that gold nanoparticles were formed with bipyramid shape (tip-to-tip distance of 88.4 ± 9.4 nm and base length of 29.9 ± 3.2 nm) and face-centered-cubic crystalline structure. Optimum parameters for preparation of NBPs are also found.

  11. Chemical Vapor Deposition Synthesis and Raman Spectroscopic Characterization of Large-Area Graphene Sheets

    Science.gov (United States)

    Liao, Chun-Da; Lu, Yi-Ying; Tamalampudi, Srinivasa Reddy; Cheng, Hung-Chieh; Chen, Yit-Tsong

    2013-10-01

    We present a chemical vapor deposition (CVD) method to catalytically synthesize large-area, transferless, single- to few-layer graphene sheets using hexamethyldisilazane (HMDS) on a SiO2/Si substrate as a carbon source and thermally evaporated alternating Ni/Cu/Ni layers as a catalyst. The as-synthesized graphene films were characterized by Raman spectroscopic imaging to identify single- to few-layer sheets. This HMDS-derived graphene layer is continuous over the entire growth substrate, and single- to trilayer mixed sheets can be up to 30 -m in the lateral dimension. With the synthetic CVD method proposed here, graphene can be grown into tailored shapes directly on a SiO2/Si surface through vapor priming of HMDS onto predefined photolithographic patterns. The transparent and conductive HMDS-derived graphene exhibits its potential for widespread electronic and opto-electronic applications.

  12. 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.

  13. Synthesis of poly(D,L-lactide-co-glycolide) copolymers and its chemical characterization by NMR and FTIR

    International Nuclear Information System (INIS)

    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. 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.

  15. Synthesis and crystal chemical characterization of the pyrochlore type MgZrSi2O7

    International Nuclear Information System (INIS)

    Highlights: → We synthesized new pyrochlore type MgZrSi2O7 at high pressure and temperature. → We characterized this MgZrSi2O7 by Rietveld method. → A-site of pyrochlore A2B2O7 is randomly occupied by two species in a 1:1 ratio. → The MgZrSi2O7 pyrochlore has higher RA/RB ratio than previous A2B2O7 pyrochlores. - Abstract: The pyrochlore type of MgZrSi2O7 was synthesized at 25 GPa and 1500 deg. C using a Kawai-type, multi-anvil apparatus. Powder X-ray diffraction and Rietveld analysis revealed that the phase assumed the pyrochlore structure (space group Fd3-bar m, cubic) with the lattice parameter a = 9.2883(1) A and the structural parameter x = 0.4295(4). Chemical analysis by the electron probe microanalysis (EPMA) confirmed the stoichiometry of MgZrSi2O7. It was demonstrated that the eight-fold coordinated 16c site is randomly occupied by both Mg2+ and Zr4+ ions in a 1:1 ratio. The high ionic radius ratio RA/RB (where A and B denote Mg + Zr and Si, respectively) of 2.22 necessitates a relatively high pressure to stabilize the pyrochlore structure.

  16. Synthesis and characterization of GaN nanowires by a catalyst assisted chemical vapor deposition

    Energy Technology Data Exchange (ETDEWEB)

    Wei Xiaofeng [College of Physics and Electronics, Shandong Normal University, Jinan, 250014 (China); Shi Feng, E-mail: sf751106@163.com [College of Physics and Electronics, Shandong Normal University, Jinan, 250014 (China)

    2011-09-15

    GaN nanowires have been fabricated on Si(1 1 1) substrates by chemical vapor deposition (CVD) method with NiCl{sub 2} as catalyst and their compositions, microstructures, morphologies and light emitting properties were characterized by X-ray diffraction (XRD), FT-IR spectrophotometer (FTIR), scanning electron microscope (SEM), high-resolution transmission electron microscope (HRTEM), Raman spectroscopy and photoluminescence (PL). The results demonstrate that the nanowires are single-crystal GaN with hexagonal wurtzite structure and high crystalline quality, having the size of 20-50 nm in diameter and several tens of microns in length with some nano-droplets on their tips, which reveals that the growth mechanism of GaN nanowires agrees with vapor-liquid-solid (VLS) process. Five first-order Raman active phonon bands move to low shift and A{sub 1}(TO), E{sub 1}(TO), and E{sub 2} (high) bands are overlapped and broaden, which is caused by uncertainty in the phonon wave vector. Five non-first-order active Raman phonons also appear, which is caused by the small dimension and high surface disorder degree. A blue-shift of the band-gap emission occurs due to quantum confinement effect.

  17. 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.

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

    International Nuclear Information System (INIS)

    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 125I-[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 125I-[Tyr2] leiurotoxin I binding and vice versa. Moreover, the peculiar effects of K+ on 125I-[Tyr2]leiurotoxin I binding are identical to those previously observed for 125I-apamin binding

  19. Synthesis and characterization of Mn doped ZnCdS core shell nanostructures QDs using a chemical precipitation route

    Science.gov (United States)

    Kaur, Manpreet; Pandey, O. P.; Sharma, Manoj

    2016-04-01

    With advancement in time, researchers has drawn great attention in the synthesis and characterization of mono dispersed alloyed nanocomposites of II-VI compounds. Ternary semiconductor alloyed ZnCdS quantum dots (QD's) exhibit properties intermediate between those of ZnS and CdS. It shows high absorption coefficients, a composition tunable and size tunable band gap. Moreover, ZnCdS alloyed NC's display unique composition dependent properties distinct from those of their bulk counterparts. The most striking feature of the alloyed NC's nanocrystals is their unusual long time stability in emission wavelength. ZnCdS alloyed QD's at room temperature has been synthesized using chemical precipitation method. Undoped and Mn2+ doped ZnCdS QDs have been synthesized and studied. UV-visible absorption spectrum shows absorbance in the visible region and photoluminescence (PL) emission spectra of the doped ZnCdS QD's shows orange emission in comparison to weak blue emission from undoped QDs. The crystallite size is calculated from the XRD patterns. The experimental results indicate that this easy synthesis route would prove a versatile approach for the preparation of doped and undoped ZnCdS QD's.

  20. 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.

  1. Low-temperature synthesis and characterization of helical carbon fibers by one-step chemical vapour deposition

    International Nuclear Information System (INIS)

    Graphical abstract: - Highlights: • HCNFs were synthesized by one-step CVD using cupric tartrate as a catalyst at temperature below 500 °C. • The synthesis of HCNFs is highly temperature-dependent at the synthesis temperature of 280–480 °C. • The addition of HCNFs makes a noticeable contribution to the reinforcement of NR/CB system. - Abstract: Helical carbon fibers (HCNFs) were synthesized by one-step chemical vapour deposition using cupric tartrate as a catalyst at temperature below 500 °C. The bound rubber of natural rubber (NR)/HCNFs were also prepared in this study. The results of thermogravimetry–differential scanning calorimetry (TG/DSC) for cupric tartrate nanoparticles show that the transformation of C4H4CuO6 → Cu reaction occurs at ∼250–310 °C. The characterization of scanning electron microscopy (SEM), transmission electron microscope (TEM), X-ray diffraction (XRD) and Raman spectrum for the synthesized products confirms that the synthesis of HCNFs is highly temperature-dependent. The straight fibers with the fiber diameter of 100–400 nm are obtained at 280 °C and HCNFs can be synthesized at higher temperature, with the coil diameter of 0.5–1 μm and fiber diameter of 100–200 nm at 380 °C, and the coil diameter of ∼100 nm and fiber diameter of ∼80 nm at 480 °C. The maximum of the bound-rubber content (37%) can be obtained with the addition of 100 wt.% HCNFs in NR, which indicates that the coiled configuration of HCNFs makes a noticeable contribution to the reinforcement of NR/CB system

  2. Low-temperature synthesis and characterization of helical carbon fibers by one-step chemical vapour deposition

    Energy Technology Data Exchange (ETDEWEB)

    Jin, Yongzhong [Department of Materials and Chemistry Engineering, Sichuan University of Science and Engineering, 643000 Zigong, Sichuan (China); Chen, Jian, E-mail: wuhangzs@163.com [Department of Materials and Chemistry Engineering, Sichuan University of Science and Engineering, 643000 Zigong, Sichuan (China); Fu, Qingshan [Department of Materials and Chemistry Engineering, Sichuan University of Science and Engineering, 643000 Zigong, Sichuan (China); Li, Binghong [China Rubber Group Carbon Black Industry Research and Design Institute, 643000 Zigong, Sichuan (China); Zhang, Huazhi; Gong, Yong [Department of Materials and Chemistry Engineering, Sichuan University of Science and Engineering, 643000 Zigong, Sichuan (China)

    2015-01-01

    Graphical abstract: - Highlights: • HCNFs were synthesized by one-step CVD using cupric tartrate as a catalyst at temperature below 500 °C. • The synthesis of HCNFs is highly temperature-dependent at the synthesis temperature of 280–480 °C. • The addition of HCNFs makes a noticeable contribution to the reinforcement of NR/CB system. - Abstract: Helical carbon fibers (HCNFs) were synthesized by one-step chemical vapour deposition using cupric tartrate as a catalyst at temperature below 500 °C. The bound rubber of natural rubber (NR)/HCNFs were also prepared in this study. The results of thermogravimetry–differential scanning calorimetry (TG/DSC) for cupric tartrate nanoparticles show that the transformation of C{sub 4}H{sub 4}CuO{sub 6} → Cu reaction occurs at ∼250–310 °C. The characterization of scanning electron microscopy (SEM), transmission electron microscope (TEM), X-ray diffraction (XRD) and Raman spectrum for the synthesized products confirms that the synthesis of HCNFs is highly temperature-dependent. The straight fibers with the fiber diameter of 100–400 nm are obtained at 280 °C and HCNFs can be synthesized at higher temperature, with the coil diameter of 0.5–1 μm and fiber diameter of 100–200 nm at 380 °C, and the coil diameter of ∼100 nm and fiber diameter of ∼80 nm at 480 °C. The maximum of the bound-rubber content (37%) can be obtained with the addition of 100 wt.% HCNFs in NR, which indicates that the coiled configuration of HCNFs makes a noticeable contribution to the reinforcement of NR/CB system.

  3. Synthesis and characterization of β-phase iron silicide nano-particles by chemical reduction

    International Nuclear Information System (INIS)

    Graphical abstract: - Highlights: • β-FeSi2 nano-particle was synthesized by reducing with Mg and by diluting with MgO. • XRD profile shows the iron di-silicide phase to be semiconducting β-FeSi2. • HRTEM and FESEM images indicate the β-FeSi2average particle size to be 60–70 nm. • Absorption, reflectance and PL spectroscopy show band gap to be direct 0.87 eV. • Nano-β-FeSi2is p-type with hole density of 4.38 × 1018 cm−3 and mobility 8.9 cm2/V s. - Abstract: Nano-particles of β-FeSi2 have been synthesized by chemical reduction of a glassy phase of [Fe2O3, 4SiO2] by Mg-metal where MgO is used as diluent to prevent the agglomeration of nano crystallites into micro-particles and also act as a negative catalyst for the formation of other phases. The sample is characterized by XRD, FESEM, HRTEM, EDX, ultra-violet-visible-infrared and PL spectroscopy and electronic properties have been investigated by Hall measurement. XRD profile shows that the synthesized powder consists of purely β-FeSi2 semiconducting phase. The average crystallite size of β-FeSi2 is determined to be around 65.4 nm from XRD peaks as well as from FESEM also. The optical absorption and PL spectroscopy shows that synthesized β-FeSi2 phase is a direct band gap semiconductor with a value of 0.87 eV. Hall measurements show that β-FeSi2 nano-particles is p-type with hole concentration of 4.38 × 1018 cm−3 and average hole mobility of 8.9 cm2/V s at 300 K

  4. 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.

  5. Synthesis and Characterization of Biomimetic Hydroxyapatite Nanoconstruct Using Chemical Gradient across Lipid Bilayer.

    Science.gov (United States)

    Koirala, Mukund Bahadur; Nguyen, Tuyen Duong Thanh; Pitchaimani, Arunkumar; Choi, Seong-O; Aryal, Santosh

    2015-12-16

    In this study, we synthesized biomimetic hydroxyapatite nanoconstruct (nanosized hydroxyapatite, NHAp) using a double emulsion technique combined with a chemical gradient across a lipid bilayer for surface modification of a titanium (Ti) implant. The synthesized NHAp was characterized by dynamic light scattering, X-ray diffraction, transmission electron microscopy, and Fourier transform infrared (FTIR) spectroscopy, and it was further tested for its biocompatibility and in vitro proliferation efficacy using normal human osteoblasts (NHOst). The results showed that the synthesized NHAp had a hydrodynamic diameter of ∼200 nm with high aqueous stability. The chemistry of the NHAp was confirmed by FTIR spectroscopic analysis. Typical FTIR vibrational bands corresponding to the phosphate group (PO4(3-)) present in hydroxyapatite (HAp) were observed at 670, 960, and 1000 cm(-1). A broad band at 3500 cm(-1) confirmed the presence of a structural -OH group in the NHAp. Powder X-ray crystallographic diffraction further confirmed the formation of NHAp with characteristic reflections in (002), (211), (130), and (213) planes at respective 2θ degrees. These reflection planes are similar to those of typical HAp crystallized toward (002) and (211) crystallographic planes. The mechanism of the formation of NHAp was studied using the fluorescence resonance energy transfer (FRET) technique. The FRET study showed the fluorescent recovery of a donor fluorophore and the mechanism of the insertion of lipids into nanodroplets obtained from the first water-in-oil (w/o) emulsion during the formation of the second oil-in-water (o/w) emulsion. With these confirmations, we further studied NHOst cell proliferation on a Ti surface. When NHOst were cultured on the Ti surface coated with the NHAp, a distinct proliferation pattern and cell-cell communication via cytoplasmic extension on the substrate surface were observed. In contrast, a bare Ti surface showed diminished cell size with minimal

  6. Synthesis and characterization of β-phase iron silicide nano-particles by chemical reduction

    Energy Technology Data Exchange (ETDEWEB)

    Sen, Sabyasachi [Department of Electronics & Electrical Communication Engineering, Indian Institute of Technology, Kharagpur 721302 (India); Gogurla, Narendar [Department of Physics, Indian Institute of Technology, Kharagpur 721302 (India); Banerji, Pallab [Materials Science Centre, Indian Institute of Technology, Kharagpur 721302 (India); Guha, Prasanta K. [Department of Electronics & Electrical Communication Engineering, Indian Institute of Technology, Kharagpur 721302 (India); Pramanik, Panchanan, E-mail: pramanik1946@gmail.com [Department of Basic Science, MCKV Institute of Engineering, Howrah, Liluah 711204 (India)

    2015-10-15

    Graphical abstract: - Highlights: • β-FeSi{sub 2} nano-particle was synthesized by reducing with Mg and by diluting with MgO. • XRD profile shows the iron di-silicide phase to be semiconducting β-FeSi{sub 2}. • HRTEM and FESEM images indicate the β-FeSi{sub 2}average particle size to be 60–70 nm. • Absorption, reflectance and PL spectroscopy show band gap to be direct 0.87 eV. • Nano-β-FeSi{sub 2}is p-type with hole density of 4.38 × 10{sup 18} cm{sup −3} and mobility 8.9 cm{sup 2}/V s. - Abstract: Nano-particles of β-FeSi{sub 2} have been synthesized by chemical reduction of a glassy phase of [Fe{sub 2}O{sub 3}, 4SiO{sub 2}] by Mg-metal where MgO is used as diluent to prevent the agglomeration of nano crystallites into micro-particles and also act as a negative catalyst for the formation of other phases. The sample is characterized by XRD, FESEM, HRTEM, EDX, ultra-violet-visible-infrared and PL spectroscopy and electronic properties have been investigated by Hall measurement. XRD profile shows that the synthesized powder consists of purely β-FeSi{sub 2} semiconducting phase. The average crystallite size of β-FeSi{sub 2} is determined to be around 65.4 nm from XRD peaks as well as from FESEM also. The optical absorption and PL spectroscopy shows that synthesized β-FeSi{sub 2} phase is a direct band gap semiconductor with a value of 0.87 eV. Hall measurements show that β-FeSi{sub 2} nano-particles is p-type with hole concentration of 4.38 × 10{sup 18} cm{sup −3} and average hole mobility of 8.9 cm{sup 2}/V s at 300 K.

  7. Synthesis, characterization and chemical modification of a cationic polyelectrolyte poly(methylene amine)

    OpenAIRE

    Kundu, Nihar Ranjan

    2007-01-01

    Polyamine polymers have attracted attention due to their ability to demonstrate pH dependent cationic nature and presence of highly reactive pendant amino groups. These amino groups make them suitable for a host of applications through cross-linking and derivatization. As a result the end use application of a polyamine is largely driven by the number of amino groups and the way they are attached to the polymer backbone. Thus, this piece of work describes the synthesis and investigation of pro...

  8. Synthesis and physicochemical characterization of chemically modified chitosan by succinic anhydride

    OpenAIRE

    Karine Gargioni Pereira Correa de Mello; Leandra de Cássia Bernusso; Ronaldo Nogueira de Moraes Pitombo; Bronislaw Polakiewicz

    2006-01-01

    The N-succinil-chitosan is a chemically modified derivative of the biopolymer chitosan. The succinic anhydride attached to the free amino groups presented along the chitosan's polymer chain imparts to the molecule different physicochemical properties not exhibited before the modification. These chemical modifications enhance chitosan's solubility in slightly acid, neutral and alkaline media. These properties are related to the long alkyl chains attached to hydrophilic parts. In this case the ...

  9. The application of zero-current potentiometry in chemical synthesis and characterization of polypyrrole using electrochemical sensors

    Energy Technology Data Exchange (ETDEWEB)

    Budimir, M.V. (Faculty of Agriculture, Univ. of Osijek (Yugoslavia)); Sak-Bosnar, M. (Pedagogical Faculty, Univ. of Osijek (Yugoslavia)); Kovac, S. (Faculty of Food Tech., Univ. of Osijek (Yugoslavia)); Duic, L. (Faculty of Tech., Inst. of Electrochemistry, Univ. of Zagreb (Yugoslavia))

    1991-01-01

    The chemical polymerization of pyrrole to highly conducting polypyrrole in aqueous and acetonitrile solutions using various oxidizing agents was studied. The course of synthesis was followed using zero-current potentiometry with a platinum reference electrode as redox sensor. The obtained results can be used for a better understanding of pyrrole polymerization kinetics. In addition, the halogenide-ion content as counter ion can be determined potentiometrically after chemical degradation of polypyrrole using a chloride-selective electrode as sensor. (orig.).

  10. Physico-chemical studies on synthesis, characterization, and magnetic properties of Li-Ca-Zn nanoferrites

    Energy Technology Data Exchange (ETDEWEB)

    Randhawa, B. S., E-mail: balwinderrandhawa@gmail.com; Singh, Jashanpreet [Guru Nanak Dev University, Department of Chemistry, Centre of Advanced Studies (India)

    2013-01-15

    The synthesis of Li{sub 0.25}Ca{sub 0.5-X}Zn{sub X}Fe{sub 2.25}O{sub 4} (LCZ) spinel nanoferrites by the solution combustion method using oxalyl-dihydrazide as a fuel leads to the formation of fine nanoparticles. Structural studies such as X-ray diffraction and transmission electron microscope confirm the formation of single phase spinel with particle size in the range 26-43 nm while Moessbauer data under the shadow of magnetic studies attribute to the superparamagnetic nature of the ferrites obtained, resulting from the transition of ferrimagnetic to superparamagnetic phase. In addition, the magnetic studies reveal an initial increase in the saturation magnetization (M{sub S}) from 33.5 emu/g for X = 0-41.4 emu/g (X = 0.3) followed by a gradual decrease to 32.8 emu/g (X = 0.5) as the concentration of zinc increases while Curie temperature lies in the range 312-527 Degree-Sign C for the same series. Keeping in view the various properties of the nanoferrites formed, variation of dielectric constant has also been carried out with both frequency (20 Hz-1 MHz) and temperature (up to 500 Degree-Sign C). We believe that the synthesized LCZ nanoferrites can be suitable for their application in nanomagnetic and nanoelectronic devices for drug delivery and bioencapsulating systems.

  11. 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.

  12. 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.

  13. Chemical synthesis, characterizations and magnetic properties of nanocrystalline Fe50Co50 alloy

    International Nuclear Information System (INIS)

    Nanocrystalline Fe50Co50 alloy has been synthesized successfully by chemical reduction route using superhydride as reducing agent and oleic acid and oleylamine as capping agents. Phase purity, crystallite size and lattice parameters of the synthesized NPs are determined by X-ray powder diffraction method. FeCo alloy crystallizes in body centered cubic (bcc) structure having crystallite size equal to 29 nm and lattice parameters equal to 2.8546 Å. The size and shape morphologies of the material were studied by SEM analysis. SEM micrograph study shows the average particle size to be 60 nm and indicates the appearance of agglomerates of the nano-particles consisting of several crystallites. The room temperature magnetic hysteresis studies indicate ferromagnetic behavior of the materials. The values of saturation magnetization and coercivity were 65 emu/g and 460 Oe, respectively. Magnetic properties of the material were interpreted on the basis of fine particle magnetism

  14. 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.

  15. 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

  16. Synthesis and physicochemical characterization of chemically modified chitosan by succinic anhydride

    Directory of Open Access Journals (Sweden)

    Karine Gargioni Pereira Correa de Mello

    2006-07-01

    Full Text Available The N-succinil-chitosan is a chemically modified derivative of the biopolymer chitosan. The succinic anhydride attached to the free amino groups presented along the chitosan's polymer chain imparts to the molecule different physicochemical properties not exhibited before the modification. These chemical modifications enhance chitosan's solubility in slightly acid, neutral and alkaline media. These properties are related to the long alkyl chains attached to hydrophilic parts. In this case the hydrophilic part of D-glucosamine promotes stronger interactions with the water molecules, and consequently, enhances the solubility of the chitosan polymer. Non-modified free chitosan is soluble only in acidic medium (pH A N-succinil-quitosana é um derivado quimicamente modificado do biopolímero quitosana. A inserção de substituintes de anidrido succínico nas aminas protonadas presentes ao longo da cadeia do polímero quitosana, conferem diferentes características físico-químicas a molécula de quitosana. Esta modificação química, possibilitou à quitosana, solubilidade em pHs que variam do ácido (2.0 a 3.0 até alcalino (13.0 a 14.0. Estas propriedades são atribuídas ao alongamento da cadeia alquílica, que afasta a parte hidrofílica da cadeia fechada da D-glicosamina, facilitando o acesso da água, a qual irá estabelecer uma interação mais forte com a molécula de quitosana. Esta propriedade não está presente em amostras de quitosana pura, a qual sabe-se que solubiliza-se apenas em pH abaixo de 5.5. Estas modificações na quitosana possibilitam novas aplicações na área de biotecnologia, uma vez que a solubilidade em meio neutro e levemente alcalino é importante na área biológica.

  17. Chemical synthesis and characterization of magnesium substituted amorphous calcium phosphate (MG-ACP)

    International Nuclear Information System (INIS)

    Amorphous calcium phosphate (ACP) was synthesized by a simple aqueous precipitation using CaCl2 and Na3PO4 in the presence of MgCl2 to ensure the formation of the ACP phase at room temperature. Magnesium substituted ACP phases corresponding to two different compositions representing the two most prominent calcium phosphate phases (hydroxyapatite: Ca + Mg/P = 1.67 and tricalcium phosphate: Ca + Mg/P = 1.5) were synthesized by this simple approach. Both compositions of ACP phases resulted in their transformation into β-tricalcium phosphate upon heat treatment in air at 600 deg. C. X-ray diffraction (XRD), heat treatment, scanning electron microscopy (SEM), Fourier transform infrared (FT-IR) and Brunauer-Emmett-Teller (BET) analyses were used to characterize the phase, thermal stability, surface area, and morphology of the synthesized ACP powders corresponding to the two different nominal Ca/P compositions. Although it is known that α-TCP is the phase that appears upon heat treatment at 600 deg. C unsubstituted ACP, substitution of magnesium ion in ACP (both TCP and HA composition) stabilized the structure of β-TCMP phase at 600 deg. C. Moreover, FT-IR analysis revealed that the ACP phase regardless of the composition, exhibited characteristic bands corresponding to that of HA, with the exception of the ACP corresponding to HA composition which exhibited a prominent OH vibrational mode.

  18. Production and structural characterization of nanolayers of LiNbO3 by wet chemical synthesis

    International Nuclear Information System (INIS)

    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.

  19. 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 in an...

  20. Synthesis, characterization and biocompatibility of silver nanoparticles synthesized from Nigella sativa leaf extract in comparison with chemical silver nanoparticles.

    Science.gov (United States)

    Amooaghaie, Rayhaneh; Saeri, Mohammad Reza; Azizi, Morteza

    2015-10-01

    Despite the development potential in the field of nanotechnology, there is a concern about possible effects of nanoparticles on the environment and human health. In this study, silver nanoparticles (AgNPs) were synthesized by 'green' and 'chemical' methods. In the wet-chemistry method, sodium borohydrate, sodium citrate and silver nitrate were used as raw materials. Leaf extract of Nigella sativa was used as reducing as well as capping agent to reduce silver nitrate in the green synthesis method. In addition, toxic responses of both synthesized AgNPs were monitored on bone-building stem cells of mice as well as seed germination and seedling growth of six different plants (Lolium, wheat, bean and common vetch, lettuce and canola). In both synthesis methods, the colorless reaction mixtures turned brown and UV-visible spectra confirmed the presence of silver nanoparticles. Scanning electron microscope (SEM) observations revealed the predominance of silver nanosized crystallites and fourier transform infra-red spectroscopy (FTIR) indicated the role of different functional groups in the synthetic process. MTT assay showed cell viability of bone-building stem cells of mice was further in the green AgNPs synthesized using black cumin extract than chemical AgNPs. IC50 (inhibitory concentrations) values for seed germination, root and shoot length for 6 plants in green AgNPs exposures were higher than the chemical AgNPs. These results suggest that cytotoxicity and phytotoxicity of the green synthesized AgNPs were significantly less than wet-chemistry synthesized ones. This study indicated an economical, simple and efficient ecofriendly technique using leaves of N. sativa for synthesis of AgNPs and confirmed that green AgNPs are safer than chemically-synthesized AgNPs. PMID:26122733

  1. HNAB: synthesis and characterization

    Energy Technology Data Exchange (ETDEWEB)

    O' Keefe, D.M.

    1976-05-01

    The laboratory and pilot-plant scale synthesis of hexanitroazobenzene (HNAB) are detailed. Some of its physical, chemical, and explosive properties are presented and discussed. Among these are included polymorphic forms, thermal behavior, spectra, solubility, compatibility, toxicity, sensitivity to gap test, detonation velocity and pressure, impact sensitivity, and explosive classification. Finally, some alternate syntheses of HNAB and its intermediates are considered; some of these were successful and some were not.

  2. 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.

  3. Synthesis and characterization of bulk Cu2ZnSnX4 (X: S, Se) via thermodynamically supported mechano-chemical process

    International Nuclear Information System (INIS)

    Materials with the general formula, Cu2ZnSnX4 (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

  4. Chemical Synthesis of Copper Nanoparticles

    Directory of Open Access Journals (Sweden)

    Hamid Reza Ghorbani

    2014-06-01

    Full Text Available Metal nanoparticles have attracted considerable interest particularly because of the size dependence of physical and chemical properties and its enormous technological potential. Among different metal nanoparticles, copper nanoparticles have attracted great attention because copper is one of the most key metals in new technology. Chemical methods are used to synthesize copper nanoparticles and among them chemical reduction is the most frequently applied method for the preparation of stable, colloidal dispersions in organic solvents. In this paper, a brief overview of the current research worldwide in the chemical synthesis of copper nanoparticles is discussed.

  5. A new nitrosyl ruthenium complex: synthesis, chemical characterization, in vitro and in vivo antitumor activities and probable mechanism of action.

    Science.gov (United States)

    Heinrich, Tassiele A; Von Poelhsitz, Gustavo; Reis, Rosana I; Castellano, Eduardo E; Neves, Ademir; Lanznaster, Maurício; Machado, Sérgio P; Batista, Alzir A; Costa-Neto, Claudio M

    2011-09-01

    This study describes the synthesis of a new ruthenium nitrosyl complex with the formula [RuCl(2)NO(BPA)] [BPA = (2-hydroxybenzyl)(2-methylpyridyl)amine ion], which was synthesized and characterized by spectroscopy, cyclic voltammetry, X-ray crystallography, and theoretical calculation data. The biological studies of this complex included in vitro cytotoxic assays, which revealed its activity against two different tumor cell lines (HeLa and Tm5), with efficacy comparable to that of cisplatin, a metal-based drug that is administered in clinical treatment. The in vivo studies showed that [RuCl(2)NO(BPA)]is effective in reducing tumor mass. Also, our results suggest that the mechanism of action of [RuCl(2)NO(BPA)] includes binding to DNA, causing fragmentation of this biological molecule, which leads to apoptosis. PMID:21665332

  6. Synthesis of chemically modified DNA.

    Science.gov (United States)

    Shivalingam, Arun; Brown, Tom

    2016-06-15

    Naturally occurring DNA is encoded by the four nucleobases adenine, cytosine, guanine and thymine. Yet minor chemical modifications to these bases, such as methylation, can significantly alter DNA function, and more drastic changes, such as replacement with unnatural base pairs, could expand its function. In order to realize the full potential of DNA in therapeutic and synthetic biology applications, our ability to 'write' long modified DNA in a controlled manner must be improved. This review highlights methods currently used for the synthesis of moderately long chemically modified nucleic acids (up to 1000 bp), their limitations and areas for future expansion. PMID:27284032

  7. Synthesis and structural characterization of tungsten trioxide nanoplatelet-containing thin films prepared by Aqueous Chemical Growth

    International Nuclear Information System (INIS)

    We report the synthesis of WO3 thin films predominantly made up of nanoplatelets, on transparent plain glass microscope slides, by the low-temperature, soft chemistry method of Aqueous Chemical Growth (ACG). During the heterogeneous growth, by ACG, of WO3 thin films onto these plain glass substrates, nanoplatelet and nanorod-like structures of WO3 were also precipitated out of the Peroxotungstic acid precursor solutions and collected as slurries which were annealed at 500 °C to give ultra-fine powders of WO3. Scanning Electron Microscopy of the thin films and powders showed that nanoplatelets formed had thicknesses generally less than 300 nm and lengths and diameters in the 1–2 μm range. The thin films formed were less than 5 μm thick. Transmission Electron Microscopy (TEM) on one of the thin films confirmed the formation of nanoplatelets as well as nanorod-like structures, while High Resolution TEM alongside X-ray Diffraction and Raman spectroscopy suggested that the WO3 thin film grown on a plain glass microscope slide was monoclinic in crystal structure. While Energy Dispersive X-ray Spectroscopy, Fourier Transform-Infrared Spectroscopy, and Attenuated Total Reflection were used to establish the purity and bond structure of WO3 within the thin film, Selected Area Electron Diffraction gave further evidence of crystallinity within the nanostructures prepared. The potential use of the WO3 nanoplatelet-containing thin films for hydrogen sensing at 300 °C was demonstrated. - Highlights: ► WO3 thin films grown on glass slides by Aqueous Chemical Growth, at 90–95 °C ► Formation of square-nanoplatelets in the thin films is confirmed. ► Raman spectroscopy confirms platelets to be monoclinic in crystal structure. ► Drop-coated thick films of WO3 nanoplatelets on glass, sensed H2 at 300 °C

  8. Synthesis and characterization of NiCrx Fe2-xO4 oxides (simulated corrosion products) for chemical decontamination

    International Nuclear Information System (INIS)

    Water-cooled nuclear power reactors such as Boiling Water Reactors (BWR), Pressurized light Water Reactors (PWR/VVER) and Pressurized Heavy Water Reactors (PHWR) face the problems of increasing radiation field on the out of core surfaces of primary systems over a period of operation. The radiation field is attributed to the activation of corrosion products by neutron flux. The main source of corrosion products are the structural material like carbon steel, stainless steel, and high nickel alloys and the oxides formed on these material surfaces also act as host for the radionuclides leading to radiation build-up due to deposition of activated corrosion products. Type of water chemistry regimes followed and the composition of the structural materials in the primary circuits lead to the formation of different type of oxides. In the case of BWRs reactor coolant circuits outer most oxide film is haematite (Fe2O3), followed by magnetite (Fe3O4), nickel and chromium substituted magnetite (NiFe2-xCrxO4) and inner film contains chromite spinels. Recently, sol-gel combustion synthesis has emerged as an attracting technique for the production of high purity and crystalline oxide powders at significantly lower temperatures compared to the conventional solid state synthetic methods. In order to understand the mechanistic aspects of decontamination, a series of chromium substituted nickel ferrites were chosen for preparation, characterization and its dissolution studies

  9. 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.

  10. 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)

  11. 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

    2016-01-01

    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. PMID:27143312

  12. 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.

  13. 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

  14. 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.

  15. Mapping student thinking in chemical synthesis

    Science.gov (United States)

    Weinrich, Melissa

    In order to support the development of learning progressions about central ideas and practices in different disciplines, we need detailed analyses of the implicit assumptions and reasoning strategies that guide students' thinking at different educational levels. In the particular case of chemistry, understanding how new chemical substances are produced (chemical synthesis) is of critical importance. Thus, we have used a qualitative research approach based on individual interviews with first semester general chemistry students (n = 16), second semester organic chemistry students (n = 15), advanced undergraduates (n = 9), first year graduate students (n = 15), and PhD candidates (n = 16) to better characterize diverse students' underlying cognitive elements (conceptual modes and modes of reasoning) when thinking about chemical synthesis. Our results reveal a great variability in the cognitive resources and strategies used by students with different levels of training in the discipline to make decisions, particularly at intermediate levels of expertise. The specific nature of the task had a strong influence on the conceptual sophistication and mode of reasoning that students exhibited. Nevertheless, our data analysis has allowed us to identify common modes of reasoning and assumptions that seem to guide students' thinking at different educational levels. Our results should facilitate the development of learning progressions that help improve chemistry instruction, curriculum, and assessment.

  16. Synthesis and characterization of the manganese cobaltite spinel prepared using two 'soft chemical' methods

    Energy Technology Data Exchange (ETDEWEB)

    Brylewski, Tomasz, E-mail: brylew@agh.edu.pl [AGH University of Science and Technology, Faculty of Materials Science and Ceramics, Al. Mickiewicza 30, 30-059 Krakow (Poland); Kruk, Andrzej; Adamczyk, Anna; Kucza, Witold; Stygar, Miroslaw; Przybylski, Kazimierz [AGH University of Science and Technology, Faculty of Materials Science and Ceramics, Al. Mickiewicza 30, 30-059 Krakow (Poland)

    2012-11-15

    Using the coprecipitation method and EDTA gel processes, manganese cobaltite (Mn{sub 1.5}Co{sub 1.5}O{sub 4}) powders were successfully synthesized. The thermal decomposition behavior of the gel precursors, phase formation and morphology of the Mn{sub 1.5}Co{sub 1.5}O{sub 4} powders were characterized by means of DTA/TGA and MS analyses, X-ray diffraction (XRD), and scanning electron microscopy (SEM), respectively. Well-crystallized dual-phase manganese cobaltite spinel, containing both the cubic and tetragonal phases, was obtained at room temperature for both types of powders calcinated at 800 Degree-Sign C for 10 h in static air, without formation of any intermediate phase. SEM investigations show that the Mn{sub 1.5}Co{sub 1.5}O{sub 4} powders prepared using two 'soft chemical' methods were agglomerates composed of approximately micron-sized particles. The structure and morphology of the bulk samples, as well as their electrical conductivity, were investigated using XRD, SEM, and EIS, respectively. Mn{sub 1.5}Co{sub 1.5}O{sub 4} spinels with different microstructure exhibited excellent electrical conductivity and structural stability. Major emphasis was placed on structural transformations of the spinel solid solutions with temperature and their effect on the electrical properties of these solutions. -- Highlights: Black-Right-Pointing-Pointer Mn{sub 1.5}Co{sub 1.5}O{sub 4} powders were prepared using coprecipitation and EDTA gel processes. Black-Right-Pointing-Pointer Approximately micron-sized particles with cubic and tetragonal grains. Black-Right-Pointing-Pointer A transition occurs in the 250-450 Degree-Sign C range. Black-Right-Pointing-Pointer Only the cubic spinel phase is observed at higher temperatures. Black-Right-Pointing-Pointer At higher temperature electrical conductivity is related to the grain volume.

  17. 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.

  18. Matrix Synthesis and Characterization

    Science.gov (United States)

    1984-01-01

    The role of NASA in the area of composite material synthesis; evaluation techniques; prediction analysis techniques; solvent-resistant tough composite matrix; resistance to paint strippers; acceptable processing temperature and pressure for thermoplastics; and the role of computer modeling and fiber interface improvement were discussed.

  19. Synthesis and characterization Bi2O2S thin film via chemical bath deposition at low pH.

    Science.gov (United States)

    Kariper, I Afşin

    2016-06-15

    Bismuth oxysulfide thin film was prepared using Bi(NO3)3 and Na2S as reactive. Since bismuth in the form of bismuth oxide is dissolved into water, bismuth and sulfide concentration of the chemical bath is very important. Bismuth oxysulfide (Bi2O2S) thin films were produced below pH2. Tested bismuth and sulfide concentrations are as follows: 2×10(-1)M, 2×10(-2)M, 2×10(-3)M, 2×10(-4)M bismuth and 1×10(-1)M, 1×10(-2)M, 1×10(-3)M, 1×10(-4)M sulfide. The structure of the films was examined via X-ray diffraction (XRD). Optical properties, such as transmission and absorbance were measured with Ultra violet-visible spectrum, and then refractive index and reflectivity were calculated. The pH of chemical bath was stabilized below pH of 2 using 13.85mL concentrated nitric acid. Deposition time and temperature of the baths were 4h and 30°C. It has been found that bismuth and sulfide concentrations affected the structure and thickness of the film. Also, optical band gap of the films varied with concentration, parallel to the change of the structure and film thickness. PMID:27043873

  20. Chemical synthesis, characterizations and magnetic properties of nanocrystalline Fe{sub 50}Co{sub 50} alloy

    Energy Technology Data Exchange (ETDEWEB)

    Dalavi, Shankar B.; Panda, Rabi Narayan, E-mail: rnp@goa.bits-pilani.ac.in [Department of Chemistry, BITS-Pilani, K. K. Birla Goa Campus, Zuarinagar, Goa-403726 (India); Raja, M. Manivel [Defence Metallurgical Research Laboratory, Hyderabad-500058 (India)

    2014-04-24

    Nanocrystalline Fe{sub 50}Co{sub 50} alloy has been synthesized successfully by chemical reduction route using superhydride as reducing agent and oleic acid and oleylamine as capping agents. Phase purity, crystallite size and lattice parameters of the synthesized NPs are determined by X-ray powder diffraction method. FeCo alloy crystallizes in body centered cubic (bcc) structure having crystallite size equal to 29 nm and lattice parameters equal to 2.8546 Å. The size and shape morphologies of the material were studied by SEM analysis. SEM micrograph study shows the average particle size to be 60 nm and indicates the appearance of agglomerates of the nano-particles consisting of several crystallites. The room temperature magnetic hysteresis studies indicate ferromagnetic behavior of the materials. The values of saturation magnetization and coercivity were 65 emu/g and 460 Oe, respectively. Magnetic properties of the material were interpreted on the basis of fine particle magnetism.

  1. Zirconia-magnesia inert matrix fuel and waste form: Synthesis, characterization and chemical performance in an advanced fuel cycle

    Science.gov (United States)

    Holliday, Kiel Steven

    There is a significant buildup in plutonium stockpiles throughout the world, because of spent nuclear fuel and the dismantling of weapons. The radiotoxicity of this material and proliferation risk has led to a desire for destroying excess plutonium. To do this effectively, it must be fissioned in a reactor as part of a uranium free fuel to eliminate the generation of more plutonium. This requires an inert matrix to volumetrically dilute the fissile plutonium. Zirconia-magnesia dual phase ceramic has been demonstrated to be a favorable material for this task. It is neutron transparent, zirconia is chemically robust, magnesia has good thermal conductivity and the ceramic has been calculated to conform to current economic and safety standards. This dissertation contributes to the knowledge of zirconia-magnesia as an inert matrix fuel to establish behavior of the material containing a fissile component. First, the zirconia-magnesia inert matrix is synthesized in a dual phase ceramic containing a fissile component and a burnable poison. The chemical constitution of the ceramic is then determined. Next, the material performance is assessed under conditions relevant to an advanced fuel cycle. Reactor conditions were assessed with high temperature, high pressure water. Various acid solutions were used in an effort to dissolve the material for reprocessing. The ceramic was also tested as a waste form under environmental conditions, should it go directly to a repository as a spent fuel. The applicability of zirconia-magnesia as an inert matrix fuel and waste form was tested and found to be a promising material for such applications.

  2. Chemical characterization of bohrium (element 107)

    Science.gov (United States)

    Eichler; Bruchle; Dressler; Dullmann; Eichler; Gaggeler; Gregorich; Hoffman; Hubener; Jost; Kirbach; Laue; Lavanchy; Nitsche; Patin; Piguet; Schadel; Shaughnessy; Strellis; Taut; Tobler; Tsyganov; Turler; Vahle; Wilk; Yakushev

    2000-09-01

    The arrangement of the chemical elements in the periodic table highlights resemblances in chemical properties, which reflect the elements' electronic structure. For the heaviest elements, however, deviations in the periodicity of chemical properties are expected: electrons in orbitals with a high probability density near the nucleus are accelerated by the large nuclear charges to relativistic velocities, which increase their binding energies and cause orbital contraction. This leads to more efficient screening of the nuclear charge and corresponding destabilization of the outer d and f orbitals: it is these changes that can give rise to unexpected chemical properties. The synthesis of increasingly heavy elements, now including that of elements 114, 116 and 118, allows the investigation of this effect, provided sufficiently long-lived isotopes for chemical characterization are available. In the case of elements 104 and 105, for example, relativistic effects interrupt characteristic trends in the chemical properties of the elements constituting the corresponding columns of the periodic table, whereas element 106 behaves in accordance with the expected periodicity. Here we report the chemical separation and characterization of six atoms of element 107 (bohrium, Bh), in the form of its oxychloride. We find that this compound is less volatile than the oxychlorides of the lighter elements of group VII, thus confirming relativistic calculations that predict the behaviour of bohrium, like that of element 106, to coincide with that expected on the basis of its position in the periodic table. PMID:10993071

  3. Chemical characterization of bohrium (element 107)

    Science.gov (United States)

    Eichler, R.; Brüchle, W.; Dressler, R.; Düllmann, Ch. E.; Eichler, B.; Gäggeler, H. W.; Gregorich, K. E.; Hoffman, D. C.; Hübener, S.; Jost, D. T.; Kirbach, U. W.; Laue, C. A.; Lavanchy, V. M.; Nitsche, H.; Patin, J. B.; Piguet, D.; Schädel, M.; Shaughnessy, D. A.; Strellis, D. A.; Taut, S.; Tobler, L.; Tsyganov, Y. S.; Türler, A.; Vahle, A.; WiIk, P. A.; Yakushev, A. B.

    2000-09-01

    The arrangement of the chemical elements in the periodic table highlights resemblances in chemical properties, which reflect the elements' electronic structure. For the heaviest elements, however, deviations in the periodicity of chemical properties are expected: electrons in orbitals with a high probability density near the nucleus are accelerated by the large nuclear charges to relativistic velocities, which increase their binding energies and cause orbital contraction. This leads to more efficient screening of the nuclear charge and corresponding destabilization of the outer d and f orbitals: it is these changes that can give rise to unexpected chemical properties. The synthesis of increasingly heavy elements, now including that of elements 114, 116 and 118, allows the investigation of this effect, provided sufficiently long-lived isotopes for chemical characterization are available. In the case of elements 104 and 105, for example, relativistic effects interrupt characteristic trends in the chemical properties of the elements constituting the corresponding columns of the periodic table, whereas element 106 behaves in accordance with the expected periodicity. Here we report the chemical separation and characterization of six atoms of element 107 (bohrium, Bh), in the form of its oxychloride. We find that this compound is less volatile than the oxychlorides of the lighter elements of group VII, thus confirming relativistic calculations that predict the behaviour of bohrium, like that of element 106, to coincide with that expected on the basis of its position in the periodic table.

  4. Tools for chemical synthesis in microsystems

    OpenAIRE

    Jensen, Klavs F.; Newman, Stephen G.; Reizman, Brandon Jacob

    2014-01-01

    Chemical synthesis in microsystems has evolved from simple proof-of-principle examples to become a general technique in academia and industry. Numerous such “flow chemistry” applications are now found in pharmaceutical and fine chemical synthesis. Much of the development has been based on systems employing macroscopic flow components and tubes, rather than the integrated chip technology envisioned by the lab-on-a-chip community. We review the major developments in systems for flow chemistry a...

  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. 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.

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

    CERN Document Server

    Yihong, Wu; Ting, Yu

    2013-01-01

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

  8. Opportunities for Merging Chemical and Biological Synthesis

    OpenAIRE

    Wallace, Stephen; Balskus, Emily P.

    2014-01-01

    Organic chemists and metabolic engineers use largely orthogonal technologies to access small molecules like pharmaceuticals and commodity chemicals. As the use of biological catalysts and engineered organisms for chemical production grows, it is becoming increasingly evident that future efforts for chemical manufacture will benefit from the integration and unified expansion of these two fields. This review will discuss approaches that combine chemical and biological synthesis for small molecu...

  9. Synthesis and characterization of N-acylaniline derivatives as potential chemical hybridizing agents (CHAs) for wheat (Triticum aestivum L.).

    Science.gov (United States)

    Chakraborty, Kajal; Devakumar, C

    2006-09-01

    Induction of male sterility by deployment of chemical hybridizing agents (CHAs) are important in heterosis breeding of self-pollinated crops like wheat, wherein the male and female organs are in the same flower. Taking a lead from the earlier work on rice, a total of 25 N-acylanilines comprising of malonanilates, acetoacetanilides, and acetanilides (including halogenated acetanilides) were synthesized and screened as CHAs on three genotypes of wheat, viz., PBW 343, HD 2046, and HD 2733 at 1500 ppm in the winter of 2001-2002. The N-acylanilines containing variations at the acyl and aromatic domain were synthesized by condensation of substituted anilines with appropriate diesters, acid chlorides, or monoesters. The test compounds with highly electronegative groups such as F/Br at the para position of the aryl ring were identified as the most potent CHAs, causing higher induction of male sterility. A variation of N-substitution at the side chain generally furnished analogues like 4'-fluoroacetoacetanilide (7) and ethyl 4'-fluoromalonanilate (1), which induced 89.12 and 84.66% male sterility, respectively, in PBW 343. Among halogenated acetanilides, the increasing number of chlorine atoms in the side chain led to an increase in the activity of 4'-fluoro (23) and 4'-bromo (24) derivatives of trichoroacetanilides, which induced >87% male sterility. Quantitative structure-activity relationship (QSAR) models indicated the positive contributions of the field effect exemplified by the Swain-Lupton constant (Fp) and negative contributions of the Swain-Lupton resonance constant (R) for the aromatic substitution. The positive influences of parachor (P) for the acyl domain have been underlined. These leads will be significant in explaining the CHA fit in the macromolecular receptor site. The CHAs appeared to act by causing an imbalance in the acid-base equilibrium in pollen mother cells resulting in dissolution of the callose wall by premature callase secretion. PMID:16939342

  10. 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.

  11. 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.

  12. Chemical synthesis of magnetic nanocrystals: Recent progress

    International Nuclear Information System (INIS)

    Colloidal chemical synthesis of various types of magnetic nanocrystals is discussed with regard to recent discoveries. We first outline the chemical preparation of single-component magnetic nanocrystals with controlled size, shape, and uniformity based on several solution-phase methods, especially thermal decomposition and/or reduction method. Then we discuss the synthetic strategies of multi-component nanocrystals incorporating at least one magnetic component by manipulating heterogeneous nucleation and growth process. Toward the end, approaches for preparing hollow/porous magnetic nanocrystals are highlighted. We believe that the summarized chemical synthesis will pave the way for the future development of extraordinary magnetic nanocrystals. (topical review - magnetism, magnetic materials, and interdisciplinary research)

  13. Chemical characterization of element 112.

    Science.gov (United States)

    Eichler, R; Aksenov, N V; Belozerov, A V; Bozhikov, G A; Chepigin, V I; Dmitriev, S N; Dressler, R; Gäggeler, H W; Gorshkov, V A; Haenssler, F; Itkis, M G; Laube, A; Lebedev, V Ya; Malyshev, O N; Oganessian, Yu Ts; Petrushkin, O V; Piguet, D; Rasmussen, P; Shishkin, S V; Shutov, A V; Svirikhin, A I; Tereshatov, E E; Vostokin, G K; Wegrzecki, M; Yeremin, A V

    2007-05-01

    The heaviest elements to have been chemically characterized are seaborgium (element 106), bohrium (element 107) and hassium (element 108). All three behave according to their respective positions in groups 6, 7 and 8 of the periodic table, which arranges elements according to their outermost electrons and hence their chemical properties. However, the chemical characterization results are not trivial: relativistic effects on the electronic structure of the heaviest elements can strongly influence chemical properties. The next heavy element targeted for chemical characterization is element 112; its closed-shell electronic structure with a filled outer s orbital suggests that it may be particularly susceptible to strong deviations from the chemical property trends expected within group 12. Indeed, first experiments concluded that element 112 does not behave like its lighter homologue mercury. However, the production and identification methods used cast doubt on the validity of this result. Here we report a more reliable chemical characterization of element 112, involving the production of two atoms of (283)112 through the alpha decay of the short-lived (287)114 (which itself forms in the nuclear fusion reaction of 48Ca with 242Pu) and the adsorption of the two atoms on a gold surface. By directly comparing the adsorption characteristics of (283)112 to that of mercury and the noble gas radon, we find that element 112 is very volatile and, unlike radon, reveals a metallic interaction with the gold surface. These adsorption characteristics establish element 112 as a typical element of group 12, and its successful production unambiguously establishes the approach to the island of stability of superheavy elements through 48Ca-induced nuclear fusion reactions with actinides. PMID:17476264

  14. Chemical characterization of element 112

    Science.gov (United States)

    Eichler, R.; Aksenov, N. V.; Belozerov, A. V.; Bozhikov, G. A.; Chepigin, V. I.; Dmitriev, S. N.; Dressler, R.; Gäggeler, H. W.; Gorshkov, V. A.; Haenssler, F.; Itkis, M. G.; Laube, A.; Lebedev, V. Ya.; Malyshev, O. N.; Oganessian, Yu. Ts.; Petrushkin, O. V.; Piguet, D.; Rasmussen, P.; Shishkin, S. V.; Shutov, A. V.; Svirikhin, A. I.; Tereshatov, E. E.; Vostokin, G. K.; Wegrzecki, M.; Yeremin, A. V.

    2007-05-01

    The heaviest elements to have been chemically characterized are seaborgium (element 106), bohrium (element 107) and hassium (element 108). All three behave according to their respective positions in groups 6, 7 and 8 of the periodic table, which arranges elements according to their outermost electrons and hence their chemical properties. However, the chemical characterization results are not trivial: relativistic effects on the electronic structure of the heaviest elements can strongly influence chemical properties. The next heavy element targeted for chemical characterization is element 112; its closed-shell electronic structure with a filled outer s orbital suggests that it may be particularly susceptible to strong deviations from the chemical property trends expected within group 12. Indeed, first experiments concluded that element 112 does not behave like its lighter homologue mercury. However, the production and identification methods used cast doubt on the validity of this result. Here we report a more reliable chemical characterization of element 112, involving the production of two atoms of 283112 through the alpha decay of the short-lived 287114 (which itself forms in the nuclear fusion reaction of 48Ca with 242Pu) and the adsorption of the two atoms on a gold surface. By directly comparing the adsorption characteristics of 283112 to that of mercury and the noble gas radon, we find that element 112 is very volatile and, unlike radon, reveals a metallic interaction with the gold surface. These adsorption characteristics establish element 112 as a typical element of group 12, and its successful production unambiguously establishes the approach to the island of stability of superheavy elements through 48Ca-induced nuclear fusion reactions with actinides.

  15. Synthesis, characterization and degradation of some polyamines

    International Nuclear Information System (INIS)

    The present assignment deals with the synthesis, characterization and thermal degradation of poly-tertiary butyl aziridine (PTBA) and its copolymers with PMMA. Macro monomer of MMA and TBA was synthesised, its polymerisation and degradation studies were also conducted. Chapter one describes the major synthetic modes and the degradative processes in polymers and the ways and means to retard the degradation are also discussed. Chapter two includes the details of analytical and thermo analytical techniques used in the present research. Chapter three describes the methods employed for purification of chemicals, experimental details and data for the synthesis of monomers and polymers, characterization methodologies and isolation techniques. Chapter four includes the characterization of poly-tertiary butyl aziridine (PTBA) which was synthesised through cationic ring opening polymerization. Significant feature being the production of oligomers in bulk quantity which were collected as cold ring fraction. The mechanisms were proposed for the degradation products. Bifunctional anionic polymerisation of MMA to the desired molecular weight, end capping it with carbon disulfide, and block copolymer synthesis of PMMA with 'living' PTBA is included in chapter five. Chapter six includes the details of the modification procedure adopted for PMMA to generate desirable 'sites' on the polymer. Living PTBA segment were later grafted onto those sites to yield PMMA-g-PTBA. The TG, TVA and SATVA shows that the copolymer is quite stable and the degradation products are almost evenly distributed in liquid and cold ring fraction with very little condensable volatile fraction. In the final chapter the details of synthesis of a new monomer N-methyl-N-tert.butyl-amino ethyl-methacrylate (MTBAEM) are given. The polymerisation and characterization of the MTBAEM is discussed in details. Thermal analysis through TG, TVA and SATVA was conducted, the major fraction was collected at the cold ring

  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. Manganese borohydride; synthesis and characterization

    OpenAIRE

    Richter, Bo; Ravnsbæk, Dorthe B.; Tumanov, Nikolay; Filinchuk, Yaroslav; Jensen, Torben R.

    2015-01-01

    Solvent-based synthesis and characterization of α-Mn(BH4)2 and a new nanoporous polymorph of manganese borohydride, γ-Mn(BH4)2, via a new solvate precursor, Mn(BH4)2·1/2S(CH3)2, is presented. Manganese chloride is reacted with lithium borohydride in a toluene/dimethylsulfide mixture at room temperature, which yields halide and solvent-free manganese borohydride after extraction with dimethylsulfide (DMS) and subsequent removal of residual solvent. This work constitutes the first example of es...

  18. Synthesis and characterization of boron nitrides nanotubes

    International Nuclear Information System (INIS)

    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)

  19. 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.

  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. ALTERNATIVE FUELS AND CHEMICALS FROM SYNTHESIS GAS

    Energy Technology Data Exchange (ETDEWEB)

    Peter J. Tijrn

    2000-09-30

    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.

  3. ALTERNATIVE FUELS AND CHEMICALS FROM SYNTHESIS GAS

    Energy Technology Data Exchange (ETDEWEB)

    Unknown

    2001-03-31

    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.

  4. ALTERNATIVE FUELS AND CHEMICALS FROM SYNTHESIS GAS

    Energy Technology Data Exchange (ETDEWEB)

    Peter J. Tijrn

    2000-06-30

    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

    1999-10-01

    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.

  6. ALTERNATIVE FUELS AND CHEMICALS FROM SYNTHESIS GAS

    Energy Technology Data Exchange (ETDEWEB)

    Unknown

    1999-07-01

    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.

  7. ALTERNATIVE FUELS AND CHEMICALS FROM SYNTHESIS GAS

    Energy Technology Data Exchange (ETDEWEB)

    Unknown

    2002-07-01

    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.

  8. 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.

  9. ALTERNATIVE FUELS AND CHEMICALS FROM SYNTHESIS GAS

    Energy Technology Data Exchange (ETDEWEB)

    Unknown

    2000-10-01

    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.

  10. ALTERNATIVE FUELS AND CHEMICALS FROM SYNTHESIS GAS

    Energy Technology Data Exchange (ETDEWEB)

    Unknown

    1998-01-01

    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.

  11. 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.

  12. 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.

  13. 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.

  14. 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.

  15. 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.

  16. 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.

  17. Efficient Biocatalytic Synthesis of Chiral Chemicals.

    Science.gov (United States)

    Zhang, Zhi-Jun; Pan, Jiang; Ma, Bao-Di; Xu, Jian-He

    2016-01-01

    Chiral chemicals are a group of important chiral synthons for the synthesis of a series of pharmaceuticals, agrochemicals, and fine chemicals. In past decades, a number of biocatalytic approaches have been developed for the green and effective synthesis of various chiral chemicals. However, the practical application of these biocatalytic processes is still hindered by the lack of highly efficient and robust biocatalysts, which usually results in the low volumetric productivity and high cost of the bioprocesses. Further step forward of biocatalysis in industrial application strongly requires the development of versatile and highly efficient biocatalysts, aiming to increase the process efficiency and facilitate the downstream processing. Recently, the fast growth of genome sequences in the database in post-genomic era offers great opportunities for accessing numerous biocatalysts with practical application potential, and the so-called genome mining approach provides time-effective and highly specific strategy for the fast identification of target enzymes with desired properties and outperforms the traditional screening of soil samples for microbial enzyme producers of interest. A number of biocatalytic processes with industrial application potential were developed thereafter. Further development of protein engineering strategies, process optimization, and cooperative work between biologists, organic chemists, and engineers is expected to make biocatalysis technology the first choice approach for the eco-friendly, highly efficient, and cost-effective synthesis of chiral chemicals in the near future. PMID:25537446

  18. Chemical Vapor Synthesis of Nanocrystalline Oxides

    Science.gov (United States)

    Djenadic, Ruzica; Winterer, Markus

    The generation of nanoparticles in the gas phase by Chemical Vapor Synthesis (CVS) may be described from the point of view of chemical engineering as a sequence of unit operations among which reactant delivery, reaction energy input, and product separation are key processes which determine the product characteristics and quality required by the applications of nanoparticles and powders. In case of CVS, the volatility of the reactants (precursors) may severely limit the possible type of products as well as the production rate. It is shown that these limits can be lifted by use of a laser flash evaporator which also enables the use of precursor mixtures for the production of complex oxides as shown for Co-doped ZnO and the pulsed operation to influence powder characteristics. The mode in which energy is supplied to the particle synthesis reactor has also substantial influence on particle and powder characteristics as is shown for TiO2 using different time-temperatureprofiles.

  19. Synthesis and optimization of integrated chemical processes

    Energy Technology Data Exchange (ETDEWEB)

    Barton, Paul I.; Evans, Lawrence B.

    2002-04-26

    This is the final technical report for the project titled ''Synthesis and optimization of integrated chemical processes''. Progress is reported on novel algorithms for the computation of all heteroazeotropic compositions present in complex liquid mixtures; the design of novel flexible azeotropic separation processes using middle vessel batch distillation columns; and theory and algorithms for sensitivity analysis and numerical optimization of hybrid discrete/continuous dynamic systems.

  20. Synthesis and characterization of a cerebral radiotracer

    International Nuclear Information System (INIS)

    The development of nuclear medicine is based on research of new radiopharmaceuticals, in particular, relying on technetium-99m, the most used radioisotope in terms of availability and low cost. A similar study on Rhenium (185/187Re) is essential for monitoring physico-chemical studies due to the high specific activity of technetium-99m. During this work, we have synthesized and labeled with technetium the N-methyl-4-hydroxy piperidinyl ferrocenyl carboxylate. The marking is done by exchange of ligands between the iron group of ferrocene and tricabonyl technetium core. We have succeeded to synthesis the N-methyl-4-hydroxy piperidinyl carboxyl cyclopentadienyl tricarbonyl rhenium (the molecular analogue of the technetium). We characterized it by MS, IR and NMR (1H, 13C) The structure of N-methyl-4-hydroxy piperidinyl carboxyl cyclopentadienyl tricarbonyl technetium is well justified.

  1. Synthesis and structural characterization of microporous glasses

    International Nuclear Information System (INIS)

    The silica powder production is one of the fundamental raw material industries, and plays an important role in chemical processing ones. For some specific applications, finer and less aggregated powders with higher purity are needed. For others, micro porosity and specific surface area plays and important role. New technologies have been implemented to establish inferior limits in size, specific surface area and porosity of these materials. Here we present the synthesis of a new microporous silica powder (purity . 98%) produced from glasses obtained from oil shale processing wastes. It comprises the acid leaching of glasses with chloridric acid at 90 deg C. XRD, SEM/EDX, FTIR, specific surface area measurements, particle size analysis and DTA/TGA were used to characterize these materials. (author)

  2. 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.

  3. 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.

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

    International Nuclear Information System (INIS)

    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 (Fe3O4). The relaxivities r2 and r2* values were determined from the transverse relaxation times T2 and T2* 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

  5. 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.

  6. 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)

  7. Chevrel phases superconductive and ultrafine powders synthesis and characterization

    International Nuclear Information System (INIS)

    This work deals with the Chevrel phases superconductive and ultrafine powders synthesis and characterization. The first part of this study presents some new way of synthesis (precipitation, coprecipitation) of Chevrel phases precursors powders (PbS, SnS, MoS2) and their characterizations (X-ray fluorescence analysis, ICP mass spectroscopy, scanning electron microscopy, transmission electron microscopy and laser granulometry). These new synthesis methods lead to quasi spherical morphology grains and very weak size grains (0.2 to 0.5 μm) whereas the chemical preparation from the solid state elements gives very different morphology grains (small plates) with a size of 1 to 20 μm. In the second part is shown the interest of the binary Mo6 S8 as precursor in the synthesis of ternary superconductive phases (Li, Ni, Cu, Pb). The last part presents the formation reaction of the phase PbMo6 S8 and its main chemical and physical properties. Thus some calorimetric measures associated with X-ray diffraction analysis have been realized and have allowed to understand the different reactions occurring during the PbMo6S8 synthesis. (O.L.). 100 refs., figs., tabs

  8. 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.

  9. 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.

  10. 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).

  11. Synthesis and characterization of ferromagnetic nanowires

    Science.gov (United States)

    Tsai, Poching

    Ferromagnetic nanocrystals with shape anisotropy have drawn great attention in the past decades because of their unique magnetic properties and for their potential applications in ultra-high-density magnetic recording media, exchange-coupled nanocomposite magnets and related nanodevices. In this thesis, synthesis and characterixation of ferromagnetic CoNi and CoFe nanowires are reported. CoNi nanocrystals with different size, shape and composition were successfully synthesized via a catalyst chemical solution method. It was found out that the structure and morphology can be controlled by altering the NaOH concentration, and the elongation of the nanowires can be adjusted by changing surfactants ratio and catalyst amount. Unlike the CoNi, CoFe nanocrystals were prepared by a non-catalyst chemistry solution method. The particle size and shape are controlled by varying parameters such as solvent amount, surfactant ratio, reducing agent and heating rate. Morphological, structural, and compositional characterizations of the nanoparticles were performed by using Transmission Electron Microscopy (TEM), high resolution TEM (HRTEM), and X-Ray Diffractometer (XRD). Magnetic properties of nanoparticles of different size were studied by Alternating Gradiant Magnetometer (AGM).

  12. Chemical characterization of atmospheric particles

    International Nuclear Information System (INIS)

    In the characterisation of complex environmental materials such as atmospheric particulate matter, analytical specificity is required to account for the many dimensions of information present in the sample. These dimensions include size, morphology, elemental composition, inorganic and organic chemical speciation, all to be performed on either single particles or on the population (or bulk sample) basis. Various techniques were developed for such measurements, including a number of bulk analysis procedures, methodologies for microscopical analysis of individual particles, and a variety of procedures for organic/inorganic chemical speciation. (author)

  13. Chemical studies on the synthesis and characterization of some ion- exchange materials and its use in the treatment of hazardous wastes

    International Nuclear Information System (INIS)

    Now inorganic ion exchange materials play an important role in analytical chemistry, based originally on their thermal and radiation resistance as well as their stability to chemical attack.Vanadate salts are one of the main categories of inorganic ion exchange materials widely used in separation and preconcentration of some toxic and hazardous elements from different waste media. Attempts in this study are focused on the preparation of two inorganic ion exchange materials ,Tin Vanadate (SnV) and Titanium Potassium Vanadate(TiKV) for treatment of hazardous waste.These material were characterized using X-ray spectra (XRD and XRF), IR, TGA-DTA and total elemental analysis studies. On the basis of distribution studies, the materials have been found that they are highly selective for Pb(II) and Cs(I)ions. Thermodynamic parameters (i.e. ΔG, ΔS and ΔH) have also been calculated for the adsorption of Pb2+, Cs+, Fe3+, Cd2+, Cu+2, Zn2+and Co2+ ions on Tin Vanadate (SnV) and Titanium Potassium Vanadate(TiKV) showing that the overall adsorption process is spontaneous and endothermic. The mechanism of diffusion of Fe3+, Co2+, Cu2+, Zn2+, Cd2+, Cs+and Pb2+ ions for Tin Vanadate (SnV) and Titanium Potassium Vanadate(TiKV) as cation exchangers were studied as a function of particle size, concentration of the exchanging ions, reaction temperatures and drying temperatures. The exchange rate was controlled by a particle diffusion mechanism as a limited batch technique and is confirmed from straight lines of B versus 1/r2 plots. The values of diffusion coefficients, activation energies and entropies of activation were calculated and their significance was discussed. The data obtained have been compared with that reported for other inorganic exchangers. Exchange isotherms for Cs+ ,Co2+and Cd2+ions were determined at 25, 45 and 65±1 degree C. These isotherms showed that Cs+ ,Co2+and Cd2+ are physically adsorbed. Finally, separations of the above mentioned cations on Tin Vanadate

  14. Chemical Characterization of Asturian Cider

    OpenAIRE

    Picinelli, A.M. (Anna); Suárez, Belén; Moreno, Javier; Rodríguez, Roberto; Caso-García, L.M. (Lourdes); Mangas, J.J. (Juan)

    2011-01-01

    Ninety-four samples of Asturian natural cider were analyzed for titratable and volatile acidities, pH, alcoholic, total polyphenol, and acidic polysaccharide contents, nonvolatile acids, polyalcohols, residual sugars, and major volatile compounds. A partial least-squares regression analysis (PLR-1) was performed to correlate the chemical composition and the origin of the raw material, the cider samples being grouped into two categories: an “odd” class, cider made from foreign appl...

  15. Synthesis and Characterization of Gold Nanoparticles

    OpenAIRE

    Hedkvist, Olof

    2013-01-01

    This thesis is focused on the synthesis of three different shapes of gold nanoparticles; the gold nanosphere, the gold nanorod and the gold nanocube. These will be synthesized using wet chemistry methods and characterized using UV-Vis- NIR spectroscopy and dynamic light scattering. The results will be used to draw some conclusions as to what factors influence the growth of gold nanoparticles.

  16. Chemical Characterization of Marajoara Pottery

    International Nuclear Information System (INIS)

    The aim of this project was to find a fingerprinting of the archaeological Marajoara pottery. For that, 330 archaeological and 36 contemporary samples were analysed using two techniques: INAA for elemental chemical analysis and ESR (Electron spin resonance) to determine the burning temperature. The results were studied by means of principal component and discriminant analysis using the SEARCH Programme from H. Mommsen from University of Bonn, Germany, showed the existence of two groups for the archaeological samples indicating that different raw material was used in the manufacturing of the prehistoric artifacts. Meanwhile, the clay used in the contemporary Marajoara ceramics is very different from the clay used in the archaeological. The temper effect in the concentration data was studied by means of correlation coefficient and showed that the tempering problem does not exist in the ceramics. The Procrustes analysis showed that the reduction of variable is viable and the chemical elements Eu, K, Yb, Cr, Fe and Th are sufficient in order to do the fingerprinting of the Marajoara pottery. The ESR studies showed that there is no difference in the burning temperature between the Marajoara's ceramics (the archaeological and contemporary ones). This Project was made in collaboration with the Museu de Arquelogia e Etnologia da Universidade de Sao Paulo, Sao Paulo, Brazil and University of Bonn, Germany by means a fellowship of IAEA in the training on the use of the SEARCH Programme. (author)

  17. The use of chemically stabilised proteolytic enzymes in peptide synthesis

    OpenAIRE

    Colleary, Sandra

    2003-01-01

    The aim of this project was to study various serine proteases, both native and chemically modified, with a view to their application in peptide synthesis. Various chemical modifications of these were carried out to improve their stability before peptide synthesis. Porcine trypsin was stabilised by reaction with ethylene glycol bis-(succinic acid Nhydroxy-succinimide ester) (EG). The enhanced stability is likely due to intramolecular crosslink(s) being formed in the enzyme. EG-tiypsin reta...

  18. Boron carbide nanowires: Synthesis and characterization

    Science.gov (United States)

    Guan, Zhe

    Bulk boron carbide has been widely used in ballistic armored vest and the property characterization has been heavily focused on mechanical properties. Even though boron carbides have also been projected as a promising class of high temperature thermoelectric materials for energy harvesting, the research has been limited in this field. Since the thermal conductivity of bulk boron carbide is still relatively high, there is a great opportunity to take advantage of the nano effect to further reduce it for better thermoelectric performance. This dissertation work aims to explore whether improved thermoelectric performance can be found in boron carbide nanowires compared with their bulk counterparts. This dissertation work consists of four main parts. (1) Synthesis of boron carbide nanowires. Boron carbide nanowires were synthesized by co-pyrolysis of diborane and methane at low temperatures (with 879 °C as the lowest) in a home-built low pressure chemical vapor deposition (LPCVD) system. The CVD-based method is energy efficient and cost effective. The as-synthesized nanowires were characterized by electron microscopy extensively. The transmission electron microscopy (TEM) results show the nanowires are single crystalline with planar defects. Depending on the geometrical relationship between the preferred growth direction of the nanowire and the orientation of the defects, the as-synthesized nanowires could be further divided into two categories: transverse fault (TF) nanowires grow normal to the defect plane, while axial fault (AF) ones grow within the defect plane. (2) Understanding the growth mechanism of as-synthesized boron carbide nanowires. The growth mechanism can be generally considered as the famous vapor-liquid-solid (VLS) mechanism. TF and AF nanowires were found to be guided by Ni-B catalysts of two phases. A TF nanowire is lead by a hexagonal phase catalyst, which was proved to be in a liquid state during reaction. While an AF nanowires is catalyzed by a

  19. Chemical characterization of CVD tungsten

    International Nuclear Information System (INIS)

    Characterization of tungsten films that have been deposited under ''selective'' conditions is presented. SEM and TEM studies indicate good conformal coverage and minimum encroachment. Cross section TEM results may indicate that some ''damage'' occurs at hole corners. Auger and SIMS depth profiles reveal very clean films. SIMS however does reveal that fluorine is a contaminant. Tungsten films were deposited at about 30A/min at 3000C with a 30/1 H/sub 2//WF/sub 6/ flow ration at 0.3 Torr. These films were selective up to film thicknesses of about 2000A. Mass spectral analysis of 99.8% WF/sub 6/ indicated no oxyfluorides and only a trace of methyl fluorosilanes that may have been an artifact of the gas sampling technique via contamination with silicone grease or lubricant. The sheet resistance of films became constant at about 8μ Ω-cm for film thicknesses (measured by profilometer after tungsten etch) greater than 4000A and increased up to about 20μ Ω-cm for very thin films (less than 500A). Auger depth profiling indicated that a thin oxide layer at the tungsten silicon interface corresponded to films having good adhesion as determined by a scribed tape pull test; where as a film deposited on a freshly HF cleaned surface with high carbon level had poor adhesion. Auger analysis indicated clean tungsten films with no evidence of fluorine. However, SIMS analysis indicated measurable levels of fluorine throughout the tungsten film and fluorine may be a significant contaminant as at higher temperatures it was found to have migrated to all interface areas as shown in SIMS study of annealed and unannealed W Six. The importance of fluorine impurities has not been correlated with any electrical properties

  20. Chemical characterization of marajoara ceramics

    International Nuclear Information System (INIS)

    In this study the elemental concentration of Ce, Co, Cr, Cs, Eu, Fe, Hf, K, La, Lu, Na, Nd, Rb, Sc, Sm, Ta, Tb, Th, U, Yb and Zn were determined by instrumental neutron activation analysis (INAA) in 204 fragments of Marajoara archaeological ceramics, of which 156 were provided by the Archaeology and Ethnology Museum of Sao Paulo University (MAE) and 48 were provided by Dr. Denise Pahl Schaan, Marajo Museum curator. Also, 9 contemporary ceramics produced and marketed at Marajo Island were analyzed. Electron paramagnetic resonance (EPR) analyses were performed in 8 archaeological samples and 1 contemporary sample in order to identify the burning temperature of the samples. X-ray diffraction (XRD) analyses were performed in 13 archaeological samples and 2 contemporary samples for the investigation of their mineralogical composition. Mahalanobis distance was used for the study of outlier while modified filter was used for the study of the temper added to the ceramic paste. Result interpretation was performed using cluster analysis, principal components analysis and discriminant analysis. Procrustes analysis was used for variable selection and it showed that the Ce, Fe, Eu, Hf, K and Th variables are adequate for the characterization of the analyzed samples. The comparative study among the archaeological and contemporary ceramics showed the arrangement of two well-defined and close groups for the archaeological samples and a third, distant group for the contemporary ones. This result indicates that the archaeological and contemporary ceramics differ in their composition. EPR and XRD analysis were inconclusive for the differentiation of archaeological and contemporary ceramics. (author)

  1. 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.

  2. Synthesis and characterization of silicon carbonitride films by plasma enhanced chemical vapor deposition (PECVD) using bis(dimethylamino)dimethylsilane (BDMADMS), as membrane for a small molecule gas separation

    Science.gov (United States)

    Kafrouni, W.; Rouessac, V.; Julbe, A.; Durand, J.

    2010-12-01

    Silicon carbonitride thin films have been deposited by plasma enhanced chemical vapor deposition (PECVD) from bis(dimethylamino)dimethylsilane (BDMADMS) as a function of X = (BDMADMS/(BDMADMS + NH 3)) between 0.1 and 1, and plasma power P (W) between 100 and 400 W. The microstructure of obtained materials has been studied by SEM, FTIR, EDS, ellipsometrie, and contact angle of water measurements. The structure of the materials is strongly depended on plasma parameters; we can pass from a material rich in carbon to a material rich in nitrogen. Single gas permeation tests have been carried out and we have obtained a helium permeance of about 10 -7 mol m -2 s -1 Pa -1 and ideal selectivity of helium over nitrogen of about 20.

  3. Synthesis, structural characterization and optical properties of multilayered Yttria-stabilized ZrO2 thin films obtained by aerosol assisted chemical vapour deposition

    International Nuclear Information System (INIS)

    Multilayered Yttria-stabilized zirconium (YSZ) oxide thin films were synthesized by aerosol assisted chemical vapour deposition onto borosilicate glass substrate. The film consisted of a periodic stack of several YSZ layer pairs. Each pair was composed of layers, a few nanometers thick, of the same composition but different density. Optically the multilayered microstructure correspond to alternating layers of high (dense layer) and low (porous layer) refraction index. The microstructure was analysed by electron and atomic force microscopy. Optical properties were evaluated by reflectance spectroscopy, and associated with the cross sectional microstructure of the films. The measured effective refractive index of the films deviates from bulk value. The discrepancy can be explained by the multilayered structure of the film

  4. Synthesis and Characterization of Manganese Carboxylates

    OpenAIRE

    Maryudi; R.M. Yunus; A.H. Nour; M.H. Abidin

    2009-01-01

    The explorations of prodegradant additives for plastics from trans-metals organic salts have been being conducted. This study reports a method of synthesis of manganese carboxylates and their characterization. The new method involves reaction between molten carboxylic acid with sodium hydroxide in alcoholic solution to produce sodium carboxylate and continued by reacting sodium carboxylate with chloride salt of manganese. First reaction and second reaction were conducted at 80-85°C and under ...

  5. The Novel Ketoprofenamides: Synthesis and Spectroscopic Characterization

    OpenAIRE

    ZOVKO, MARIJANA; ZORC, BRANKA; Jadrijević-Mladar Takač, Milena; Metelko, Biserka; Novak, Predrag

    2003-01-01

    Synthesis of a series of new ketoprofenamides (3a-h) is described. Amide formation was achieved by aminolysis of ketoprofen benzotriazolide (2) with various amines: primary, secondary, hydroxylamine and amino acid β-alanine. The structures of synthesized compounds were characterized by means of IR, 1H and 13C NMR spectroscopies and elemental analysis. The synthesized compounds are potential prodrugs of a well-known NSAID ketoprofen.

  6. Chemical synthesis and characterization of hydroxyapatite (HAp)-poly (ethylene co vinyl alcohol) (EVA) nanocomposite using a phosphonic acid coupling agent for orthopedic applications

    Energy Technology Data Exchange (ETDEWEB)

    Pramanik, Nabakumar; Mohapatra, Sasmita [Department of Chemistry, Indian Institute of Technology Kharagpur, Kharagpur - 721302, West Bengal (India); Bhargava, Parag [Metallurgical Engineering and Materials Science, Indian Institute of Technology Bombay, Mumbai-400076 (India); Pramanik, Panchanan [Department of Chemistry, Indian Institute of Technology Kharagpur, Kharagpur - 721302, West Bengal (India)], E-mail: pramanik@chem.iitkgp.ernet.in

    2009-01-01

    A novel bio-analogue hydroxyapatite (HAp)-poly (ethylene co vinyl alcohol) (EVA) nanocomposite has been synthesized by a solution-based chemical methodology with varying HAp contents from 10 to 60% (w/w). The surface of HAp particles has been modified with 2-carboxyethylphosphonic acid in order to enhance the interfacial bonding interaction between HAp and EVA, and hence to improve the mechanical properties of the composite. The interfacial modification has been investigated through Fourier transform infrared absorption spectra (FTIR), X-ray diffraction (XRD) and thermal analyses. 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 use of phosphonic acid coupling agent promotes the uniform dispersion of HAp particles in the polymer matrix with strong particle-polymer interfacial bonding, which leads to a significant improvement in mechanical properties of the composite. The cell viability test indicates that the HAp-EVA nanocomposite is cytocompatible. The developed HAp-EVA nanocomposite may be potentially used as bone substitutes.

  7. Chemical synthesis and characterization of hydroxyapatite (HAp)-poly (ethylene co vinyl alcohol) (EVA) nanocomposite using a phosphonic acid coupling agent for orthopedic applications

    International Nuclear Information System (INIS)

    A novel bio-analogue hydroxyapatite (HAp)-poly (ethylene co vinyl alcohol) (EVA) nanocomposite has been synthesized by a solution-based chemical methodology with varying HAp contents from 10 to 60% (w/w). The surface of HAp particles has been modified with 2-carboxyethylphosphonic acid in order to enhance the interfacial bonding interaction between HAp and EVA, and hence to improve the mechanical properties of the composite. The interfacial modification has been investigated through Fourier transform infrared absorption spectra (FTIR), X-ray diffraction (XRD) and thermal analyses. 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 use of phosphonic acid coupling agent promotes the uniform dispersion of HAp particles in the polymer matrix with strong particle-polymer interfacial bonding, which leads to a significant improvement in mechanical properties of the composite. The cell viability test indicates that the HAp-EVA nanocomposite is cytocompatible. The developed HAp-EVA nanocomposite may be potentially used as bone substitutes

  8. 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.

  9. One pot synthesis of Curcumin-NSAIDs prodrug, spectroscopic characterization, conformational analysis, chemical reactivity, intramolecular interactions and first order hyperpolarizability by DFT method

    Science.gov (United States)

    Srivastava, Sangeeta; Gupta, Preeti; Sethi, Arun; Singh, Ranvijay Pratap

    2016-08-01

    A novel Curcumin-NSAIDs prodrug 4-((1E, 3Z, 6E)-3-hydroxy-(4-hydroxy-3-methoxyphenyl)-5-oxohepta-1,3,3-trienyl)-2-methoxyphenyl-2-(4-isobutylphenyl) propanoate (2) derivative was synthesized by Steglich esterification in high yield and characterized with the help of 1H, 13C NMR, 1H-1H COSY, UV, FT-IR spectroscopy and mass spectrometry. The molecular geometry of synthesized compound was calculated in ground state by Density functional theory (DFT/B3LYP) using two different basis set 6-31G (d, p) and 6-311G (d, p). Conformational analysis of 2 was carried out to determine the most stable conformation. Stability of the molecule as a result of hyperconjugative interactions and electron delocalization were analysed using Natural bond orbital (NBO) analysis. Intramolecular interactions were analysed by AIM (Atom in molecule) approach. Global and local reactivity descriptors were calculated to study the reactive site within molecule. The electronic properties such as HOMO and LUMO energies were calculated using time dependent Density Functional Theory (TD-DFT). The vibrational wavenumbers were calculated using DFT method and assigned with the help of potential energy distribution (PED). First hyperpolarizability value has been calculated to describe the nonlinear optical (NLO) property of the synthesized compound. Molecular electrostatic potential (MEP) for synthesized compounds have also been determined to check their electrophilic or nucleophilic reactivity.

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

    International Nuclear Information System (INIS)

    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 13C 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 (Hg2+, Cd2+, Pb2+, Cu2+, Zn2+, K+, Na+ and Li+) 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)

  11. 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)

  12. 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.

  13. Synthesis, spectroscopic characterizations and quantum chemical computational studies of (Z)-4-[(E)-(4-fluorophenyl)diazenyl]-6-[(3-hydroxypropylamino)methylene]-2-methoxycyclohexa-2,4-dienone.

    Science.gov (United States)

    Albayrak, Ciğdem; Odabaşoğlu, Mustafa; Ozek, Arzu; Büyükgüngör, Orhan

    2012-01-01

    In this study, the molecular structure and spectroscopic properties of the title compound were characterized by X-ray diffraction, FT-IR and UV-vis spectroscopies. These properties were also investigated using DFT method. The most convenient conformation of title compound was firstly determined. The geometry optimizations in gas phase and solvent media were performed by DFT methods with B3LYP adding 6-31G(d) basis set. The differences between crystal and computational structures are due to crystal packing in which hydrogen bonds play an important role. UV-vis spectra were recorded in different organic solvents. The results show that title compound exists in both keto and enol forms in DMSO, EtOH but it tends to shift towards enol form in benzene. The polar solvents facilitate the proton transfer by decreasing the activation energy needed for Transition State. The formation of both keto and enol forms in DMSO and EtOH is due to decrease in the activation energy. TD-DFT calculations starting from optimized geometry were carried out in both gas and solution phases to calculate excitation energies of the title compound. The non-linear optical properties were computed at the theory level and the title compound showed a good second order non-linear optical property. In addition, thermodynamic properties were obtained in the range of 100-500K. PMID:22001007

  14. Synthesis and characterization of novel cardanol based benzoxazines.

    Science.gov (United States)

    Minigher, Andrea; Benedetti, Elena; De Giacomo, Ornela; Campaner, Pietro; Aroulmoji, Vincent

    2009-04-01

    Benzoxazines are a class of phenolic compounds extensively studied in polymer science because of their properties as fiber reinforcements, fire-retardants and curing agents. In this article is described a solvent-less process, based on a Mannich reaction involving a primary amine and an aldehyde, for the preparation of new benzoxazines deriving from cardanol (a well known phenol obtained as a renewable organic resource and harmful by-product of the cashew industry). Particular attention is given to the synthesis and chemical characterization (both by 1H NMR spectroscopy and HPLC), while the thermal polymerization process has been monitored by differential scanning calorimetry. PMID:19475998

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

    International Nuclear Information System (INIS)

    Bismuth Telluride (Bi2Te3) 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

  16. 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

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

    OpenAIRE

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

    2015-01-01

    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,...

  18. Electrochemical synthesis and characterization of hydroxyapatite powders

    International Nuclear Information System (INIS)

    Electrochemical synthesis of hydroxyapatite powders was performed galvanostatically from homogeneous solution of Na2H2EDTA.2H2O, NaH2PO4 and CaCl2 at a concentration relationship Ca/EDTA/PO43- of 0.25/0.25/0.15 M at current densities of 137 and 207 mA cm-2 and pH values of 9.0 and 12.0. The hydroxyapatite powders were characterized by X-ray diffraction, size distribution measurements, transmission electron microscopy, scanning electron microscopy and thermogravimetric and differential thermal analysis. The influence of the electrochemical synthesis parameters, e.g. applied current density and pH value, on the phase composition, crystallite size, morphology and thermal characteristics of hydroxyapatite powders were investigated

  19. Synthesis and characterization of new ionic liquids

    International Nuclear Information System (INIS)

    In recent years, ionic liquids have been highlighted for its potential in various industrial applications. Among them, the salts of Broensted has a promising profile for the low toxicity, low cost and simple synthesis. This paper presents the synthesis and characterization of new salts of Bronsted with branched (lactate) or large chain anions (oleate) for future use as additives promoters of proton conductivity in fuel cells of ethanol. Experimental data were measured for density, sound velocity and conductivity of pure ionic liquids and mixtures. The density decreases linearly with increasing temperature, and sound velocity shows a similar trend, but not linear. The conductivity increases according to the Arrhenius model with activation energy less than 10 J/mol. Tests NMR, FTIR and TGA confirm ionic structure and thermal stability up to 165 deg C. (author)

  20. 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.

  1. SYNTHESIS AND CHARACTERIZATION OF NEW HALOGENATED CURCUMINOIDS

    Directory of Open Access Journals (Sweden)

    Eugenio Torres

    2013-12-01

    Full Text Available In this work a novel procedure of synthesis of compounds analogues to curcumin with halogens atoms in its structure is described, which can increase its solubility and biological activity. Four halogenated curcuminoids were obtained with great pharmacological interest, none of them reported in literature before. Synthesis was carried out by means of the aldol condensation assisted by microwaves of halogenated aromatic aldehydes and acetylacetona, using morpholine as basic catalyst, in absence of solvent, and the reaction just needed 1 min. The products were purified by treatment of the reaction mixture with methanol under ultrasound irradiation, followed by chromatographic column. All obtained compounds were characterized by infrared spectroscopy, nuclear magnetic resonance, quantitative elementary analysis and high resolution mass spectrometry. The RMN-1H data demonstrate in all structures of synthesized curcuminoids the enol form is the most favored.

  2. Synthesis and characterization of iodinated polyurethane with inherent radiopacity.

    Science.gov (United States)

    Kiran, S; James, Nirmala R; Joseph, Roy; Jayakrishnan, A

    2009-10-01

    The synthesis and characterization of polyurethane (PU) with excellent radiopacity for medical and allied applications are reported. Bisphenol-A (BPA) was iodinated to obtain 4,4'-isopropylidinedi-(2,6-diiodophenol) (IBPA) which was used as a chain extender for the preparation of a radiopaque PU. The PU was prepared by reacting 4,4'-methylenebis(phenyl isocyanate) (MDI), poly(tetramethylene glycol) (PTMG) and IBPA in 2.2:1.2:1 molecular ratio and is characterized by infrared spectroscopy (IR), thermogravimetry (TGA), dynamic mechanical analysis (DMA), energy dispersive X-ray analysis (EDX), gel permeation chromatography (GPC) and X-radiography. X-ray images showed that the PU prepared using IBPA as the chain extender is highly radiopaque. An in vitro cytotoxicity test using L929 mouse fibroblast cells shows that the PU is non-cytotoxic. The outlined synthesis of a PU with radiocontrast properties opens up the possibility of synthesizing many different kinds of radiopaque PUs with desirable range of physical properties exploiting the versatility in their chemical synthesis. PMID:19596151

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

    Energy Technology Data Exchange (ETDEWEB)

    Chen, W.

    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.

  4. Synthesis, characterization and application of electrode materials

    Energy Technology Data Exchange (ETDEWEB)

    He, L.

    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-Ti{sub 4}O{sub 7} and Pt-Ti{sub 4}O{sub 7} 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 Ti{sub 4}O{sub 7} ceramic 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 Bi{sub 2}Ru{sub 2}O{sub 7.3} and Bi{sub 2}Ir{sub 2}O{sub 7} electrodes are described in paper 2 and paper 3, respectively. Details are reported for the synthesis and characterization of composite Bi{sub 2}Ru{sub 2}O{sub 7.3} 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 H{sub 2}O with simultaneous evolution of O{sub 2}. Paper 3 includes electrocatalytic activities of composite Bi{sub 2}Ir{sub 2}O{sub 7} disk electrodes for the oxidation of I{sup -} and the reduction of IO{sub 3}{sup -}.

  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. Synthesis and characterization of acidic mesoporous borosilicate thin films.

    Science.gov (United States)

    Xiu, Tongping; Liu, Qian; Wang, Jiacheng

    2009-02-01

    Work on the synthesis and characterization of acidic wormhole-like ordered mesoporous borosilicate thin films (MBSTFs) on silicon wafers is described in this paper. The MBSTFs coated by the dip-coating method were prepared through an evaporation-induced self-assembly (EISA) process using nonionic block copolymers as structure-directing agents. Fourier transform infrared (FT-IR) spectroscopy confirmed the formation of borosiloxane bonds (Si-O-B). High-resolution transmission electron microscopy (HRTEM) and N2 sorption evidenced a wormhole-like mesoporous structure in the MBSTFs obtained. Scanning electron microscopy (SEM) images of the cross sections and surfaces of the samples showed that MBSTFs on silicon wafers were continuous, homogeneous and did not crack. The acidic properties of the MBSTFs were characterized by FT-IR spectra of chemisorbed pyridine. The MBSTFs thus prepared may find their future applications in many fields including chemical sensors, catalysis, optical coating, molecule separation, etc. PMID:19441565

  7. 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

  8. Routes to deagglomerated nanopowder by chemical synthesis

    OpenAIRE

    Burgard, Detlef; Kropf, Christian; Nass, Rüdiger; Schmidt, Helmut K.

    1994-01-01

    The concept of tailored interfaces has been applied to the synthesis of nano-scaled Y2O3/ZrO2 powders. The microemulsion technique as well as the thermodynamically controlled growth reaction have been utilized for this purpose. Both methods yielded agglomerate free amorphous powders with particles sized of 8 nm and 15 nm, respectively. Cubic zirconia was obtained by calcination between 300 and 400°C and crystallite coarsening was not observed. The calcined powders could be redispersed by trea...

  9. Synthesis of fine chemical over zeolites

    Czech Academy of Sciences Publication Activity Database

    Voláková, Martina; Čejka, Jiří

    Kerala : Transworld Research Network, 2008 - (Čejka, J.; Peréz-Pariente, J.; Roth, W.), s. 263-297 ISBN 978-81-7895-330-4 R&D Projects: GA ČR GA104/05/0192; GA ČR GA203/05/0197; GA ČR GA104/07/0383; GA AV ČR 1QS400400560; GA AV ČR 1ET400400413 Institutional research plan: CEZ:AV0Z40400503 Keywords : zeolites * synthesis * molecular sieves Subject RIV: CF - Physical ; Theoretical Chemistry

  10. Advances in chemical synthesis and application of metal-metalloid amorphous alloy nanoparticulate catalysts

    Institute of Scientific and Technical Information of China (English)

    WU Zhijie; LI Wei; ZHANG Minghui; TAO Keyi

    2007-01-01

    This paper reviews the advances in the chemical synthesis and application of metal-metalloid amorphous alloy nanoparticles consisting of transition metal (M) and metalloid elements (B,P).After a brief introduction on the history of amorphous alloy catalysts,the paper focuses on the properties and characterization of amorphous alloy catalysts,and recent developments in the solution-phase synthesis of amorphous alloy nanoparticles.This paper further outlines the applications of amorphous alloys,with special emphasis on the problems and strategies for the application of amorphous alloy nanoparticles in catalytic reactions.

  11. Synthesis and characterization of hydrocarbon sphere

    International Nuclear Information System (INIS)

    With glucose as starting material, hydrocarbon sphere which was rich in oxygen containing functional groups was synthesized by hydrothermal carbonization process, and characterized by SEM and FTIR techniques. The results show that the size and dispersion of carbon spheres depend on many factors, including the concentration of glucose, the reaction temperature and the adulterated organic monomer. The obtained hydrocarbon spheres contain rich functional groups which can greatly improve the hydrophilicity and chemical reactivity. (authors)

  12. Indium Antimonide Nanowires: Synthesis, Characterization, and Applications

    OpenAIRE

    Penchev, Miroslav Valentinov

    2012-01-01

    Indium Antimonide (InSb) nanowires with a diameter ranging from 30 nm to 200 nm, were synthesized by electrochemical disposition in anodized alumina and polycarbonate porous membranes. In addition, epitaxial single crystalline InSb nanowires with diameters ranging from 5 nm to 100 nm, were synthesized by chemical vapor deposition (CVD) using Au nanoparticles as catalyst. Structural and material characterization of InSb nanowires was carried out by scanning electron microscopy (SEM), energy di...

  13. SYNTHESIS AND CHARACTERIZATION OF COPPER CARBONATE NANOPARTICLES

    OpenAIRE

    R.Hepzi Pramila Devamani; Sabeena, M.

    2014-01-01

    Copper carbonate nanoparticles were synthesized via chemical co-precipitation method from copper sulphate and sodium carbonate. The formed nanoparticle is characterized by powder x-ray diffraction, scanning electron microscopy, ultra-violet spectroscopy and fourier transform infrared spectroscopy, confirmed the preferential growth of copper carbonate nanoparticles that width is 90.55nm. The SEM image shows the synthesized copper carbonate show well crystallized particles with ...

  14. Ion-exchange membranes in chemical synthesis – a review

    Directory of Open Access Journals (Sweden)

    Jaroszek Hanna

    2016-12-01

    Full Text Available The applicability of ion-exchange membranes (IEMs in chemical synthesis was discussed based on the existing literature. At first, a brief description of properties and structures of commercially available ion-exchange membranes was provided. Then, the IEM-based synthesis methods reported in the literature were summarized, and areas of their application were discussed. The methods in question, namely: membrane electrolysis, electro-electrodialysis, electrodialysis metathesis, ion-substitution electrodialysis and electrodialysis with bipolar membrane, were found to be applicable for a number of organic and inorganic syntheses and acid/base production or recovery processes, which can be conducted in aqueous and non-aqueous solvents. The number and the quality of the scientific reports found indicate a great potential for IEMs in chemical synthesis.

  15. Nanograined WC-Co Composite Powders by Chemical Vapor Synthesis

    Science.gov (United States)

    Ryu, Taegong; Sohn, H. Y.; Han, Gilsoo; Kim, Young-Ugk; Hwang, Kyu Sup; Mena, M.; Fang, Zhigang Z.

    2008-02-01

    Nanograined tungsten carbide (WC) Co composite powders were prepared by a chemical vapor synthesis (CVS) process that has previously been used for preparing the aluminides of titanium and nickel and other metallic and intermetallic powders at the University of Utah. To determine the optimum condition for producing nanograined WC-Co composite powders, the effects of carburization temperature, CH4 to WCl6 ratio, CH4 to H2 ratio, CoCl2 contents, and residence time of WC on the powder composition and particle size were investigated. The reduction and carburization of the vaporized chlorides by CH4-H2 mixtures produced nanograined WC and Co composite powder, which sometimes contained small levels of W2C, W, or the η (Co3W3C) phase. The presence of these incompletely carburized phases can be tolerated because they can be fully carburized during the subsequent sintering process. These phases can also be fully carburized by a separate post-treatment. The products were characterized by using X-ray diffraction (XRD) and a transmission electron microscope (TEM). As a result, nanograined WC-Co composite with the particle size less than 30 nm was obtained.

  16. Chemical synthesis and immunosuppressive activity of dipalmitoyl phosphatidylinositol hexamannoside.

    Science.gov (United States)

    Ainge, Gary D; Compton, Benjamin J; Hayman, Colin M; Martin, William John; Toms, Steven M; Larsen, David S; Harper, Jacquie L; Painter, Gavin F

    2011-06-17

    Phosphatidylinositol mannosides (PIMs) isolated from mycobacteria have been identified as an important class of phosphoglycolipids with significant immune-modulating properties. We present here the synthesis of dipalmitoyl phosphatidylinositol hexamannoside (PIM(6)) 1 and the first reported functional biology of a synthetic PIM(6). Key steps in the synthetic protocol included the selective glycosylation of an inositol 2,6-diol with a suitably protected mannosyl donor and construction of the glycan core utilizing a [3 + 4] thio-glycosylation strategy. The target 1 was purified by reverse phase chromatography and characterized by standard spectroscopic methods, HPLC, and chemical modification by deacylation to dPIM(6). The (1)H NMR spectrum of synthetic dPIM(6) obtained from 1 matched that of dPIM(6) obtained from nature. PIM(6) (1) exhibited dendritic cell-dependent suppression of CD8(+) T cell expansion in a human mixed lymphocyte reaction consistent with the well established immunosuppressive activity of whole mycobacteria. PMID:21574597

  17. 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.

  18. DNA and RNA induced enantioselectivity in chemical synthesis

    NARCIS (Netherlands)

    Roelfes, Gerard

    2007-01-01

    One of the hallmarks of DNA and RNA structures is their elegant chirality. Using these chiral structures to induce enantioselectivity in chemical synthesis is as enticing as it is challenging. In recent years, three general approaches have been developed to achieve this, including chirality transfer

  19. 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...

  20. 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

  1. 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.

  2. Green synthesis and characterization of graphene nanosheets

    International Nuclear Information System (INIS)

    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

  3. 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.

  4. SYNTHESIS AND CHARACTERIZATION OF NEW CHITOSAN-O-ETHYL PHOSPHONATE

    Directory of Open Access Journals (Sweden)

    GLORIA PALMA

    2005-12-01

    Full Text Available The chitin is a natural polymer that is extracted commercially from the shells of crustaceans generated as raw material from the fishing industry. Their chemical structure is constituted by residual units of N-acetyl glucosamine linked by b (1 ® 4 and its derivatives can be obtained from alkaline chitosan. The chitin, chitosan and their derivatives present very good perspectives to be used in agriculture. These derivatives are biodegradable and they exhibit fungicides, germicides, nemacides properties and natural defensive mechanisms of the plants. The chlorophosphonic-2-acid (Ethephon® is a commercial product employed for the early maturation of fruits. The objective of the present work is the synthesis and characterization of chitosan-O-ethyl phosphonate chitosan to obtain a controlled released system with potential plant growth regulation properties. Alkaline chitosan was obtained; and then reacted with the 2-chlorophosphonic acid. The synthesis of new chitosan derivatives and its complete characterization by FT-IR, 13C, ¹H and 31P NMR is described and gas chromatographic, the effects on field blueberries are also tested. A chitosan 99 % deacetylated and Mv = 89,000 g/mol is prepared. The O-(ethyl phosphonic chitosan (QOEP with a degree of substitution of 58% is obtained

  5. Chemically stabilized subtilisins in peptide synthesis

    OpenAIRE

    Colleary, Sandra; Ó'Fágáin, Ciarán

    2008-01-01

    We have stabilized alcalaseTM and subtilisin Carlsberg (SC) against heat by chemical modification with ethylene glycol bis-succinimidyl succinate (EGNHS), a procedure not previously reported for subtilisins. The increases in thermal stability at 65oC were 1.8-fold and 4.7-fold respectively. Caseinolytic activity of alcalase in aqueous buffer was unchanged following modification but apparent Km of SC decreased 2.5-fold. Native and modified forms of both enzymes synthesized the tripeptide Z-...

  6. Synthesis and characterization of an additive type super plasticizers obtained from plastics cups of polystyrene

    International Nuclear Information System (INIS)

    This paper aims to describe the synthesis of an additive type superplasticizer from alternative material - plastic cups used of polystyrene - and characterize it physically and chemically in order to verify their efficiency and compare it with a commercial use superplasticizer. Following the search, the synthesized superplasticizer is used in mortars to assess their efficiency

  7. The total chemical synthesis of polymer/graphene nanocomposite films.

    Science.gov (United States)

    Salvatierra, Rodrigo V; Cava, Carlos E; Roman, Lucimara S; Oliveira, Marcela M; Zarbin, Aldo J G

    2016-01-28

    A versatile and room temperature synthesis of thin films of polymer/graphene is reported. Drastically differing from other methods, not only the polymer but also the graphene are completely built from their simplest monomers (thiophene and benzene) in a one-pot polymerization reaction at a liquid-liquid interface. The materials were characterized and electronic properties are presented. PMID:26658554

  8. Brazilian oil spills chemical characterization : case studies

    International Nuclear Information System (INIS)

    The Petrobras Research Centre has been active in responding to some significant oil spills in Brazil in the past decade. The centre has characterized spilled oil, monitored the affected ecosystems and determined the fate of oil in the environment. This paper described the use of some advanced chemical analytical techniques used in Brazilian oil spill studies to determine fractions and individual petroleum hydrocarbons in water, groundwater, sediment, sand, fish and the spilled oil itself. Some of the most recent oil spill cases were discussed in terms of chemical characterization of the spilled oil and the environmental samples from different matrices of the affected ecosystems for determining the fate of the oil in the environment and to assess environmental damage. In particular, methods such as gas chromatography/flame ionization detector, P and T/GC/PID and gas chromatography/mass spectrometry have been used to examine crude and fuel oil spills in Guanabara Bay, Barigui and Iguassu Rivers, and the Sao Sebastiao Channel. The chemical analytical methods are used to determine total petroleum hydrocarbons, n-alkanes, isoprenoids, unresolved complex mixtures, volatile monoaromatic compounds such as BTEX (benzene, toluene, ethylbenzene and xylenes), as well as parent and alkylated homologues polycyclic aromatic hydrocarbons (PAH) and terpanes and steranes. Acute ecotoxicity data for water and sediment samples was also included. It was determined that with certain limitations, PAH ratios can help determine the origin of hydrocarbons as being either petrogenic or pyrolytic. However, alkylated PAH homologues and parent compounds such as dibenzothiophene and perylene give more precise interpretation of the data. 30 refs., 9 tabs., 11 figs

  9. 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

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

    International Nuclear Information System (INIS)

    Graphical abstract: NiWO4 nanoparticles were prepared via precipitation technique. Experimental parameters of procedure were optimized statistically. Highlights: ► NiWO4 spherical nanoparticles were synthesized via direct precipitation method. ► Taguchi robust design was used for optimization of synthesis reaction parameters. ► Composition and structural properties of NiWO4 nanoparticles were characterized. ► EDAX, XRD, SEM, FT-IR, UV–vis and photoluminescence techniques were employed. ► 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. 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.

  11. Synthesis and Characterization of Photoresponsive Azo Polyelectrolytes

    Institute of Scientific and Technical Information of China (English)

    WU Lifeng; PENG Huagen; WANG Xiaogong; LIU Deshan; ZHOU Qixiang

    2001-01-01

    Optical active azo polymers are very important functional materials because of their photoresponsive properties.This paper investigates three kinds of aromatic azo polyelectrolytes synthesized by chemical modification of poly(acryloyl chloride)which was prepared by free radical polymerization.Poly was esterified with three different kinds of aromatic azo compounds containing hydroxyl groups to give polymeric intermediates,which were used to prepare the azo polyelectrolytes by hydrolysis.The products were characterized by elementary analysis,IR,1H-NMR,and UV-Vis spectrography.

  12. SYNTHESIS AND CHARACTERIZATION OF COPPER CARBONATE NANOPARTICLES

    Directory of Open Access Journals (Sweden)

    R.Hepzi Pramila Devamani

    2014-04-01

    Full Text Available Copper carbonate nanoparticles were synthesized via chemical co-precipitation method from copper sulphate and sodium carbonate. The formed nanoparticle is characterized by powder x-ray diffraction, scanning electron microscopy, ultra-violet spectroscopy and fourier transform infrared spectroscopy, confirmed the preferential growth of copper carbonate nanoparticles that width is 90.55nm. The SEM image shows the synthesized copper carbonate show well crystallized particles with spherical morphology. The FTIR spectrum is used to study the stretching and bending frequencies of molecular functional groups in the sample. From UV spectrum, the band gap of copper carbonate nanoparticles is found to be 3.4eV.

  13. Electrochemical synthesis and characterization of copolyviologen films

    International Nuclear Information System (INIS)

    Two cyanopyridine-based monomers were synthesized and utilized for the cathodic electropolymerization of polyviologen (BPV) and copolyviologen (CoPV) films onto glassy carbon (GC) electrodes. One of the monomer material is branched (BCP) whereas the other one has a linear structure (LCP) the former bearing three the latter two polymerizable cyanopyridinium groups. The electrochemical synthesis of the polyviologen and copolyviologen films were made in aqueous solutions and the film properties were characterized by electrochemical and spectroscopic techniques. Atomic force microscopy was used in order to study the surface morphologies of the films. The BPV and CoPV films undergo a two-step reduction reaction and show redox properties typical for viologen derivatives in monomer free electrolyte solutions. In comparison to the polyviologen film, electrochemically synthesized from the branched monomer (BCP), the redox property of the copolymer was changed. The results from in situ UV–vis spectra show that the copolyviologen film has good stability and undergoes reversible electron transfer reactions successfully. The structure of the copolyviologen film was characterized by FTIR spectroscopy, confirming successful polymerization of both monomer materials. The copolymerization therefore opens up a direct electrochemical method to form viologen films with large cavities. This feature gives a potential to apply the partly conjugated copolyviologen film with redox properties as a conducting host material for immobilization of macromolecules

  14. Synthesis and characterization of functionalized magnetic nanoparticles

    Science.gov (United States)

    Biswal, Dipti; Peeples, Brianna N.; Spence, Destiny D.; Peeples, Caryn; Bell, Crystal N.; Pradhan, A. K.

    2012-04-01

    Magnetic nanoparticles have been used in a wide array of industrial and biomedical applications due to their unique properties at the nanoscale level. They are extensively used in magnetic resonance imaging (MRI), magnetic hyperthermia treatment, drug delivery, and in assays for biological separations. Furthermore, superparamagnetic nanoparticles are of large interest for in vivo applications. However, these unmodified nanoparticles aggregate and consequently lose their superparamagnetic behaviors, due to high surface to volume ratio and strong dipole to dipole interaction. For these reasons, surface coating is necessary for the enhancement and effectiveness of magnetic nanoparticles to be used in various applications. In addition to providing increased stability to the nanoparticles in different solvents or media, stabilizers such as surfactants, organic/inorganic molecules, polymer and co-polymers are employed as surface coatings, which yield magnetically responsive systems. In this work we present the synthesis and magnetic characterization of Fe3O4 nanoparticles coated with 3-aminopropyltriethoxy silane (APS) and citric acid. The particles magnetic hysteresis was measured by a superconducting quantum interference device (SQUID) magnetometer with an in-plane magnetic field. The uncoated and coated magnetic nanoparticles were characterized by using fourier transform infrared (FTIR), UV-vis, X-ray diffraction, transmission electron microscopy, and thermo-gravimetric analysis.

  15. Synthesis and characterization of the natural and burned hydrotalcite

    International Nuclear Information System (INIS)

    The synthesis and the structural and surface properties of the natural and burned hydrotalcite using salts of AlCl3 and MgCl2.6H2O its were studied. Its were used those analysis of BET, IR, XRD, TGA and SEM to characterize these materials. The obtained product was identified as the natural or carbonated hydrotalcite of chemical formula Mg6Al2(OH)16CO3.4H2O. The hydrotalcite was roasted at 500 C during 5 h and the was obtained roasted hydrotalcite (HTC) that is a material of high selectivity toward the anions that it can be efficiently used as adsorbent material in studies of adsorption for the treatment of anionic radioactive waste present in watery solution. (Author)

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

    Science.gov (United States)

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

    2013-01-01

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

  17. Microwave synthesis and spectroscopic characterization of manganese oxalate nanocrystals

    Institute of Scientific and Technical Information of China (English)

    S.Lakshmi Reddy; G.Udayabashkar Reddy; R.Ramasubba Reddy; G.Siva Reddy; Ray L.Frost; Tamio Endo

    2013-01-01

    The microwave synthesis of MnC2O4·2H2O nanoparticles was performed through the thermal double decomposition of oxalic acid dihydrate (C2H2O4·2H2O) and Mn(OAc)2·4H2O solutions using a CATA-2R microwave reactor.Structural characterization was performed using X-ray diffraction (XRD),particle size and shape were analyzed using transmission electron microscopy (TEM).The chemical in the structures was investigated using electron paramagnetic resonance (EPR) as well as optical absorption spectra and near-infrared (NIR) spectroscopies.The nanocrystals produced with this method were pure and had a distorted rhombic octahedral structure.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2002-07-01

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

  19. Synthesis, Characterization and Application Of PbS Quantum Dots

    International Nuclear Information System (INIS)

    Lead Chalcogenides (PbS, PbSe, PbTe) quantum dots (QDs) are ideal for fundamental studies of strongly quantum confined systems with possible technological applications. Tunable electronic transitions at near--infrared wavelengths can be obtained with these QDs. Applications of lead chalcogenides encompass quite a good number of important field viz. the fields of telecommunications, medical electronics, optoelectronics etc. Very recently, it has been proposed that 'memristor'(Memory resistor) can be realized in nanoscale systems with coupled ionic and electronic transports. The hystersis characteristics of 'memristor' are observed in many nanoscale electronic devices including semiconductor quantum dot devices. This paper reports synthesis of PbS QDs by chemical route. The fabricated samples are characterized by UV-Vis, XRD, SEM, TEM, EDS, etc. Observed characteristics confirm nano formation. I-V characteristics of the sample are studied for investigating their applications as 'memristor'.

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

    Directory of Open Access Journals (Sweden)

    Newton M. Barbosa Neto

    2011-07-01

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

  1. Synthesis and characterization of fluorine compounds

    International Nuclear Information System (INIS)

    The (18 F) D-glucose, 2-deoxy fluorine (18 FDG) is a radio pharmaceutic that is used in nuclear medicine it is utilized mainly in the glucose metabolism. It allows recently to observe the tumors accumulation and growing. The obtention of this radio pharmaceutic can realize by a nucleophilic or electrophilic process through the use of different fluorinated agents obtained as intermediates for introducing the 18 F radionuclide in a final step of synthesis. The first methods already has been studied in the National Institute of Nuclear Research. The second one which is based this work and it was realized through the reaction of acetyl hypo fluorite (CH3COOF) with tri acetyl glucal (TAG) in turn they require the obtention of several fluorated compounds that they serve as intermediates for their obtention so that objective of this work was to find the adequate technique for the obtention of anhydride hydrofluoric acid (HF), KF.2 HF and elemental fluorine so as the design and construction of the systems and equipment used for carry out each one of the reactions. Moreover it was designed the system that will be used for the obtention of acetyl hypo fluoride and the synthesis of composite tetraacetilide 3,4,6 tri-D-glucopyranosil fluoride (TAG-F) for that finally by hydrolysis it was obtained the 2-deoxy fluoride-D-glucose (TAG) in inactive. In this system were realized several preliminary tests. The results are showed in the content of this work also the techniques for compounds characterization were given. (Author)

  2. Synthesis and Characterization of Nano Scale YBCO

    International Nuclear Information System (INIS)

    Synthesis and characterization of the nano scale YBCO superconductor have been performed. The nano scale superconductor was synthesized from YBCO system (YBa2Cu3O7-X). Raw materials, namely Y2O3, BaCO3, and Cu°, were balanced and mixed with ethanol using magnetic steering as a churn in a beaker glass. Then, the precursor was calcined at Tk = 900°C for 5 hours and repeated it until three times. The resulting precursor was ground by using High Energy Milling (HEM) for t = 0, 30, 50, 70, and 90 hour and hereinafter precursors are successively referred as YKM-00, YKM-30, YKM-50, YKM-70, and YKM-90. The resulting powders phase were characterized by means of x-ray diffraction technique using the Rietveld analysis method. Precursor of YKM-90 was pressed into pellets, and then sintered at various temperatures and periods. The sample phase was then characterized by using the Rietveld analysis method based on the x-ray diffraction data. The crystallites size were calculated using Scherrer formula. Results of analysis indicate that by minimizing crystallites size, period of sinter can be shortened from 10 to 1 hour, resulting crystallite size of D = 925 Å, critical current density of Jc = 4 A / cm2, and can be grown of about 15 weight % of 211-phase in a matrix of 123-phase. The decrease of crystallite size will generate a change in physical properties dramatically, if the crystallite size of the material, D is smaller or equal to the coherence length of 10 Å. (author)

  3. Synthesis and characterization of carbon nanotubes decorated with platinum nanoparticles

    Directory of Open Access Journals (Sweden)

    L.A. Dobrzański

    2010-04-01

    Full Text Available Purpose: In presented work results of synthesis of carbon nanotubes decorated with platinum nanoparticles by organic colloidal process as an example of direct formation of nanoparticles onto CNTs are reported.Design/methodology/approach: CNT were grown by chemical vapour deposition (CVD by the catalytic decomposition of CO. To improve metal deposition onto CNTs the purification procedure with a mixture of concentrated HNO3–H2SO4 and H2O2 reduction reagent was applied. CNT–nanocrystal composite was fabricated by direct deposition of nanoparticles onto the surface of CNTs. Chemical composition and crystallographic structure of the obtained Pt/CNT composites were confirmed by energy dispersive X-ray spectroscopy (EDS and by X-ray diffraction (XRD measurements, while transmission (TEM and scanning electron microscopy (SEM were used for characterization of the morphology of composite as well as the distribution of nanocrystals on the CNTs surfaces.Findings: High efficiency of proposed method was confirmed as well as possibility of the coating of Pt nanoparticles onto CNTs, without aggregation of these particles.Research limitations/implications: Many others noble metals such as palladium, platinum, gold and iridium can be used for deposition on the CNTs using described procedure.Originality/value: Obtained material can be employed in constructing various electrochemical sensors. As a result of increasing of the surface area of Pt caused by the reduction of the size of used particles, fabricated sensor may be characterized by higher sensitivity.

  4. Graphene synthesis and characterization on copper

    Science.gov (United States)

    Mohsin, Ali

    Graphene, two dimensional sheet of carbon atoms has recently gained attention as some of its properties are promising for electronics applications e.g. higher mobility that translates to higher operating frequency for devices geared towards radio frequency applications. Excellent optical transmittance combined with its semi metallic behavior makes it an important material for transparent contacts in solar cells. To bring graphene to the production level, synthesis methods are needed for its growth on wafer scale. It has been shown that chemical vapor deposition (CVD) is one of the techniques that can potentially synthesize wafer scale graphene. Recently copper has gained popularity as an important substrate material for graphene growth due to its lower carbon solubility, which allows better control over number of graphene layers. Here we report optimization of graphene growth on copper foils with our home made atmospheric pressure chemical vapor deposition (APCVD) setup. Graphene growth on copper under APCVD was non self-limiting similar to other reports. It was found that apart from growth parameters surface texture plays a very important role in graphene growth. In fact, few layer and bilayer graphene were obtained on the regions where copper surface was not uniform, confirmed by Raman spectroscopy. To improve copper surface texture thin layer of copper film was evaporated by electron beam evaporation before the graphene growth process. After this modification, monolayer graphene was obtained on areas as large as 300 microm x 300 microm confirmed by Raman area maps. Graphene transfer procedure was also optimized so that graphene on metal surface could be transferred to insulating substrate.

  5. The Evolving Role of Chemical Synthesis in Antibacterial Drug Discovery

    OpenAIRE

    Wright, Peter M.; Seiple, Ian B.; Myers, Andrew G.

    2014-01-01

    The discovery and implementation of antibiotics in the early twentieth century transformed human health and wellbeing. Chemical synthesis enabled the development of the first antibacterial substances, organoarsenicals and sulfa drugs, but these were soon outshone by a host of more powerful and vastly more complex antibiotics from nature: penicillin, streptomycin, tetracycline, and erythromycin, among others. These primary defences are now significantly less effective as an unavoidable consequ...

  6. Chemical characterization of some substituted hydroxyapatites

    Directory of Open Access Journals (Sweden)

    Ibrahim Doreya

    2011-11-01

    Full Text Available Abstract Synthetic multi-substituted hydroxyapatite nano powders containing silicon and or carbonate prepared by a wet chemical method. The process parameters are set up to allow the simultaneous substitution of carbonate and silicon ions in the place of phosphorus. The chemical and structural characterizations of the prepared powders are determined with the aid of; XRF, ICP, XRD and FTIR. The results show that, the ion substitution in the crystal lattice of HA caused a change in the unit cell dimensions and affected the degree of crystallization of the produced powders. The apatite formation abilityy of the prepared discs from the synthesized powders is determined by immersing in SBF solution for different periods. The degree of ion release was determined in the obtained solutions. The examined surface of the immersed discs under SEM and analyzed by CDS showed a more dense HA layer than those of un-substituted ones. The HA with the substituted silicon and carbonate ions, showed the highest solubility with greater rate of ion release, compared with carbonate-free powder. All prepared powders took sodium ion from the SBF solution during immersion, which was not recorded before.

  7. 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.

  8. Lanthipeptides: chemical synthesis versus in vivo biosynthesis as tools for pharmaceutical production.

    Science.gov (United States)

    Ongey, Elvis Legala; Neubauer, Peter

    2016-01-01

    Lanthipeptides (also called lantibiotics for those with antibacterial activities) are ribosomally synthesized post-translationally modified peptides having thioether cross-linked amino acids, lanthionines, as a structural element. Lanthipeptides have conceivable potentials to be used as therapeutics, however, the lack of stable, high-yield, well-characterized processes for their sustainable production limit their availability for clinical studies and further pharmaceutical commercialization. Though many reviews have discussed the various techniques that are currently employed to produce lanthipeptides, a direct comparison between these methods to assess industrial applicability has not yet been described. In this review we provide a synoptic comparison of research efforts on total synthesis and in vivo biosynthesis aimed at fostering lanthipeptides production. We further examine current applications and propose measures to enhance product yields. Owing to their elaborate chemical structures, chemical synthesis of these biomolecules is economically less feasible for large-scale applications, and hence biological production seems to be the only realistic alternative. PMID:27267232

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

    Science.gov (United States)

    Koroleva, Elena V.; Gusak, K. N.; Ignatovich, Zh V.

    2010-10-01

    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.

  10. 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.

  11. 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

  12. 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.

  13. Magnetic ionic liquids: synthesis and characterization

    International Nuclear Information System (INIS)

    The synthesis of magnetic ionic liquids (MILs) based on the stable dispersions of magnetic nanoparticles (MNPs) of γ-Fe2O3, Fe3O4, and CoFe2O4 in the ionic liquid 1-n-butyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide (BMI.NTf2) is reported. The MNPs were obtained by the coprecipitation method. The surface of the α-Fe2O3, Fe3O4, and CoFe2O4 MNPs with mean sizes (XRD) of 9.3, 12.3, and 11.0 nm, respectively were functionalized by 1-n-butyl-3-(3'-trimethoxypropylsilane)- imidazolium chloride. The non functionalized and functionalized MNPs were further characterized by Raman, FTIR-ATR, and FTNIR spectroscopy and by TGA. The stability of the MILs was assigned to the formation of at least one monolayer of the surface modifier agent that mimics the structure of the BMI.NTf2 IL. (author)

  14. : Synthesis, Characterization, and Enhanced Photocatalytic Activity

    Science.gov (United States)

    Gao, Xiaoming; Fu, Feng; Li, Wenhong

    2014-12-01

    3D hierarchical microspheres of Cu-loaded Bi2WO6 are successfully prepared by the hydrothermal synthesis method on a large scale. The as-prepared samples are characterized by UV-Vis DRS, BET, XRD, XPS, and SEM. The results reveal that the light absorption of Cu-loaded Bi2WO6 has higher intensity in the visible range and a bathochromic shift of the absorption edge compared to that of pure Bi2WO6. The photocatalytic activity is evaluated by phenol removal from aqueous solution under visible-light irradiation. The results demonstrate that loaded Cu significantly enhances the photocatalytic activity of Bi2WO6, for the loaded Cu acts as the electron receptor on the surface of Bi2WO6, and inhibits the recombination of photogenerated electron-hole. The content of loaded Cu has an impact on the catalytic activity, and the 1.0 wt.% Cu-loaded Bi2WO6 exhibits the best photocatalytic activity in the degradation of phenol. Furthermore, the reaction kinetics of phenol removal from aqueous solution over the Cu-loaded Bi2WO6 is established by the way of the Langmuir-Hinshelwood model. The results indicate that the process of photodegradation of phenol on Cu-loaded Bi2WO6 match the Langmuir-Hinshelwood kinetic model.

  15. Novel metallomesogenic polyurethanes: Synthesis, characterization and properties

    International Nuclear Information System (INIS)

    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 (Mn = 650, 2000) and 2,4-toluene diisocyanate (TDI), or 4,4′-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, 1H and 13C 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: ► Design and synthesis of metallomesogenic diols. ► Metallomesogenic polyurethanes were prepared using these diols as chain extenders. ► Liquid crystalline and mechanical properties were studied. ► A square pyramidal structure for the copper(II) complexes have been proposed. ► Polyurethanes exhibited enantiotropic smectic A phases.

  16. 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.

  17. Synthesis, characterization and toxicological evaluation of carbon-based nanostructures

    OpenAIRE

    Mendes, Rafael Gregorio

    2015-01-01

    The synthesis, characterization and biological evaluation of different graphene-based nanoparticles with potential biomedical applications are explored. The results presented within this work show that eukaryotic cells can respond differently not only to different types of nanoparticles, but also identify slight differences in the morphology of nanoparticles, such as size. This highlights the great importance of the synthesis and thorough characterization of nanoparticles in the design of eff...

  18. 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.

  19. 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.

  20. 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.

  1. Temperature lowering in cryogenic chemical-synthesis techniques and system

    International Nuclear Information System (INIS)

    When evaluating a chemical synthesis process for a reaction that occurs on the cryogenically cooled walls, it is sometimes necessary to reduce the wall temperatures to enhance the chemical process. To evaluate the chemical process at lower than atmospheric boiling of liquid nitrogen, we built a system and used it to reduce the temperature of the liquid nitrogen. The technique of lowering the liquid nitrogen temperature by reducing the pressure of the boil-off is established knowledge. This paper presents the engineering aspects of the system, design features, equipment requirements, methods of control, and results of the chemical synthesis. The heat input to the system was ∼400 watts, placing a relatively large demand on the pumping system. Our system is a scale-up of the small laboratory experiment, and it provides the information needed to design an effective system. The major problem encountered was the large quantity of liquid escaping the system during the processing, placing a large gas load on the vacuum system

  2. Vanadium oxide based materials: Synthesis, characterization and gas sensing properties

    Science.gov (United States)

    Ayesh, Samar I.

    In recent years, the demand for gas sensors based on safety and process control requirements has been expanding. The reason for such demand sterns from environmental and safety concerns since the toxic gases released from automobile exhausts and chemical plants can directly or indirectly pollute our environment and affect our health. Among the chemicals studied, nitrogen oxide (NOx) gases are among the most dangerous air pollutants. Transition metal oxide clusters (or polyoxometalates) provide an exciting opportunity for the design and synthesis of a new generation of materials for efficient NOx sensing. Polyoxometalates are an important and fast emerging class of compounds that exhibit many remarkable properties. Chapter 1 provides introduction and background of chemical sensors. It describes the need for gas sensors and the current status of research in the area of NOx gas sensors in particular. A description of polyoxmetalates and their relevance as potential novel gas sensor materials is also given. Chapter 2 describes the synthesis and characterization by FTIR spectroscopy, elemental analysis, thermogravimetric analysis, manganometric titration, bond valence sum calculation, temperature dependent magnetic properties studies, electron paramagnetic resonance, and complete single crystal X-ray diffraction analysis of newly prepared vanadium oxide based-systems that have been discovered during the course of this work. First, the system containing arrays of decavanadates networked by extensive hydrogen bonding with cyclic nitrogen bases are described. This is followed by the mixed-valence vanadium oxide cluster, [VV 13VIV3O42(Cl)]-7, containing a hitherto unknown vanadium oxide framework structure. Finally the synthesis of 3D-framework materials is described. These compounds have highly symmetrical closely related three-dimensional framework structures consisting vanadium oxide shells {V18O42(XO4)} linked via heterometallic atoms {M' = Cd, Zn} into three

  3. Green and sustainable chemical synthesis using flow microreactors.

    Science.gov (United States)

    Yoshida, Jun-ichi; Kim, Heejin; Nagaki, Aiichiro

    2011-03-21

    Several features that allow flow microreactors contribute to green and sustainable chemical synthesis are presented: (1) For extremely fast reactions, kinetics often cannot be used because of the lack of homogeneity of the reaction environment when they are conducted in batch macroreactors. Better controllability, by virtue of fast mixing based on short diffusion paths in microreactors, however, leads to a higher selectivity of the products, based on kinetics considerations. Therefore, less waste is produced. (2) Reactions involving highly unstable intermediates usually require very low temperatures when they are conducted in macrobatch reactors. By virtue of short residence times, flow microreactors enable performing such reactions at ambient temperatures, avoiding cryogenic conditions and minimizing the energy required for cooling. (3) By virtue of the precise residence time control, flow microreactors allow to avoid the use of auxiliary substances such as protecting groups, enabling highly atom- and step-economical straightforward syntheses. The development of several test plants based on microreaction technology has proved that flow microreactor synthesis can be applied to the green and sustainable production of chemical substances on industrial scales. (4) Microreactor technology enables on-demand and on-site synthesis, which leads to less energy for transportation and easy recycling of substances. PMID:21394921

  4. Synthesis and characterization of poly iodine anilines by plasma

    International Nuclear Information System (INIS)

    The polymers and organic materials present a numberless quantity of applications. However, it has not been but until recent times that it has been found that some of these materials can possess semiconductor properties. This has generated a great interest for the investigation in the area of semiconductor polymers. The poly aniline (Pan) it is one of the main semiconductor polymers because their electric properties change depending on the doping and of the state of oxidation to the one the molecules are subjected. The synthesis of this material has been carried out by means of chemical oxidation or electrochemistry. In this work a study is presented on the formation of poly aniline polymers with halogens chemically united to the aniline ring, poly(m-iodine aniline) (m-PAnI) and poly(m-chloroaniline) (m-PAnCI) for plasma. The plasma is generated by means of discharges of splendor with an r f amplifier to 13.5 MHz to drops pressures (10-2 mbar). The synthesized polymers were obtained in form of thin film in the walls of the reactor and in the substrate introduced in the one. The electric properties of the polymers were evaluated in function of the time of reaction. Also, the conductivity of the polymers was compared synthesized in this work with reported data of synthesized poly aniline and doped with iodine for plasma. The highest values in conductivity are obtained in the poly aniline where the halogens are chemically connected to the ring that if it is doped with iodine. The atomic proportion in the surface of the polymers was analyzed by dispersive energy spectroscopy with which is deduced that the halogens come off of the molecules of the monomers or of the polymer in formation and that the atoms of iodine get lost more easily than those of chlorine. Other techniques that were used to characterize to the poly aniline were scanning electron microscopy, infrared spectroscopy, thermal gravimetric analysis and X-ray diffraction. The results are presented in function

  5. Synthesis, structural, and spectroscopic (FT-IR, NMR, and UV) Characterization of 1-(Cyclohexylmethyl)-2-(pyridin-2-yl)-1 H-benzo[ d]imidazole by experimental techniques and quantum chemical calculations

    Science.gov (United States)

    Özdemir, Namık; Dayan, Osman; Demirmen, Selin

    2016-05-01

    The title compound ( II), 1-(cyclohexylmethyl)-2-(pyridin-2-yl)-1 H-benzo[ d]imidazole (C19H21N3), was synthesized via N-alkylation of 2-(pyridin-2-yl)-1 H-benzo[ d]imidazole ( I). Both compounds I and II were characterized by IR, NMR and UV-vis spectroscopy. Solid-state structure of compound II was determined by single-crystal X-ray diffraction technique. Furthermore, quantum chemical calculations employing density functional theory (DFT/B3LYP) method with the 6-311++ G( d, p) basis set were performed for the theoretical characterization of the molecular and spectroscopic features of the compounds. Using the TD-DFT method, electronic absorption spectra of the compounds have been predicted at same level. When the obtained results were compared with the experimental findings, it is seen that theoretical results support the experimental data and a good agreement exists between them.

  6. 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.

  7. 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.

  8. Graphene Oxide: Synthesis, Characterization, Electronic Structure, and Applications

    Science.gov (United States)

    Stewart, Derek A.; Mkhoyan, K. Andre

    While graphite oxide was first identified in 1855 [1, 2], the recent discovery of stable graphene sheets has led to renewed interest in the chemical structure and potential applications of graphene oxide sheets. These structures have several physical properties that could aid in the large scale development of a graphene electronics industry. Depending on the degree of oxidization, graphene oxide layers can be either semiconducting or insulating and provide an important complement to metallic graphene layers. In addition, the electronic and optical properties of these films can be controlled by the selective removal or addition of oxygen. For example, selective oxidationof graphene sheets could lead to electronic circuit fabrication on the scale of a single atomic layer. Graphene oxide is also dispersible in water and other solvents and this provides a facile route for graphene deposition on a wide range of substrates for macroelectronics applications. Although graphite oxide has been known for roughly 150 years, key questions remain in regards to its chemical structure, electronic properties, and fabrication. Answering these issues has taken on special urgency with the development of graphene electronics. In this chapter, we will provide an overview of the field with special focus on synthesis, characterization, and first principles analysis of bonding and electronic structures. Finally, we will also address some of the most promising applications for graphene oxide in electronics and other industries.

  9. Synthesis and characterization of CuO at nanoscale

    Energy Technology Data Exchange (ETDEWEB)

    Bozkurt, Gamze [Nanoscience and Nanoengineering Department, Atatürk University, Erzurum 25240 (Turkey); Bayrakçeken, Ayşe [Chemical Engineering Department, Atatürk University, Erzurum 25240 (Turkey); Özer, A. Kadir, E-mail: kadirozer@atauni.edu.tr [Chemical Engineering Department, Atatürk University, Erzurum 25240 (Turkey)

    2014-11-01

    Highlights: • CuO structures were synthesized by chemical precipitation method. • Effects of different reactants and surfactants were investigated. • Morphologies were significantly changed with respect to the synthesis conditions. - Abstract: CuO structures were synthesized by chemical precipitation method at nanoscale. The effects of different reactants including KOH + NH{sub 3}·H{sub 2}O, NH{sub 3}·H{sub 2}O + KOH, KOH or NaOH in addition to Cu(NO{sub 3}){sub 2}·3H{sub 2}O on the properties of CuO structures were investigated. Effects of different surfactants including zwitterionic 3-(N,N-dimethyldodecylammonio) propane-sulfonate (SB12), cationic cetyl trimethylammonium bromide (CTAB) and anionic sodium dodecyl sulfate (SDS) were also investigated. Synthesized samples were characterized by X-ray diffraction (XRD), thermal gravimetric analysis (TGA), Fourier Transform Infrared (FTIR) spectra, scanning electron microscopy (SEM) and cyclic voltammetry (CV) techniques. XRD and SEM results showed that the morphologies were significantly changed with respect to the reactant used. The significant effects of different surfactants on the structures were also observed from the experiments. The specific capacitances were changed according to the utilization of different reactants.

  10. Influence of the synthesis parameters on the physico-chemical and catalytic properties of cerium oxide for application in the synthesis of diethyl carbonate

    International Nuclear Information System (INIS)

    Synthesis of cerium (IV) oxide by means of room temperature precipitation method was carried out. The effect of preparation variables such as synthesis time, calcination temperature and pH of the solution on resulting CeO2 properties was discussed. Moreover, the comparison of CeO2 samples prepared in a static and rotation mode of synthesis is presented. The solid catalysts were characterized by means of X-ray powder diffraction, scanning electron microscopy, transmission electron microscope, nitrogen physisorption, X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy using pyridine as a probe molecule and temperature programmed desorption of CO2. Significant variations in physico-chemical properties of CeO2 by varying the preparation conditions were observed. Furthermore, the catalytic performances of CeO2 catalysts were compared in the synthesis of diethyl carbonate starting from ethanol and CO2 using butylene oxide as a dehydrating agent. The dependence of CeO2 properties on its catalytic activity is evaluated in detail. - Highlights: • Synthesis of cerium (IV) oxide by precipitation method. • Influence of synthesis time, calcination temperature, mode of stirring and solution pH on properties. • Characterization by XRD, SEM, TEM, nitrogen physisorption, XPS, FTIR. • Catalytic performance diethyl carbonate synthesis from ethanol and CO2

  11. Synthesis and characterization of hexaarylbenzenes with five or six different substituents enabled by programmed synthesis

    Science.gov (United States)

    Suzuki, Shin; Segawa, Yasutomo; Itami, Kenichiro; Yamaguchi, Junichiro

    2015-03-01

    Since its discovery in 1825, benzene has served as one of the most used and indispensable building blocks of chemical compounds, ranging from pharmaceuticals and agrochemicals to plastics and those used in organic electronic devices. Benzene has six hydrogen atoms that can each be replaced by different substituents, which means that the structural diversity of benzene derivatives is intrinsically extraordinary. The number of possible substituted benzenes from n different substituents is (2n + 2n2 + 4n3 + 3n4 + n6)/12. However, owing to a lack of general synthetic methods for making multisubstituted benzenes, this potentially huge structural diversity has not been fully exploited. Here, we describe a programmed synthesis of hexaarylbenzenes using C-H activation, cross-coupling and [4+2] cycloaddition reactions. The present method allows for the isolation and structure-property characterization of hexaarylbenzenes with distinctive aryl substituents at all positions for the first time. Moreover, the established protocol can be applied to the synthesis of tetraarylnaphthalenes and pentaarylpyridines.

  12. Synthesis and Characterization of New Polyamides from 1,2-Bis hydrazine Derivatives

    International Nuclear Information System (INIS)

    Preparation of polyamides having different chemical structures allows obtaining new materials with different mechanical and physical properties. The difference in the chemical structure depends mainly on the starting reactants used in condensation polymerization of polyamides. In this paper the synthesis of new polyamides based on the condensation polymerization of 1,2- Bis(3-carboxyacryloyl or carboxybenzoyl) hydrazine derivatives and various diamines has been described. The polymers obtained were characterized using spectroscopic and X-ray analysis. Besides thermal stability and electrical conductivity have been evaluated and correlated with the chemical structure of the polyamides obtained

  13. Synthesis in Characterization of Tapioca Starch-High Density Polyethylene Composite

    International Nuclear Information System (INIS)

    Synthesis and characterization of tapioca starch - High Density Polyethylene (HDPE) composite have been done. The aim of this research is to make plastic that could be degrade in natural known as biodegradable plastic. This research is conducted in step of synthesis of tapioca starch in nanometer scale, synthesis of tapioca starch-HDPE composite and characterizing this composite. Synthesis of tapioca starch in nanometer scale is done by milling process using planetary ball mill. Synthesis of tapioca starch-HDPE composite is done by blending the HDPE and tapioca starch in laboplastomill. The characterization of particle size of tapioca starch is done by using scanning electron microscope (SEM). Mechanical properties was determined by using stograph R-1 tensile strength test. Characterization of functional group is done by using FT-IR (Fourier Transform-Infra Red) spectroscopy. The added of tapioca starch in nanometer scale into HDPE matrix caused the decreasing of tensile strength. The bonding between tapioca starch as filler with HDPE as matrix is physical bonding not chemical bonding express with no new spectrum in FT-IR. (author)

  14. Enabling Technologies for the Future of Chemical Synthesis.

    Science.gov (United States)

    Fitzpatrick, Daniel E; Battilocchio, Claudio; Ley, Steven V

    2016-03-23

    Technology is evolving at breakneck pace, changing the way we communicate, travel, find out information, and live our lives. Yet chemistry as a science has been slower to adapt to this rapidly shifting world. In this Outlook we use highlights from recent literature reports to describe how progresses in enabling technologies are altering this trend, permitting chemists to incorporate new advances into their work at all levels of the chemistry development cycle. We discuss the benefits and challenges that have arisen, impacts on academic-industry relationships, and future trends in the area of chemical synthesis. PMID:27163040

  15. Synthesis and characterization of chitosan alkyl urea.

    Science.gov (United States)

    Wang, Jing; Jiang, Ji-Zhou; Chen, Wei; Bai, Zheng-Wu

    2016-07-10

    Chitosan is a versatile material employed for various purposes in many fields including the development of chiral stationary phases for enantioseparation. Chitosan alkyl urea is a kind of intermediate used to prepare enantioseparation materials. In order to synthesize the intermediates, in the present work, a new way to prepare chitosan alkyl urea has been established: chitosan was first reacted with methyl chloroformate yielding N-methoxyformylated chitosan, which was then converted to chitosan alkyl urea through amine-ester exchange reaction. With a large excess of methyl chloroformate and primary amine of low stereohindrance, the amino group in chitosan could be almost completely converted to ureido group. The as-prepared chitosan alkyl urea derivatives were characterized by IR, (1)H NMR, (13)C NMR,(1)H-(1)H COSY and (1)H-(13)C HSQC NMR spectra. The chemical shifts of hydrogen and carbon atoms of glucose unit were assigned. It was found that the degree of substitution was obviously lower if cyclopropyl amine, aniline, tert-butyl amine and diethyl amine were used as reactants for the amine-ester exchange reaction. The reason was explained with the aid of theoretical calculations. PMID:27106154

  16. Synthesis and characterization of struvite nano particles

    Science.gov (United States)

    Rathod, K. R.; Jogiya, B. V.; Chauhan, C. K.; Joshi, M. J.

    2015-06-01

    Struvite, Ammonium Magnesium Phosphate Hexahydrate [(AMPH) - (NH4)MgPO4.6(H2O)], is one of the fascinating inorganic phosphate minerals. Struvite is one of the components of the urinary stones. Struvite occurs as crystallites in urine and grows as a type of kidney stone. In this study, struvite nano particles were synthesized by wet chemical technique. The aqueous solutions containing dissolved Mg(CH3COO)2.4H2O and (NH4)H2PO4 mixed at the Mg/P molar ratio of 1.00. The synthesized struvite nano particles were characterized by XRD, FT-IR, Thermal Analysis and TEM. From XRD, crystal structure of the nano particle was found to be orthorhombic and crystalline size was found to be within 11 to 26 nm. The FT-IR spectrum for the struvite nano particles confirmed the presence of a water molecule and metal-oxygen stretching vibration, O-H stretching and bending, N-H bending and stretching, P-O bending and stretching vibrations. The Thermal Analysis was carried out from room temperature to 900°C. From TEM analysis, particle size was 23 to 30 nm. All the results were compared with bulk struvite.

  17. Total chemical synthesis of human proinsulin†‡

    OpenAIRE

    Luisier, Samuel; Avital-Shmilovici, Michal; Weiss, Michael A.; Kent, Stephen B H

    2010-01-01

    A convergent synthetic strategy based on modern chemical ligation methods was used to make human proinsulin. The synthetic protein was characterized by LCMS, CD spectroscopy, and by 1D- and 2D-NMR spectroscopy. Synthetic human proinsulin had full biochemical activity in a receptor-binding assay.

  18. Single-step chemical synthesis of ferrite hollow nanospheres

    International Nuclear Information System (INIS)

    We report a single-step chemical synthesis of iron oxide hollow nanospheres with 9.3 nm in diameter. The sample presents a narrow particle diameter distribution and chemical homogeneity. The hollow nature of the particles is confirmed by HRTEM and HAADF STEM analysis. Electron and x-ray diffraction show that the outer material component is constituted by 2 nm ferrite crystals. Moessbauer data provide further evidence for the formation of iron oxide with high structural disorder, magnetically ordered at 4.2 K and superparamagnetism at room temperature. An unusual magnetic behavior under an applied field is reported, which can be explained by the large fraction of atoms existing at both inner and outer surfaces.

  19. Synthesis and characterization of macromolecular layers grafted to polymer surfaces

    Science.gov (United States)

    Burtovyy, Oleksandr

    The composition and behavior of surfaces and interfaces play a pivotal role in dictating the overall efficiency of the majority of polymeric materials and devices. Surface properties of the materials can be altered using surface modification techniques. It is necessary to highlight that successful methods of surface modification should affect only the upper layer of the polymer material without changing bulk properties. The processes must introduce new functionalities to the surface, optimize surface roughness, lubrication, hydrophobicity, hydrophilicity, adhesion, conductivity, and/or biocompatibility. Research presented in this dissertation is dedicated to the synthesis, characterization, and application of thin macromolecular layers anchored to polymer substrates. Specifically, attachment of functional polymers via a "grafting to" approach has been extensively studied using PET and nylon model substrates. First, poly(glycidyl methacrylate) was used to introduce permanent functionalities to the model substrates by anchoring it to model films. Then, three different functional polymers were grafted on top of the previous layer. As one part of this study, the temperature and time dependence of grafting functional layers were studied. The surface coverage by hydrophobic polymer was determined from experimental data and predicted by a model. In general, the model has a high degree of predictive capability. Next, surface modification of polymeric fibers and membranes is presented as an important application of the polymer thin layers targeted in the study. Specifically, the procedures developed for surface modification of model substrates was employed for modification of PET, nylon, and cotton fabrics as well as PET track-etched membranes. Since epoxy groups are highly reactive in various chemical reactions, the approach becomes virtually universal, allowing both various surfaces and end-functionalized macromolecules to be used in the grafted layer synthesis. PET

  20. 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).

  1. Peptide protected gold clusters: chemical synthesis and biomedical applications

    Science.gov (United States)

    Yuan, Qing; Wang, Yaling; Zhao, Lina; Liu, Ru; Gao, Fuping; Gao, Liang; Gao, Xueyun

    2016-06-01

    Bridging the gap between atoms and nanoparticles, noble metal clusters with atomic precision continue to attract considerable attention due to their important applications in catalysis, energy transformation, biosensing and biomedicine. Greatly different to common chemical synthesis, a one-step biomimetic synthesis of peptide-conjugated metal clusters has been developed to meet the demand of emerging bioapplications. Under mild conditions, multifunctional peptides containing metal capturing, reactive and targeting groups are rationally designed and elaborately synthesized to fabricate atomically precise peptide protected metal clusters. Among them, peptide-protected Au Cs (peptide-Au Cs) possess a great deal of exceptional advantages such as nanometer dimensions, high photostability, good biocompatibility, accurate chemical formula and specific protein targeting capacity. In this review article, we focus on the recent advances in potential theranostic fields by introducing the rising progress of peptide-Au Cs for biological imaging, biological analysis and therapeutic applications. The interactions between Au Cs and biological systems as well as potential mechanisms are also our concerned theme. We expect that the rapidly growing interest in Au Cs-based theranostic applications will attract broader concerns across various disciplines.

  2. Synthesis and in situ characterization of graphene on copper substrates

    OpenAIRE

    Callens, Lien

    2014-01-01

    This thesis focuses on the synthesis and study of graphene, a rising star on the horizon of materials science with many applications in (bio)electronics, photonics, bioengineering, etc.. Still, a controlled synthesis of good quality graphene on a wafer-size scale remains a challenge. This project takes a first step towards the in situ preparation and characterization of graphene. The growth process, executed under ultra high vacuum, was analysed in situ by different spectroscopy methods. W...

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

    OpenAIRE

    Jingfei Luan; Zhitian Hu; Lingyan Zhang

    2011-01-01

    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 organobis...

  4. PHYTO-ASSISTED SYNTHESIS AND CHARACTERIZATION OF SILVER NANOPARTICLES FROM AMARANTHUS DUBIUS

    OpenAIRE

    M. Jannathul Firdhouse; Lalitha, P.

    2012-01-01

    The aqueous extract of Amaranthus dubius was used for the green synthesis of silver nanoparticles from silver nitrate solution under various conditions. The silver nanoparticles were characterized by spectrophotometric, physical and theoretical methods. The size of silver nanoparticles ranged from 10-70nm. The present approach of biosynthesis of silver nanoparticles using aqueous extract of A.dubius appears to be cost efficient, eco-friendly and an easy alternative to conventional chemical me...

  5. Systematic Synthesis and Characterization of a Series of Tetra(5-aryl-2-thienyl)thiophenes

    OpenAIRE

    Muraoka, Hiroki; Tanifuji, Takanori; Ogawa, Satoshi

    2011-01-01

    We have succeeded in the synthesis of a series of tetra(5-aryl-2-thienyl)thiophenes as aryl-functionalized tetrathienylthiophenes. Characterization of these chemicals was performed by physical and spectroscopic means. The electrochemical properties were examined by cyclic voltammetry. The CV of all compounds showed that the redox behavior and potentials were controlled by the electronic effect of the p-substituted phenyl groups introduced at the outer α-positions on the four thiophene units l...

  6. Synthesis and EPR Characterization of Exohedrally Perfluoroalkylated Paramagnetic Lanthanum Metallofullerenes: A Fluorous Phase Approach

    Science.gov (United States)

    Tagmatarchis, Nikos; Taninaka, Atsushi; Shinohara, Hisanori; Prato, Maurizio

    2002-10-01

    A strategy to chemically derivatize the outer sphere of endohedral metallofullerenes by using a modern organic technique that utilizes a fluorous synthesis-partitioning approach has been developed. The newly synthesized materials were found to be paramagnetic species and were characterized by electron paramagnetic resonance spectroscopy (EPR), laser desorption time-of-flight spectrometry (LD-TOF) and electronic absorption spectroscopy (UV-VIS-NIR). The systematic study of exohedrally derivatized endohedral metallofullerenes should ultimately provide technologically intriguing novel nano-materials.

  7. Synthesis and characterization of UiO-67-BNDC MOF

    OpenAIRE

    Wu, Lianpao

    2015-01-01

    In this study, the 1,1'-binaphthyl-4,4'-dicarboxylic acid (BNDC) linker has been synthesized by six-step synthesis route in five gram level. Meanwhile, a four-step synthesis route was also explored in a milligram scale. Then a new Zr-MOF with the BNDC linker was prepared by the conventional method. The synthesis of this MOF single crystal was also tested.This new Zr-MOF was characterized by a various methods including powder X-ray diffraction (PXRD), thermogravimetric analysis (TGA), N2 adsor...

  8. Synthesis and characterizations of novel polymer electrolytes

    Science.gov (United States)

    Chanthad, Chalathorn

    Polymer electrolytes are an important component of many electrochemical devices. The ability to control the structures, properties, and functions of polymer electrolytes remains a key subject for the development of next generation functional polymers. Taking advantage of synthetic strategies is a promising approach to achieve the desired chemical structures, morphologies, thermal, mechanical, and electrochemical properties. Therefore, the major goal of this thesis is to develop synthetic methods for of novel proton exchange membranes and ion conductive membranes. In Chapter 2, new classes of fluorinated polymer- polysilsesquioxane nanocomposites have been designed and synthesized. The synthetic method employed includes radical polymerization using the functional benzoyl peroxide initiator for the telechelic fluorinated polymers with perfluorosulfonic acids in the side chains and a subsequent in-situ sol-gel condensation of the prepared triethoxylsilane-terminated fluorinated polymers with alkoxide precursors. The properties of the composite membranes have been studied as a function of the content and structure of the fillers. The proton conductivity of the prepared membranes increases steadily with the addition of small amounts of the polysilsesquioxane fillers. In particular, the sulfopropylated polysilsesquioxane based nanocomposites display proton conductivities greater than Nafion. This is attributed to the presence of pendant sulfonic acids in the fillers, which increases ion-exchange capacity and offers continuous proton transport channels between the fillers and the polymer matrix. The methanol permeability of the prepared membranes has also been examined. Lower methanol permeability and higher electrochemical selectivity than those of Nafion have been demonstrated in the polysilsesquioxane based nanocomposites. In Chapter 3, the synthesis of a new class of ionic liquid-containing triblock copolymers with fluoropolymer mid-block and imidazolium methacrylate

  9. Synthesis and Characterization of Nanostructured Sulfated Zirconias

    Czech Academy of Sciences Publication Activity Database

    Lutecki, M.; Šolcová, Olga; Werner, S.; Breitkopf, C.

    2010-01-01

    Roč. 53, č. 1 (2010), s. 13-20. ISSN 0928-0707 Grant ostatní: DFG(DE) BR2068/2-1; DFG(DE) BR2068/2-2 Institutional research plan: CEZ:AV0Z40720504 Keywords : sulfated zirconia * template assisted synthesis * porous materials Subject RIV: CA - Inorganic Chemistry Impact factor: 1.525, year: 2010

  10. Characterizing Molecular Interactions in Chemical Systems

    OpenAIRE

    Guenther, David; Alvarez-Boto, Roberto; Contreras-Garcia, Julia; Piquemal, Jean-Philip; Tierny, Julien

    2014-01-01

    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 ...

  11. Properties Characterization of Chemically Modified Hemp Hurds

    OpenAIRE

    Nadezda Stevulova; Julia Cigasova; Adriana Estokova; Eva Terpakova; Anton Geffert; Frantisek Kacik; Eva Singovszka; Marian Holub

    2014-01-01

    The effect of chemical treatment of hemp hurds slices in three solutions (EDTA (Ethylenediaminetetraacetic acid), NaOH and Ca(OH)2) on the properties of natural material was discussed in this paper. Changes in the morphology, chemical composition and structure as well as thermal stability of hemp hurds before and after their modification were investigated by using FTIR (Fourier transform infrared spectroscopy), XRD (X-ray powder diffraction analysis) and TG (thermogravimetry)/DSC (differentia...

  12. Chemical characterization of a marine conditioning film

    Digital Repository Service at National Institute of Oceanography (India)

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

    in marine waters. Abundance and composition of neutral sugars and its composition are useful tools to assess the sources of organic matter (Cowie and Hedges, 1984; Skoog and Benner, 1997; D’Souza et al., 2005). Carbohydrate polymers appear to play... procedures and substratum surface properties may influence the chemical composition and the amount of the adsorbed material (Little and Zsolnay, 1985; Taylor et al., 1997; Compere et al., 2001). Changes in the chemical composition of the conditioning film...

  13. 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.

  14. 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.

  15. Nanocrystalline hydroxyapatite bioceramic using microwave radiation: Synthesis and characterization

    International Nuclear Information System (INIS)

    In this work, we synthesized bioactive hydroxyapatite (Ca10(PO4)6(OH)2, HAp) ceramic powder in the lower-end of nano-regime using microwave radiation, which offers several advantages. The powder was synthesized using calcium nitrate tetrahydrate and sodium phosphate dibasic anhydrous as the starting materials. EDTA served as the complex reagent. The pH of the final suspension was adjusted to 9 by adding ammonium hydroxide. Applied microwave power of 600 W, pH of the suspension, mole ratio of Ca/P in the staring chemicals, and the chelating effect of EDTA served as the factors in the synthesis of nanocrystalline HAp powder. The synthesized powder was studied using various characterizing techniques viz., XRD, SEM, HR-TEM, EDS, TG/DTA and FT-IR to determine powder morphology, particle-size, crystallinity, phases, elemental composition and thermal behavior. Results confirmed highly crystalline nano-powder (5-30 nm) with elemental composition of Ca and P in HAp phase and possessed mixed (elliptical and rod-shape) morphology. Using the Scherrer formula, the average crystallite size was found to be 12 nm. The FT-IR confirmed that the powder is of typical apatite structure. Thermal analysis showed a remarkably lower initial dehydroxylation temperature, compared to micron sized HAp, as reported in literature.

  16. 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.

  17. Synthesis, characterization, applications, and challenges of iron oxide nanoparticles.

    Science.gov (United States)

    Ali, Attarad; Zafar, Hira; Zia, Muhammad; Ul Haq, Ihsan; Phull, Abdul Rehman; Ali, Joham Sarfraz; Hussain, Altaf

    2016-01-01

    Recently, iron oxide nanoparticles (NPs) have attracted much consideration due to their unique properties, such as superparamagnetism, surface-to-volume ratio, greater surface area, and easy separation methodology. Various physical, chemical, and biological methods have been adopted to synthesize magnetic NPs with suitable surface chemistry. This review summarizes the methods for the preparation of iron oxide NPs, size and morphology control, and magnetic properties with recent bioengineering, commercial, and industrial applications. Iron oxides exhibit great potential in the fields of life sciences such as biomedicine, agriculture, and environment. Nontoxic conduct and biocompatible applications of magnetic NPs can be enriched further by special surface coating with organic or inorganic molecules, including surfactants, drugs, proteins, starches, enzymes, antibodies, nucleotides, nonionic detergents, and polyelectrolytes. Magnetic NPs can also be directed to an organ, tissue, or tumor using an external magnetic field for hyperthermic treatment of patients. Keeping in mind the current interest in iron NPs, this review is designed to report recent information from synthesis to characterization, and applications of iron NPs. PMID:27578966

  18. 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.

  19. Properties Characterization of Chemically Modified Hemp Hurds

    Directory of Open Access Journals (Sweden)

    Nadezda Stevulova

    2014-12-01

    Full Text Available The effect of chemical treatment of hemp hurds slices in three solutions (EDTA (Ethylenediaminetetraacetic acid, NaOH and Ca(OH2 on the properties of natural material was discussed in this paper. Changes in the morphology, chemical composition and structure as well as thermal stability of hemp hurds before and after their modification were investigated by using FTIR (Fourier transform infrared spectroscopy, XRD (X-ray powder diffraction analysis and TG (thermogravimetry/DSC (differential scanning calorimetry. Size exclusion chromatography (SEC measurements were used for determination of degree of cellulose polymerization of hemp hurd samples. Chemical modification is related to the partial removal of non-cellulosic components of lignin, hemicellulose and pectin as well as waxes from the surface of hemp hurd slices. Another effect of the chemical treatment applied is connected with increasing the crystallinity index of cellulose determined by FTIR and XRD methods. Decrease in degree of cellulose polymerization and polydispersity index in chemically modified hemp hurds compared to the original sample was observed. Increase in thermal stability of treated hemp hurd was found. The most significant changes were observed in alkaline treated hemp hurds by NaOH.

  20. 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.

  1. Synthesis of Colloidal Ruthenium Nanocatalyst by Chemical Reduction Method

    OpenAIRE

    Patharkar, R. G.; S. U. Nandanwar; Chakraborty, M.

    2013-01-01

    Colloidal ruthenium nanoparticles were prepared by chemical reduction of ruthenium trichloride (RuCl3) using sodium borohydrate (NaBH4) as reducing agent and sodium dodecyl sulfate (SDS) as a stabilizer. Size and size distribution of synthesized colloidal Ru nanoparticles were studied by varying different parameters such as molar ratio (MR) of SDS/RuCl3, NaBH4/RuCl3, effects of different stabilizers, and reducing agents. Prepared nanoparticles were characterized by transmission electron micro...

  2. Synthesis, characterization and applications of magnetite nanoparticles

    Science.gov (United States)

    Kanmukhla, Vikram Kumar

    In the past few years, the synthesis of magnetic nanoparticles has received considerable attention due to their potential use in clinical applications. Since the properties of these nanoparticles depend strongly on their size, shape and crystallinity, there is a need for a general method to produce these particles with a controlled size, shape and crystal type. Of the many magnetic materials (Co, Ni, and Fe), the magnetite (Fe3O 4) is least toxic and hence most promising for applications in medical diagnostics. Microemulsion-based synthesis utilizes the local aqueous environment within a reverse micelle as a nano-scale reactor and allows synthesizing nanoparticles with a hydrophilic surface for subsequent functionalization. By controlling the water-to-surfactant ratio, the type of surfactants, and the ionic strength of the aqueous core, one can control the size and shape of the resulting particles. We developed such a system that allows the multi-step synthesis of surface-functionalized, magnetic nanoparticles in a one-pot synthesis reaction. By altering the system chemistry, we were further able to produce either spheres or cylinders of controlled dimension in the size range of 5 nm to 30 nm. Using standard bio-conjugation techniques, we successfully immobilized an enzyme onto the nanoparticles. We also developed a theoretical model for the separation and fractionation of nanoparticles based on their size and magnetic properties. Using the multiphysics and finite element modeling capabilities of FEMLAB(TM), we solved the coupled system of PDEs describing the interaction of magnetic particles within a magnetic field for either static (cylindrical beaker) or convective flow (capillary) conditions. A net retention time as high as 310 s is achieved for 200 nm particles at field strength of 1250 kA/m. The model allows the design of a magnetic, field-flow fractionation (MFFF) system to separate nanoparticles by size.

  3. Plasma-Chemical Synthesis of Nanosized Powders-Nitrides, Carbides, Oxides, Carbon Nanotubes and Fullerenes

    International Nuclear Information System (INIS)

    In this article the plasma-chemical synthesis of nanosized powders (nitrides, carbides, oxides, carbon nanotubes and fullerenes) is reviewed. Nanosized powders - nitrides, carbides, oxides, carbon nanotubes and fullerenes have been successfully produced using different techniques, technological apparatuses and conditions for their plasma-chemical synthesis. (plasma technology)

  4. 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.

  5. 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...

  6. New approach for direct chemical synthesis of hexagonal Co nanoparticles

    Science.gov (United States)

    Abel, Frank M.; Tzitzios, Vasilis; Hadjipanayis, George C.

    2016-02-01

    In this paper, we explore the possibility of producing hexagonal Cobalt nanoparticles, with high saturation magnetization by direct chemical synthesis. The nanoparticles were synthesized by reduction of anhydrous cobalt (II) chloride by NaBH4 in tetraglyme at temperatures in the range of 200-270 °C under a nitrogen-hydrogen atmosphere. The reactions were done at high temperatures to allow for the formation of as-made hexagonal cobalt. The size of the particles was controlled by the addition of different surfactants. The best magnetic properties so far were obtained on spherical hexagonal Co nanoparticles with an average size of 45 nm, a saturation magnetization of 143 emu/g and coercivity of 500 Oe. the saturation magnetization and coercivity were further improved by annealing the Co nanoparticles leading to saturation magnetization of 160 emu/g and coercivity of 540 Oe.

  7. Chemical Synthesis of Human Insulin-Like Peptide-6.

    Science.gov (United States)

    Wu, Fangzhou; Mayer, John P; Zaykov, Alexander N; Zhang, Fa; Liu, Fa; DiMarchi, Richard D

    2016-07-01

    Human insulin-like peptide-6 (INSL-6) belongs to the insulin superfamily and shares the distinctive disulfide bond configuration of human insulin. In this report we present the first chemical synthesis of INSL-6 utilizing fluorenylmethyloxycarbonyl-based (Fmoc) solid-phase peptide chemistry and regioselective disulfide bond construction protocols. Due to the presence of an oxidation-sensitive tryptophan residue, two new orthogonal synthetic methodologies were developed. The first method involved the identification of an additive to suppress the oxidation of tryptophan during iodine-mediated S-acetamidomethyl (Acm) deprotection and the second utilized iodine-free, sulfoxide-directed disulfide bond formation. The methodologies presented here offer an efficient synthetic route to INSL-6 and will further improve synthetic access to other multiple-disulfide-containing peptides with oxidation-sensitive residues. PMID:27259101

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

    International Nuclear Information System (INIS)

    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. - Highlights: • La1−xDyxCo1−yFeyO3 nanoparticles were prepared in the range 20–60 nm. • 12 Fold increase in DC resistivity achieved for La0.40Dy0.60Co0.40Fe0.60O3. • Paramagnetic to ferromagnetic behavior was observed for La1−xDyxCo1−yFeyO3 nanoparticles

  9. Synthesis and characterization of La2O3 nano particles for future CMOS applications

    International Nuclear Information System (INIS)

    This research paper deals with the preliminary studies on synthesis and characterization of lanthanum oxide or lanthana (La2O3) nano particles by chemical combustion using urea as fuel. The fuel urea is varied for different fuel to oxidizer ratios (O/F) or Ψ. The starting material (oxidizer) is the lanthanum nitrate (La(NO3)3.6H2O) and fuel as urea. The synthesized lanthana nano particles were characterized by X-ray diffraction (XRD) for crystal structure analysis, scanning electron microscopy (SEM) for morphological and particle size determination. (author)

  10. Laser ablation synthesis and spectral characterization of ruby nanoparticles

    Science.gov (United States)

    Baranov, M. S.; Bardina, A. A.; Savelyev, A. G.; Khramov, V. N.; Khaydukov, E. V.

    2016-04-01

    The laser ablation method was implemented for synthesis of ruby nanoparticles. Nanoparticles were obtained by nanosecond ablation of bulk ruby crystal in 10% ethanol water solution. The nanoparticles enable water colloid stability and exhibit narrow photoluminescent line at 694 nm when pumped at blue-green spectral range. The ruby nanoparticles were characterized by SEM and Z-sizer.

  11. 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.

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

    DEFF Research Database (Denmark)

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

    2009-01-01

    The synthesis and biophysical characterization of four prodrug ether phospholipid conjugates are described. The lipids are prepared from the anticancer drug chlorambucil and have C16 and C18 ether chains with phosphatidylcholine or phosphatidylglycerol headgroups. All four prodrugs have the abili...

  13. 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.

  14. Protein synthesis by native chemical ligation: Expanded scope by using straightforward methodology

    OpenAIRE

    Tilman M Hackeng; Griffin, John H.; Dawson, Philip E.

    1999-01-01

    The total chemical synthesis of proteins has great potential for increasing our understanding of the molecular basis of protein function. The introduction of native chemical ligation techniques to join unprotected peptides next to a cysteine residue has greatly facilitated the synthesis of proteins of moderate size. Here, we describe a straightforward methodology that has enabled us to rapidly analyze the compatibility of the native chemical ligation strategy for X–Cys ligation sites, where X...

  15. SYNTHESIS OF CARBON NANOSTRUCTURES BY PLASMA ENHANCED CHEMICAL VAPOUR DEPOSITION AT ATMOSPHERIC PRESSURE

    OpenAIRE

    Jašek Ondřej; Synek Petr; Zajíčková Lenka; Eliáš Marek; Kudrle Vít

    2010-01-01

    Carbon nanostructures present leading field in nanotechnology research. Wide range of chemical and physical methods was used for carbon nanostructures synthesis including arc discharges, laser ablation and chemical vapour deposition. Plasma enhanced chemical vapour deposition (PECVD) with its application in modern microelectronics industry became soon target of research in carbon nanostructures synthesis. The selection of the ideal growth process depends on the application. Most of PECVD tech...

  16. Synthesis and characterization of hybrid nanostructures

    Directory of Open Access Journals (Sweden)

    Taleb Mokari

    2011-05-01

    Full Text Available There has been significant interest in the development of multicomponent nanocrystals formed by the assembly of two or more different materials with control over size, shape, composition, and spatial orientation. In particular, the selective growth of metals on the tips of semiconductor nanorods and wires can act to couple the electrical and optical properties of semiconductors with the unique properties of various metals. Here, we outline our progress on the solution-phase synthesis of metal-semiconductor heterojunctions formed by the growth of Au, Pt, or other binary catalytic metal systems on metal (Cd, Pb, Cu-chalcogenide nanostructures. We show the ability to grow the metal on various shapes (spherical, rods, hexagonal prisms, and wires. Furthermore, manipulating the composition of the metal nanoparticles is also shown, where PtNi and PtCo alloys are our main focus. The magnetic and electrical properties of the developed hybrid nanostructures are shown.

  17. Chemical synthesis of superconducting MgB2 nanopowder

    International Nuclear Information System (INIS)

    Highlights: • MgB2 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 MgB2 filaments. - Abstract: Superconducting MgB2 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 MgB2 powder was evaluated to be 33 nm. The superconducting transition temperature of the MgB2 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

  18. 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). PMID:24982609

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

    Directory of Open Access Journals (Sweden)

    Seyed Abolghasem Kahani

    2014-01-01

    Full Text Available 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.

  20. Synthesis and optical properties of copper nanoparticles prepared by a chemical reduction method

    International Nuclear Information System (INIS)

    Copper nanoparticles, due to their interesting properties, low cost preparation and many potential applications in catalysis, cooling fluid or conductive inks, have attracted a lot of interest in recent years. In this study, copper nanoparticles were synthesized through the chemical reduction of copper sulfate with sodium borohydride in water without inert gas protection. In our synthesis route, ascorbic acid (natural vitamin C) was employed as a protective agent to prevent the nascent Cu nanoparticles from oxidation during the synthesis process and in storage. Polyethylene glycol (PEG) was added and worked both as a size controller and as a capping agent. Cu nanoparticles were characterized by Fourier transform infrared (FT-IR) spectroscopy to investigate the coordination between Cu nanoparticles and PEG. Transmission electron microscopy (TEM) and UV–vis spectrometry contributed to the analysis of size and optical properties of the nanoparticles, respectively. The average crystal sizes of the particles at room temperature were less than 10 nm. It was observed that the surface plasmon resonance phenomenon can be controlled during synthesis by varying the reaction time, pH, and relative ratio of copper sulfate to the surfactant. The surface plasmon resonance peak shifts from 561 to 572 nm, while the apparent color changes from red to black, which is partly related to the change in particle size. Upon oxidation, the color of the solution changes from red to violet and ultimately a blue solution appears

  1. 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.

  2. 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.

  3. 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

  4. Synthesis and characterization of two dimensional transition metal dichalcogenides

    Science.gov (United States)

    Gao, Jian

    Two-dimensional transition metal dichalcogenides (TMDs) are an emerging class of atomically thin semiconductors that show potential in next-generation electronics, optoelectronics, and energy storage batteries. The successful synthesis and doping of TMDs is the key to their applications. I have synthesized monolayer MoS2, WS2, and multilayer ReS2 flakes by CVD, and studied an unprecedented one-pot synthesis for transition-metal substitution doping in large-area, synthetic monolayer TMDs. Electron microscopy, optical and electronic transport characterization and ab initio calculations indicate that our doping strategy preserves the attractive qualities of TMD monolayers, including semiconducting transport and strong direct-gap luminescence. The Re doping of MoS2 greatly improve the contact quality (one of the biggest issue in TMDs) and the FET shows Ohmic contact even at low temperature (4K). These results potentially enables next-generation optoelectronic technology in the atomically-thin regime. Besides, TMDs are generally considered to be 'air-stable', however, we have found that they exhibit poor long-term stability in air in morphology, chemical states, photo-emission, and demonstrated a potential solution to this problem by encapsulation of the monolayer sheet with transparent parylene C. Synthetic TMDs tend to grow parallel to the growth substrate, however, high performance energy conversion and storage devices prefer flakes with high exposed surface area. Therefore by choosing the right precursors and appropriate tuning of the CVD growth conditions, we have grown vertical ReS2 nanosheets on various growth substrates. We show that these structural features of the vertically grown ReS2 sheets can be exploited to significantly improve their performance as electrochemical catalysts in Lithium-Sulfur (Li-S) batteries and in hydrogen evolution reactions (HER). After 300 cycles, the specific capacity of the Li-S battery with vertical-ReS2 catalyst is retained above

  5. 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...

  6. Synthesis of the heaviest chemical elements - results and perspectives

    Energy Technology Data Exchange (ETDEWEB)

    Herrmann, G.

    1988-11-01

    All 17 artificially produced elements heavier than uranium were discovered by nuclear-chemical synthesis. The three heaviest ones - elements 107, 108 and 109 - were snythesized at the heavy-ion accelerator UNILAC in Darmstadt by nuclear fusion from the heaviest stable nuclei, lead-208 and bismuth-209, and the most neutron-rich stable isotopes of chromium and iron: element 107 from bismuth-209 (atomic number Z=83) and chromium-54 (Z=24), element 108 from lead-208 (Z=82) and iron-58 (Z=26), and element 109 from bismuth-209 and iron-58. The first isotopes detected were those with mass numbers 262 (Z=107), 265 (Z=108) and 266 (Z=109); these nuclei are short-lived ed -emitters with half-lives of 8.2 ms, 1.8 ms and 3.4 ms, respectively. The yields of these reactions are extremely small; only three atoms of element 109 have ever been observed. Experiments to synthesize element 110 have given ambiguous results. All attempts to detect the 'superheavy' elements with proton numbers near Z=114 and neutron numbers near N=184 have thus far failed. These elements have been predicted theoretically, and many attempts to synthesize them have been made, e.g. at UNILAC by fusion of calcium-48 (Z=20) with curium-248 (Z=96), or by transference of protons in the collision of two very heavy nuclei such as uranium-238 (Z=92). Surprisingly, the heaviest known nuclei are far more stable toward spontaneous fission into two fragments than was expected, but their synthesis is strongly hindered - much more than was initially anticipated. It is this hindrance rather than the decreasing nuclear stability which seems to presently limit the extent of the periodic table: even heavier elements should be able to exist, but no way has yet been found to produce them.

  7. Synthesis of chiral polyaniline films via chemical vapor phase polymerization

    DEFF Research Database (Denmark)

    Chen, J.; Winther-Jensen, B.; Pornputtkul, Y.; West, K.; Kane-Maquire, L.; Wallace, G.G.

    2006-01-01

    Electrically and optically active polyaniline films doped with (1)-(-)-10- camphorsulfonic acid were successfully deposited on nonconductive substrates via chemical vapor phase polymerization. The above polyaniline/ R- camphorsulfonate films were characterized by electrochemical and physical...... methods, such as cyclic voltammetry (CV), UV- vis spectroscopy, four- point probe conductivity measurement, Raman spectroscopy, circular dichroism spectroscopy, and scanning electron microscopy. The polyaniline films grown by this method not only showed high electrochemical activity, supported by CV and...... Raman spectrum, but also exhibited optical activity corresponding to the polymer chains as observed by circular dichroism spectra. (c) 2005 The Electrochemical Society....

  8. Synthesis of Colloidal Ruthenium Nanocatalyst by Chemical Reduction Method

    Directory of Open Access Journals (Sweden)

    R. G. Patharkar

    2013-01-01

    Full Text Available Colloidal ruthenium nanoparticles were prepared by chemical reduction of ruthenium trichloride (RuCl3 using sodium borohydrate (NaBH4 as reducing agent and sodium dodecyl sulfate (SDS as a stabilizer. Size and size distribution of synthesized colloidal Ru nanoparticles were studied by varying different parameters such as molar ratio (MR of SDS/RuCl3, NaBH4/RuCl3, effects of different stabilizers, and reducing agents. Prepared nanoparticles were characterized by transmission electron microscope (TEM and dynamic light scattering (DLS. Stability of colloidal nanoparticles was detected by Turbiscan. Stable Ru nanoparticles were dispersed on γ-Al2O3 to prepare Ru/γ-Al2O3 catalyst. This catalyst was characterized by X-ray Diffraction (XRD and transmission electron microscope (TEM.

  9. Synthesis and characterization of luminescent oxide nanocrystals

    Science.gov (United States)

    Seo, Sooyeon

    Oxide nanocrystals with controlled geometries exhibit unique shape dependent optical and structural properties. Shape-controlled synthesis of rare earth doped gadolinium oxide (Gd2O3: Eu3+, Tb3+ or Er3+) and zinc gallate (ZnGa2O 4:Eu3+) nanocrystals by non-hydrolytic high temperature (˜300°C) methods are reported. Various shapes of Gd2O 3 nanocrystals were synthesized, including spheres and plates and advanced shapes such as curved rods and triangles. The nanocrystal shape was shown to be a function of the synthesis parameters, such as metal precursors (acetate, acetyl acetonate, chloride or octanoate) and surfactant type (tri-octyl phosphine oxide-TOPO, or hexadecanediol-HDD) and concentration (metal precursor: surfactant molar ratios of 1:2 to 1:5), as well as heating rate (5-25°C/min.) between pre-heat (200°C) and reaction (290°C) temperatures. The effects of these parameters upon nanocrystal shape were explained based on nucleation and growth of oxide nanocrystals. The photoluminescence intensity from Gd 2O3:Eu3+ was shown to increase as the concentration of dopant incorporated into the nanocrystals increased. The doping efficiency, defined to be the percentage of dopant incorporated into the nanocrystals, ranged from 0.57-6.1 mol%, was a function of shape of the Gd2O 3: Eu3 and was discussed in terms of the rate of reaction, product yield and crystal structure. To be used for labeling biomolecules such as DNA, RNA, or proteins, water soluble luminescent nanocrystals are required. Doped Gd2O 3 nanocrystals prepared by the non-hydrolytic hot solution method are hydrophobic and are not soluble in water due to organic surfactant encapsulation. A general strategy to convert hydrophobic luminescent nanocrystals (e.g. Gd 2O3) to water soluble particles by over-coating the hydrophobic surface with amphiphilic polymers is reported. Specifically, octylamine modified surfaces were coated with poly (acrylic acid) and water dispersions of Gd 2O3: Eu3+ were still

  10. 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.

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

    OpenAIRE

    Russo, Carmela

    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...

  12. Green synthesis and characterization of palladium nanoparticles and its conjugates from solanum trilobatum leaf extract

    Institute of Scientific and Technical Information of China (English)

    Amarnath Kanchana; Saveetha Devarajan

    2010-01-01

    An important area of research in nanotechnology deals with the synthesis of nanoparticles of different chemical compositions, sizes and controlled monodispersity. Currently, there is a growing need to develop environmentally benign nanoparticle synthesis in which no toxic chemicals are used in the synthesis protocol. Palladium nanoparticles (PdNp) are of interest because of their catalytic properties and affinity for hydrogen. Our protocol for the phyto-synthesis of PdNp under moderate pH and room temperature offers a new means to develop environmentally benign nanoparticles. Solanum trilobatum is enlightened in our present study as it is enriched with phytochemicals to reduce palladium chloride ions. Poly MVA a dietary supplement based on the nontoxic chemotherapeutic lipoic acid-palladium complex (LA-Pd) is been hypothesized as the new paradigm of cancer therapy. Hence forth we successfully conjugated lipoic acid (S-PdNp-LA) and vitamins (S-PdNp-Vitamin-LA) to palladium nanoparticles synthesised from Solanum trilobatum leaf extract. These nanoparticles (S-PdNp, S-PdNp-LA, S-PdNp-Vitamin-LA) were characterized with UV-Vis Spectroscopy, SEM and FTIR analysis, which revealed that S-PdNp are polydisperse and of different morphologies ranging from 60~70 nm (S-PdNp), 65~80 nm (S-PdNp-LA) and 75~100 nm (S-PdNp-Vitamin-LA) in size.

  13. Novel double prodrugs of the iron chelator N,N'-bis(2-hydroxybenzyl)ethylenediamine-N,N'-diacetic acid (HBED): Synthesis, characterization, and investigation of activation by chemical hydrolysis and oxidation.

    Science.gov (United States)

    Thiele, Nikki A; Abboud, Khalil A; Sloan, Kenneth B

    2016-08-01

    The development of iron chelators suitable for the chronic treatment of diseases where iron accumulation and subsequent oxidative stress are implicated in disease pathogenesis is an active area of research. The clinical use of the strong chelator N,N'-bis(2-hydroxybenzyl)ethylenediamine-N,N'-diacetic acid (HBED) and its alkyl ester prodrugs has been hindered by poor oral bioavailability and lack of conversion to the parent chelator, respectively. Here, we present novel double prodrugs of HBED that have the carboxylate and phenolate donors of HBED masked with carboxylate esters and boronic acids/esters, respectively. These double prodrugs were successfully synthesized as free bases (7a-f) or as dimesylate salts (8a-c,e), and were characterized by (1)H, (13)C, and (11)B NMR; MP; MS; and elemental analysis. The crystal structure of 8a was solved. Three of the double prodrugs (8a-c) were selected for further investigation into their abilities to convert to HBED by stepwise hydrolysis and H2O2 oxidation. The serial hydrolysis of the pinacol and methyl esters of N,N'-bis(2-boronic acid pinacol ester benzyl)ethylenediamine-N,N'-diacetic acid methyl ester dimesylate (8a) was verified by LC-MS. The macro half-lives for the hydrolyses of 8a-c, measured by UV, ranged from 3.8 to 26.3 h at 37 °C in pH 7.5 phosphate buffer containing 50% MeOH. 9, the product of hydrolysis of 8a-c and the intermediate in the conversion pathway, showed little-to-no affinity for iron or copper in UV competition experiments. 9 underwent a serial oxidative deboronation by H2O2 in N-methylmorpholine buffer to generate HBED (k = 10.3 M(-1) min(-1)). The requirement of this second step, oxidation, before conversion to the active chelator is complete may confer site specificity when only localized iron chelation is needed. Overall, these results provide proof of principle for the activation of the double prodrugs by chemical hydrolysis and H2O2 oxidation, and merit further investigation into the

  14. Synthesis Array Topology Metrics in Location Characterization

    Science.gov (United States)

    Shanmugha Sundaram, GA

    2015-08-01

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

  15. Synthesis and characterization of melanin in DMSO

    Science.gov (United States)

    Bronze-Uhle, Erika S.; Batagin-Neto, Augusto; Xavier, Pedro H. P.; Fernandes, Nicole I.; de Azevedo, Eduardo R.; Graeff, Carlos F. O.

    2013-09-01

    Recently soluble melanin derivatives have been obtained by a synthetic procedure carried out in DMSO (D-melanin). In this work a comparative study of the structural characteristics of synthetic melanin derivatives obtained by oxidation of L-DOPA in H2O and DMSO are presented. To this end, Fourier-transform infrared spectroscopy as well as proton and carbon nuclear magnetic resonance techniques has been employed. In addition, aging effects have been investigated for D-melanin. The results suggest that sulfonate groups (-SO2CH3) from the oxidation of DMSO, are incorporated into melanin, which confers protection to the phenolic hydroxyl group present in its structure. The solubility of D-melanin in DMSO is attributed to the presence of these groups. When D-melanin is left in air for long time periods, the sulfonate groups leave the structure, and an insoluble compound is obtained. NaOH and water have been used, in order to accelerate the release of the sulfonate groups attached to D-melanin, thereby corroborating the proposed structure and the synthesis mechanism.

  16. The synthesis and characterization of polydibromoacetylene

    OpenAIRE

    Leben, Stanko; Janevski, Aco; Sebenik, Anton; Osredkar, Uci

    1992-01-01

    Polydibromoacetylenes were synthesized under different polymerization conditions and with Al-Ti coordinative catalysts. For the characterization of the polymers and for the study of the correlation between polymerization conditions and properties of the polymers, 13C MAS NMR, ESR and UV spectroscopies were used. The electrical conductivity of the polymers was measured in dependence on temperature. The energy gap decreased with increased crystallinity. As compared to polyacetylene the conducti...

  17. Uranium and thorium based phosphate matrix: synthesis, characterizations and lixiviation

    International Nuclear Information System (INIS)

    In the framework of the search for a ceramic material usable in the radioactive waste storage, uranium and thorium phosphates have been investigated. Their experimental synthesis conditions have been entirely reviewed, they lead to the preparation of four new compounds: U(UO2)(PO4)2, U2O(PO4)2, UCIPO4, 4H2O, and Th4(PO4)4P2O7. Experimental evidenced are advanced for non existent compounds such as: U3(PO4)4, U2O3P2O7 and Th3 (PO4)4. Characterization by several techniques (X-rays and neutron powder diffractions, UV-Visible and Infra-red spectroscopies, XPS,...) were performed. The ab initio structure determination of U(UO2)(PO4)2 has been achieved by X-rays and refined by neutron diffractions. Through its physico-chemical analysis, we found that this compound was a new mixed valence uranium phosphate in which U4+ and UO22+ ions are ordered in pairs along parallel chains according to a new type of arrangement. Reaction mechanism, starting from UCIPO4, 4H2O and based on redox processes of uranium in solid state was set up. From two main matrices U(UO2)(PO4)2 and Th4(PO4)4P2O7, solid solutions were studied. They consist of replacement of U(IV) by Th(IV) and reversely. The leaching tests on pure, loaded and doped matrices were performed in terms of storage time, pH of solutions, and determined by the use of solids labelled with 230U or by the measurement of uranyl concentration by Laser-Induced Time-Resolved Spectro-fluorimetry. Average concentration of uranium in the liquid phase is around 10-4 M to 10-6 M. Taking into account the very low solubilities of the studied phosphate ceramics, we estimated their chemical performances promising as an answer to the important nuclear waste problem, if we compare them to the glasses used at the present time. (author)

  18. Size-controlled synthesis of transition metal nanoparticles through chemical and photo-chemical routes

    Science.gov (United States)

    Tangeysh, Behzad

    The central objective of this work is developing convenient general procedures for controlling the formation and stabilization of nanoscale transition metal particles. Contemporary interest in developing alternative synthetic approaches for producing nanoparticles arises in large part from expanding applications of the nanomaterials in areas such as catalysis, electronics and medicine. This research focuses on advancing the existing nanoparticle synthetic routes by using a new class of polymer colloid materials as a chemical approach, and the laser irradiation of metal salt solution as a photo-chemical method to attain size and shape selectivity. Controlled synthesis of small metal nanoparticles with sizes ranging from 1 to 5nm is still a continuing challenge in nanomaterial synthesis. This research utilizes a new class of polymer colloid materials as nano-reactors and protective agents for controlling the formation of small transition metal nanoparticles. The polymer colloid particles were formed from cross-linking of dinegatively charged metal precursors with partially protonated poly dimethylaminoethylmethacrylate (PDMAEMA). Incorporation of [PtCl6]2- species into the colloidal particles prior to the chemical reduction was effectively employed as a new strategy for synthesis of unusually small platinum nanoparticles with narrow size distributions (1.12 +/-0.25nm). To explore the generality of this approach, in a series of proof-of-concept studies, this method was successfully employed for the synthesis of small palladium (1.4 +/-0.2nm) and copper nanoparticles (1.5 +/-0.6nm). The polymer colloid materials developed in this research are pH responsive, and are designed to self-assemble and/or disassemble by varying the levels of protonation of the polymer chains. This unique feature was used to tune the size of palladium nanoparticles in a small range from 1nm to 5nm. The procedure presented in this work is a new convenient room temperature route for synthesis of

  19. 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. PMID:27077333

  20. Synthesis of oxide superconductors by soft-chemical techniques

    International Nuclear Information System (INIS)

    Our recent works on the synthesis of oxide superconductors using soft-chemical techniques are reviewed. First, Li-intercalation into layered perovskites has been carried out. We have found new Li-intercalated superconductors of the Ruddlesden-Popper phase of LixSr2CuO2X2 (X = Br, I) with Tc = 7-8 K and the Dion-Jacobson phase of LixASr2Nb3O10 (A = Rb, Cs) with Tc ∼6 K. However, no superconductivity has appeared in Aurivillius phases of LixBi4Ti3O10 and LixBi2MO6 (M = Mo, W). Next, we have succeeded in preparing insulating La2CuO4 with the Nd2CuO4-type (T') structure and superconducting Ba0.6K0.4BiO3 by the direct precipitation from molten alkaline-metal hydroxides at a temperature as low as 260-350 deg. C

  1. 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.

  2. Synthesis and characterization of porous calcium phosphate

    International Nuclear Information System (INIS)

    The porous calcium phosphate was prepared by the continuous precipitation method using Ca(NO3)2.4H2O and NH4H2PO4 salts. The synthesized material was structurally and superficially characterized using the XRD, BET, IR TGA and SEM techniques. The obtained inorganic material was identified as calcium phosphate that presents a great specific area for what can be efficiently used as adsorbent material for adsorption studies in the radioactive wastes treatment present in aqueous solution. (Author)

  3. Synthesis and characterization of aminated lignin.

    Science.gov (United States)

    Pan, Hong; Sun, Gang; Zhao, Tao

    2013-08-01

    Amination of lignin can bring reactive amino groups onto the natural polymer and enable it to be employed in engineering materials. The amination reaction was successfully implemented after some of the hydroxyl groups on lignin were epoxidized. The resulted products showed a great quantity of primary amine group and secondary amine group which can be used as curing agents of epoxy resin. The results revealed that several factors including reaction temperature and time, as well as ratios of compounds, could influence the epoxidation and amination reactions. The resulted products were characterized by FT-IR spectra, (1)H NMR, (13)C NMR, element analysis, XPS and thermogravimetry analysis. PMID:23618954

  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. Synthesis and characterization of organically linked ZnO nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Chory, Christine; Riedel, Ingo; Parisi, Juergen [Energy and Semiconductor Research Laboratory (EHF), University of Oldenburg, Carl-von Ossietzky-Strasse 9-11, 26129 Oldenburg (Germany); Kruska, Carsten; Heimbrodt, Wolfram [Department of Physics and Material Sciences Center, Philipps-University Marburg, Renthof 5, 35032 Marburg (Germany); Feser, Clemens [NEXT ENERGY - EWE Research Centre for Energy Technology e.V., Carl-von Ossietzky-Strasse 15, 26129 Oldenburg (Germany); Beenken, Wichard J.D. [Department of Theoretical Physics I, Ilmenau University of Technology, Weimarer Strasse 25, 98693 Ilmenau (Germany); Hoppe, Harald [Department of Experimental Physics I, Ilmenau University of Technology, Weimarer Strasse 32, 98693 Ilmenau (Germany)

    2012-11-15

    We report on the solution-based synthesis and characterization of three-dimensional networks of ZnO nanoparticles where the formation of structures is achieved by covalently linking the nanocrystals with bifunctional organic ligands. The colloidal synthesis will be presented with application of two ligands that vary in size and binding sites. Furthermore we report on structural characterization of dried powders and thin films by means of X-ray diffraction and electron microscopy in order to examine the regularity of the structures. We also present first investigations of the optical properties and electrical conductance behavior in lateral direction of the differently linked hybrid ZnO networks. (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  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 POLYBENZOXAZINE CONTAINING PHOSPHORUS

    Institute of Scientific and Technical Information of China (English)

    Ting-ting Zhang; Wei-wei Men; Ying Liu; Zai-jun Lu

    2012-01-01

    The novel benzoxazine monomer containing phosphorus has been synthesized based on multifunctional amine route from bis(4-aminophenyl)phenylphosphate,p-cresol and formaldehyde.Subsequently,the benzoxazine monomer was thermo-cured into polybenzoxazine containing phosphorus.The chemical structures were identified by nuclear magnetic resonance (NMR),Fourier transform infrared spectroscopy (FT-IR).The curing reaction was monitored by differential scanning calorimetry (DSC) and FT-IR.The thermal and flame-retardant properties of obtained polybenzoxazine were evaluated by dynamic mechanical thermal analysis (DMA),thermal gravimetric analysis (TGA) and oxygen index meter,respectively.The results show that the novel polybenzoxazine has high limiting oxygen index (38.1) and glass transition temperature (232℃).

  8. 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

  9. 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

  10. Synthesis and electrochemical characterization of substituted indolizine carboxylates

    OpenAIRE

    Soare Maria-Laura; Ungureanu Eleonora-Mihaela; Georgescu Emilian; Birzan Liviu

    2013-01-01

    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 structur...

  11. 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.

  12. Synthesis and characterization of new amino acyl-4-thiazolidones

    Directory of Open Access Journals (Sweden)

    Ana Cristina Lima Leite

    2007-04-01

    Full Text Available A series of heterocyclic compounds with a 4-thiazolidone nucleus and amino acyl moiety were synthesized by protection reaction of thiosemicarbazide using the symmetrical anhydride (Boc2O and cyclization with chloroacetic acid under mild conditions. Trifluoroacetic acid was used to obtain 4-thiazolidone and the alpha-amino acid condensation reactions were carried out using strategies for peptide synthesis. The characterization of this new class of compounds was performed using IR and ¹H-NMR spectroscopy.

  13. Synthesis and Characterization of Amorphous Carbide-based Thin Films

    OpenAIRE

    Folkenant, Matilda

    2015-01-01

    In this thesis, research on synthesis, structure and characterization of amorphous carbide-based thin films is presented. Crystalline and nanocomposite carbide films can exhibit properties such as high electrical conductivity, high hardness and low friction and wear. These properties are in many cases structure-related, and thus, within this thesis a special focus is put on how the amorphous structure influences the material properties. Thin films within the Zr-Si-C and Cr-C-based systems hav...

  14. Synthesis, characterization and potential applications of iron-platinum nanoparticles

    Science.gov (United States)

    Nandwana, Vikas

    Monodisperse FePt nanoparticles with controlled size and geometry have drawn great attention in the last decade for fundamental scientific studies and for their potential applications in advanced materials and devices such as ultra-high-density magnetic recording media, exchange-coupled nanocomposite magnets, biomedicines and nanodevices. This dissertation focuses on the synthesis and characterization of FePt nanoparticles and their use in potential applications. The FePt nanoparticles of different size (2 to 16 nm) and shape (spherical, cubic, rod) were synthesized by a chemical solution method. The size and shape of these particles were controlled by adjusting reaction parameters. The as-synthesized FePt nanoparticles have chemically disordered fcc structure and are superparamagnetic at room temperature. Upon heat treatment the nanoparticles were transformed into ordered L10 structure, and high coercivity up to 27 kOe was achieved. Magnetic properties of annealed FePt nanoparticles including magnetization and coercivity were strongly dependent on particle size, shape, composition and annealing temperature. FePt/Fe3O4 bimagnetic nanoparticles with two different morphologies, core/shell and heterodimer, were prepared by coating or attaching Fe3O4 on surface of FePt nanoparticles. The size of FePt and Fe3O4 was tuned very finely to obtain most effective exchange coupling. The heterodimer nanoparticles resulted in relatively poor magnetic properties compared to the core/shell nanoparticles due to insufficient exchange coupling. By optimizing the dimensions of the FePt and Fe3O 4 in core/shell bimagnetic nanoparticles, energy products up to 17.8 MGOe were achieved. FePt/Fe3O4 core/shell and FePt+Fe3O 4 mixed nanoparticles with similar magnetic properties were compacted under 2.0 GPa at 400°C, 500°C and 600°C. A density up to 84% of the full density was achieved. After annealing at 650°C in forming gas, the FePt/Fe3O4 compacted samples were converted into L10 Fe

  15. Synthesis and characterization of tannin grafted polycaprolactone.

    Science.gov (United States)

    Song, Ping; Jiang, Suchen; Ren, Yajun; Zhang, Xue; Qiao, Tiankui; Song, Xiaofeng; Liu, Qimin; Chen, Xuesi

    2016-10-01

    Tannin and biodegradable polyester have attracted increasing interest for biomedical applications. To improve their compatibility, a novel tannin grafted polycaprolactone (TA-g-PCL) has been synthesized via ring-opening polymerization reaction. The structure of the product is characterized with FTIR, (1)H NMR and GPC. GPC results show that the experimental molecular weight is far less than the theoretical due to complicated stereo structure and large steric hindrance of tannic molecule, but the polydispersity of the product is narrow. At 115.76:1 of molar ratio of CL to tannin, molecular weight of the product reaches the maximum. Thermodynamics properties and dissolubility of TA-g-PCL are closely related to its molecular weight. With PCL molecular chain grows, TA-g-PCL changes from amorphous form to crystalline structure, and its dissolubility in chloroform is also enhanced significantly. PMID:27388129

  16. 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,...

  17. Synthesis and characterization of biocompatible magnetic glyconanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Kekkonen, Viktoria; Lafreniere, Nelson [Department of Chemistry and Biochemistry, Biomolecular Sciences Program, Laurentian University, 935, Ramsey Lake Road, Sudbury, ON, P3E2C6 (Canada); Ebara, Mitsuhiro; Saito, Atsuhiro; Sawa, Yoshiki [Medical Center for Translational Research, Osaka University Hospital, 2-15, Yamada-oka, Suita, Osaka 565-0871 (Japan); Narain, Ravin [Department of Chemistry and Biochemistry, Biomolecular Sciences Program, Laurentian University, 935, Ramsey Lake Road, Sudbury, ON, P3E2C6 (Canada)], E-mail: rnarain@laurentian.ca

    2009-05-15

    Magnetic glyconanoparticles were synthesized via the co-precipitation method. Iron (II) and iron (III) chloride were co-precipitated out of solution by the addition of ammonium hydroxide in an aqueous solution containing carbohydrate stabilizers such as D-gluconic acid, lactobionic acid and Ficoll at 75-80 deg. C. Stable magnetic glyconanoparticles were formed in a simple and direct process. Dynamic light scattering and transmission electron microscopy were used to characterize the surface-coated magnetic nanoparticles. In vitro cell viability studies of the glyconanoparticles were conducted with the mouse fibroblast cell lines. The magnetic glyconanoparticles revealed to be non-toxic at a concentration as high as 0.1 mg/mL.

  18. Synthesis and characterization of biocompatible magnetic glyconanoparticles

    Science.gov (United States)

    Kekkonen, Viktoria; Lafreniere, Nelson; Ebara, Mitsuhiro; Saito, Atsuhiro; Sawa, Yoshiki; Narain, Ravin

    2009-05-01

    Magnetic glyconanoparticles were synthesized via the co-precipitation method. Iron (II) and iron (III) chloride were co-precipitated out of solution by the addition of ammonium hydroxide in an aqueous solution containing carbohydrate stabilizers such as D-gluconic acid, lactobionic acid and Ficoll ® at 75-80 °C. Stable magnetic glyconanoparticles were formed in a simple and direct process. Dynamic light scattering and transmission electron microscopy were used to characterize the surface-coated magnetic nanoparticles. In vitro cell viability studies of the glyconanoparticles were conducted with the mouse fibroblast cell lines. The magnetic glyconanoparticles revealed to be non-toxic at a concentration as high as 0.1 mg/mL.

  19. 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.

  20. 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.

  1. 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.

  2. Synthesis and characterization of biocompatible magnetic glyconanoparticles

    International Nuclear Information System (INIS)

    Magnetic glyconanoparticles were synthesized via the co-precipitation method. Iron (II) and iron (III) chloride were co-precipitated out of solution by the addition of ammonium hydroxide in an aqueous solution containing carbohydrate stabilizers such as D-gluconic acid, lactobionic acid and Ficoll at 75-80 deg. C. Stable magnetic glyconanoparticles were formed in a simple and direct process. Dynamic light scattering and transmission electron microscopy were used to characterize the surface-coated magnetic nanoparticles. In vitro cell viability studies of the glyconanoparticles were conducted with the mouse fibroblast cell lines. The magnetic glyconanoparticles revealed to be non-toxic at a concentration as high as 0.1 mg/mL.

  3. Expanding the chemical toolbox for the synthesis of large and uniquely modified proteins

    Science.gov (United States)

    Bondalapati, Somasekhar; Jbara, Muhammad; Brik, Ashraf

    2016-05-01

    Methods to prepare proteins that include a specific modification at a desired position are essential for understanding their cellular functions and physical properties in living systems. Chemical protein synthesis, which relies on the chemoselective ligation of unprotected peptides, enables the preparation of modified proteins that are not easily fabricated by other methods. In contrast to recombinant approaches, chemical synthesis can be used to prepare protein analogues such as D-proteins, which are useful in protein structure determination and the discovery of novel therapeutics. Post-translationally modifying proteins is another example where chemical protein synthesis proved itself as a powerful approach for preparing samples with high homogeneity and in workable quantities. In this Review, we discuss the basic principles of the field, focusing on novel chemoselective peptide ligation approaches such as native chemical ligation and the recent advances based on this method with a proven record of success in the synthesis of highly important protein targets.

  4. 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.

  5. Synthesis and characterization of a pH responsive folic acid functionalized polymeric drug delivery system.

    Science.gov (United States)

    Li, Xia; McTaggart, Matt; Malardier-Jugroot, Cecile

    2016-01-01

    We report the computational analysis, synthesis and characterization of folate functionalized poly(styrene-alt-maleic anhydride), PSMA for drug delivery purpose. The selection of the proper linker between the polymer and the folic acid group was performed before conducting the synthesis using Density Functional Theory (DFT). The computational results showed the bio-degradable linker 2, 4-diaminobutyric acid, DABA as a good candidate allowing flexibility of the folic acid group while maintaining the pH sensitivity of PSMA, used as a trigger for drug release. The synthesis was subsequently carried out in multi-step experimental procedures. The functionalized polymer was characterized using InfraRed spectroscopy, Nuclear Magnetic Resonance and Dynamic Light Scattering confirming both the chemical structure and the pH responsiveness of PSMA-DABA-Folate polymers. This study provides an excellent example of how computational chemistry can be used in selection process for the functional materials and product characterization. The pH sensitive polymers are expected to be used in delivering anti-cancer drugs to solid tumors with overly expressed folic acid receptors. PMID:27183249

  6. 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.

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

    International Nuclear Information System (INIS)

    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. Nutrient-substituted hydroxyapatites: synthesis and characterization

    Science.gov (United States)

    Golden, D. C.; Ming, D. W.

    1999-01-01

    Incorporation of Mg, S, and plant-essential micronutrients into the structure of synthetic hydroxyapatite (HA) may be advantageous for closed-loop systems, such as will be required on Lunar and Martian outposts, because these apatites can be used as slow-release fertilizers. Our objective was to synthesize HA with Ca, P, Mg, S, Fe, Cu, Mn, Zn, Mo, B, and Cl incorporated into the structure, i.e., nutrient-substituted apatites. Hydroxyapatite, carbonate hydroxyapatite (CHA), nutrient-substituted hydroxyapatite (NHA), and nutrient-substituted carbonate hydroxyapatite (NCHA) were synthesized by precipitating from solution. Chemical and mineralogical analysis of precipitated samples indicated a considerable fraction of the added cations were incorporated into HA, without mineral impurities. Particle size of the HA was in the 1 to 40 nm range, and decreased with increased substitution of nutrient elements. The particle shape of HA was elongated in the c-direction in unsubstituted HA and NHA but more spherical in CHA and NCHA. The substitution of cations and anions in the HA structure was confirmed by the decrease of the d[002] spacing of HA with substitution of ions with an ionic radius less than that of Ca or P. The DTPA-extractable Cu ranged from 8 to 8429 mg kg-1, Zn ranged from 57 to 1279 mg kg-1, Fe from 211 to 2573 mg kg-1, and Mn from 190 to 1719 mg kg-1, depending on the substitution level of each element in HA. Nutrient-substituted HA has the potential to be used as a slow-release fertilizer to supply micronutrients, S, and Mg in addition to Ca and P.

  9. 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).

  10. 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.

  11. Synthesis and characterization of biomorphic ceramics

    International Nuclear Information System (INIS)

    Biotemplating represents a recently developed technology for manufacturing of biomorphous ceramics from naturally grown plant structures. This approach allows the production of ceramic materials with cellular structure, where the microstructural features of the ceramic product are similar to the native plant. After processing, the biomorphic ceramic exhibits directed pore morphology in the micrometer range. Biomorphic SiC fibers were produced from bamboo by carbothermal reduction of SiO2 originally present in the bamboo structure. Bamboo pieces were heated up to 1500 deg C in argon to promote the reaction between carbon and silica. Biomorphic alumina, mullite and zirconia ceramics were manufactured via the sol-gel route by repeated infiltration of low viscous oxide precursors (sols) into rattan, pine and bamboo structures. The raw samples were pyrolyzed at 800 deg C in nitrogen for 1h and subsequently annealed at 1550 deg C in air. The microstructure and physical properties of the biomorphic ceramics were characterized by X-ray diffraction (XRD) and high temperature-XRD, scanning electron microscopy (SEM), porosimetry and picnometry. Thermal analysis (TGA/DTA) was performed on the infiltrated samples in order to evaluate the reactions and the total weight loss during the thermal process. The mechanical properties were evaluated by compressive strength tests. In contrast to conventional processed ceramic foam of similar porosity, the microstructure highly porous biomorphic ceramics shows uniaxial pore morphology with anisotropic properties. These properties are favorable for applications in catalyst support, filters or low-density heat insulation structures, or as biomaterials. (author)

  12. Synthesis of Silver-Doped Zinc Oxide Nanocomposite by Pulse Mode Ultrasonication and Its Characterization Studies

    OpenAIRE

    Siva Vijayakumar, T.; Karthikeyeni, S.; S Vasanth; Arul Ganesh; G Bupesh; Ramesh, R.; Manimegalai, M.; P Subramanian

    2013-01-01

    The synthesis of silver-doped zinc oxide (Ag:ZnO) nanocomposite material was achieved using a simple chemical coprecipitation method, in which 0.2 M zinc chloride and 0.001 M silver nitrate coprecipitated with 25% ammonia solution by pulse mode dispersion using ultrasonicator. The obtained silvery white precipitate was dried overnight at 110°C in hot air oven, and the powder was collected. The resulted Ag:ZnO nanocomposite was structurally and optically characterized using various techniques....

  13. Evolution of Fe species during the synthesis of over-exchanged Fe/ZSM5 obtained by chemical vapor deposition of FeCl3

    NARCIS (Netherlands)

    Battiston, AA; Bitter, JH; de Groot, FMF; Overweg, AR; Stephan, O; van Bokhoven, JA; Kooyman, PJ; van der Spek, C; Vanko, G; Koningsberger, DC

    2003-01-01

    The evolution of iron in over-exchanged Fe/ZSM5 prepared via chemical vapor deposition of FeCl3 was studied at each stage of the synthesis. Different characterization techniques (EXAFS, HR-XANES, Fe-57 Mossbauer spectroscopy, Al-27 NMR, EELS, HR-TEM, XRD, N-2 physisorption, and FTIR spectroscopy) we

  14. 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.

  15. CHEMICAL AND BIOLOGICAL CHARACTERIZATION OF LEACHATES FROM COAL SOLID WASTES

    Science.gov (United States)

    The report gives results of the chemical and mineralogical characterization of coal solid wastes. The wastes included three Lurgi gasification ashes, mineral residues from the SRC-1 and H-Coal liquefaction processes, two chars, two coal-cleaning residues, and a fly-ash-and-water-...

  16. 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...

  17. Synthesis, characterization, and photocatalytic properties of core/shell mesoporous silica nanospheres supporting nanocrystalline titania

    International Nuclear Information System (INIS)

    The facile bulk synthesis of silica nanospheres makes them an attractive support for the transport of chemical compounds such as nanocrystalline titanium dioxide. In this contribution we present a promising route for the synthesis of mesoporous silica nanospheres (m-SiO2) with diameter in range 200 nm, which are ideal supports for nanocrystalline titanium dioxide (TiO2). The detailed microscopic and spectroscopic characterizations of core/shell structure (m-SiO2/TiO2) were conducted. Moreover, the photocatalytic potential of the nanostructures was investigated via phenol decomposition and hydrogen generation. A clear enhancement of photoactivity in both reactions as compared to commercial TiO2-Degussa P25 catalyst is detected.

  18. Synthesis and characterization of ZnO nanowires for nanosensor applications

    International Nuclear Information System (INIS)

    In this paper we report the synthesis of ZnO nanowires via chemical vapor deposition (CVD) at 650 oC. It will be shown that these nanowires are suitable for sensing applications. ZnO nanowires were grown with diameters ranging from 50 to 200 nm depending on the substrate position in a CVD synthesis reactor and the growth regimes. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), photoluminescence (PL), and Raman spectroscopy (RS) have been used to characterize the ZnO nanowires. To investigate the suitability of the CVD synthesized ZnO nanowires for gas sensing applications, a single ZnO nanowire device (50 nm in diameter) was fabricated using a focused ion beam (FIB). The response to H2 of a gas nanosensor based on an individual ZnO nanowire is also reported.

  19. 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. PMID:26456245

  20. 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.

  1. Synthesis and characterization of nanosized lead oxide

    Science.gov (United States)

    Laak, Sheau Tyan

    Nanosized lead oxide as well as copper-doped lead oxide are prepared using two different synthetic techniques; hydrothermal and precipitation. The precipitation method involves simply reacting lead (IV) acetate with distilled water. On the other hand, the hydrothermal process used an autoclave with the presence of Polyvinyl Pyrrolidone (PVP) to prepare lead oxide (PbO 2) hollow spheres, and lead oxide (Pb3O4) microtubes at reaction temperatures of 90°C and 180°C, respectively. Characterization of the synthesized material was carried out using X-Ray Diffraction (XRD), Thermal Gravimetric Analysis (TGA), Differential Thermal Analysis (DTA), and Scanning Electron Microscopy (SEM). X-Ray Diffraction shows that the prepared lead oxides using the hydrothermal process with a reaction a temperature of 90°C is crystalline α PbO 2. SEM shows that the prepared particles are hollow spheres. It also shows uniformity in shape and size. In contrast, X-Ray Diffraction and SEM show that the prepared lead oxide using the hydrothermal process with a reaction temperature of 180°C is nanofiber crystalline α PbO2. It also shows uniformity in shape and size. As to the precipitation method, X-Ray Diffraction shows that the sample is crystalline β PbO2. X-Ray Diffraction revealed that these lead oxides show two different transitions, from β PbO2 to Pb3O4, and Pb3O4 to PbO. These observations were supported by TGA and DTA at 400°C and 700°C, respectively. SEM analysis shows that the prepared β PbO2 sample does not show uniformity, neither in size nor in shape. Indeed, particles appear to congregate and form much larger particles. The results from our study suggest that simple precipitation can lead to the product of PbO2, it however cannot guarantee uniformity. The use of an autoclave in the presence of a polymer such as PVP allowed the precipitation of uniform nano PbO2. In addition, the temperature appeared to affect the morphology of the final product. When low temperature is

  2. Synthesis and characterization of LiFePO{sub 4} cathode preparation by low temperature method

    Energy Technology Data Exchange (ETDEWEB)

    Rajesh, Desapogu, E-mail: rajesh.desapogu@gmail.com; Srinivas Naik, V.; Sunandana, C.S., E-mail: sunandana@gmail.com

    2015-05-01

    We review in detail the physics and technology of the novel material LiFePO{sub 4}, a potential cathode material for Li-ion batteries. In the present work, nano crystalline LiFePO{sub 4} 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 LiFePO{sub 4} 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. Fe{sup 3+} impurity characterization has been done by using ESR.

  3. Peptide o-aminoanilides as crypto-thioesters for protein chemical synthesis.

    Science.gov (United States)

    Wang, Jia-Xing; Fang, Ge-Min; He, Yao; Qu, Da-Liang; Yu, Min; Hong, Zhang-Yong; Liu, Lei

    2015-02-01

    Fully unprotected peptide o-aminoanilides can be efficiently activated by NaNO2 in aqueous solution to furnish peptide thioesters for use in native chemical ligation. This finding enables the convergent synthesis of proteins from readily synthesizable peptide o-aminoanilides as a new type of crypto-thioesters. The practicality of this approach is shown by the synthesis of histone H2B from five peptide segments. Purification or solubilization tags, which are sometimes needed to improve the efficiency of protein chemical synthesis, can be incorporated into the o-aminoanilide moiety, as demonstrated in the preparation of the cyclic protein lactocyclicin Q. PMID:25475965

  4. 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.

  5. 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.

  6. Cholesteric bonded stationary phases for high performance liquid chromatography II: synthesis, physico-chemical characterization and chromatographic behavior of a phospho-cholesteric bonded support. A new way to mimic drug/membrane interactions?

    OpenAIRE

    Courtois, Cédric; Allais, Christophe; Constantieux, Thierry; Rodriguez, Jean; Caldarelli, Stefano; Delaurent, Corinne

    2008-01-01

    International audience Among the various methods exploitable to deter- mine the bioavailability of drugs, reversed-phase liquid chromatography (RPLC) appears to be suited to creation of patterns of prediction. In this context a new stationary phase was designed in this work to reproduce, in terms of chemical structure, as accurately as possible, the main elements of cellular membranes; which include phospholipids and cho- lesterol molecules. An efficient synthetic pathway was developed to ...

  7. 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. PMID:26716586

  8. 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

    2015-10-01

    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 1H and 13C NMR). Quantum chemical investigations have been employed to investigate the structural and spectral properties. The molecular structure, vibrational assignments, 1H and 13C 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.

  9. New Synthesis of TATB. Scaleup and Product Characterization

    International Nuclear Information System (INIS)

    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

  10. Green synthesis and characterization of se nanoparticles and nanorods

    Science.gov (United States)

    Chen, Huiyu; Yoo, Ji-Beom; Liu, Yaqing; Zhao, Guizhe

    2011-12-01

    Selenium nanoparticles and nanorods were successfully prepared in a mixed solvent of ethylene glycol and water at a relatively low temperature of 85°C. No other surfactant or template was employed, and glucose was used as a green and mild reducing reagent in the current synthesis. The volume ratio of ethylene glycol to water played an important role for controlling the shapes of selenium products. The obtained selenium samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), Raman spectra, and UV-vis absorption spectra. The evolution process from amorphous selenium to a trigonal phase complied with a "solid-solution-solid" formation mechanism. HRTEM and SAED results indicate that the trigonal selenium nanorods grow along the [001] direction. This method might provide an environmentally-friendly and low cost route for the synthesis of other related nanomaterials with controlled morphologies.

  11. 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

  12. Synthesis of nano hydroxyapatite ceramic powders using different surfactant templates and their characterization

    International Nuclear Information System (INIS)

    In the present study synthesis of nano hydroxyapatite; HA, Ca/sub 10/(PO/sub 4/)6(OH)/sup 2/ using different surfactants as templates are exploited. Three surfactants such as Cetyl Trimethyl Ammonium Bromide; CTAB (cationic), Sodium Dodecyl Sulphate; SDS (anionic) and Polyoxyethylene sorbitane monolaurate; Tween 20 (nonionic) surfactants have been used as nano reactors for the synthesis of hydroxyapatite ceramic powders. Precipitation route has been used for synthesis with same calcium and phosphate precursors. The effect of different templates on the synthesis, morphology and particle size has been investigated. Considerable influence of templates on the morphology and particle size of the synthesized HA is observed. The samples are characterized using XRD, FTIR and SEM to evaluate the quality, morphology and particle size. The chemical and structural compositions of the products are examined by FTIR. SEM micrographs reveal a rod like structure of HA; possessing various thickness and length in nano range; vary in contrast of each template while the XRD spectra show some other minor phases along with HA. (author)

  13. 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.

  14. Bio-assisted synthesis and characterization of nanostructured bismuth (III) sulphide using Clostridium acetobutylicum

    International Nuclear Information System (INIS)

    Nanostructured bismuth (III) sulphide is synthesized at room temperature using a hydrogen sulphide producing microorganism namely Clostridium acetobutylicum. On contrary to chemical routes involving both the high and room temperature methods, the present experimental procedure involves a bio-assisted approach. This method is free from the usage of toxic and hazardous chemicals making it an environment friendly route. The synthesized bismuth sulphide is characterized using transmission electron microscope (TEM), powder X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and cyclic voltammetry (CV). From our experiments we find that bismuth sulphide produced using this bio-assisted approach exhibits a hexagonal shaped plate-like structures and is stabilized by the extracellular proteins present in the culture medium. - Graphical abstract: A green chemistry approach towards the synthesis of bismuth (III) sulphide nanostructures at room temperature using a hydrogen sulphide producing microorganism namely, Clostridium acetobutylicum is demonstrated. - Highlights: • Environmentally benign (greener) route towards synthesis of Bi2S3 nanostructures. • Bio-assisted synthesis of Bi2S3 at room temperature using Clostridium acetobutylicum. • Extracellular proteins in H2S producing microorganism as stabilizer for Bi2S3 NPs. • Hexagonal platelets of Bi2S3 possessing an orthorhombic crystalline structure

  15. Bio-assisted synthesis and characterization of nanostructured bismuth (III) sulphide using Clostridium acetobutylicum

    Energy Technology Data Exchange (ETDEWEB)

    Kamaraj, Sathish Kumar; Venkatachalam, Ganesh; Arumugam, Palaniappan; Berchmans, Sheela, E-mail: sheelaberchmans@yahoo.com

    2014-02-14

    Nanostructured bismuth (III) sulphide is synthesized at room temperature using a hydrogen sulphide producing microorganism namely Clostridium acetobutylicum. On contrary to chemical routes involving both the high and room temperature methods, the present experimental procedure involves a bio-assisted approach. This method is free from the usage of toxic and hazardous chemicals making it an environment friendly route. The synthesized bismuth sulphide is characterized using transmission electron microscope (TEM), powder X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and cyclic voltammetry (CV). From our experiments we find that bismuth sulphide produced using this bio-assisted approach exhibits a hexagonal shaped plate-like structures and is stabilized by the extracellular proteins present in the culture medium. - Graphical abstract: A green chemistry approach towards the synthesis of bismuth (III) sulphide nanostructures at room temperature using a hydrogen sulphide producing microorganism namely, Clostridium acetobutylicum is demonstrated. - Highlights: • Environmentally benign (greener) route towards synthesis of Bi{sub 2}S{sub 3} nanostructures. • Bio-assisted synthesis of Bi{sub 2}S{sub 3} at room temperature using Clostridium acetobutylicum. • Extracellular proteins in H{sub 2}S producing microorganism as stabilizer for Bi{sub 2}S{sub 3} NPs. • Hexagonal platelets of Bi{sub 2}S{sub 3} possessing an orthorhombic crystalline structure.

  16. Synthesis and enhanced hydrogen desorption kinetics of magnesium hydride using hydriding chemical vapor synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Jin-Ho [Icheon Branch, Korea Institute of Ceramic Engineering and Technology (KICET), Icheon-si, Gyeonggi-do (Korea, Republic of); Kim, Byung-Goan [Korea Energy Materials Co.Ltd., 409, Daegu Technopark, 1-11, Hosan-Dong, Dalse-Gu 704-230 (Korea, Republic of); Kang, Yong-Mook, E-mail: dake@kaist.ac.kr [Department of Chemistry, Dongguk University-Seoul, 100715 Seoul (Korea, Republic of)

    2012-07-15

    Highlights: Black-Right-Pointing-Pointer We synthesized pure MgH{sub 2} by a hydriding chemical vapor synthesis process in a hydrogen atmosphere. Black-Right-Pointing-Pointer The particle size HCVS-MgH{sub 2} was drastically reduced to the sub-micron or micrometer-scale. Black-Right-Pointing-Pointer HCVS-MgH{sub 2} showed different shapes (needle-like nanofibers and angulated plate) depending on the deposited position. Black-Right-Pointing-Pointer HCVS-MgH{sub 2} desorbed hydrogen up to about 7.2 wt% and 7.1 wt%. - Abstract: This paper describes the hydriding chemical vapor synthesis (HCVS) of the hydrogen storage alloy MgH{sub 2} in a hydrogen atmosphere and the product's hydrogenation properties. Mg powder was used as a starting material to produce submicron MgH{sub 2} and uniformly heated to a temperature of 600 Degree-Sign C for Mg vaporization. The effects of deposited positions in HCVS reactor on the morphology and the composition of the obtained products were examined by using X-ray diffraction (XRD), scanning electron microscopy (SEM), and Brunauer-Emmett-Teller (BET) analyses. It is clearly seen that after the HCVS process, the particle size of synthesized MgH{sub 2} was drastically reduced to the sub-micron or micrometer-scale and these showed different shapes (needle-like nanofibers and angulated plate) depending on the deposited position. The hydrogen desorption temperatures of HCVS-MgH{sub 2} were measured using a differential scanning calorimeter (DSC). It was found that after the HCVS process, the desorption temperature of HCVS-MgH{sub 2} decreased from 430 to 385 Degree-Sign C and, simultaneously, the smallest particle size and the highest specific surface area were obtained. These observations indicate that the minimum hydrogen desorption temperature of HCVS-MgH{sub 2} powder with needle-like form can be obtained, and that this temperature is dependent on the particle size and the specific surface area of the products. The thermogravimetric

  17. Synthesis and characterization of a nanostructured matrix hydroxyapatite ceramic bone reconstruction

    International Nuclear Information System (INIS)

    The nanostructured ceramics have been shown promise as biomaterials for bone reconstruction. Among calcium phosphates, hydroxyapatite Ca/P ratio = 1.67 mol stands out because of its crystallographic similarity with the mineral bone phase and biocompatibility. This work was based on synthesis and characterization of a nanostructured hydroxyapatite for use in reconstituting bone tissue. The synthesis method for obtaining the bioceramic powder occurred at process of dissolution/precipitation, involving CaO solid/liquid and phosphoric acid required for forming the composition of Ca/P = 1.67 mole. The material recovered from the synthesis was calcined at 900 ° C/2h, providing the hydroxyapatite powder nanometer. This was subjected to mechanical fragmentation process in mill attritor, providing a hydroxyapatite with modified surface morphology. The results presented relate to morphological characterization studies (SEM), mineralogical (XRD), chemical (FTIR) and particle size distribution, using the laser particle size analysis method. Such results showed the formation of hydroxyapatite phase and morphology satisfactory for use in reconstituting bone tissue

  18. Synthesis, characterization and radiation processing of carboxymethyl-chitosan

    International Nuclear Information System (INIS)

    Chitosan is natural polymer derived from chitin, a polysaccharide found in the exoskeleton of shrimps, crabs, fungi and others. Chitosan is a naturally occurring substance that is chemically similar to cellulose. Chitosan possesses a positive ionic charge give ability to chemically bond with negatively charged fats. Chitosan is soluble in organic acid but insoluble in water. Carboxymethyl-chitosan (cm-chitosan) is a derivative of chitosan which is water-soluble was then prepared by carboxymethylation process of chitosan produced from local shrimp shell. A simple method for synthesis of cm-chitosan has been developed at 55 degree C in aqueous sodium hydroxide / propanol with chloroacetic acid (CAA) or sodium chloroacetate salt (SCA). The modification of chitosan to water-soluble chitosan can be used in hydrogel as anti-bacterial and anti-fungal agent, and it overcome the problem of bad smell using organic acid. (Author)

  19. Chevrel phases superconductive and ultrafine powders synthesis and characterization; Synthese et caracterisation de poudres ultrafines supraconductrices de phases de Chevrel

    Energy Technology Data Exchange (ETDEWEB)

    Even-Boudjada, S.

    1994-12-01

    This work deals with the Chevrel phases superconductive and ultrafine powders synthesis and characterization. The first part of this study presents some new way of synthesis (precipitation, coprecipitation) of Chevrel phases precursors powders (PbS, SnS, MoS{sub 2}) and their characterizations (X-ray fluorescence analysis, ICP mass spectroscopy, scanning electron microscopy, transmission electron microscopy and laser granulometry). These new synthesis methods lead to quasi spherical morphology grains and very weak size grains (0.2 to 0.5 {mu}m) whereas the chemical preparation from the solid state elements gives very different morphology grains (small plates) with a size of 1 to 20 {mu}m. In the second part is shown the interest of the binary Mo{sub 6} S{sub 8} as precursor in the synthesis of ternary superconductive phases (Li, Ni, Cu, Pb). The last part presents the formation reaction of the phase PbMo{sub 6} S{sub 8} and its main chemical and physical properties. Thus some calorimetric measures associated with X-ray diffraction analysis have been realized and have allowed to understand the different reactions occurring during the PbMo{sub 6}S{sub 8} synthesis. (O.L.). 100 refs., figs., tabs.

  20. Plasma chemical synthesis of boride ultra-dispersed powders, their properties and application

    International Nuclear Information System (INIS)

    Special features of equipment's getting up and technological regularities of plasma-chemical reductional synthesis of ultra-dispersed powders of borides of titanium, zirconium, vanadium and chromium are investigated. The chemical and phase composition of compounds obtained, their crystallographical structure, thermo-oxidizing and corrosion resistance, particle's size distribution, gas-saturation of particle's surface are studied. (author)

  1. 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.

  2. The effect of chemical additives on the synthesis of ethanol

    Energy Technology Data Exchange (ETDEWEB)

    Chuang, S.S.C.

    1992-03-06

    The objective of this research was to investigate the reaction mechanism of higher alcohol and aldehyde synthesis from syngas and the role of additives in the synthesis. An in situ IR reaction system and probe molecule technique were developed to study adsorbed species, active sites, and reaction pathway during reaction. The catalysts used for this study included silica-supported Rh, Ru, and Ni. (VC)

  3. 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...

  4. On-line monitoring of continuous flow chemical synthesis using a portable, small footprint mass spectrometer.

    Science.gov (United States)

    Bristow, Tony W T; Ray, Andrew D; O'Kearney-McMullan, Anne; Lim, Louise; McCullough, Bryan; Zammataro, Alessio

    2014-10-01

    For on-line monitoring of chemical reactions (batch or continuous flow), mass spectrometry (MS) can provide data to (1) determine the fate of starting materials and reagents, (2) confirm the presence of the desired product, (3) identify intermediates and impurities, (4) determine steady state conditions and point of completion, and (5) speed up process optimization. Recent developments in small footprint atmospheric pressure ionization portable mass spectrometers further enable this coupling, as the mass spectrometer can be easily positioned with the reaction system to be studied. A major issue for this combination is the transfer of a sample that is representative of the reaction and also compatible with the mass spectrometer. This is particularly challenging as high concentrations of reagents and products can be encountered in organic synthesis. The application of a portable mass spectrometer for on-line characterization of flow chemical synthesis has been evaluated by coupling a Microsaic 4000 MiD to the Future Chemistry Flow Start EVO chemistry system. Specifically, the Hofmann rearrangement has been studied using the on-line mass spectrometry approach. Sample transfer from the flow reactor is achieved using a mass rate attenuator (MRA) and a sampling make-up flow from a high pressure pump. This enables the appropriate sample dilution, transfer, and preparation for electrospray ionization. The capability of this approach to provide process understanding is described using an industrial pharmaceutical process that is currently under development. The effect of a number of key experimental parameters, such as the composition of the sampling make-up flow and the dilution factor on the mass spectrometry data, is also discussed. PMID:25106707

  5. 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.

  6. 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.

  7. 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.

  8. Synthesis and characterization of Ba/MCM-41

    OpenAIRE

    Kaya, Emine; OKTAR, Nuray; KARAKAŞ, Gürkan

    2010-01-01

    Mesoporous Ba/MCM-41 type materials (Ba/MCM-41) with high Ba/Si molar ratios between 0.025 and 0.1 were synthesized by direct hydrothermal synthesis. The samples were characterized by XRD, nitrogen adsorption, TGA-DTA, FTIR, SEM-EDS, and TEM techniques. BET surface areas of samples with various Ba loadings were found between 722 and 931 m2/g with 28 Å average pore size, which is consistent with the pore size of 30 Å for pure MCM-41 samples synthesized by the same procedure. The crys...

  9. 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

  10. PtCo/Au nanocomposite: Synthesis, characterization, and magnetic properties

    Science.gov (United States)

    Dai, Jingtao; Du, Yukou; Wang, Fangwei; Yang, Ping

    2007-09-01

    Magnetic PtCo/Au nanocomposites with narrow size distribution were synthesized in a reverse micelle, followed by a post-synthesis handling of the stabilizer-exchange technique. The PtCo/Au nanocomposites were characterized by ultraviolet visible spectroscopy, X-ray diffraction and transmission electron microscopy, respectively. Superconducting quantum interference device studies revealed that the nanocomposites were superparamagnetic above the blocking temperature ( TB=69 K), while the samples were ferromagnetic with Hc (628 Oe) and Ms (2.97 emu /g) at 5 K.

  11. 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.

  12. Synthesis characterization, and properties of rubber lattices; a review

    International Nuclear Information System (INIS)

    Latex is a stable dispersion of polymeric material in an aqueous medium. Lattices are present in natural as well as in synthetic forms. The range of applications of latex is extensive in carpet underlay, fabric back-coating, paper and paints coatings, adhesive, binder, leather finish, floor polish, waterproof clothing, bounded fiber, pigment printing, latex thread, cement and asphalt, foam scraps binders, can closure, thickeners, box toes and shoes counters, sealant and mastics, modifiers, protein reduction, enzyme treatment and peroxide vulcanization. In this review we are presenting synthesis, characterization, properties, manufacturing and processing of latex. (author)

  13. Uranium complexes with macrosyclic polyethers. Synthesis and structural chemical analysis

    International Nuclear Information System (INIS)

    This dissertation reports about studies on the chemical coordination behaviour of uranium of oxidation stages IV and VI with regard to twelve different macrocyclic ligands. For the preparation of the complexes, for every system a different method has been developed. The elementary analysis of the various complexes including the uranium had been done by X-ray fluorescence analysis, and the structural characterization proceeded via vibrational, uv-vis and emission spectroscopy as well as 1H-NMR and 13C-spin-lattice relaxation time studies. Conformational analysis of the polyethers used allowed the structural changes in the complexes to be observed. The structural analysis of the hydrous uranium VI crown ether complexes yielded information of characteristic features of these types of complexes. The first coordination sphere of the uranyl ion with covalently bonded anion remains unchanged. As to the water content, there is a certain range. Depending upon the solvent used, the complexes have two or four H2O molecules per formula unit. (orig./EF)

  14. 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

  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. 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.

  17. Designing chemical soil characterization programs for mixed waste sites

    International Nuclear Information System (INIS)

    The Weldon Spring Site Remedial Action Project is a remedial action effort funded by the U.S. Department of Energy. The Weldon Spring Site, a former uranium processing facility, is located in east-central Missouri on a portion of a former ordnance works facility which produced trinitrotoluene during World War II. As a result of both uranium and ordnance production, the soils have become both radiologically and chemically contaminated. As a part of site characterization efforts in support of the environmental documentation process, a chemical soil characterization program was developed. This program consisted of biased and unbiased sampling program which maximized areal coverage, provided a statistically sound data base and maintained cost effectiveness. This paper discusses how the general rationale and processes used at the Weldon Spring Site can be applied to other mixed and hazardous waste sites

  18. Control of the chemical synthesis of polyurethane by means of FTIR spectroscopy

    International Nuclear Information System (INIS)

    An analytical technique is used for the control of complex chemical synthesis and allows to value the security of the method, by means of the bands that characteristic the chemical groups in the reaction. The chemical reaction between sucrose and toluendiisocyanate (TDI), to form urethane, is measured by the disappearance, in the spectrum, of the vibration bands of the isocyanate groups, the appearance of characteristic absorptions of urethane groups and the maintenance of sucrose cyclic structure, as well as the TDI aromatic structure

  19. Lanthanum and yttrium oxysulfides activated by europium: (Ln1-x Eux)2 O2 S - Synthesis and characterization

    International Nuclear Information System (INIS)

    The synthesis of lanthanum and yttrium oxysulfides activated by europium were obtained by thermal decomposition of lanthanum and yttrium oxalates doped with europium, under an argon and sulphur atmosphere. The thermal decomposition of these compounds is studied by differential thermal analysis (DTA). The characterization of these oxysulfides were made by chemical analyses, infrared spectroscopy, X-ray diffraction, scanning electron microscopy and emission spectroscopy. (M.V.M.)

  20. Characterization of Chemical and Mechanical Properties of Polymer Based Nanocomposites

    OpenAIRE

    Wafy, Tamer

    2013-01-01

    Characterization of Chemical and Mechanical Properties of Polymer Based NanocompositesThe University of ManchesterTamer Wafy Doctor of Philosophy17 January, 2013One of the most significant issues in nanocomposite performance is improving the dispersion of carbon nanotubes (CNTs) in thermosetting or thermoplastic polymers in order to gain good mechanical properties. Several studies have investigated the fabrication of nanocomposites based on carbon nanotubes and analysed properties, but there ...

  1. Synthesis of Mn3O4 nanoparticles via chemical precipitation approach for supercapacitor application

    International Nuclear Information System (INIS)

    Highlights: • Facile synthesis of Mn3O4 nanoparticles at room temperature via simple chemical precipitation method. • Fabricated supercapacitor device shows maximum specific capacitance in 1 M Na2SO4. • 77% of specific capacitance is retained even after 1000 cycles. - Abstract: A simple chemical precipitation method has been used for the preparation of Mn3O4 nanoparticles at room temperature. The crystal structure and morphology studies of the resulting Mn3O4 nanoparticles were characterized by powder X-ray diffraction (XRD), Fourier transform-infrared spectroscopy (FT-IR), Raman spectroscopy, scanning electron microscope (SEM), transmission electron microscope (TEM), N2 adsorption and desorption and X-ray photoelectron spectroscopy (XPS). The electrochemical properties of the Mn3O4 nanoparticles were then investigated using cyclic voltammetry (CV), galvanostatic charge–discharge and electrochemical impedance spectroscopy (EIS) analysis. The supercapacitive properties of Mn3O4 nanoparticles in the presence of 1 M Na2SO4 exhibited a high specific capacitance of 322 F g−1 at a current density of 0.5 mA cm−2 in the potential range from −0.1 to +0.9 V and about 77% of the initial capacitance was retained after 1000 cycles, indicating that the Mn3O4 electrode owns a good electrochemical stability and capacitance retention capability. The results suggest that the obtained Mn3O4 nanoparticles is a promising electrode material for supercapacitor applications

  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.

    2015-07-01

    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. Electrochemical synthesis and characterization of copper (I oxide

    Directory of Open Access Journals (Sweden)

    Bugarinović Sanja J.

    2009-01-01

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

  4. Synthesis and characterization of termini azobenzene-dendrimer

    Directory of Open Access Journals (Sweden)

    Omid Louie

    2013-10-01

    Full Text Available Some of the organic molecules can be isomerized upon photoirradiation and when they are accompanied by a change in the visible absorption spectrum, it can be called photochromism. Azobenzenes which are important parts of molecular machines and nanotechnology can be called photoisomerizationazobenzene (azo chromophores, and have been incorporated into a wide variety of materials and molecular architectures, including polymers, dendrimers, and molecular glasses. We synthesized and characterized the AB2 type polyamidoamine (PAMAM dendrimers by single active site. PAMAM diazobenzenedendrimer was synthesized and characterized by FTIR and NMR (1H, 13C and CHN-O Elementary analysis. A simple method can be used for the synthesis of azobenzene derivative PAMAM dendrimer and other similar compounds.

  5. Synthesis and characterization of nanorods for magnetic rotational spectroscopy

    Science.gov (United States)

    Aprelev, Pavel; Gu, Yu; Burtovyy, Ruslan; Luzinov, Igor; Kornev, Konstantin G.

    2015-08-01

    Magnetic rotational spectroscopy (MRS) with magnetic nanoprobes is a powerful method for in-situ characterization of minute amounts of complex fluids. In MRS, a uniformly rotating magnetic field rotates magnetic micro- or nano-probes in the liquid and one analyzes the features of the probe rotation to extract rheological parameters of liquids. Magnetic properties of nanoprobes must be well characterized and understood to make results reliable and reproducible. Ni and Co nanorods synthesized by electrochemical template synthesis in alumina membranes are discussed in applications to MRS. We employ alternating gradient field magnetometry, X-ray diffraction, and magnetic force microscopy to evaluate and compare properties of these nanorods and study their performance as the MRS probes. It is shown that nickel nanorods do not seem to violate any assumptions of the MRS rigid dipole theory, while cobalt nanorods do.

  6. Synthesis and study of structural, dielectric, magnetic and magnetoelectric characterization of BiFeO3–NiFe2O4 nanocomposites prepared by chemical solution method

    International Nuclear Information System (INIS)

    Highlights: • Synthesized nanocomposites of xNiFe2O4–(1−x)BiFeO3 (x = 0.1, 0.2, 0.3, 0.4). • The average particles size is around 30–70 nm. • Anomaly in dielectric constant is a signature of magnetoelectric coupling (γ). • γ calculated from fractional change of Δε ∼ γM2 by varying magnetic field. • Magnetic properties greatly enhanced with increase in nickel ferrite content. -- Abstract: Magnetoelectric (ME) nanocomposites of xNiFe2O4–(1−x)BiFeO3 (x = 0.1, 0.2, 0.3, 0.4) have been prepared by chemical solution method. The samples have been calcined at various temperatures ranging from 500 to 700 °C and X-ray diffraction analysis showed phase formation of xNiFe2O4–(1−x)BiFeO3 nanocomposites calcined at 500 °C. The effect of annealing temperature on structural and magnetic properties was studied. TEM shows the formation of powders of nano order size and the average crystal size was found to be around 30–70 nm. Variation of dielectric constant and dielectric loss with frequency showed dispersion in the low frequency range and an anomaly in the temperature variation of dielectric constant is an evidence of presence of magnetoelectric coupling in the prepared nanocomposites. The magnetic behavior is found to be strongly dependent upon nickel ferrite content and annealing temperature. Magnetic field-induced relative change of the dielectric constant was observed in the nanocomposites. The fractional change of magnetic field induced in dielectric constant can also be expressed by Δε ∼ γM2 (where γ is magnetoelectric coupling coefficient)

  7. Transition metal complexes with thiosemicarbazide-based ligands. Part46. Synthesis and physico-chemical characterization of mixed ligand cobalt(III-complexes with salicylaldehyde semi-, thiosemi- and isothiosemicarbazone and pyridine

    Directory of Open Access Journals (Sweden)

    VUKADIN M. LEOVAC

    2003-12-01

    Full Text Available Mixed ligand octahedral cobalt(III complexes with the tridentate salicylaldehyde semi-, thiosemi- and isothiosemicarbazone and pyridine of general formula [CoIII(L11-3(py3]X (H2L1 = salicylaldehyde semicarbazone, X = [CoIICl3(py]-, ClO4- . H2O, I- . 0.5 I2; H2L2 = salicylaldehyde thiosemicarbazone, X = [CoIICl3(py]-, [CoIIBr3(py]-, ClO4- . H2O, I3-; H2L3 = salicylaldehyde S-methylisothiosemicarbazone, X = [ CoIIBr3(py ]-, ClO4- . H2O, BF4- were synthesized. The tridentate coordination of all the three dianionic forms of the ligands involves the phenol oxygen, hydrazine nitrogen and the chalcogen (O or S in case of salicylaldehyde semi-, thiosemicarbazone and the terminal nitrogen atom in the case of isothiosemicarbazone. For all the complexes, a meridial octahedral arrangement is proposed, which is a consequence of the planarity of the chelate ligand. The compounds were characterized by elemental analysis, molar conductivity, magnetic susceptibility, IR and electronic absorption spectra. The thermal decomposition of the complexes was investigated by thermogravimetry, coupled TG-MS measurements and DSC.

  8. Synthesis, molecular structure, spectroscopic characterization and quantum chemical calculation studies of (2E)-1-(5-chlorothiophen-2-yl)-3-(2,3,4-trimethoxyphenyl)prop-2-en-1-one

    Science.gov (United States)

    Chidan Kumar, C. S.; Govindarasu, K.; Fun, Hoong-Kun; Kavitha, E.; Chandraju, Siddegowda; Quah, Ching Kheng

    2015-04-01

    High quality single crystal of efficient novel nonlinear optical (NLO) chalcone derivative (2E)-1-(5-chlorothiophen-2-yl)-3-(2,3,4-trimethoxyphenyl)prop-2-en-1-one crystal has been grown and its structure has been characterized by Fourier Transform Infrared (4000-400 cm-1), Fourier Transform Raman (3500-50 cm-1) and single-crystal X-ray diffraction techniques. The vibrational wavenumbers were computed using Density Functional Theory (DFT) and are assigned with the help of potential energy distribution (PED) method. The geometrical parameters of the title compound obtained from X-ray diffraction (XRD) studies are compared with the calculated (DFT) values using 6-31G(d,p) basis set. Stability of the molecule, hyperconjugative interactions, charge delocalization and intramolecular hydrogen bond has been analyzed by using natural bond orbital (NBO) analysis. Electronic structures were discussed by Time Dependent Density Functional Theory (TD-DFT) and the relocation of the electron density was determined. Nonlinear optical (NLO) properties were also investigated. The Time Dependent Density Functional Theory (TD-DFT) method has been used to calculate energies, oscillator strengths of electronic singlet-singlet transitions and the absorption wavelengths. The Higher occupied molecular orbital (HOMO) and the Lower unoccupied molecular orbital (LUMO) analysis are used to determine the charge transfer within the molecule. Comprehensive theoretical and experimental structural studies on the molecule have been carried out by FT-IR, FT-Raman and Ultra Violet-visible spectrometry (UV-Vis).

  9. Characterization of Carbon Nanotubes Grown by Chemical Vapor Deposition

    Science.gov (United States)

    Cochrane, J. C.; Zhu, Shen; Su, Ching-Hua; Lehoczky, S. L.; Rose, M. Franklin (Technical Monitor)

    2001-01-01

    Since the superior properties of multi-wall carbon nanotubes (MWCNT) could improve numerous devices such as electronics and sensors, many efforts have been made in investigating the growth mechanism of MWCNT to synthesize high quality MWCNT. Chemical vapor deposition (CVD) is widely used for MWCNT synthesis, and scanning electron microscopy (SEM) and energy dispersive x-ray spectroscopy (EDS) are useful methods for analyzing the structure, morphology and composition of MWCNT. Temperature and pressure are two important growth parameters for fabricating carbon nanotubes. In MWCNT growth by CVD, the plasma assisted method is normally used for low temperature growth. However a high temperature environment is required for thermal CVD. A systematic study of temperature and pressure-dependence is very helpful to understanding MWCNT growth. Transition metal particles are commonly used as catalysis in carbon nanotube growth. It is also interesting to know how temperature and pressure affect the interface of carbon species and catalyst particles

  10. Carbazole Containing Copolymers: Synthesis, Characterization, and Applications in Reversible Holographic Recording

    Directory of Open Access Journals (Sweden)

    Bénédicte Mailhot-Jensen

    2010-01-01

    Full Text Available Carbazolic copolymers have been developed to be used in reversible holographic recording. This paper describes a complete analysis, from synthesis of the material to its applications, together with the corresponding characterizations. The investigated materials were photosensitive copolymers obtained from carbazolylalkylmethacrylates (CEM and octylmethacrylate (OMA. A detailed investigation was undertaken involving infrared spectroscopy and NMR techniques, 1H, 13C, COSY, and HSQC, in order to establish the chemical structure and the composition of the copolymers. Holographic recording characteristics were investigated with one- and two-layer photothermoplastic carriers. The two-layer carrier contains separate photosensitive and thermoplastic layers and gives the best holographic response. The surface of microstructured samples has been characterized by atomic force microscopy analysis. It is shown that via a photothermoplastic recording process, it is possible to record and read holograms practically in real time (~3 s with a diffraction efficiency of 10% and a spatial resolution higher than 1000 mm−1.

  11. Synthesis and Characterization of a New TRIPHOS Ligand Derivative and the Corresponding Pd(II) Complexes

    Energy Technology Data Exchange (ETDEWEB)

    Miller, Deanna L.; Boro, Brian J.; Grubel, Katarzyna; Helm, Monte L.; Appel, Aaron M.

    2015-12-01

    The synthesis of the new bis(2-(diphenylphosphino)ethyl)methylhydroxyphosphine tridentate phosphine ligand, LCH2OH/Ph, is reported. The ligand reacts with [Pd(Cl)2(PhCN)2 to form [Pd(LCH2OH/Ph)Cl]Cl. Exchange of the chloride ions for triflate (OTf–) using AgOTf yielded pure [Pd(LCH2OH/Ph)OTf]OTf. In addition to spectral characterization the free ligand, LCH2OH/Ph, and Pd(II) complex, [Pd(LCH2OH/Ph)OTf]OTf, are structurally characterized. This research was supported by the US Department of Energy (DOE), Office of Science, Office of Basic Energy Sciences, Division of Chemical Sciences, Biosciences, and Geosciences. Pacific Northwest National Laboratory is a multiprogram national laboratory operated by Battelle for DOE.

  12. Native Chemical Ligation to Minimize Aspartimide Formation during Chemical Synthesis of Small LDLa Protein.

    Science.gov (United States)

    Tailhades, Julien; Sethi, Ashish; Petrie, Emma J; Gooley, Paul R; Bathgate, Ross A; Wade, John D; Hossain, Mohammed A

    2016-01-18

    The inhibition of the G protein-coupled receptor, relaxin family peptide receptor 1 (RXFP1), by a small LDLa protein may be a potential approach for prostate cancer treatment. However, it is a significant challenge to chemically produce the 41-residue and three-disulfide cross-bridged LDLa module which is highly prone to aspartimide formation due to the presence of several aspartic acid residues. Known palliative measures, including addition of HOBt to piperidine for N(α) -deprotection, failed to completely overcome this side reaction. For this reason, an elegant native chemical ligation approach was employed in which two segments were assembled for generating the linear LDLa protein. Acquisition of correct folding was achieved by using either a regioselective disulfide bond formation or global oxidation strategies. The final synthetic LDLa protein obtained was characterized by NMR spectroscopic structural analysis after chelation with a Ca(2+) ion and confirmed to be equivalent to the same protein obtained by recombinant DNA production. PMID:26612092

  13. 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.

  14. Solution-Chemical Synthesis of Cobalt and Iron:Zinc Oxide Nanocomposite Films

    OpenAIRE

    Lagerqvist, Ulrika

    2016-01-01

    The potentially most important challenges today are related to energy and the environment. New materials and methods are needed in order to, in a sustainable way, convert and store energy, reduce pollution, and clean the air and water from contaminations. In this, nanomaterials and nanocomposites play a key role, and hence knowledge about the relation between synthesis, structure, and properties of nanosystems is paramount. This thesis demonstrates that solution-chemical synthesis, using amin...

  15. Synthesis and characterization of carbon nano fibers for its application in the adsorption of toxic gases

    International Nuclear Information System (INIS)

    The production of carbon nano fibers (CNF's) by diverse techniques as the electric arc, laser ablation, or chemical deposition in vapor phase, among other, they have been so far used from final of the 90's. However, the synthesis method by discharge Glow arc of alternating current and high frequency developed by Pacheco and collaborators, is a once alternative for its obtaining. In the plasma Application Laboratory (LAP) of the National Institute of Nuclear Research (INlN) it was designed and manufactured a reactor of alternating current and high frequency that produces a Glow arc able to synthesize carbon nano fibers. Its were carried out nano fibers synthesis with different catalysts to different proportions and with distinct conditions of vacuum pressure and methane flow until obtaining the best nano fibers samples and for it, this nano structures were characterized by Scanning and Transmission Electron Microscopy, X-ray Diffraction, Raman spectrometry and EDS spectrometry. Once found the optimal conditions for the nano fibers production its were contaminated with NO2 toxic gas and it was determined if they present adsorption, for it was used the thermal gravimetric analysis technique. This work is divided in three parts, in the first one, conformed by the chapters 1, at the 3, they are considered the foundations of the carbon nano fibers, their history, their characteristics, growth mechanisms, synthesis techniques, the thermal gravimetric analysis principles and the adsorption properties of the nano fibers. In the second part, consistent of the chapters 4 and 5, the methodology of synthesis and characterization of the nano fibers is provided. Finally, in third part its were carried out the activation energy calculation, the adsorption of the CNF's is analyzed and the conclusions are carried out. The present study evaluates the adsorption of environmental gas pollutants as the nitrogen oxides on carbon nano fibers at environmental or near conditions. Also, they

  16. Synthesis and Characterization of Thermoelectric Oxides at Macro- and Nano-scales

    Science.gov (United States)

    Ma, Feiyue

    Thermoelectric materials can directly convert a temperature difference into electrical voltage and vice versa. Due to this unique property, thermoelectric materials are widely used in industry and scientific laboratories for temperature sensing and thermal management applications. Waste heat harvesting, another potential application of thermoelectric materials, has long been limited by the low conversion efficiency of the materials. Potential high temperature applications, such as power plant waste heat harvesting and combustion engine exhaust heat recovery, make thermoelectric oxides a very promising class of thermoelectric materials. In this thesis, the synthesis and characterization of thermoelectric oxide materials are explored. In the first part of this thesis, the measurement methodologies and instrumentation processes employed to investigate different thermoelectric properties, such as the Seebeck coefficient and carrier concentration at the bulk scale and the thermal conductivity at the nanoscale, are detailed. Existing scientific and engineering challenges associated with these measurements are also reviewed. To overcome such problems, original parts and methodologies have been designed. Three fully functional systems were ultimately developed for the characterization of macroscale thermoelectric properties as well as localized thermal conductivity. In the second part of the thesis, the synthesis of NaxCo 2O4, a thermoelectric oxide material, is discussed. Modification of both composition and structure were carried out so as to optimize the thermoelectric performance of NaxCo2O4. Nanostructuring methods, such as ball milling, electrospinning, auto-combustion synthesis, and core-shell structure fabrication, have been developed to refine the grain size of NaxCo2O4 in order to reduce its thermal conductivity. However, the structure of the nanostructured materials is very unstable at high temperature and limited improvement on thermoelectric performance is

  17. Synthesis Characterization and Quantum Chemical Studies on Two Isoquinolin-7-Ones%两种异喹啉-7-酮的合成、表征及量化计算研究

    Institute of Scientific and Technical Information of China (English)

    顾静和; 王成; 程宇; 徐雨辞; 宋洁; 赵朴素

    2014-01-01

    7H-benzimidazo[2,1,-a]benz[de] isoquinolin-7-one (1) and 4-bromo-7H-benzimidazo[2,1,-a] benz [ de ] isoquinolin-7-one ( 2 ) have been synthesized and characterized by elemental analysis , IR, 1 HNMR, UV-Vis and fluorescence spectra .For the two compounds , density functional theory ( DFT) calcula-tions of the structures and natural population atomic charge analysis have been performed at B 3 LYP/6-311G** level of theory.By using TD-DFT method, electron spectra of 1 and 2 have been predicted, which are in agreement with the experimental ones .Comparative studies on 1 and 2 indicate that introducing an elec-tron-withdrawing group of Br in 4-position of naphthalene ring will change the peak intensity and peak locations both in electron spectra and fluorescence spectra .%合成了异喹啉-7-酮衍生物,7H-苯并咪唑[2,1,-a]联苯[de]异喹啉-7-酮(1)和4-溴代-7H-苯并咪唑[2,1,-a]联苯[de]异喹啉-7-酮(2),并用红外、核磁共振、紫外可见光谱和荧光光谱进行了表征。对于这两个化合物,使用密度泛函( DFT )方法,在B3 LYP/6-311 G**水平上,计算了它们几何结构和原子电荷自然布居分析。使用 TD-DFT 方法,预测了化合物1和化合物2的电子光谱,结果表明与实验电子光谱相吻合。在萘环的4位处引入Br吸电子基团将会改变化合物1和化合物2电子光谱和荧光光谱峰的强度和位置。

  18. 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.

  19. Synthesis and characterization of cellulose derivatives obtained from bacterial cellulose

    International Nuclear Information System (INIS)

    The chemical modification of cellulose leads to production of derivatives with different properties from those observed for the original cellulose, for example, increased solubility in more traditional solvents. In this work we synthesized four derivatives of cellulose: microcrystalline cellulose, cellulose acetate, methylcellulose and carboxymethylcellulose using bacterial cellulose as a source. These were characterized in terms of chemical and structural changes by examining the degree of substitution (DS), infrared spectroscopy (FTIR) and nuclear magnetic resonance spectroscopy - NMR 13C. The molecular weight and degree of polymerization were evaluated by viscometry. The characterization of the morphology of materials and thermal properties were performed with the techniques of X-ray diffraction, electron microscopy images, differential scanning calorimetry (DSC) and thermogravimetric analysis. (author)

  20. N-Methylcysteine-Mediated Total Chemical Synthesis of Ubiquitin Thioester

    OpenAIRE

    Erlich, Lesly A.; Ajish Kumar, K. S.; Haj-Yahya, Mahmood; Dawson, Philip E.; Brik, Ashraf

    2010-01-01

    Ubiquitin thioester is a key intermediate in the ubiquitylation of proteins and is formed enzymatically through the activation of α-COOH of ubiquitin in an ATP dependent manner using the E1 enzyme. The current methods used for the preparation of ubiquitin thioester rely on either the enzymatic machinery or on expressed protein ligation technology. In this article, we report a new chemical strategy, combining native chemical ligation and N-methylcysteine containing peptides, to chemically prep...

  1. Synthesis and Characterization of Biodegradable Polyurethane for Hypopharyngeal Tissue Engineering

    OpenAIRE

    Shen, Zhisen; Lu, Dakai; Li, Qun; Zhang, Zongyong; Zhu, Yabin

    2015-01-01

    Biodegradable crosslinked polyurethane (cPU) was synthesized using polyethylene glycol (PEG), L-lactide (L-LA), and hexamethylene diisocyanate (HDI), with iron acetylacetonate (Fe(acac)3) as the catalyst and PEG as the extender. Chemical components of the obtained polymers were characterized by FTIR spectroscopy, 1H NMR spectra, and Gel Permeation Chromatography (GPC). The thermodynamic properties, mechanical behaviors, surface hydrophilicity, degradability, and cytotoxicity were tested via d...

  2. Sodium meta-autunite colloids: Synthesis, characterization, stability

    OpenAIRE

    Zheng, Zuoping; Wan, Jiamin; Tokunaga, Tetsu K.

    2004-01-01

    Waste forms of U such as those in the United States Department of Energy's Hanford Site often contain high concentrations of Na and P. Low solubility sodium uranyl phosphates such as sodium meta-autunite have the potential to form mobile colloids that can facilitate transport of this radionuclide. In order to understand the geochemical behavior of uranyl phosphate colloids, we synthesized sodium meta-autunite colloids, and characterized their morphology, chemical composition, structure, ...

  3. Synthesis and Characterization of the TAPO-5 Molecular Sieve

    OpenAIRE

    Sarah P.O. Rios; Ricardo Pereira; Dilson Cardoso

    2002-01-01

    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 los...

  4. 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.

  5. Chemical characterization of Sacha Inchi (Plukenetia volubilis L.) oil.

    Science.gov (United States)

    Fanali, Chiara; Dugo, Laura; Cacciola, Francesco; Beccaria, Marco; Grasso, Simone; Dachà, Marina; Dugo, Paola; Mondello, Luigi

    2011-12-28

    A chemical characterization of the major components, namely, triacylglycerols (TAGs), polyphenols, and tocopherols in a Sacha inchi oil derived from cold pressing of the seed, is hereby reported. To tackle such a task, high-performance liquid chromatography in combination with photodiode array (PDA), fluorescence (RF), and mass spectrometry (MS) detection was employed. The latter was interfaced with atmospheric pressure chemical ionization and with electrospray ionization for the analysis of TAGs and polyphenols, respectively, whereas RF detection was tested for the determination of tocopherol content. Furthermore, fatty acid methyl esters (FAMEs) were evaluated by gas chromatography-flame ionization detector. A 93% amount of total fatty acids was represented by unsaturated FAMEs with the greatest percentage represented by linoleic (L) and linolenic (Ln) accounting for approximately 50 and 36%, respectively. The main TAGs (>10%) were represented by LLnL, LnLnLn, and LnLLn; the latter was present in the oil sample at the highest percentage (22.2%). Among tocopherols, γ-tocopherol was detected to be the most abundant component (over 50%). The polyphenolic composition was also investigated, and a total of 15 compounds were positively identified, through the complementary analytical information coming from PDA and MS data. To the best of our knowledge, this is the first report providing a thorough chemical characterization of a Plukenetia volubilis L. oil. PMID:22053706

  6. Combustion synthesis and characterization of uranium and thorium tellurides

    International Nuclear Information System (INIS)

    This report describes an investigation of the chemical systems uranium-tellurium and thorium-tellurium. A novel synthesis technique, combustion synthesis, which uses the exothermic heat of reaction rather than externally supplied heat, was utilized to form the phases UTe, U3Te4, and UTe2 in the U-Te system and the phases ThTe, Th2Te3, and ThTe2 in the Th-Te system from reactions of the type U/sub x/ + Te/sub y/ = U/sub x/Te/sub y/. With this synthetic method, U-Te and Th-Te products could be formed in a matter of seconds, and the purity of the products was often greater than that of the starting materials used. Control over final product stoichiometry was found to be very difficult. The product phase distribution observed in combustion products, as determined by x-ray diffraction, electron microprobe, and optical metallographic methods, was found to be spatially complex. Lattice constants were calculated from x-ray diffraction patterns for the compounds UTe, U3Te4, and ThTe. SOLGASMIX thermodynamic equilibrium calculations were performed using available and estimated thermodynamic data on the system U-Te-O in an attempt to understand the products formed by combustion. Adiabatic combustion reaction temperatures for specific U-Te and Th-Te reactions were also calculated utilizing available and estimated thermodynamic data. 71 refs., 31 figs., 15 tabs

  7. 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.

  8. Synthesis and characterization of a porous wollastonite for filteration applications

    International Nuclear Information System (INIS)

    The present research describes the synthesis and fabrication of a porous Wollastonite based glass-ceramic body by using the conventional ceramic processing method. The major chemical ingredients incorporated were Si0/sub 2/ and CaO, with small additions of AI/sub 2/0/sub 3/, Na/sub 2/0, MgO and K/sub 2/O as mineralizers in stoichiometric proportions. Wet milled and dried powder mixture was binded with PV A and green samples were prepared by cold die pressing in the from of flat disks. Partial calcinations were conducted at 850 degree C that was followed by sintering at 1100 degree C according to thermo gravimetric analysis (TGA) report. Average pore diameter in the range of 10-20 micro meters and interconnected porosity was observed through scanning electron microscope (SEM). The wollastonite phase was identified by X-ray diffraction analysis (XRD) of the sintered sample. (author)

  9. 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.

  10. Synthesis, characterization and behaviour of trans-bis (argininate) copper (II) to gamma radiation

    International Nuclear Information System (INIS)

    The synthesis, the characterization and the behaviour to gamma radiation of trans-bis (argininate) copper (II) are presented. The synthesis is made from copper sulfate, sodium hydroxide and hydrochloride of L (+) arginine, in aqueous medium, and the characterization by infrared spectroscopy, visible and ultraviolet spectroscopy and elementary analysis. (C.G.C.)

  11. 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.

  12. Molybdenum disulfide nanowires and nanoribbons by electrochemical/chemical synthesis.

    Science.gov (United States)

    Li, Q; Walter, E C; van der Veer, W E; Murray, B J; Newberg, J T; Bohannan, E W; Switzer, J A; Hemminger, J C; Penner, R M

    2005-03-01

    Molybdenum disulfide nanowires and nanoribbons have been synthesized by a two-step, electrochemical/chemical synthetic method. In the first step, MoO(x) wires (a mixture of MoO(2) and MoO(3)) were electrodeposited size-selectively by electrochemical step-edge decoration on a highly oriented pyrolytic graphite (HOPG) surface. Then, MoO(x) precursor wires were converted to MoS(2) by exposure to H(2)S either at 500-700 degrees C, producing "low-temperature" or LT MoS(2) nanowires that were predominantly 2H phase, or above 800 degrees C producing "high-temperature" or HT MoS(2) ribbons that were predominantly 3R phase. The majority of these MoS(2) wires and ribbons were more than 50 microm in length and were organized into parallel arrays containing hundreds of wires or ribbons. MoS(2) nanostructures were characterized by X-ray photoelectron spectroscopy, scanning and transmission electron microscopy, selected area electron diffraction, X-ray diffraction, UV-visible absorption spectrometry, and Raman spectroscopy. HT and LT MoS(2) nanowires were structurally distinct: LT MoS(2) wires were hemicylindrical in shape and nearly identical in diameter to the MoO(x) precursor wires from which they were derived. LT MoS(2) wires were polycrystalline, and the internal structure consisted of many interwoven, multilayer strands of MoS(2); HT MoS(2) ribbons were 50-800 nm in width and 3-100 nm thick, composed of planar crystallites of 3R-MoS(2). These layers grew in van der Waals contact with the HOPG surface so that the c-axis of the 3R-MoS(2) unit cell was oriented perpendicular to the plane of the graphite surface. Arrays of MoS(2) wires and ribbons could be cleanly separated from the HOPG surface and transferred to glass for electrical and optical characterization. Optical absorption measurements of HT MoS(2) nanoribbons reveal a direct gap near 1.95 eV and two exciton peaks, A1 and B1, characteristic of 3R-MoS(2). These exciton peaks shifted to higher energy by up to 80 meV as

  13. 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.

  14. Physical Characterization and Steam Chemical Reactivity of Carbon Fiber Composites

    Energy Technology Data Exchange (ETDEWEB)

    Anderl, Robert Andrew; Pawelko, Robert James; Smolik, Galen Richard

    2001-05-01

    This report documents experiments and analyses that have been done at the Idaho National Engineering and Environmental Laboratory (INEEL) to measure the steam chemical reactivity of two types of carbon fiber composites, NS31 and NB31, proposed for use at the divertor strike points in an ITER-like tokamak. These materials are 3D CFCs constituted by a NOVOLTEX preform and densified by pyrocarbon infiltration and heat treatment. NS31 differs from NB31 in that the final infiltration was done with liquid silicon to reduce the porosity and enhance the thermal conductivity of the CFC. Our approach in this work was twofold: (1) physical characterization measurements of the specimens and (2) measurements of the chemical reactivity of specimens exposed to steam.

  15. "Human Health Impact Characterization of Toxic Chemicals for Sustainable Design and Manufacturing

    OpenAIRE

    Yuan, Chris; Dornfeld, David

    2009-01-01

    A schematic method to characterize the human health impact of toxic chemicals is presented. This schematic method uses a streamlined three-tiered hierarchy process which includes intake, toxicity and persistence of a chemical release for its impact characterization. The human health impact of a chemical is represented by its position in a two-dimensional characterization plot, which enables the benchmarking of chemicals to be easily made by comparing the relative positions of the chemicals in...

  16. Synthesis and characterization of ferrous phosphate (vivianite) and its behavior in aqueous media

    International Nuclear Information System (INIS)

    The synthesis and characterization of materials that can be useful in Environmental Chemistry is very important because their characteristics are exposed and its behavior in chemical phenomena as the sorption in aqueous media is understand to use it in the human being benefit. With the object of using, in a future, the octa hydrated ferrous phosphate (vivianite) as a potential candidate for matrix confinement in contention walls for the storage of radioactive waste of long half life, it was synthesized and it characterized physico chemically and their properties of surface of this compound were evaluated. Presently work was carried out the synthesis and structural characterization of the iron phosphate II by infrared spectroscopy with having Fourier transform, high vacuum scanning electron microscopy, X-ray diffraction, thermal gravimetric analysis, the BET multipoint surface area and Moessbauer spectroscopy; as well as, the determination between aqueous media of the isoelectric point and the density of sites of surface of the compound. The octa hydrated ferrous phosphate was obtained pure. The results indicate that the product corresponds to the prospective mineral, the vivianite. The thermal gravimetric analysis demonstrated that the ferrous phosphate is a stable salt after the lost of water. The isoelectric point is since an important parameter because allows to know the behavior of the surface of the material in aqueous systems, in this case the isoelectric point, of the octa hydrated ferrous phosphate, in distilled water is of pH 4.20 and in solution of potassium nitrate 0.5 M is of pH = 3.75. This indicates that the material has an amphoteric surface depending on the pH. On the other hand, the density of active sites of surface obtained by titrations acid-base is of 20 sites by nm2. (Author)

  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. Cysteine functionalized copper organosol: synthesis, characterization and catalytic application

    International Nuclear Information System (INIS)

    We herein report a facile one-pot synthesis, stabilization, redispersion and Cu-S interaction of L-cysteine and dodecanethiol (DDT) protected copper organosol in toluene from precursor copper stearate using sodium borohydride in toluene under a nitrogen atmosphere. Surface modification of the synthesized copper organosol with an amino acid L-cysteine and an alkanethiol (dodecanethiol, DDT) is accomplished by a thiolate bond between the used ligands and nanoparticle surface. The cysteine molecule binds the copper surface via a thiolate and amine linkage but not through electrostatic interaction with the carboxylate group due to the solvent polarity and dielectric medium. Fourier transform infrared (FTIR) analysis was performed to confirm the surface functionalization of the amino acid and DDT to the copper surface. Copper organosol has been characterized by optical spectroscopy (UV/vis), transmission electron microscopy (TEM), x-ray photoelectron spectroscopy (XPS) and x-ray diffraction (XRD). The as-synthesized particles are spherical in shape and exhibit a Mie scattering profile with an absorption maxima in the visible range. Copper nanoparticles capped by cysteine and/or DDT in non-aqueous media are found to represent an interesting catalytic approach for the synthesis of octylphenyl ether

  19. Nuclear, chemical, and physical characterization of nuclear materials

    International Nuclear Information System (INIS)

    The goal of nuclear forensics is to establish an unambiguous link between illicitly trafficked nuclear material and its origin. The Los Alamos National Laboratory (LANL) Nuclear Materials Signatures Program has implemented a graded 'conduct of operations' type analysis flow path approach for determining the key nuclear, chemical, and physical signatures needed to identify the manufacturing process, intended use, and origin of interdicted nuclear material. This analysis flow path includes both destructive and non-destructive characterization techniques and has been exercized against different nuclear materials from LANL's special nuclear materials archive. Results obtained from the case study will be presented to highlight analytical techniques that offer the critical attribution information. (author)

  20. Synthesis, Chemical and Physical Characterization of TKX-50

    Science.gov (United States)

    Klapoetke, Thomas

    2015-06-01

    TKX-50 (bis(hydroxylammonium) 5,5'-bis(tetrazolate-1 N-oxide)) is one of the most promising ionic salts as a possible replacement for RDX. The thermal behavior of TKX-50 (bis(hydroxylammonium) 5,5'-(tetrazolate-1 N-oxide)) and the kinetics of its thermal decomposition were studied using differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). The calculated results of the detonation parameters and equations of state for the detonation products (EOS DP) of explosive materials TKX-50 and MAD-X1 and several of their derivatives were obtained using the computer program EXPLO5 V.6.01. These values were also calculated for standard explosive materials which are commonly used such as TNT, PETN, RDX, HMX as well as for the more powerful explosive material CL-20 to allow comparisons to be made. The determination of the detonation parameters and EOS DP was conducted both for explosive materials having the maximum crystalline density and for porous right up to 50% in volume materials. The influence of the content of plastic binder polyisobutylene used (up to 20% in volume) on all of the investigated properties was also examined. Calculated results on shock wave loading of different inert barriers in a wide range of their dynamic properties under explosion on their surfaces of concrete size charges of different explosive materials in various initial states were obtained with the use of the one-dimensional computer hydrocode EP. Barriers due to materials such as polystyrene, textolite, magnesium, aluminum, zinc, copper, tantalum or tungsten were examined (Fig. 1). Initial values of pressure and other parameters of loading on the interface explosive-barrier were determined in the process of conducted calculations. Phenomena of propagation and attenuation of shock waves in barrier materials were considered too for all possible situations. From these calculations, an essentially complete overview of the explosion properties and characteristics of shock wave action onto barriers was obtained for several new and also for several standard explosive materials as a comparison. Work done in collaboration with Golubev/Fischer/Stierstorfer/Bohanek/Dobrilovic.

  1. Preparation and characterization of calcium aluminate by chemical synthesis

    Institute of Scientific and Technical Information of China (English)

    2006-01-01

    Saturated Ca(OH)2 and AlCl3 solutions were used to synthesize calcium aluminate hydrate precipitates at room temperature; high purity calcium aluminate powders with stable phases were made by calcination of the precursors at a temperature as low as1100℃. PSD and BET analysis revealed the particles with sizes ranging from submicrometer to several micrometers and with a specific area of 13 m2/g. The measurement of hydraulic exotherm revealed that the exothermal rate is in peak for about 2 h. The exothermal quantities are 449.24 J/g at 12 h and 488.38 J/g at 24 h. Its strength development is quick and the 1 day curing strength is almost equal to 100% of the 3 days curing strength in the mortar test.

  2. Synthesis and characterization of a new silicone multiblock polymer

    Energy Technology Data Exchange (ETDEWEB)

    Riley, M.O.; Kolb, J.R.; Jessop, E.S.

    1982-05-10

    The Lawrence Livermore National Laboratory (LLNL) has an active interest in the synthesis of new polysiloxanes as base polymers for cellular silicone materials. These elastomers have properties uniquely suited to very specific engineering requirements. While the polymers which we have prepared via random equilibrium of various cyclic tetrasiloxanes have adequate properties for certain applications, there is evidence to suggest that alternating block polysiloxanes prepared via condensation-polymerization techniques have properties more suited to our end uses as flexible foam materials (cushions). The synthetic sequence developed to prepare these materials involves reactions of functionally terminated (silylamino and silanol) polysiloxane oligomers to produce alternating multiblock (ABAB...) materials of high molecular weight. Dialkylamines are condensation byproducts in this reaction. The analysis and characterization of these multiblock polymers is reported.

  3. Synthesis and Characterization of Bionic Nano-silicon-substituted Hydroxyapatite

    Directory of Open Access Journals (Sweden)

    ZHAI Qian-Qian, ZHAO Shi-Gui, WANG Xiao-Hai, LI Xiu-Zhi, LI Wen-Jie, ZHENG Ya-Sen

    2013-01-01

    Full Text Available To explore the synthesis condition of the bionic nano-silicon-substituted hydroxyapatite and the impact of the silicon content on its crystallization properties, hydroxyapatite of different silicon content were synthesized from Ca(NO32, (NH42HPO4 and Si(OCH2CH34(TEOS via an aqueous precipitation reaction. Fourier transform infrared spectroscopy (FTIR, X-ray fluorescence spectrum (XRF, X-ray diffraction (XRD and transmission electron microscopy (TEM were used for hydroxyapatite characterization. The results show that relative low temperature (40¡䧠is conducive to obtain pure bionic nano-silicon-substituted hydroxyapatite. Under this condition, SiO44- enters the lattice of hydroxyapatite and replaces part of PO43-. The more the content of silicon is, the lower the crystallinity is, the smaller the grain size is and the higher the lattice parameters a and c are.

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

    Directory of Open Access Journals (Sweden)

    Doadrio Antonio L.

    2002-01-01

    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.

  5. Phytochemical Synthesis and Preliminary Characterization of Silver Nanoparticles Using Hesperidin

    International Nuclear Information System (INIS)

    his paper is the first of its kind for development of rapid and ecofriendly method for synthesis of silver nanoparticles from aqueous solution of silver nitrate using the flavonoid “hesperidin” and optimization of the methodology. There is formation of stable spherical silver nanoparticles in the size range of 20–40nm. Optimization of methodology in terms of concentration of reactants and pH of the reaction mixture reduced the reaction time for silver nanoparticle formation to 2mins. Silver nanoparticles (AgNPs) were characterized by UV-Vis spectroscopy and transmission electron microscopy (TEM). UV-vis spectroscopy derived spectrum demonstrated a peak of 430nm which corresponds to the plasmon absorbance of silver nanoparticles. Transmission electron microscopy revealed spherical shaped silver nanoparticles in the size range of 20–40nm.

  6. Synthesis, characterization and catalytic activity of CdO nanocrystals

    Energy Technology Data Exchange (ETDEWEB)

    Singh, G., E-mail: gsingh4us@yahoo.com [Department of Chemistry, D.D.U. Gorakhpur University, Gorakhpur 273009 (India); Kapoor, I.P.S.; Dubey, Reena; Srivastava, Pratibha [Department of Chemistry, D.D.U. Gorakhpur University, Gorakhpur 273009 (India)

    2011-02-15

    In this paper, we report the synthesis of nanocrystalline cadmium oxide (CdO) and its characterization by X-ray diffraction (XRD) and transmission electron microscopy (TEM). Its catalytic activity was investigated on the thermal decomposition of 1,2,5,7-tetranitro-1,3,5,7-tetraazacyclooctane (HMX), ammonium perchlorate (AP), hydroxyl terminated polybutadiene (HTPB) and composite solid propellants (CSPs) using thermogravimetric analysis (TG), simultaneous thermogravimerty and differential scanning calorimetry (TG-DSC) and ignition delay measurements. Kinetics of thermal decomposition of AP + CdO has also been investigated using model free (isoconversional) and model-fitting approaches which have been applied to data for isothermal TG decomposition. All these studies show enhancement in the rate of decomposition of AP, HTPB and CSPs but no effect on HMX. The burning rate of CSPs has also been found to be increased with CdO nanocrystals.

  7. 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.

  8. 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.

  9. Synthesis and Characterization of Carbazole-Linked Porphyrin Tweezers.

    Science.gov (United States)

    Chang, Yi; Michelin, Clément; Bucher, Léo; Desbois, Nicolas; Gros, Claude P; Piant, Sébastien; Bolze, Frédéric; Fang, Yuanyuan; Jiang, Xiaoqin; Kadish, Karl M

    2015-08-17

    Herein the synthesis, spectroscopic characterization, two-photon absorption and electrochemical properties of 3,6-disubstituted carbazole tweezers is reported. A dimer resulting from a Glaser homocoupling was isolated during a Sonogashira coupling reaction between a diethynyl-carbazole spacer and a 5-bromo-triarylporphyrin and the properties of this original compound were compared with the 3,6-disubstituted carbazole bisporphyrin tweezers. The dyads reported herein present a two-photon absorption maximum at 920 nm with two-photon absorption cross-section in the 1200 GM range. Despite a strong linear absorption in the Soret region and moderate fluorescence quantum yield, they both lead to a high brightness reaching 30 000 M(-1)  cm(-1) . PMID:26177731

  10. 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.

  11. 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 (cells.

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

    OpenAIRE

    Seyed Abolghasem Kahani; Zahra Yagini

    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...

  13. Synthesis and characterization of hollow mesoporous BaFe12O19 spheres

    International Nuclear Information System (INIS)

    A facile method is reported to synthesize hollow mesoporous BaFe12O19 spheres using a template-free chemical etching process. Hollow BaFe12O19 spheres were synthesized by conventional spray pyrolysis. The mesoporous structure is achieved by alkaline ethylene glycol etching at 185 °C, with the porosity controlled by the heating time. The hollow porous structure is confirmed by SEM, TEM, and FIB-FESEM characterization. The crystal structure and magnetic properties are not significantly affected after the chemical etching process. The formation mechanism of the porous structure is explained by grain boundary etching. - Graphical abstract: Hollow spherical BaFe12O19 particles are polycrystalline with both grains and grain boundaries. Grain boundaries have less ordered structure and lower stability. When the particles are exposed to high temperature alkaline ethylene glycol, the grain boundaries are etched, leaving small grooves between grains. These grooves allow ethylene glycol to diffuse inside to further etch the grains. As the grain size decreases, gaps appear on the particle surfaces, and a porous structure is finally formed. - Highlights: • Two-step synthesis method for hollow mesoporous BaFe12O19 spheres is proposed. • Porosity of the product can be regulated by controlling the second step of chemical etching. • The crystal structure and magnetic properties are examined to be little affected during the chemical etching. • The mesoporous structure formation mechanism is explained by grain boundary etching

  14. Chemical equilibrium of glycerol carbonate synthesis from glycerol

    International Nuclear Information System (INIS)

    Research highlights: → Transesterification of glycerol with cyclic carbonates or alkyl carbonates is thermodynamically favourable for the preparation of glycerol carbonate from glycerol. → The reaction of glycerol and carbon dioxide is thermodynamically limited. → High temperature and low pressure is favourable to the reaction of glycerol and urea. → Increasing temperature can increase the chemical equilibrium constant for the reaction of glycerol and dimethyl carbonate. → For the reaction of glycerol and ethylene carbonate, increasing temperature can decrease the chemical equilibrium constant. - Abstract: In this paper, the chemical equilibrium for the glycerol carbonate preparation from glycerol was investigated. The chemical equilibrium constants were calculated for the reactions to produce glycerol carbonate from glycerol. The theoretical calculation was compared with the experimental results for the transesterification of glycerol with dimethyl carbonate. Transesterification of glycerol with cyclic carbonates or alkyl carbonates is thermodynamically favourable for producing glycerol carbonate from glycerol according to the equilibrium constant. Increasing temperature can increase the chemical equilibrium constant for the reaction of glycerol with dimethyl carbonate. For the reaction of glycerol with ethylene carbonate, increasing temperature can decrease the chemical equilibrium constant. The reaction of glycerol with carbon dioxide is thermodynamically limited. High temperature and low pressure are favourable to the reaction of glycerol and urea.

  15. 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…

  16. Parallel combinatorial chemical synthesis using single-layer poly(dimethylsiloxane) microfluidic devices

    OpenAIRE

    Dexter, Joseph P.; Parker, William

    2009-01-01

    Improving methods for high-throughput combinatorial chemistry has emerged as a major area of research because of the importance of rapidly synthesizing large numbers of chemical compounds for drug discovery and other applications. In this investigation, a novel microfluidic chip for performing parallel combinatorial chemical synthesis was developed. Unlike past microfluidic systems designed for parallel combinatorial chemistry, the chip is a single-layer device made of poly(dimethylsiloxane) ...

  17. Energy-dependent existence of soliton in the synthesis of chemical elements

    OpenAIRE

    Iwata, Yoritaka

    2014-01-01

    Light chemical elements are, for instance, produced through ion collisions taking place in the core of stars, where fusion is particularly important to the synthesis of chemical elements. Meanwhile soliton provides non-interacting transparency leading to the hindrance of fusion cross section. In order to explain high fusion cross section actually observed in low incident energies, it is necessary to discover the suppression mechanism of soliton propagation. In this paper, based on a systemati...

  18. 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.

  19. Structural diversity and chemical synthesis of peroxide and peroxide-derived polyketide metabolites from marine sponges.

    Science.gov (United States)

    Norris, Matthew D; Perkins, Michael V

    2016-07-28

    Covering: up to early 2016Marine sponges are widely known as a rich source of natural products, especially of polyketide origin, with a wealth of chemical diversity. Within this vast collection, peroxide and peroxide-derived secondary metabolites have attracted significant interest in the fields of natural product isolation and chemical synthesis for their structural distinction and promising in vitro antimicrobial and anticancer properties. In this review, peroxide and peroxide-derived polyketide metabolites isolated from marine sponges in the past 35 years are summarised. Efforts toward their synthesis are detailed with a focus on methods that utilise or attempt to elucidate the complex biosynthetic interrelationships of these compounds beyond enzymatic polyketide synthesis. Recent isolations, advances in synthetic methodology and theories of biogenesis are highlighted and critically evaluated. PMID:27163115

  20. Activation of aluminum as an effective reducing agent by pitting corrosion for wet-chemical synthesis.

    Science.gov (United States)

    Li, Wei; Cochell, Thomas; Manthiram, Arumugam

    2013-01-01

    Metallic aluminum (Al) is of interest as a reducing agent because of its low standard reduction potential. However, its surface is invariably covered with a dense aluminum oxide film, which prevents its effective use as a reducing agent in wet-chemical synthesis. Pitting corrosion, known as an undesired reaction destroying Al and is enhanced by anions such as F⁻, Cl⁻, and Br⁻ in aqueous solutions, is applied here for the first time to activate Al as a reducing agent for wet-chemical synthesis of a diverse array of metals and alloys. Specifically, we demonstrate the synthesis of highly dispersed palladium nanoparticles on carbon black with stabilizers and the intermetallic Cu₂Sb/C, which are promising candidates, respectively, for fuel cell catalysts and lithium-ion battery anodes. Atomic hydrogen, an intermediate during the pitting corrosion of Al in protonic solvents (e.g., water and ethylene glycol), is validated as the actual reducing agent. PMID:23390579

  1. Parallel combinatorial chemical synthesis using single-layer poly(dimethylsiloxane) microfluidic devices

    Science.gov (United States)

    Dexter, Joseph P.; Parker, William

    2009-01-01

    Improving methods for high-throughput combinatorial chemistry has emerged as a major area of research because of the importance of rapidly synthesizing large numbers of chemical compounds for drug discovery and other applications. In this investigation, a novel microfluidic chip for performing parallel combinatorial chemical synthesis was developed. Unlike past microfluidic systems designed for parallel combinatorial chemistry, the chip is a single-layer device made of poly(dimethylsiloxane) that is extremely easy and inexpensive to fabricate. Using the chip, a 2×2 combinatorial series of amide-formation reactions was performed. The results of this combinatorial synthesis indicate that the new device is an effective platform for running parallel organic syntheses at significantly higher throughput than with past methodologies. Additionally, a design algorithm for scaling up the 2×2 combinatorial synthesis chip to address more complex cases was developed. PMID:20216962

  2. 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.

  3. 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.

  4. Mechano-chemical synthesis and optical properties of ZnS nanoparticles

    International Nuclear Information System (INIS)

    In the present work, we report the synthesis and optical properties of ZnS nanoparticles produced by the mechano-chemical route. We used zinc acetate and sodium sulphide as source materials in a high energy planetary ball mill at rotation speed of 300 rpm and vial rotation speed of 600 rpm with ball to powder (BPR or charge ratio CR) 5:1 for 30 and 90 min. The milled powders were washed with methanol to remove impurity and dried at 300 °C for 1 h. The prepared nanoparticles have been characterized using X-ray diffraction (XRD), Field emission scanning electron microscope (FESEM), UV-vis-NIR spectrophotometer and Fluorescence spectroscopy. The crystallite size of the synthesized ZnS nanoparticles is found to be in the range 7-8 nm which was calculated using Debye-Scherer's formula. The value of optical band gap has been found to be in the range 3.80-4.15 eV. Room temperature photoluminescence (PL) spectrum of ZnS samples exhibit a blue emission peaked at 466 nm under UV excitation.

  5. Mechano-chemical synthesis and optical properties of ZnS nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Pathak, C.S., E-mail: chandrashekharpathak09@gmail.com [Department of Physics, Bharat Institute of Technology, Meerut, UP 250103 (India); Agarwala, V. [Department of Metallurgical and Materials Engineering, Indian Institute of Technology, Roorkee 247667 (India); Mandal, M.K. [Department of Physics, National Institute of Technology, Durgapur 713209 (India)

    2012-09-01

    In the present work, we report the synthesis and optical properties of ZnS nanoparticles produced by the mechano-chemical route. We used zinc acetate and sodium sulphide as source materials in a high energy planetary ball mill at rotation speed of 300 rpm and vial rotation speed of 600 rpm with ball to powder (BPR or charge ratio CR) 5:1 for 30 and 90 min. The milled powders were washed with methanol to remove impurity and dried at 300 Degree-Sign C for 1 h. The prepared nanoparticles have been characterized using X-ray diffraction (XRD), Field emission scanning electron microscope (FESEM), UV-vis-NIR spectrophotometer and Fluorescence spectroscopy. The crystallite size of the synthesized ZnS nanoparticles is found to be in the range 7-8 nm which was calculated using Debye-Scherer's formula. The value of optical band gap has been found to be in the range 3.80-4.15 eV. Room temperature photoluminescence (PL) spectrum of ZnS samples exhibit a blue emission peaked at 466 nm under UV excitation.

  6. Synthesis of mono and multidomain YIG particles by chemical coprecipitation or ceramic procedure

    International Nuclear Information System (INIS)

    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 oC when the nitrate precursors were used. However, calcination temperatures of up to 1100 oC 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/cm3, after calcination at 800 oC. 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 oC. 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.

  7. Characterizing chemical systems with on-line computers and graphics

    International Nuclear Information System (INIS)

    Incorporating computers and graphics on-line to chemical experiments and processes opens up new opportunities for the study and control of complex systems. Systems having many variables can be characterized even when the variable interactions are nonlinear, and the system cannot a priori be represented by numerical methods and models. That is, large sets of accurate data can be rapidly acquired, then modeling and graphic techniques can be used to obtain partial interpretation plus design of further experimentation. The experimenter can thus comparatively quickly iterate between experimentation and modeling to obtain a final solution. We have designed and characterized a versatile computer-controlled apparatus for chemical research, which incorporates on-line instrumentation and graphics. It can be used to determine the mechanism of enzyme-induced reactions or to optimize analytical methods. The apparatus can also be operated as a pilot plant to design control strategies. On-line graphics were used to display conventional plots used by biochemists and three-dimensional response-surface plots

  8. 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

  9. 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…

  10. Synthesis of polysaccharide chemical gels by gamma-irradiation

    International Nuclear Information System (INIS)

    Recently many biodegradable hydrogel systems have been developed in the area of controlled drug delivery. In previous studies, the authors prepared biodegradable hydrogels by crosslinking natural polymers, such as albumin and dextran, using gamma-irradiation. Natural polymers were functionalized by introducing double bonds through reaction with glycidyl acrylate. The functionalized polymers were then crosslinked to form chemical gels by exposure to gamma-irradiation. In this study, they examined the ability of various polysaccharides to form chemical gels by gamma-irradiation. Dextran, alginic acid, hyaluronic acid, benzyl esters of hyaluronic acid, and gellan were functionalized. The effects of the polymer concentration and the gamma-irradiation dose on the hydrogel formation were examined. All the polysaccharides used formed chemical gels, although the extent of gel formation was different. For alginic acid, hyaluronic acid, and benzyl ester of hyaluronic acid at 25% of esterification degree, the chemical gels were formed at lower polymer concentration and at lower gamma-irradiation dose, if the solution was acidified to pH 3. The ability to form chemical gels with various natural polymers would be useful in the development of controlled drug delivery systems

  11. Synthesis and characterization of nanostructured Ag on porous titania

    International Nuclear Information System (INIS)

    In this work, porous titania was prepared on bulk Ti by chemical oxidation, and then nanostructured silver (Ag) was deposited on titania surface by ion beam sputtering. After annealing treatment, Ag/TiO2 composites were characterized using X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Results indicated that a nano-porous titania layer with mean pore size of 150 nm and thickness of 1 μm was formed by chemical oxidation at 80 deg. C for 45 min. There were three Ag species (Ag (0), Ag (1+), and Ag (2+)) on composites surface after annealing treatment, and metallic Ag content achieved maximum value with annealing temperature of 500 deg. C in air. Ag showed high thermal stability being partly attributed to the inhibiting the diffusion of Ag by the underlying porous titania.

  12. 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.

  13. Physical and chemical characterization of waste wood derived biochars.

    Science.gov (United States)

    Yargicoglu, Erin N; Sadasivam, Bala Yamini; Reddy, Krishna R; Spokas, Kurt

    2015-02-01

    Biochar, a solid byproduct generated during waste biomass pyrolysis or gasification in the absence (or near-absence) of oxygen, has recently garnered interest for both agricultural and environmental management purposes owing to its unique physicochemical properties. Favorable properties of biochar include its high surface area and porosity, and ability to adsorb a variety of compounds, including nutrients, organic contaminants, and some gases. Physical and chemical properties of biochars are dictated by the feedstock and production processes (pyrolysis or gasification temperature, conversion technology and pre- and post-treatment processes, if any), which vary widely across commercially produced biochars. In this study, several commercially available biochars derived from waste wood are characterized for physical and chemical properties that can signify their relevant environmental applications. Parameters characterized include: physical properties (particle size distribution, specific gravity, density, porosity, surface area), hydraulic properties (hydraulic conductivity and water holding capacity), and chemical and electrochemical properties (organic matter and organic carbon contents, pH, oxidation-reduction potential and electrical conductivity, zeta potential, carbon, nitrogen and hydrogen (CHN) elemental composition, polycyclic aromatic hydrocarbons (PAHs), heavy metals, and leachable PAHs and heavy metals). A wide range of fixed carbon (0-47.8%), volatile matter (28-74.1%), and ash contents (1.5-65.7%) were observed among tested biochars. A high variability in surface area (0.1-155.1g/m(2)) and PAH and heavy metal contents of the solid phase among commercially available biochars was also observed (0.7-83 mg kg(-1)), underscoring the importance of pre-screening biochars prior to application. Production conditions appear to dictate PAH content--with the highest PAHs observed in biochar produced via fast pyrolysis and lowest among the gasification

  14. Synthesis of MCM-41 by Hydrothermal and Sonochemical Methods and Characterization

    OpenAIRE

    Gedikli, Ümran; Mısırlıoğlu, Zarife; Acar Bozkurt, Pınar; CANEL, Muammer

    2015-01-01

    One of the known groups of mesoporous materials is MCM-41 that has been applied as catalyst for various chemical reactions [1-2]. In this work, using water as solvent, cetylytrimethylammonium bromide (CTAB) as template, sodium silicate and tetraethylortosilicate (TEOS) as silica source, mesoporous MCM-41 were synthesized by direct hydrothermal synthesis method and sonochemical synthesis method. Furthermore, the effects of silica source and synthesis method on the distribution of products were...

  15. 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  |

  16. 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.

  17. Synthesis and structural characterization of manganese olivine lithium phosphate

    International Nuclear Information System (INIS)

    Highlights: • LiMnPO4 was obtained by sol gel method and crystallization in reducing atmosphere. • Magnetic and electric properties are reported for LiMnPO4. • Electrochemical properties are also found and enhanced by adding carbon. • SEM and HRTEM show the submicron powder nature. • The multifunctional behavior of LiMnPO4 is experimentally demonstrated. - Abstract: The manganese olivine lithium phosphate is a multifunctional material. If carbon is added to form a composite LiMnPO4–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 LiMnPO4 is obtained by sol gel chemical method and according to X-ray diffraction patterns, pure LiMnPO4 is obtained after calcination in a reducing atmosphere (10% H2 – 90% Ar). Nanostructured LiMnPO4 is a material with very interesting properties that deserves attentions

  18. Technology Evaluation Workshop Report for Tank Waste Chemical Characterization

    International Nuclear Information System (INIS)

    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

  19. Synthesis and Characterization of Carbon Nanotubes Decorated with Gold Nanoparticles

    International Nuclear Information System (INIS)

    In presented work we report results of simple and viable method for producing Au/CNT composites. Chemical composition and crystallographic structure of the Au/CNT composites was confirmed by X-ray diffraction measurements, while transmission and scanning electron microscopy were used to characterize the morphology of nanocrystals as well as the distribution of nanocrystals in the composite. The obtained particles with relatively small diameter (less than 9 nm) were found to be spatially well dispersed on the carbon nanotubes. The density of attached Au-nanoparticles is not sufficient, and cannot be improved by simple increasing gold loading. (authors)

  20. 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.

  1. Synthesis and characterization of GaN nanowires

    International Nuclear Information System (INIS)

    In this work, GaN nanowires were fabricated on Si substrates coated with NiCl2 thin films using chemical vapor deposition (CVD) method by evaporating Ga2O3 powder at 1100 deg. C in ammonia gas flow. X-ray diffraction (XRD), scanning electron microscopy (SEM), high-resolution transmission electron microscope (HRTEM) and photoluminescence (PL) spectrum are used to characterize the samples. The results demonstrate that the nanowires are single-crystal GaN with hexagonal wurtzite structure. The growth mechanism of GaN nanowires is also discussed.

  2. 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.

  3. Synthesis and characterization of blue light emitting materials containing imidazole

    International Nuclear Information System (INIS)

    A series of novel imidazole derivatives as blue light emitting materials were synthesized by heck coupling reaction and characterized with respect to their chemical, luminescence and thermal properties. The results were shown that the imidazole derivatives were strongly blue fluorescent (λ = 455-487 nm) with high fluorescence quantum yields (Φf = 0.28-0.63). All of these compounds have excellent thermal properties (382-423 deg. C) due to the molecular structure introduced by imidazole heterocycles, and the imidazole derivatives (M1 and M2) can be polymerized as monomers

  4. 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

  5. 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.

  6. Synthesis and characterization of carbon fibers obtained through plasma techniques

    International Nuclear Information System (INIS)

    The study of carbon, particularly the nano technology is a recent field, the one which has important implications in the science of new materials. It investigation is of great interest for industries producers of ceramic, metallurgy, electronic, energy storage, biomedicine, among others. The diverse application fields are a reason at national as international level, so that many works are focused in the production of nano fibers of carbon. The Thermal plasma applications laboratory (LAPT) of the National Institute of Nuclear Research (ININ), it is carrying out works about carbon nano technology. The present work has as purpose to carry out the synthesis and characterization of the carbon nano fibers which are obtained by electric arch of alternating current (CA) to high frequencies and by a plasma gun of non transferred arch, where are used hydrocarbons like benzene, methane, acetylene like carbon source and ferrocene, nickel, yttrium and cerium oxide like catalysts. For both techniques its were thought about a relationship among hydrocarbon-catalyst that it favored to the nano fibers production. The obtained product of each experiment outlined it was analyzed by transmission electron microscopy (TEM), scanning electron microscopy (SEM) and X-ray diffraction (XRD), analysis with those were obtained pictures and diffraction graphs, which were observed to arrive to one conclusion on the operation conditions, same analysis with those were characterized the tests carried out according to the nano structures formation of carbon. (Author)

  7. Electrochemical synthesis and characterization of branched viologen derivatives

    International Nuclear Information System (INIS)

    In this work two three-branched cyanopyridine based monomers were synthesized and used as starting materials for the preparation of viologen derivatives with branched structures. The film synthesis was performed using reductive electropolymerization in aqueous solution. Both electrochemical and spectroelectrochemical characterization proved that the viologen films undergo a well-defined and reversible two step redox reaction, which is the typical performance for viologen materials. Furthermore, FTIR and SEM were utilized to characterize their structures and morphologies. SEM studies showed that the viologen films have a highly porous structure. Additionally, discharging experiments confirmed that the viologen films show different intercalation behavior as size of electrolyte anion had various effects on the redox potential. Finally, it has been proven that these two viologen derivative materials have the potential to be utilized as a supporting material with intrinsic redox activity and with excellent properties for hosting especially negatively charged particles, molecules and macromolecules. The promising properties of these materials make them good candidates in electronics and also in organic solar cells when loaded with large molecules such as fullerenes. In the organic rechargeable battery applications they can be used as anode-active materials as they exhibit high charging-discharging capacity at negative potentials

  8. Nanoparticle synthesis of zinc peroxide: structural and morphological characterization for bactericidal applications

    International Nuclear Information System (INIS)

    Zinc peroxide (ZnO2) nanoparticles were synthesized by sol-gel technique. The chemicals used for the synthesis were zinc acetate di-hydrate (Zn(CH3COO)2.2H2O) and hydrogen peroxide (H2O2) at 30 % in an aqueous solution with sonication. The structure of the ZnO2 nanoparticles was characterized by X-ray diffraction. While the morphology and the cluster size were determined using scanning and transmission electron microscopy. For a preliminary evaluation of the bactericidal properties of the ZnO2, the material was exposed to Staphylococcus aureus, Escherichia coli y Bacillus subtili, and the nanoparticles presented good bactericidal properties. (author)

  9. Synthesis and characterization of zeolite material from coal ashes modified by surfactant

    International Nuclear Information System (INIS)

    Coal ash was used as starting material for zeolite synthesis by means of hydrothermal treatment. The surfactant-modified zeolite (SMZ) was prepared by adsorbing the cationic surfactant hexadecyltrimethylammonium bromide (HDTMA-Br) on the external surface of the zeolite from coal ash. The zeolite structure stability was monitored during the characterization of the materials by FTIR, XDR and SEM. The structural parameters of surfactant-modified zeolite are very close to that of corresponding non-modified zeolite which indicates that the crystalline nature of the zeolite remained intact after required chemical treatment with HDTMA-Br molecules and heating treatment for drying. The most intense peaks in the FTIR spectrum of HDTMA-Br were observed in SMZ spectrum confirming adsorption of surfactant on zeolites. (author)

  10. 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.

  11. Synthesis and characterization of free-isocyanate polyurethane as renewable coating materials

    Science.gov (United States)

    Saputra, O. A.; Apriany, K.; Putri, F. R.; Firdaus, M.

    2016-02-01

    Green synthesis of diethyl ethane-1,2-diyldicarbamate (M1) as starting dimer of free-isocyanate polyurethane from an excess of diethyl carbonate and ethylene diamine catalyzed by TBD (1,5,7-triazabicyclo-[4,4,0]dec-5-ene) at 80 °C for 4 hours has been carried out. The product has high yield and purity up to 92% and 99,18%, respectively. The product was obtained in the form of rod-shaped white crystals and characterized with 1H-NMR, 13C-NMR and FTIR spectroscopy. Polyurethane (P1) has successfully synthesized via polycondensation methods by reacting of M1 with cis-2-butene-1,4-diol. This reaction also catalyzed by TBD organo catalyst. P1 chemical structure has been confirmed using 1H-NMR and FTIR techniques.

  12. 1.7 nm Platinum Nanoparticles: Synthesis with Glucose Starch, Characterization and Catalysis

    DEFF Research Database (Denmark)

    Engelbrekt, Christian; Sørensen, Karsten Holm; Lubcke, T.;

    2010-01-01

    Monodisperse platinum nanoparticles (PtNPs) were synthesized by a green recipe. Glucose serves as a reducing agent and starch as a stabilization agent to protect the freshly formed PtNP cores in buffered aqueous solutions. Among the ten buffers studied, 2-(N-morpholino)ethanesulfonic acid (MES......), ammonium acetate and phosphate are the best media for PtNP size control and fast chemical preparation. The uniform sizes of the metal cores were determined by transmission electron microscopy (TEM) and found to be 1.8 +/- 0.5, 1.7 +/- 0.2 and 1.6 +/- 0.5 nm in phosphate, MES and ammonium acetate buffer......, respectively. The estimated total diameter of the core with a starch coating layer is 5.8-6.0 nm, based on thermogravimetric analysis (TGA). The synthesis reaction is simple, environmentally friendly, highly reproducible, and easy to scale up. The PtNPs were characterized electrochemically and show high...

  13. 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.

  14. Synthesis of graphene platelets by chemical and electrochemical route

    International Nuclear Information System (INIS)

    Graphical abstract: A schematic showing the overall reduction process of graphite to reduced graphene platelets by chemical and electrochemical route. - Highlights: • Graphene was prepared by diverse routes viz. chemical and electrochemical methods. • NaBH4 was effective for removing oxygen functional groups from graphene oxide. • Sodium borohydride reduced graphene oxide (SRGO) showed high specific capacitance. • Electrochemical rendered a cheap route for production of graphene in powder form. - Abstract: Graphene platelets were synthesized from graphene oxide by chemical and electrochemical route. Under the chemical method, sodium borohydride and hydrazine chloride were used as reductants to produce graphene. In this paper, a novel and cost effective electrochemical method, which can simplify the process of reduction on a larger scale, is demonstrated. The electrochemical method proposed in this paper produces graphene in powder form with good yield. The atomic force microscopic images confirmed that the graphene samples prepared by all the routes have multilayers of graphene. The electrochemical process provided a new route to make relatively larger area graphene sheets, which will have interest for further patterning applications. Attempt was made to quantify the quantum of reduction using cyclic voltammetry and choronopotentiometry techniques on reduced graphene samples. As a measure in reading the specific capacitance values, a maximum specific capacitance value of 265.3 F/g was obtained in sodium borohydride reduced graphene oxide

  15. Preparation of nanostructured nickel aluminate spinel powder from spent NiO/Al2O3 catalyst by mechano-chemical synthesis

    OpenAIRE

    Nazemi, M.K.; Sheibani, S; Rashchi, F; González-Delacruz, V.M.; Caballero, Alfonso

    2012-01-01

    In this paper, the possibility of mechano-chemical synthesis, as a single step process for preparation of nanostructured nickel aluminate spinel powder from NiO/Al2O3 spent catalyst was investigated. Powder samples were characterized in terms of composition, morphology, structure, particle size and surface area using complementary techniques such as X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), differential thermal analysis (DTA) and volu...

  16. 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. PMID:26833854

  17. 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.

  18. Synthesis and Characterization of Nanocrystalline YSZ Powder by Smoldering Combustion Synthesis

    Directory of Open Access Journals (Sweden)

    Mari-Ann Einarsrud

    2006-07-01

    Full Text Available Nanocrystalline yttria-stabilized zirconia (YSZ powders with 8 mol% Y2O3 have been produced using smoldering combustion synthesis with glycine as fuel and nitrate as oxidizer. The YSZ powders prepared by using different glycine to nitrate ratios (0.20–1.0 have been characterized by X-ray diffraction (crystallite size, thermogravimetry, infrared spectroscopy, surface area analysis, transmission electron microscopy, and dilatometry to determine the parameters giving the powder the best properties when it comes to densification properties. The influence of calcination temperature on crystallite size, surface area, and carbonate species remaining from the smoldering combustion reaction has been studied especially for the G/N ratio of 0.23 to reveal the optimal synthesis conditions. A G/N ratio of 0.23 and calcination in the range 650–900ºC in oxygen flow gave high quality powder with a crystallite size less than 10 nm. Densities of sintered bodies exhibit an increase for calcination temperatures above 600ºC, where most of the residual carbonate species has been removed.

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

    International Nuclear Information System (INIS)

    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 (Ca10(PO4)6(OH)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 oC. 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 oC and 1300 oC for 6 h, separately, in air. A maximum average sintered density of 3.29 g/cm3 was achieved in structures sintered at 1300 oC, 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

  20. 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.

  1. Synthesis and characterization of EVA/LLDE-cloisite nanocomposites

    International Nuclear Information System (INIS)

    Ethylene vinyl co-acetate/linear low density polyethylene (EVA/LLDPE) based nanocomposites were prepared using organically modified montmorillonite (cloisite) as reinforcing material. Lowering of processing temperature for polymer nanocomposites (PNCs) synthesis with cloisite was successfully done. Different compositions of EVA: LDPE blends such as 70:30, 60:40 and 50:50 were prepared. Cloisite added in the EVA/LLDPE (50:50) blend at 130 degree C in Haake MiniLab to get the polymer nanocomposites. The extent of exfoliation was studied using XRD. The effect of the processing time in the extruder over the extent of was also studied with different residence times for two systems. . Further characterizations of mechanical and thermal properties are carried out. Initially, on the addition of 5 wt% cloisite in pure cloisite at its processing temperature. XRD pattern showed peak shift from 4.8 degree to 6.2 degree. This shifting to higher 20 value reflected the collapse of interlayer spacing. This may be due to partial degradation of the organic modifier or may be due to the change in spatial arrangement of modifier present in the galleries on sodium montmorillonite. Then with the addition of LLDPE processing temperature lowered and PNCs were synthesized. Synthesis at low temperature showed a shift of peak from high 20θ to lower 2θ value in XRD depicting partial exfoliation of the clay. Further, with the increase of residence time in MiniLab, more force is applied by the screws which separated the layers and enhanced the extent of exfoliation and the improvement in the mechanical properties were obtained with the increase in the residence time. (author)

  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. Synthesis and characterization of aluminosilicate catalyst impregnated by nickel oxide

    Science.gov (United States)

    Maulida, Iffana Dani; Sriatun, Taslimah

    2015-09-01

    Aluminosilicate as a catalyst has been synthesized by pore-engineering using CetylTrimethylAmmonium-Bromide (CTAB) as templating agent. It can produce bigger aluminosilicate pore therefore it will be more suitable for bulky molecule. The aims of this research are to synthesize aluminosilicate supported by Nickel, using CTAB surfactant as templating agent for larger pore radius than natural zeolite and characterize the synthesis product, consist of total acid sites and surface area characteristic. This research has been done with following steps. First, making sodium silicate and sodium aluminate. Second, aluminosilicate was synthesized by direct methods, calcined at 550, 650 and 750°C variation temperature, characterized product by X-RD and FTIR spectrometer. Third, NiCl2 was impregnated to the aluminosilicate that has the best cristallinity and main TO4 functional groups product (550 sample). Variation of NiCl2:aluminosilicate (w/w) ratio were 25%:75%, 50%:50% and 75%:25%. Last but not least characterization of catalytic properties was performed. It comprised total acidity test (gravimetric method) and Surface Area Analyzer. The result shows that the product synthesized by direct method at 550oC calcination temperature has the best cristallinity and main functional groups of TO4. The highest total acid sites was 31.6 mmole/g (Imp-A sample). Surface Area Analyzer shows that Imp-B sample has the best pore distribution and highest total pore volume and specific surface area with value 32.424 cc/g and 46.8287 m2/g respectively. We can draw the conclusion that the most potential catalyst is Imp-A sample compared to Imp-B and Imp-C because it has the highest total acid sites. However the most effective catalyst used for product selectivity was Imp-B sample among all samples.

  4. 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.

  5. Green Chemical Synthesis of II-VI Semiconductor Quantum Dots

    OpenAIRE

    Shahid, Robina

    2012-01-01

    Nanotechnology is the science and technology of manipulating materials at atomic and molecular scale with properties different from bulk. Semiconductor QDs are important class of nanomaterials with unique physical and chemical properties owing to the quantum confinement effect. Size dependent optical properties make research on semiconductor QDs more attractive in the field of nanotechnology. Semiconductor QDs are usually composed of combination of elements from groups II–VI, III–V, or IV–VI ...

  6. Bioinspired greigite magnetic nanocrystals: chemical synthesis and biomedicine applications

    OpenAIRE

    Mei Feng; Yang Lu; Yuan Yang; Meng Zhang; Yun-Jun Xu; Huai-Ling Gao; Liang Dong; Wei-Ping Xu; Shu-Hong Yu

    2013-01-01

    Large scale greigite with uniform dimensions has stimulated significant demands for applications such as hyperthermia, photovoltaics, medicine and cell separation, etc. However, the inhomogeneity and hydrophobicity for most of the as prepared greigite crystals has limited their applications in biomedicine. Herein, we report a green chemical method utilizing β-cyclodextrin (β-CD) and polyethylene glycol (PEG) to synthesize bioinspired greigite (Fe3S4) magnetic nanocrystals (GMNCs) with similar...

  7. Generation of synthesis gas for fuels and chemicals production

    OpenAIRE

    Tunå, Per

    2013-01-01

    Many scientists believe that the oil production will peak in the near future, if the peak has not already occurred. Peak oil theories and uncertain future oil deliveries have stimulated interest in alternative sources of fuel and chemicals. This interest has been enhanced by concerns about energy security and about the climate change caused by emissions of carbon dioxide. The result has been increased interest in substituting fossil fuels with renewable energy sources such as wind, solar and ...

  8. 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.

  9. Synthesis and characterization of cobalt-manganese oxides

    International Nuclear Information System (INIS)

    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 Mn4+ to Mn3+. 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.

  10. 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.

  11. Characterization of tin dioxide film for chemical vapors sensor

    Energy Technology Data Exchange (ETDEWEB)

    Hafaiedh, I. [Unite de Recherche de Physique des Semi-conducteurs et Capteurs, IPEST, 2070 La Marsa (Tunisia)], E-mail: imen_haf@yahoo.fr; Helali, S.; Cherif, K.; Abdelghani, A. [Unite de Recherche de Physique des Semi-conducteurs et Capteurs, IPEST, 2070 La Marsa (Tunisia); Tournier, G. [Ecole des Mines de Saint-Etienne, 158 cours Fauriel, 42023 Saint-Etienne (France)

    2008-07-01

    Recently, oxide semiconductor material used as transducer has been the central topic of many studies for gas sensor. In this paper we investigated the characteristic of a thick film of tin dioxide (SnO{sub 2}) film for chemical vapor sensor. It has been prepared by screen-printing technology and deposited on alumina substrate provided with two gold electrodes. The morphology, the molecular composition and the electrical properties of this material have been characterized respectively by Atomic Force Spectroscopy (AFM), Fourier Transformed Infrared Spectroscopy (FTIR) and Impedance Spectroscopy (IS). The electrical properties showed a resistive behaviour of this material less than 300 deg. C which is the operating temperature of the sensor. The developed sensor can identify the nature of the detected gas, oxidizing or reducing.

  12. Characterization of tin dioxide film for chemical vapors sensor

    International Nuclear Information System (INIS)

    Recently, oxide semiconductor material used as transducer has been the central topic of many studies for gas sensor. In this paper we investigated the characteristic of a thick film of tin dioxide (SnO2) film for chemical vapor sensor. It has been prepared by screen-printing technology and deposited on alumina substrate provided with two gold electrodes. The morphology, the molecular composition and the electrical properties of this material have been characterized respectively by Atomic Force Spectroscopy (AFM), Fourier Transformed Infrared Spectroscopy (FTIR) and Impedance Spectroscopy (IS). The electrical properties showed a resistive behaviour of this material less than 300 deg. C which is the operating temperature of the sensor. The developed sensor can identify the nature of the detected gas, oxidizing or reducing

  13. Synthesis and characterization of silver nanoarticles from extract of Eucalyptus citriodora

    OpenAIRE

    Qureshi, MZ; T. Bashir; Khursheed, S; Ismail, T.; Ayub, M.; Reynolds, A.; Hussain, G.

    2014-01-01

    The primary motivation for the study to develop simple eco-friendly green synthesis of silver nanoparticles using leaf extract of Eucalyptus citriodora as reducing and capping agent. The green synthesis process was quite fast and silver nanoparticles were formed within 0.5 h. The synthesis of the particles was observed by UV-visible spectroscopy by noting increase in absorbance. Characterization of the particles was carried out by X-ray diffraction, FTIR and electron microscopy. The developed...

  14. Synthesis, characterization and exploration of the catalytic, supramolecular and biological applications of dinuclear complexes

    OpenAIRE

    Johnpeter, Justin Paul Raj; Therrien, Bruno

    2014-01-01

    The work presented in this thesis involves the synthesis and characterization of dinuclear ruthenium, rhodium and iridium complexes. The catalytic, supramolecular and biological applications of these dinuclear complexes will be discussed. In the first part, the synthesis of sawhorse-type diruthenium tetracarbonyl complexes and their catalytic applications in the supercritical carbon dioxide (scCO2) are presented. Synthesis of sawhorse-type molecular tweezers derived from pyrenyl and porphyrin...

  15. Temperature buffer test. Hydro-mechanical and chemical/ mineralogical characterizations

    International Nuclear Information System (INIS)

    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

  16. Comparative study between bioapatite and synthetic hydroxyapatite obtained by chemical precipitation and mechanochemical synthesis

    International Nuclear Information System (INIS)

    A comparative study between the inorganic component of a human bone tissue with respect of apatite synthesized by chemical precipitation, mechanochemical synthesis and a sample of commercial hidroxyapatite are shown. The samples were studied by X-ray diffraction, atomic absorption spectroscopy and Fourier transform infrared spectroscopy. The results show similar structural characteristics among all samples identifying that sample prepared by mechanochemical synthesis is a kind of hydroxyapatite which has substitutions of carbonate in its crystalline structure, similar to the inorganic component of bone tissue. (author).

  17. 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.

  18. 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.

  19. 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.

  20. Micro-chemical synthesis of molecular probes on an electronic microfluidic device

    OpenAIRE

    Keng, Pei Yuin; Chen, Supin; Ding, Huijiang; Sadeghi, Saman; Shah, Gaurav J.; Dooraghi, Alex; Michael E. Phelps; Satyamurthy, Nagichettiar; Chatziioannou, Arion F; Kim, Chang-Jin “CJ”; van Dam, R. Michael

    2011-01-01

    We have developed an all-electronic digital microfluidic device for microscale chemical synthesis in organic solvents, operated by electrowetting-on-dielectric (EWOD). As an example of the principles, we demonstrate the multistep synthesis of [18F]FDG, the most common radiotracer for positron emission tomography (PET), with high and reliable radio-fluorination efficiency of [18F]FTAG (88 ± 7%, n = 11) and quantitative hydrolysis to [18F]FDG (> 95%, n = 11). We furthermore show that batches of...