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Sample records for cyclam synthesis characterization

  1. Synthesis and structural studies of amido, hydrazido and imido zirconium(IV) complexes incorporating a diamido/diamine cyclam-based ligand.

    Science.gov (United States)

    Munhá, Rui F; Veiros, Luis F; Duarte, M Teresa; Fryzuk, Michael D; Martins, Ana M

    2009-09-28

    The preparation, characterisation and structural analysis of a series of zirconium(IV) complexes that incorporate the diamido/diamine macrocyclic ligand Bn2Cyclam (Bn2Cyclam = 1,8-dibenzyl-1,4,8,11-tetraazacyclotetradecane) are described. The reaction of one or two equivalents of the appropriate LiNHR reagents with [(Bn2Cyclam)ZrCl2] give the corresponding amido-chloride [(Bn2Cyclam)ZrCl(NHR)] (R = tBu, (2,6-iPr)Ph) or bis(amido) [(Bn2Cyclam)Zr(NHR)2] (R = iPr, tBu, (2,6-Me)Ph) complexes, respectively. Treatment of [(Bn2Cyclam)ZrCl(NH(2,6-iPr)Ph)] with one equiv. of MgClMe gives the base-free, monomeric imido complex [(Bn2Cyclam)Zr(N(2,6-iPr)Ph)]. The reaction of the tBu analog with MgClMe generates a dimeric bridging imido species [{(Bn2Cyclam)Zr}2(mu-NR)2], which can also be obtained by thermal decomposition of [(Bn2Cyclam)Zr(NHtBu)2] in toluene. The bis(hydrazido) complex [(Bn2Cyclam)Zr(NHNPh2)2] was obtained by reaction of [(Bn2Cyclam)ZrCl2] and two equiv. of LiNHNPh2. A hydrazido-chloride compound [(Bn2Cyclam)ZrCl(N(Ph)NBu(Ph))] was generated in a one-pot reaction between [(Bn2Cyclam)ZrCl2], LiBu and azobenzene. DFT calculations on [(Bn2Cyclam)ZrXY] complexes indicate that the coordination geometry adopted by these species is dictated by the steric bulk of the ligands X and Y, varying between six-coordinate prismatic and four-coordinate tetrahedral.

  2. Saccharin/cyclamates: epidemiological evidence.

    Science.gov (United States)

    Armstrong, B K

    1985-01-01

    Adequate data on the carcinogenicity of saccharin and cyclamate to humans are available only for the urinary bladder. In the studies available, exposure to saccharin and to cyclamate cannot be distinguished readily. Descriptive studies have shown no evidence of time trends in bladder cancer that can be related to use of saccharin or cyclamate. Likewise, studies of diabetics, who have used more saccharin and cyclamate than other people, have shown no evidence of an increased risk of bladder cancer. This association, however, is probably confounded negatively by cigarette smoking. Thirteen case-control studies have addressed the relationship of saccharin and cyclamate intake to bladder cancer in individuals. While statistically significant positive associations have been observed, a similar number of significant negative associations has also been observed. Studies of the dose-response relationships have also shown no consistent pattern. Studies of saccharin and cyclamate use with smoking habits have shown no consistent interaction with heavy smoking, as might be expected from a promotional effect. In some studies, however, an increased risk with saccharin and cyclamate use has been observed in female non-smokers--a group otherwise at low risk for bladder cancer.

  3. Synthesis and optical behaviour of mesoporous silica functionalized by organometallic molecules

    Energy Technology Data Exchange (ETDEWEB)

    Laskowski, L; Kassiba, A; Errien, N [Laboratoire de Physique de l' Etat Condense LPEC, UMR CNRS n0 6087, Universite du Maine Avenue Olivier Messiaen 72085 - Le Mans CEDEX 9 France (France); Makowska-Janusik, M; Swiatek, J [Institute of Physics, Jan dlugosz University, Al. Armii Krajowej 13/15, 42-200 Czestochowa (Poland); Mehdi, A, E-mail: m.makowska@ajd.czest.pl [Institut Charles Gerhardt, UMR 5253 Chimie Moleculaire et Organisation du Solide, CC 1701 Universite Montpellier II Place E. Bataillon, F-34095 Montpellier Cedex 5 (France)

    2011-04-01

    Mesoporous silica SBA-15 functionalized by (1,4,8,11-tetraazacyclotetradecane) cyclam groups chelating nickel ions (Ni-cyclam) were synthesized by two different approaches. Characterizations by transmission electron microscopy TEM and UV-VIS absorption spectroscopy were performed to monitor the structure and optical properties of the material with regard to the used synthesis methods. The assignment of the experimental UV-VIS absorption spectra is carried out by using the support of suitable numerical simulations based on quantum chemistry DFT codes developed on the modelled (Ni-cyclam) system as free molecule and also constrained in the pores of mesoporous silica matrices.

  4. SYNTHESIS, CHARACTERIZATION AND ANTIBACTERIAL ...

    African Journals Online (AJOL)

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    SYNTHESIS, CHARACTERIZATION AND ANTIBACTERIAL EVALUATION OF. SOME NOVEL DERIVATIVES OF ... ABSTRACT. In the present study, synthesis, and biological evaluation of some novel derivatives of 2- .... dried over anhydrous sodium sulphate and concentrated under vacuum to give the desired product.

  5. SYNTHESIS, CHARACTERIZATION AND ANTIMICROBIAL ...

    African Journals Online (AJOL)

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    ______. *Corresponding author. E-mail: srachem@yahoo.com; Tel: +92 915641658/915843456. SYNTHESIS, CHARACTERIZATION AND ANTIMICROBIAL STUDIES OF. TRANSITION METAL COMPLEXES OF IMIDAZOLE DERIVATIVE. Saeed-ur-Rehman*, Muhammad Ikram, Sadia Rehman, Alia Faiz and Shahnawaz.

  6. SYNTHESIS, CHARACTERIZATION AND PHOTOCATALYTIC ...

    African Journals Online (AJOL)

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    SYNTHESIS, CHARACTERIZATION AND PHOTOCATALYTIC ACTIVITIES OF. Ag-N-CODOPED ZnO NANOPARTICLES FOR DEGRADATION OF METHYL RED. Tesfay Welderfael1, O.P. Yadav1, Abi M. Taddesse1* and Jyotsna Kaushal2. 1Chemistry Department, Haramaya University, P.B. Box 138, Dire Dawa, Ethiopia.

  7. Manganese (III) cyclam complexes with aqua, iodo, nitrito, perchlorato and acetic acid/acetato axial ligands

    DEFF Research Database (Denmark)

    Mossin, Susanne; Sørensen, Henning Osholm; Weihe, Høgni

    2005-01-01

    The syntheses, structures and magnetic properties of five new manganese (III) cyclam complexes, trans-[Mn(cyclam)(OH2)(2)]-(CF3SO3)(3)center dot-H2O, trans-[Mn(cyclam)I-2]I, trans-[Mn(cyclam)(ONO)(2)]ClO4, trans-[Mn(cyclam)(OClO3)(2)]ClO4 and trans-[Mn(cyclam) (CH3COO)(CH3COOH)](ClO4)(2), are rep...

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

    Science.gov (United States)

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

    2001-08-13

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

  9. Formation, Characterization, and O-O Bond Activation of a Peroxomanganese(III) Complex Supported by a Cross-Clamped Cyclam Ligand.

    Science.gov (United States)

    Colmer, Hannah E; Howcroft, Anthony W; Jackson, Timothy A

    2016-03-07

    Although there have been reports describing the nucleophilic reactivity of peroxomanganese(III) intermediates, as well as their conversion to high-valent oxo-bridged dimers, it remains a challenge to activate peroxomanganese(III) species for conversion to high-valent, mononuclear manganese complexes. Herein, we report the generation, characterization, and activation of a peroxomanganese(III) adduct supported by the cross-clamped, macrocyclic Me2EBC ligand (4,11-dimethyl-1,4,8,11-tetraazabicyclo[6.6.2]hexadecane). This ligand is known to support high-valent, mononuclear Mn(IV) species with well-defined spectroscopic properties, which provides an opportunity to identify mononuclear Mn(IV) products from O-O bond activation of the corresponding Mn(III)-peroxo adduct. The peroxomanganese(III) intermediate, [Mn(III)(O2)(Me2EBC)](+), was prepared at low-temperature by the addition of KO2 to [Mn(II)(Cl)2(Me2EBC)] in CH2Cl2, and this complex was characterized by electronic absorption, electron paramagnetic resonance (EPR), and Mn K-edge X-ray absorption (XAS) spectroscopies. The electronic structure of the [Mn(III)(O2)(Me2EBC)](+) intermediate was examined by density functional theory (DFT) and time-dependent (TD) DFT calculations. Detailed spectroscopic investigations of the decay products of [Mn(III)(O2)(Me2EBC)](+) revealed the presence of mononuclear Mn(III)-hydroxo species or a mixture of mononuclear Mn(IV) and Mn(III)-hydroxo species. The nature of the observed decay products depended on the amount of KO2 used to generate [Mn(III)(O2)(Me2EBC)](+). The Mn(III)-hydroxo product was characterized by Mn K-edge XAS, and shifts in the pre-edge transition energies and intensities relative to [Mn(III)(O2)(Me2EBC)](+) provide a marker for differences in covalency between peroxo and nonperoxo ligands. To the best of our knowledge, this work represents the first observation of a mononuclear Mn(IV) center upon decay of a nonporphyrinoid Mn(III)-peroxo center.

  10. synthesis, physical characterization, antibacterial activity

    African Journals Online (AJOL)

    [19-23], we report here the synthesis, characterization and spectral studies of the new complexes. [Co(Chel)(PBu3)]ClO4.H2O ... Synthesis of five coodrdinate cobalt(III) Schiff base complexes. Bull. Chem. Soc. Ethiop. ...... Hofman, K. The Chemistry of Hetrocyclic Compounds, Imidazole and Its Derivatives, Part I,. Interscience ...

  11. SYNTHESIS, CHARACTERIZATION AND DENSITY FUNCTIONAL ...

    African Journals Online (AJOL)

    B. S. Chandravanshi

    3Research Center for Advanced Materials Science, King Khalid University, Abha 61413, P.O. ... (System 3) were synthesized by direct tricyanovinylation of .... Synthesis, characterization and DFT study of low cost hydrazone sensitizers. Bull.

  12. Oxidation of hydrogen peroxide by [Ni (cyclam)] in aqueous acidic ...

    Indian Academy of Sciences (India)

    III. (cyclam)]. 3+ in aqueous acidic media. SANKARAN ANURADHA and VENKATAPURAM RAMANUJAM VIJAYARAGHAVAN. ∗. Department of Physical ... oxidation was followed spectrophotometrically by examining the oxidation of nickel(II) complexes of macro- .... stock solution of copper perchlorate was prepared by.

  13. SYNTHESIS, CHARACTERIZATION AND ANTIBACTERIAL ...

    African Journals Online (AJOL)

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    KEY WORDS: 1,10-Phenanthroline, Imidazole, Cobalt complex, Nickel complex, Copper complex,. Antibacterial activity. INTRODUCTION. Metal complexes containing diimine ligands such as 1,10-phenanthroline and its derivatives have gained importance because of their versatile roles as building blocks for the synthesis ...

  14. SYNTHESIS, CHARACTERIZATION AND ANTIBACTERIAL ...

    African Journals Online (AJOL)

    Metal complexes of Co(II), Ni(II), Cu(II), Zn(II), Cd(II) and Hg(II) with a new Schiff base derived from 3-aminodibenzofuran and 2-furancarboxaldehyde are reported. The complexes have been characterized using chemical analysis, spectroscopic methods (IR, UV-vis, 1H NMR and ESR), conductometric and magnetic data.

  15. 21 CFR 189.135 - Cyclamate and its derivatives.

    Science.gov (United States)

    2010-04-01

    ... Register of October 21, 1969 (34 FR 17063). (c) The analytical methods used for detecting cyclamate in food are in sections 20.162-20.172 of the “Official Methods of Analysis of the Association of Official Analytical Chemists,” 13th Ed. (1980), which is incorporated by reference. Copies may be obtained from the...

  16. Synthesis, characterization, hydrolase and catecholase activity of a dinuclear iron(III) complex: Catalytic promiscuity.

    Science.gov (United States)

    Camargo, Tiago P; Maia, Fernanda F; Chaves, Cláudia; de Souza, Bernardo; Bortoluzzi, Adailton J; Castilho, Nathalia; Bortolotto, Tiago; Terenzi, Hernán; Castellano, Eduardo E; Haase, Wolfgang; Tomkowicz, Zbigniew; Peralta, Rosely A; Neves, Ademir

    2015-05-01

    Herein, we report the synthesis and characterization of the new di-iron(III) complex [(bbpmp)(H2O)(Cl)Fe(III)(μ-Ophenoxo)Fe(III)(H2O)Cl)]Cl (1), with the symmetrical ligand 2,6-bis{[(2-hydroxybenzyl)(pyridin-2-yl)methylamino]methyl}-4-methylphenol (H3bbpmp). Complexes 2 with the unsymmetrical ligand H2bpbpmp - {2-[[(2-hydroxybenzyl)(2-pyridylmethyl)]aminomethyl]-6-bis(pyridylmethyl) aminomethyl}-4-methylphenol and 3 with the ligand L(1)=4,11-dimethyl-1,8-bis{2-[N-(di-2-pyridylmethyl)amino]ethyl}cyclam were included for comparison purposes. Complex 1 was characterized through elemental analysis, X-ray crystallography, magnetochemistry, electronic spectroscopy, electrochemistry, mass spectrometry and potentiometric titration. The magnetic data show a very weak antiferromagnetic coupling between the two iron centers of the dinuclear complex 1 (J=-0.29cm(-1)). Due to the presence of labile coordination sites in both iron centers the hydrolysis of both the diester model substrate 2,4-BDNPP and DNA was studied in detail. Complex 1 was also able to catalyze the oxidation of the substrate 3,5-di-tert-butylcatechol (3,5-DTBC) to give the corresponding quinone, and thus it can be considered as a catalytically promiscuous system. Copyright © 2015 Elsevier Inc. All rights reserved.

  17. Synthesis and characterization of Taurine

    Directory of Open Access Journals (Sweden)

    B Bayarmaa

    2014-10-01

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

  18. Synthesis and characterization of tetraethylammonium tetrachloro ...

    Indian Academy of Sciences (India)

    Unknown

    Synthesis and characterization of tetraethylammonium tetrachloro- cobaltate crystals. M A KANDHASWAMY and V SRINIVASAN*. Department of Physics, Sri Ramakrishna Mission Vidyalaya College of Arts and Science, Coimbatore 641 020, India. MS received 7 February 2000; revised 27 December 2001. Abstract.

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

    Indian Academy of Sciences (India)

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

  20. short communication the synthesis, characterization and biological ...

    African Journals Online (AJOL)

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    ______. *Corresponding author. E-mail: ahmadi.mina63@gmail.com. SHORT COMMUNICATION. THE SYNTHESIS, CHARACTERIZATION AND BIOLOGICAL EVALUATION OF A. STABLE PHOSPHORUS YLIDE AND AN IMIDAZOLE AS NOVEL COMPOUNDS. Mina Ahmadi*, Rahebeh Amiri and Soutodeh Mohammadi.

  1. Synthesis, Characterization and Properties of Copper Clusters

    OpenAIRE

    Vilar Vidal, Noelia

    2013-01-01

    This study displays the electrochemical synthesis of different copper clusters (CuCLs) sizes, their characterization and possible applications. These CuCLs exhibit great photoluminescence and catalytic properties, making them promising materials in a wide range of applications.

  2. Hydrothermal synthesis, characterization and luminescent ...

    Indian Academy of Sciences (India)

    methods, hydrothermal synthesis allows excellent control over particle size, shape, distribution and crystallinity of the material. Synthesis is conducted in a ... terns were recorded on Tecnai G2 S-twin transmission elec- tron microscope with field emission gun operating at 200 kV. Samples for TEM measurements were ...

  3. Polyamide-scorpion cyclam lexitropsins selectively bind AT-rich DNA independently of the nature of the coordinated metal.

    Directory of Open Access Journals (Sweden)

    Anthony T S Lo

    Full Text Available Cyclam was attached to 1-, 2- and 3-pyrrole lexitropsins for the first time through a synthetically facile copper-catalyzed "click" reaction. The corresponding copper and zinc complexes were synthesized and characterized. The ligand and its complexes bound AT-rich DNA selectively over GC-rich DNA, and the thermodynamic profile of the binding was evaluated by isothermal titration calorimetry. The metal, encapsulated in a scorpion azamacrocyclic complex, did not affect the binding, which was dominated by the organic tail.

  4. SYNTHESIS AND CHARACTERIZATION OF FUNCTIONALIZED ...

    African Journals Online (AJOL)

    As a consequence, the synthesis of dihydropyrimidinone derivatives has attracted significant attention by .... (CDCl3, 75 MHz) δ 169.6 (CHO), 167.5 (C=O ester), 160.7 (C=O ester), 150.9 (N2C=O), 150.4. (CN2), 72.6 (C) .... one-pot synthesis of dihydropyrimidinones/thiones under solvent-free conditions. Lett. Org. Chem.

  5. SYNTHESIS, CHARACTERIZATION STUDIES OF 2-[(2 ...

    African Journals Online (AJOL)

    User

    2016-06-01

    Jun 1, 2016 ... Antioxidant picryhydrazyl (DPPH) and the results were the ligand and copper (II) complexes pos ... r (II) complexes possess antioxidant property while zinc (II) comp bial, Antioxidant, Characterization, Ligand, ..... complexes of copper and zinc were synthesi the compounds were characterized. Antimicrob.

  6. SYNTHESIS, CHARACTERIZATION, AND CRYSTAL STRUCTURE ...

    African Journals Online (AJOL)

    a

    guest chemistry, catalysis, electrical .... of architectures and topologies but also because of their fascinating potential applications in functional solid ... Synthesis of a new coordination polymer, {[Ba2(Hpydc)2(pydc)(H2O)3].H2O.(H2pydc)}n. Bull.

  7. synthesis, optical and electrochemical characterization

    African Journals Online (AJOL)

    a

    characterised using a photodetector, a Hamamatus silicon photodiode (1010BR), an electrometer. (Keithley 617) and a picoamperemeter (Keithley 485). All preparations and characterisations were carried out in ambient atmosphere. RESULTS AND DISCUSSION. Synthesis of monomers. The syntheses of the monomeric ...

  8. Isolation, characterization and chemical synthesis

    African Journals Online (AJOL)

    The new toxin consists of 26 amino-acid residues and contains three disulfide bonds. The amino-acid sequence was determined by Edman analysis as CKGKGSOCSOTMYNCCRTGCLSGKCT where O = 4-trans-L-hydroxyproline. The sequence of new toxin was further verified by chemical synthesis and coelution studies ...

  9. Synthesis and characterization of polypyrrole grafted chitin

    Science.gov (United States)

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

    2017-05-01

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

  10. Synthesis, Characterization and In-vitro Evaluation

    African Journals Online (AJOL)

    Babazadeh M, Edjlali L, Rashidian L. Application of 2- hydroxyethyl methacrylate polymers in controlled release of 5-amino salicylic acid as a colon-specific drug. J Polym Res 2007; 14: 207-213. 27. Babazadeh M. Synthesis, characterization, and in vitro drug-release properties of. 2-hydroxyethyl methacrylate copolymers.

  11. Microwave synthesis and mechanical characterization of functionally ...

    Indian Academy of Sciences (India)

    Microwave synthesis and mechanical characterization of functionally graded material for applications in fusion devices ... compact with fine microstructure and good mechanical property has been synthesized by employing microwave heating method at a temperature of 800 °C and in a short processing time of 30 min.

  12. Synthesis and characterization of carboxymethyl chitosan hydrogel ...

    Indian Academy of Sciences (India)

    Home; Journals; Bulletin of Materials Science; Volume 35; Issue 7. Synthesis and characterization of carboxymethyl chitosan hydrogel: Application as site specific delivery for lercanidipine hydrochloride. Subhash S Vaghani Madhabhai M Patel C S Satish Kandarp M Patel N P Jivani. Volume 35 Issue 7 December 2012 pp ...

  13. Synthesis, characterization and photoluminescence properties of ...

    Indian Academy of Sciences (India)

    Synthesis of a new nano hybrid of 5,10,15,20-mesotetra(4-aminophenyl) porphyrin (TAP) functionalized with multi-walled carbon nanotubes (MWCNTs) through an amide linkage is reported for the first time. ThisMWCNT-TAP hybrid was characterized by Raman, Fourier transform infrared (FT-IR), Transmissionelectron ...

  14. Synthesis, characterizations and applications of some ...

    Indian Academy of Sciences (India)

    Home; Journals; Pramana – Journal of Physics; Volume 65; Issue 4. Synthesis, characterizations and applications of some nanomaterials (TiO2 and SiC nanostructured films, organized CNT structures, ZnO structures and CNT{blood platelet clusters). O N Srivastava A Srivastava D Dash D P Singh R M Yadava P R Mishra J ...

  15. Synthesis, Characterization and Antimicrobial Activity of Mixed ...

    African Journals Online (AJOL)

    ADOWIE PERE

    www.bioline.org.br/ja. Synthesis, Characterization and Antimicrobial Activity of Mixed Transition Metal. Complexes of Salicylic Acid ... All the complexes synthesized were of octahedral geometry.Antimicrobial activity of the mixed ..... Diarmiud Jeffreys (2005), "Aspirin the remarkable story of a wonder drug", By: Bloomsubry, ...

  16. Synthesis, Characterization, Antimicrobial Activity and Antioxidant ...

    African Journals Online (AJOL)

    MBI

    2015-12-08

    Dec 8, 2015 ... ABSTRACT. Transition metal complexes of Co(II) and Ni(II) with Schiff base ligand (HL) derived from condensation of 2- ..... Chemistry,. W.B. Sauders. Company,2nd edition, pp 115-125. Asharf M. A. and Mohamood K. and Waajid A. (2011): Synthesis, Characterization and. Biological Activity of Schiff bases, ...

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

    African Journals Online (AJOL)

    MBI

    2014-06-05

    Jun 5, 2014 ... 39. Synthesis, Characterization and Antibacterial Evaluations of the Schiff. Base 2-(1-(2-(Piperazin-1-yl)ethylimino)ethyl)Phenol and its Complexes of. Mn(II), Ni(II) and Zn(II). Salga, M. S., Sada, I. and Abdullahi, A. Department of Pure and Industrial Chemistry, Umaru Musa 'Yar Adua University, Katsina.

  18. Synthesis, spectroscopic characterization and catalytic oxidation ...

    Indian Academy of Sciences (India)

    Home; Journals; Journal of Chemical Sciences; Volume 123; Issue 3. Synthesis, spectroscopic characterization and catalytic oxidation properties of ONO/ONS donor Schiff base ruthenium(III) complexes containing PPh3/AsPh3. Priyarega M Muthu Tamizh R Karvembu R Prabhakaran K Natarajan. Volume 123 Issue 3 May ...

  19. Synthesis and characterization of mononuclear copper (II ...

    Indian Academy of Sciences (India)

    Synthesis and characterization of mononuclear copper(II) complexes of pyridine 2-carboxamide: Their application as catalyst in peroxidative oxidation and antimicrobial agents. Suvendu Samanta Shounak Ray Sutapa Joardar Supriya Dutta. Regular Articles Volume 127 Issue 8 August 2015 pp 1451-1463 ...

  20. Synthesis and characterization of a reduced heteropoly ...

    Indian Academy of Sciences (India)

    Home; Journals; Journal of Chemical Sciences; Volume 114; Issue 2. Synthesis and characterization of a reduced heteropolytungstovanadate: (NH4)7[VVO4 W 10 VI V 2 IV O36]·ca. 22H2O. Vaddypally Shivaiah Samar K Das. Inorganic and Analytical Volume 114 Issue 2 April 2002 pp 107-114 ...

  1. 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.

  2. HYDROTHERMAL SYNTHESIS AND CHARACTERIZATION OF A ...

    African Journals Online (AJOL)

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    HYDROTHERMAL SYNTHESIS AND CHARACTERIZATION OF A BINUCLEAR. COMPLEX AND A COORDINATION POLYMER OF COPPER(II). Masoumeh Tabatabaee1*, Reza Mohamadinasab1, Kazem Ghaini1 and Hamid Reza Khavasi2. 1Department of Chemistry, Islamic Azad University, Yazd Branch, Yazd, Iran.

  3. Synthesis, Characterization and Application of Nano Lepidocrocite ...

    African Journals Online (AJOL)

    Degradation of halogenated organic compounds using nanoparticles is one of the innovative technologies in environmental remediation. In the present study, the synthesis, characterization and application of lepidocrocite (FeOOH) and magnetite (Fe3O4) nanoparticles for the remediation of water contaminated with carbon ...

  4. Synthesis and optical characterization of copper nanoparticles ...

    Indian Academy of Sciences (India)

    Home; Journals; Bulletin of Materials Science; Volume 40; Issue 1. Synthesis and optical characterization of copper nanoparticles prepared by laser ablation. SAMIRA MONIRI MAHMOOD GHORANNEVISS MOHAMMAD REZA HANTEHZADEH MOHSEN ASADI ASADABAD. Volume 40 Issue 1 February 2017 pp 37-43 ...

  5. Synthesis and characterization of gold nanoparticles incorporated ...

    Indian Academy of Sciences (India)

    Synthesis and characterization of gold nanoparticles incorporated bentonite clay for electrocatalytic sensing of arsenic(III). Pankaj Kumar Rastogi Dharmendra Kumar Yadav Shruti Pandey Vellaichamy Ganesan Piyush Kumar Sonkar Rupali Gupta. Regular Articles Volume 128 Issue 3 March 2016 pp 349-356 ...

  6. synthesis, physical characterization, antibacterial activity

    African Journals Online (AJOL)

    ABSTRACT. Some five-coordinated cobalt(III) complexes were synthesized and characterized using elemental analysis, 1H NMR and IR spectra. The formation constants and the thermodynamic parameters were measured spectrophotometrically for the 1:1 adduct formation of [Co(Chel)(PBu3)]ClO4.H2O where Chel ...

  7. Synthesis, characterization, photoluminescence and thermally ...

    Indian Academy of Sciences (India)

    Administrator

    Abstract. Sm3+-doped ZnAl2O4 phosphor was synthesized by citrate sol–gel method and characterized using. X-ray diffraction and scanning electron microscopy to identify the crystalline phase and determine the parti- cle size. Photoluminescence (PL) studies on the sample showed emission peaks at 563, 601, 646 and ...

  8. Photocatalytic semiconductors synthesis, characterization, and environmental applications

    CERN Document Server

    Hernández-Ramírez, Aracely

    2014-01-01

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

  9. Synthesis, characterization and phosphotriesterase mimetic activity ...

    Indian Academy of Sciences (India)

    We report here the synthesis and characterization of a few phenolate-based ligands bearing tertamino substituent and their Zn(II) and Cu(II) metal complexes. Three mono/binuclear Zn(II) and Cu(II) complexes [Zn(L1)(H2O)].CH3OH.H2O (1) (H2 L1 = 6,6′-(((2-dimethylamino)ethylazanediyl)bis(methylene))bis(2, ...

  10. Synthesis and Characterization of Several Fullerene Polyadducts

    OpenAIRE

    Knutson, Nicholas Scott

    2017-01-01

    This dissertation describes the synthesis and characterization of several types of fullerene polyadducts including: 6,9,12,15,18-pentakisorgano-1-hydro[60]fullerenes, 6,9,12,15-tetrakisorgano[60]fullerenes, and 1,4-bisbenzyl[60]fullerenes as well as the performance of several in photovoltaic devices. Several of these projects are collaborations with material scientists and some are original research projects.

  11. On-cartridge derivatisation using matrix solid phase dispersion for the determination of cyclamate in foods

    Energy Technology Data Exchange (ETDEWEB)

    Li, Jianjun, E-mail: bootan12@126.com [Key Laboratory of Synthetic and Natural Functional Molecule Chemistry of Ministry of Education, Northwest University, Xi' an 710069 (China); National Engineering Research Center for Miniaturized Detection Systems, Xi' an 710069 (China); Liu, Yun [College of Food Engineering and Nutritional Science, Shaanxi Normal University, Xi' an 710062 (China); Liu, Qianping [National Engineering Research Center for Miniaturized Detection Systems, Xi' an 710069 (China); Hui, Junfeng [Key Laboratory of Synthetic and Natural Functional Molecule Chemistry of Ministry of Education, Northwest University, Xi' an 710069 (China); Liu, Yangzi [National Engineering Research Center for Miniaturized Detection Systems, Xi' an 710069 (China)

    2017-06-15

    A novel method for determination of sodium cyclamate in foods was developed. In this method, a syringe was loaded with the homogeneous mixture of the sample, KMnO{sub 4} powder and silica dispersant and used as a matrix solid phase dispersion (MSPD) reactor. As the reactor was infiltrated with small amounts of concentrated HCl, cyclamate was converted to 2-chlorocyclohexanone quickly and effectively within 5 min and determined by HPLC on a reversed-phase column using UV detection at a wavelength of 310 nm. Comparing with the traditional derivatisation in solution, the better clean-up was provided using on-cartridge derivatisation of MSPD, and much time, labor, and expense were saved. The results showed good linearity (r{sup 2} = 0.9998) over the concentration range of 1–500 mg/L. The limit of detection (LOD) and limits of quantification (LOQ) of the cyclamate were 0.3 mg/L and 1 mg/L respectively. The recoveries ranged from 91.6% to 101.3% with the relative standard deviations (RSDs) in the range of 2.5%–4.3%. - Highlights: • A novel method was developed for the determination of cyclamate in foods. • On cartridge derivatisation, using matrix solid phase dispersion, was developed. • A new derivatisation reaction for cyclamate conversion to 2-chlorocyclohexanone was developed. • The method was rapid, simple, inexpensive, effective.

  12. 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.

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

    CERN Document Server

    bin M Yusoff, Abdul Rashid

    2014-01-01

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

  14. Ciclamato de sódio e rim fetal Sodium cyclamate and fetal kidney

    Directory of Open Access Journals (Sweden)

    José Germano Ferraz de Arruda

    2003-06-01

    Full Text Available O ciclamato é usado como adoçante artificial não calórico em diversos alimentos e bebidas, sendo 30 vezes mais doce que a sacarose sem o sabor amargo da sacarina. Aparece na composição dos produtos como ciclamato de sódio, ciclamato de cálcio e ácido ciclâmico. O ciclamato e a ciclohexilamina, seu principal metabólito, atravessam a barreira placentária em humanos e desse modo podem ser expostos ao feto. O rim de ratos pode ser afetado por elevadas doses de ciclamato de sódio. Estudos sobre efeitos do ciclamato de sódio na espécie humana são necessários, pois, além de poder substituir a sacarose - prejudicial em casos de diabetes ou quando o controle e a redução do peso corporal são essenciais para a saúde dos pacientes - não propicia desenvolvimento de cárie dentária.Cyclamate is used as an artificial non-caloric sweetener in a variety of foods and beverages, being 30 times as sweet as sugar without the bitter after-taste of saccharin. It is present in the formula of products such as sodium and calcium cyclamates and cyclamic acid. Cyclamate and cyclohexylamine, its principal metabolite, can cross the human placenta exposing the fetus. It has been demonstrated in rats that the kidney may be adversely affected by high doses of cyclamate. Studies on the effects of sodium cyclamate in the human species are necessary, because in addition to replacing saccharose - harmful in individuals with diabetes or patients in whom weight reduction and control are essential for health - it does not cause dental caries.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1997-06-24

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

  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. Stevia, cyclamate and saccharin - natural and artificial sweeteners - exert no effect on sulfane levels in tissues.

    Science.gov (United States)

    Wilinski, Bogdan; Opoka, Wlodzimierz; Somogyi, Eugeniusz; Piotrowska, Joanna; Wilinski, Jerzy

    2013-01-01

    The interactions among natural and artificial sweeteners and endogenous sulfur metabolism have never been investigated. CBA strain mice were administered orally stevia, cyclamate or saccharin in doses of 5 mg/kg of body weight in water solutions each. The measurements of the free and acid-labile sulfane (H2S) tissue concentrations in brain, heart, liver and kidney were performed with Siegel spectrophotometric modified method. No differences in comparisons between hydrogen sulfide concentrations in the control group and each sweetener group within every tissue type were noted. In conclusion, stevia, cyclamate and saccharine do not change the endogenous sulfur metabolism to the extent of causing sulfane tissue levels alterations.

  18. Oxidation of hydrogen peroxide by [Ni III (cyclam)] 3 in aqueous ...

    Indian Academy of Sciences (India)

    The kinetics of oxidation of H2O2 by [NiIII(cyclam)]3+, [NiIIIL1], was studied in aqueous acidic media at 25°C and I = 0.5M (NaClO4). The [NiIIIL1] to [NiIIL1] reduction was found to be fast in the presence of Cu(II) ion than the oxidation of the cyclam ligand by ·OH. The rate constant showed an inverse acid dependence on H+ ...

  19. Synthesis and characterization of peapods and DWCNTs

    Energy Technology Data Exchange (ETDEWEB)

    Anis, B.; Kuntscher, C.A. [Experimentalphysik 2, Universitaet Augsburg, 86195 Augsburg (Germany); Fischer, M.; Schreck, M. [Experimentalphysik 4, Universitaet Augsburg, 86195 Augsburg (Germany); Haubner, K.; Dunsch, L. [Center of Spectroelectrochemistry, IFW Dresden, P.O. Box 270116, 01171 Dresden (Germany)

    2012-12-15

    We report the synthesis and characterization of C{sub 60} rate at SWCNT peapods and double-walled carbon nanotubes (DWCNTs) derived from the peapods. Single-walled carbon nanotubes (SWCNTs), C{sub 60} rate at SWCNT peapods, and DWCNTs were characterized by Raman and optical spectroscopy. The radial breathing modes (RBMs) of the tubes in C{sub 60} rate at SWCNT peapods are shifted to higher energies compared to the RBMs in SWCNTs, while in the case of DWCNTs the RBMs related to the outer tubes are shifted to lower energies compared to SWCNTs. A similar trend is observed for the absorption bands. These results suggest that the filling of the SWCNTs with C{sub 60} molecules decreases the average diameter of the electron cloud around the tubes, whereas the filling with an inner tube increases it. (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  20. Synthesis, characterization and application of electrode materials

    Energy Technology Data Exchange (ETDEWEB)

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

    1995-07-07

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

  1. Anion receptors containing coordinatively unsaturated metal ions: copper(II) complexes with cyclam derivatives

    National Research Council Canada - National Science Library

    Fabbrizzi, Luigi; Fusco, Nadia; Mangano, Carlo; Broglia, Arturo; Boiocchi, Massimo

    2014-01-01

    .... The formation of a five-cordinate complex is favored by the trans-I configuration of the [Cu(Bn 4 cyclam)] 2+ receptor, but it is contrasted by the severe steric repulsions exerted by the benzyl substituents on the macrocyclic framework...

  2. On the synthesis, characterization and photocatalytic applications of ...

    Indian Academy of Sciences (India)

    Home; Journals; Bulletin of Materials Science; Volume 31; Issue 3. On the synthesis, characterization and photocatalytic applications ... These catalysts have been prepared through sol–gel technique using titanium tetra-isopropoxide as a raw material for synthesis. Characterization techniques such as XRD, SEM and TEM ...

  3. Synthesis and characterization of innovative insulation materials

    Directory of Open Access Journals (Sweden)

    Skaropoulou Aggeliki

    2018-01-01

    Full Text Available Insulation elements are distinguished in inorganic fibrous and organic foamed materials. Foamed insulation materials are of great acceptance and use, but their major disadvantage is their flammability. In case of fire, they tend to transmit the flame producing toxic gases. In this paper, the synthesis and characterization of innovative inorganic insulation materials with properties competitive to commercial is presented. Their synthesis involves the mixing of inorganic raw material and water with reinforcing agent or/and foaming agent leading to the formation of a gel. Depending on raw materials nature, the insulation material is produced by freeze drying or ambient drying techniques of the gel. The raw material used are chemically benign and abundantly available materials, or industrial by-products and the final products are non-toxic and, in some cases, non-flammable. Their density and thermal conductivity was measured and found 0.02-0.06 g/cm3 and 0.03-0.04 W/mK, respectively.

  4. 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.

  5. Synthesis and characterization of anisotropic magnetic hydrogels

    Science.gov (United States)

    Hinrichs, Stephan; Nun, Nils; Fischer, Birgit

    2017-06-01

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

  6. Synthesis, characterization and optical applications of nanomaterials

    Science.gov (United States)

    Xu, Fen

    Nanomaterials have been studied extensively due to their potential application in electronics, photonics and nanodevices. There are a wide variety of methods developed to create the nano-scale materials. Chemical colloidal synthesis is the way most used since it is reproducible and high efficiency. Nanoparticles lie at the heart of nanoscience for their novel electronic, magnetic and optical properties. In this dissertation, there are two parts where researches have been performed based on the synthesis of metal and semiconductor nanoparticles. In part I, Semiconductor type-II core-shell quantum dots (QDs) ZnO-CdS have been synthesized by chemical colloidal method which was carried out in a two-step process. We initially synthesized ZnO core nanoparticles and overcoat them with CdS shell. UV-Visible spectra, photoluminescence spectra (PL), high resolution TEM images and X-ray microanalysis for composition studies of the core-shell nanoparticles were characterized. PL lifetime measurements showed this type-II ZnO-CdS core-shell QDs presented extended exciton lifetime due to the spatial separation of electrons and holes between the core and the shell, which opens various useful applications in biosensors and photovoltaic devices. In part II, normal Raman (NR) and surface enhanced Raman scattering (SERS) spectra of 3-hydroxyflavone (3-HF) have been measured. The SERS spectra were obtained both on a Ag electrode surface and on Ag colloidal nanoparticles. The experimental results support the DFT geometry calculations, which show that an adatom site at the vertex of Ag20 cluster binding with the 3-HF molecular plane tilted at an angle of about 53° to the surface is a low-energy structure. This is consistent with the enhancement of in-plane vibrational modes. Furthermore, the effect of fluence level on the discoloration of marble surfaces after the removal of the encrustation by 355 nm laser pulses was comparatively studied. Considering the thermochemical reaction

  7. Polypyrrole-silver Nanocomposite: Synthesis and Characterization

    Directory of Open Access Journals (Sweden)

    D. M. Nerkar

    2016-07-01

    Full Text Available Polypyrrole-Silver (PPy-Ag nanocomposite has been successfully synthesized by the chemical oxidative polymerization of pyrrole with iron (III chloride as an oxidant, in the presence of a colloidal suspension of silver nanoparticles. Turkevich method (Citrate reduction method was used for the synthesis of silver nanoparticles (Ag NPs. The silver nanoparticles were characterized by UV-Visible spectroscopy which showed an absorption band at 423 nm confirming the formation of nanoparticles. PPy-Ag nanocomposite was characterized by Transmission Electron Microscopy (TEM, Scanning Electron Microscopy (SEM, Fourier Transform Infrared Spectroscopy (FTIR and X-ray diffraction (XRD techniques for morphological and structural confirmations. TEM and SEM images revealed that the silver nanoparticles were well dispersed in the PPy matrix. XRD pattern showed that PPy is amorphous but the presence of the peaks at 2q values of 38.24°, 44.57°, 64.51° and 78.45° corresponding to a cubic phase of silver, revealed the incorporation of silver nanoparticles in the PPy matrix. A possible formation mechanism of PPy-Ag nanocomposite was also proposed. The electrical conductivity of PPy-Ag nanocomposite was studied using two probe method. The electrical conductivity of the PPy-Ag nanocomposite prepared was found to be 4.657´10- 2 S/cm, whereas that of pure PPy was found to be 9.85´10-3 S/cm at room temperature (303 K. The value of activation energy (Ea for pure PPy was 0.045 eV while it decreased to 0.034 eV for PPy-Ag nanocomposite. The synthesized nanocomposite powder can be utilized as a potential material for fabrication of gas sensors operating at room temperature.

  8. Synthesis and Characterization of 2-D Materials

    Science.gov (United States)

    Pazos, S.; Sahoo, P.; Afaneh, T.; Rodriguez Gutierrez, H.

    Atomically thin transition-metal dichacogenides (TMD), graphene, and boron nitride (BN) are two-dimensional materials where the charge carriers (electrons and holes) are confined to move in a plane. They exhibit distinctive optoelectronic properties compared to their bulk layered counterparts. When combined into heterostructures, these materials open more possibilities in terms of new properties and device functionality. In this work, WSe2 and graphene were grown using Chemical Vapor Deposition (CVD) and Physical Vapor Deposition (PVD) techniques. The quality and morphology of each material was checked using Raman, Photoluminescence Spectroscopy, and Scanning Electron Microscopy. Graphene had been successfully grown homogenously, characterized, and transferred from copper to silicon dioxide substrates; these films will be used in future studies to build 2-D devices. Different morphologies of WSe2 2-D islands were successfully grown on SiO2 substrates. Depending on the synthesis conditions, the material on each sample had single layer, double layer, and multi-layer areas. A variety of 2-D morphologies were also observed in the 2-D islands. This project is supported by the NSF REU Grant #1560090 and NSF Grant #DMR-1557434.

  9. 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.

  10. Enzymatic synthesis and characterization of galactosyl monoesters.

    Science.gov (United States)

    An, Dong; Zhao, Xiaohui; Ye, Zhiwen

    2015-09-23

    Enzyme-catalyzed synthesis of several fatty acyl-amino acid esters based on D-galactose, as well as their chemical evaluation, was performed. These novel galactosyl fatty acyl-amino acid monoesters were synthesized by utilizing lipase from lipozyme TL IM in tert-butanol with D-galactose and fatty acyl-amino acids as starting materials. The products were characterized by (1)H NMR, (13)C NMR and MS analysis. In addition, their primary physical properties, such as hydrophilic-lipophilic balance (HLB), critical micellar concentration (CMC), solubility in water, maximum surface excess (Γmax), and minimal surface tension (Amin) were measured. The experimental results showed that their CMC values are between 5 and 0.4 mM. The HLB values of galactosyl esters 15-17 indicate that they are useful as oil-in-water emulsions or detergents, whereas 18-22 can be employed as water-in-oil emulsifiers or wetting agents. Copyright © 2015 Elsevier Ltd. All rights reserved.

  11. Electronic structures of [Ru(II)(cyclam)(Et(2)dtc)](+), [Ru(cyclam)(tdt)](+), and [Ru(cyclam)(tdt)](2+): an X-ray absorption spectroscopic and computational study (tdt = toluene-3,4-dithiolate; Et(2)dtc = N,N-diethyldithiocarbamate(1-)).

    Science.gov (United States)

    Milsmann, Carsten; Bill, Eckhard; Weyhermüller, Thomas; DeBeer George, Serena; Wieghardt, Karl

    2009-10-19

    The reaction of [Ru(III)(cyclam)Cl(2)]Cl with 2 equiv of sodium N,N-diethyldithiocarbamate in methanol afforded [Ru(II)(cyclam)(Et(2)dtc)](BPh(4)) (1(BPh(4))). The same reaction with only 1 equiv of toluene-3,4-dithiol and a base yielded [Ru(cyclam)(tdt)](PF(6)) (2(PF(6))) which was oxidized by 1 equiv of ferrocenium hexafluorophosphate generating [Ru(cyclam)(tdt)](PF(6))(2) (2(ox)(PF(6))(2)). The crystal structures of 1 and 2 have been determined by X-ray crystallography at 100 K. The electronic structures of diamagnetic 1(BPh(4)), paramagnetic 2(PF(6)) (S = (1)/(2)), and diamagnetic 2(ox)(PF(6))(2) have been studied by magnetochemistry, spectroelectrochemistry, electron paramagnetic resonance spectroscopy, and (1)H NMR spectroscopy. X-ray absorption spectroscopy on Ru K- and L-edges as well as S K-edges has been employed. Finally, the molecular and electronic structures of all three species have been calculated by using density functional theory (B3LYP). It is shown that 2(ox) comprises an electronic structure which is best described by three resonance structures {[Ru(II)(cyclam)(tdt(0))](2+) [Ru(III)(cyclam)(tdt(*))](2+) [Ru(IV)(cyclam)(tdt(2-))](2+)} with a closed-shell singlet ground state. This is in stark contrast to the isoelectronic iron species, namely, [Fe(III)(cyclam)(tdt(*))](2+) which is a singlet diradical with a low-spin ferric ion coupled intramolecularly antiferromagnetically to a ligand pi radical monoanion (tdt(*))(-).

  12. Functionalized TUD-1 : Synthesis, characterization and (photo-)catalytic performance

    NARCIS (Netherlands)

    Saad, M.S.Hamdy M.

    2005-01-01

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

  13. Synthesis, spectroscopic and DFT characterization of 4 β -(4- tert ...

    African Journals Online (AJOL)

    Synthesis, spectroscopic and DFT characterization of 4 β -(4-tert-butylphenoxy) phthalocyanine positional isomers for non-linear optical absorption. Denisha Gounden, Grace N. Ngubeni, Marcel S. Louzada, Samson Khene, Jonathan Britton, Nolwazi Nombona ...

  14. synthesis, characterization, electrical and catalytic studies of some

    African Journals Online (AJOL)

    B. S. Chandravanshi

    SYNTHESIS, CHARACTERIZATION, ELECTRICAL AND CATALYTIC STUDIES. OF SOME COORDINATION COMPOUNDS DERIVED FROM UNSYMMETRICAL. SCHIFF BASE LIGAND. Gaurav B. Pethe, Amit R. Yaul and Anand S. Aswar*. Department of Chemistry, Sant Gadge Baba Amravati University, Amravati-444 602 ...

  15. Synthesis and characterization of core–shell magnetic molecularly ...

    Indian Academy of Sciences (India)

    Home; Journals; Bulletin of Materials Science; Volume 39; Issue 3. Synthesis and characterization of core–shell magnetic molecularly imprinted polymer nanoparticles for selective extraction of tizanidine in human plasma. GOLALEH SHEYKHAGHAEI MOAYAD HOSSAINI SADR SALAH KHANAHMADZADEH. Volume 39 ...

  16. Tris (catecholato) silicates of nickel: Synthesis, characterization and ...

    Indian Academy of Sciences (India)

    catecholato)silicates of nickel: Synthesis, characterization and first observation of inter-ion ligand transfer. J Vijeyakumar Kingston G S M Sundaram M N Sudheendra Rao. Volume 112 Issue 3 June 2000 pp 402-402 ...

  17. Saccharin, cyclamate, and human bladder cancer. No evidence of an association.

    Science.gov (United States)

    Kessler, I I; Clark, J P

    1978-07-28

    An epidemiologic study designed to elucidate the possible roles of the artificial sweeteners saccharin and cyclamate in human urinary bladder cancer was recently completed. The previous intake of each of these substances among 519 patients with histopathologically confirmed bladder cancer and an equal number of matching controls in metropolitan Baltimore did not differ significantly in frequency, quantity, or duration. These normal findings persisted after simultaneous adjustment for the effects of smoking, occupation, age, diabetes mellitus, and a number of other potentially confounding factors. They are substantiated by the failure of the relative risk of bladder cancer to increase with increasing exposure to artificial sweeteners. It is concluded that neither saccharin nor cyclamate is likely to be carcinogenic in man, at least at the moderate dietary ingestion levels reported by the patient sample.

  18. 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

  19. [Synthesis and characterization of dihydroeugenol acrylate].

    Science.gov (United States)

    Liu, Xiao-Huan; Wang, Chun-Peng; Wang, Ji-Fu; Xu, Yu-Zhi; Chu, Fu-Xiang

    2014-04-01

    Dihydroeugenol acrylate was synthesized by the reaction of acryloyl chloride (AC) with lignin mode compound dihydroeugenol (DH) in the presence of TEA and characterized by using FTIR, GC/MS, 1H-NMR and GPC. FTIR spectra showed that, after the esterification with acryloyl chloride, the intensity of stretching vibration peak of O-H (centered at 3 495 cm(-1)) of DH was disappeared. At the same time, a new peak appeared at 1 762 cm(-1) which was assigned to ester group. Additionally, the appearance of 1 631 and 981 cm(-1) were attributed to the carbon - carbon double bond confirmed the success in the synthesis of DH-AC. 1H-NMR spectra showed that, after the esterification with acryloyl chloride, the proton signal of O-H at 5.5 ppm was disappeared. Meanwhile, the appearance of three new proton signals at 6.0 ppm, 6.4 and 6.7 ppm, attributed to the vinylic protons, indicated that acryloyl chloride was successfully grafted onto DH. The results further confirmed the structures of the DH-AC. GC-MS results showed the DH-AC had a high purity of 98.63%. GPC results showed that dihydroeugenol acrylate could polymerize in the 1,4-dioxane using a thermal initiator of AIBN (2.0 Wt% of total monomers). The weight average molecular mass (Mw) of the homopolymer is 37 400 g x mol(-1), and the number average molecular mass is 23 400 g x mol(-1)' with a polydispersity index Mw/Mn of 1.60, indicating that the dihydroeugenol acrylate has high polymerization activity. This strategy provides a novel approach for extending the comprehensive utilization of lignin.

  20. 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.

  1. Silicon carbonitride nanolayers - Synthesis and chemical characterization

    Energy Technology Data Exchange (ETDEWEB)

    Hoffmann, P.S., E-mail: dg7j@ca.tu-darmstadt.de [Technische Universitaet Darmstadt, Materials Science, Petersenstr. 23, 64287 Darmstadt (Germany); Fainer, N.I. [Nikolaev Institute of Inorganic Chemistry, SB RAS, Acad. Lavrentjev Pr. 3, Novosibirsk 630090 (Russian Federation); Baake, O. [Technische Universitaet Darmstadt, Materials Science, Petersenstr. 23, 64287 Darmstadt (Germany); Kosinova, M.L.; Rumyantsev, Y.M.; Trunova, V.A. [Nikolaev Institute of Inorganic Chemistry, SB RAS, Acad. Lavrentjev Pr. 3, Novosibirsk 630090 (Russian Federation); Klein, A. [Technische Universitaet Darmstadt, Materials Science, Petersenstr. 23, 64287 Darmstadt (Germany); Pollakowski, B.; Beckhoff, B. [Physikalisch-Technische Bundesanstalt, Abbestr. 2-12, 10587 Berlin (Germany); Ensinger, W. [Technische Universitaet Darmstadt, Materials Science, Petersenstr. 23, 64287 Darmstadt (Germany)

    2012-07-01

    SiC{sub x}N{sub y} thin films were produced by plasma-enhanced chemical vapor deposition and characterized by ellipsometry, Fourier transform infrared and Raman spectroscopy, X-ray diffraction, X-ray photoelectron spectroscopy, as well as, by near-edge X-ray absorption fine structure measurements in total-reflection X-ray fluorescence geometry. The temperature of synthesis was varied between 100 Degree-Sign C and 800 Degree-Sign C, the precursors hexamethyldisilazane or hexamethylcyclotrisilazane were used with an addition of N{sub 2}, He, and NH{sub 3}, respectively. The composition of the products was determined to be constant in Si with about 20 at.%, whereas the sum of C and N results in 80 at.% (each varying between 20 and 60 at.%). Consequently, it can be stated, that in the produced silicon carbonitride a network of Si is built with Si-C-Si, Si-C-C-Si, and Si-N-Si bridges. The comparison of the chemical composition and of the physical properties shows for the samples produced with He or N{sub 2}, respectively (without NH{sub 3}) that the refractive index and the absorption coefficient are increasing with an increasing content of carbon in the final formula SiC{sub 4-n}N{sub n} (with n = 1, 2, or 3). - Highlights: Black-Right-Pointing-Pointer Silicon carbonitride nanolayers were produced by chemical vapor deposition. Black-Right-Pointing-Pointer The chemical bonds Si-C, Si-N, and C-C were identified. Black-Right-Pointing-Pointer The tetragonal structure contains cross-linking Si-C-Si, Si-N-Si, and Si-C-C-Si. Black-Right-Pointing-Pointer The elemental composition can be given as SiC{sub 4-n}N{sub n} (n = 1, 2, 3)

  2. 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

  3. Synthesis, Characterization and Antimicrobial Activity of Copper(II ...

    African Journals Online (AJOL)

    This study presents the synthesis, characterization and antimicrobial activity of copper(II) complexes of some ortho-substituted aniline Schiff bases (L1–L8). The Schiff bases and their respective copper(II) complexes were characterized by a combination of elemental analysis, infrared and UV/Visible studies. The structures of ...

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

    Indian Academy of Sciences (India)

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

  5. Synthesis and characterization of Eichhornia-mediated copper oxide ...

    Indian Academy of Sciences (India)

    Synthesis and characterization of Eichhornia-mediated copper oxide nanoparticles and assessing their antifungal activity against plant pathogens ... characterized by UV–visible spectroscopy, Fourier transform infrared spectroscopy (FTIR), Field emission scanning electron microscopy (FESEM) and Energy dispersive X-ray ...

  6. Synthesis, characterization, and X-ray crystal structures of cyclam derivatives. 5. Copper(II) binding studies of a pyridine-strapped 5,12-dioxocyclam-based macrobicycle.

    Science.gov (United States)

    Meyer, Michel; Frémond, Laurent; Espinosa, Enrique; Guilard, Roger; Ou, Zhongping; Kadish, Karl M

    2004-09-06

    The copper(II) binding properties of the macrobicyclic diamide 1,9,12,18,22-pentaazatricyclo[7.6.6.1(3,7)]docosa-3,5,7(22)-triene-13,19-dione (L1) have been fully investigated by spectroscopic (IR, UV-vis, EPR, MALDI-TOF MS), X-ray diffraction, potentiometric, electrochemical, and spectroelectrochemical methods. This constrained receptor possesses a hemispherical cavity created by cross-bridging the 1 and 8 positions of trans-dioxocyclam (1,4,8,11-tetraazacyclotetradecane-5,12-dione, L2) with a 2,6-pyridyl strap. Treatment of L1 with a copper salt in methanol produces a red complex of [Cu(L1H(-1))]+ formula in which the copper atom is embedded in a 13-membered ring and coordinated by both amines as well as the pyridine and one deprotonated amide nitrogen atoms. Infrared spectroscopy provides evidence for protonation of the carbonyl oxygen atom belonging to the copper-bound amide of [Cu(L1H(-1))]+ under strongly acidic conditions. The resulting conversion of the amidate into an iminol group highlights the inert character of the corresponding complexes, which do not dissociate at low pH values. In contrast, both secondary amides of L1 deprotonate in the presence of a weak base, thus affording a blue pentacoordinated [Cu(L1H(-2))] compound where the copper atom sits in the center of the 14-membered dioxocyclam fragment. In aqueous solution, both complexes undergo a pH-driven (pK(a) = 8.73(2)) molecular reorganization, which is reminiscent of a glider motion. The copper(II) cation switches rapidly and reversibly from a four-coordinate flattened tetrahedral arrangement of the donor atoms in the red species to a five-coordinate environment in the blue species, which is intermediate between a square pyramid and a trigonal bipyramid. Conversion of the red to the blue form was also demonstrated to occur upon reduction of [Cu(L1H(-1))]+ by cyclic voltammetry (E(pc) = -0.64 V/SCE in CH(3)CN).

  7. Synthesis and Characterization of Magnesium Hydroxide Nanoparticles via Hydrothermal Method

    OpenAIRE

    Sierra-Fernandez, A.; Flores-Carrasco, Gregorio; Gómez-Villalba, Luz Stella; Milošević, Olivera; Fort, R.; Rabanal, Maria Eugenia

    2014-01-01

    The interest in the nanostructured magnesium hydroxide (Mg(OH)2) is rapidly growing due to the fact that its physical and chemical properties makes it appropriate for multiple applications. So far, it has been used in medicine, industry, or more recently, in the conservation of cultural heritage. The current research is based on the synthesis and the characterization of functional and nanocrystalline Mg(OH)2 with different particle sizes, morphologies and high purity. The synthesis was carrie...

  8. Zeolite from fly ash: synthesis and characterization

    Indian Academy of Sciences (India)

    Unknown

    scanning electron microscopy, Fourier transform infrared spectroscopy, BET method for surface area mea- surement etc. The synthesis conditions were optimized to obtain highly crystalline ... Mondragón et al 1990; Yang and Kirkpatrick 1990; Shige- moto et al 1992; Lin and Hsi 1995; Park and Choi 1995;. Shin et al 1995; ...

  9. Synthesis and characterization of saturated polyester and ...

    Indian Academy of Sciences (India)

    and nanocomposites derived from glycolyzed PET waste with varied compositions. SUNAIN KATOCH. ∗ ... Water vapour transmission (WVT) was determined for saturated polyester nanocomposite sheets according to ... ing the synthesis of saturated polyester (from GPET waste). This has been done for the estimation of the ...

  10. electrochemical synthesis and spectroscopic characterization of poly ...

    African Journals Online (AJOL)

    a

    The films electrodeposited on these electrode surfaces constitute promising materials for practical applications [8-10], owing to their good environmental stability, electrical conductivity, mechanical and luminescence properties. The synthesis and corrosion protection ability of conducting polymer films have been studied.

  11. Synthesis and characterization of silver molybdate nanowires ...

    Indian Academy of Sciences (India)

    Wintec

    organic free hydrothermal process using ammonium molybdate and silver nitrate solutions. The powder X-ray diffraction ... luminescence (PL) spectrum exhibits UV emission at 335 nm, violet emission at 408 nm and a weak green emission at 540 nm. ... Few reports are related to the synthesis of metal molybdates through ...

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

    African Journals Online (AJOL)

    Figure 1: Biologically active pyrazole and barbituric acid scaffolds. Scheme-1: Protocol for the synthesis of 4a-o .... preparation of 4a-o was ensued via cascade. Aldol-Michael addition of N,N-dimethyl barbituric ..... Woessner KM, Simon RA, Stevenson DD. The safety of celecoxib in patients with aspirin‐sensitive asthma.

  13. Synthesis, spectral characterization and in vitro antibacterial ...

    African Journals Online (AJOL)

    Shafqat Nadeem

    2015-12-17

    Dec 17, 2015 ... analysis. Abstract The paper emphasizes on the synthesis of Palladium(II) iodide complexes containing based ligands. The new ... tural chemistry and biological properties of Palladium–sulfur interaction, in this paper, we .... The antibacterial activity of all synthesized metal complexes has been investigated ...

  14. synthesis, optical and electrochemical characterization of ...

    African Journals Online (AJOL)

    a

    containing polyfluorene copolymers (P1-P3) have been synthesized and characterized. The preparation and characterization of the corresponding blue light-emitting devices are also reported. Polymers P2 and P3 show high photoluminescence.

  15. 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.

  16. Platinum acetate blue: synthesis and characterization.

    Science.gov (United States)

    Cherkashina, Natalia V; Kochubey, Dmitry I; Kanazhevskiy, Vladislav V; Zaikovskii, Vladimir I; Ivanov, Vladimir K; Markov, Alexander A; Klyagina, Alla P; Dobrokhotova, Zhanna V; Kozitsyna, Natalia Yu; Baranovsky, Igor B; Ellert, Olga G; Efimov, Nikolai N; Nefedov, Sergei E; Novotortsev, Vladimir M; Vargaftik, Michael N; Moiseev, Ilya I

    2014-08-18

    Platinum acetate blue (PAB) of the empirical formula Pt(OOCMe)2.5±0.25, a byproduct in the synthesis of crystalline platinum(II) acetate Pt4(OOCMe)8, is an X-ray amorphous substance containing platinum in the oxidation state between (II) and (III). Typical PAB samples were studied with X-ray diffraction, differential thermal analysis-thermogravimetric, extended X-ray absorption fine structure, scanning electron microscopy, transmission electron microscopy, magnetochemistry, and combined quantum chemical density functional theory-molecular mechanics modeling to reveal the main structural features of the PAB molecular building blocks. The applicability of PAB to the synthesis of platinum complexes was demonstrated by the preparation of the new homo- and heteronuclear complexes Pt(II)(dipy)(OOCMe)2 (1), Pt(II)(μ-OOCMe)4Co(II)(OH2) (2), and Pt(III)2(OOCMe)4(O3SPhMe)2 (3) with the use of PAB as starting material.

  17. Synthesis and Characterization of Pyridine Functionalized ...

    African Journals Online (AJOL)

    picolyl) imidazolium salts (1). Treatment of the synthesized imidazolium salt with silver(I) oxide resulted in the formation of bis NHC silver(I) complex (2). The compound was characterized spectroscopically (NMR, mass spectrometry), by elemental ...

  18. Synthesis and characterization of thermotropic liquid crystalline ...

    Indian Academy of Sciences (India)

    The synthesised mesogens were characterized by different techniques including nuclear magnetic resonance and Fourier transform infrared spectroscopy. Liquid crystalline polymers (LCPs) were synthesised using pyromellitic dianhydride and 4-[(4-aminobenzylidene)amino]aniline or 4-aminophenyl-4-aminobenzoate.

  19. Synthesis, characterization and electrochemistry of heterobimetallic ...

    African Journals Online (AJOL)

    dimethylpyrazolyl) borate with a series of manganese(II) Schiff bases have been synthesized. Characterization by UV, IR, MS and elemental analysis support their formulations. Cyclic and differential pulse voltammograms of manganese(II) Schiff base ...

  20. Synthesis and characterization of germa[n]pericyclynes.

    Science.gov (United States)

    Tanimoto, Hiroki; Nagao, Tomohiko; Nishiyama, Yasuhiro; Morimoto, Tsumoru; Iseda, Fumiyasu; Nagato, Yuko; Suzuka, Toshimasa; Tsutsumi, Ken; Kakiuchi, Kiyomi

    2014-06-14

    The synthesis and characterization of novel pericyclynes comprising germanium atoms and acetylenes, germa[n]pericyclynes, are described. The prepared germa[4]-, [6]-, and [8]pericyclynes were compared by (13)C NMR spectroscopy, X-ray crystallography, cyclic voltammetry, UV-visible spectroscopy, fluorescence emission spectroscopy, Raman spectroscopy, and density functional theory calculation analyses.

  1. Synthesis, characterization and emission properties of quinolin-8 ...

    Indian Academy of Sciences (India)

    Home; Journals; Journal of Chemical Sciences; Volume 116; Issue 5. Synthesis, characterization and emission properties of quinolin-8-olato chelated ruthenium ... Author Affiliations. Bikash Kumar Panda1. Department of Inorganic Chemistry, Indian Association for the Cultivation of Science, Kolkata 700 032, India ...

  2. Synthesis, characterization and emission properties of quinolin-8 ...

    Indian Academy of Sciences (India)

    Unknown

    Synthesis, characterization and emission properties of quinolin-8-olato chelated ruthenium organometallics. BIKASH KUMAR PANDA. Department of Inorganic Chemistry, Indian Association for the Cultivation of Science, Kolkata 700 032,. India e-mail: b_panda@hotmail.com. MS received 2 June 2004; revised 21 July 2004.

  3. Synthesis & Characterization of New bis-Symmetrical Adipoyl ...

    African Journals Online (AJOL)

    Full Title: Synthesis and Characterization of New bis-Symmetrical Adipoyl, Terepthaloyl, Chiral Diimido-di-L-alanine Diesters and Chiral Phthaloyl-L-alanine Ester of Tripropoxy p-tert-Butyl Calix[4]arene and Study of Their Hosting Ability for Alanine and Na+. Bis-symmetrical tripropoxy p-tert-butyl calix[4]arene esters were ...

  4. Large scale synthesis and characterization of Ni nanoparticles by ...

    Indian Academy of Sciences (India)

    ... Refresher Courses · Symposia · Live Streaming. Home; Journals; Bulletin of Materials Science; Volume 31; Issue 1. Large scale synthesis and characterization of Ni nanoparticles by solution reduction method. Huazhi Wang Xinli Kou Jie Zhang Jiangong Li. Nanomaterials Volume 31 Issue 1 February 2008 pp 97-100 ...

  5. Synthesis and characterization of zinc oxide thin films prepared by ...

    African Journals Online (AJOL)

    Synthesis and characterization of zinc oxide thin films prepared by chemical the bath technique. ... The band gap energy of the samples deduced from the fundamental absorption edge gave the values of 1.60 – 2.80 eV for the direct ... Keywords: Chemical bath technique, zinc oxide thin films, x-ray, photovoltaic cells ...

  6. Synthesis and characterization of magnetite/hydroxyapatite tubes ...

    Indian Academy of Sciences (India)

    Synthesis and characterization of magnetite/HAp tubes. 515 oxide nanoparticles on kapok fibre can be visualized under. FE-SEM. The air entrapment inside the fibre disappeared after coating with iron oxide nanoparticle. The structure became completely flattened. The overall tubular structure was retained and unbroken.

  7. Synthesis, surface characterization and optical properties of 3 ...

    Indian Academy of Sciences (India)

    Home; Journals; Bulletin of Materials Science; Volume 34; Issue 5. Synthesis, surface characterization and optical properties of 3-thiopropionic acid capped ZnS:Cu nanocrystals ... The optical studies were done using UV-VIS spectroscopy and particle size and diameter polydispersity index (DPI) were calculated.

  8. Synthesis and characterization of six-membered pincer ...

    Indian Academy of Sciences (India)

    Home; Journals; Journal of Chemical Sciences; Volume 129; Issue 8. Synthesis and characterization of six-membered pincer nickelacycles and application in alkylation of benzothiazole. HANUMANPRASAD PANDIRI DIPESH M SHARMA RAJESH G GONNADE BENUDHAR PUNJI. REGULAR ARTICLE Volume 129 Issue ...

  9. Synthesis and characterization of mixed ligand complexes of Zn (II ...

    Indian Academy of Sciences (India)

    Home; Journals; Journal of Chemical Sciences; Volume 117; Issue 3. Synthesis and characterization of mixed ligand complexes of Zn(II) and Co(II) with amino acids: Relevance to zinc binding sites in zinc fingers. P Rabindra Reddy M Radhika P Manjula. Volume 117 Issue 3 May 2005 pp 239-246 ...

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

    Indian Academy of Sciences (India)

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

  11. Synthesis and Characterization of a Schiff Base Cobalt (III) Complex ...

    African Journals Online (AJOL)

    2017-12-18

    Dec 18, 2017 ... Synthesis and Characterization of a Schiff Base Cobalt (III) Complex and. Assessment of its Anti-Cancer Activity. Gwaram, N. S.. Department of Pure and Industrial Chemistry, Umaru Musa Yar'Adua University. P.M.B. 2211, Katsina, ... compounds of cobalt, copper, nickel, manganese, zinc, palladium ...

  12. synthesis and spectra characterization of mixed- ligand complexes ...

    African Journals Online (AJOL)

    BARTH EKWUEME

    “Let's Twist Again”-Double-Stranded,. Triple-Stranded, and Circular Helicates. Chemical Reviews 101(11): 3457-3498. Belfrekh, N., Dietrich-Buchecker, C. and Sauvage, J. P.. 2000. Synthesis and Characterization of Dinuclear Metal. Complexes Stabilized by Tetradentate Schiff base ligands.Inorganic Chemistry 39: 5169-.

  13. Synthesis, spectral characterization and antihaemostatic activity of 1 ...

    Indian Academy of Sciences (India)

    Home; Journals; Journal of Chemical Sciences; Volume 118; Issue 2. Synthesis, spectral characterization and antihaemostatic activity of 1,2,4-triazoles ... Author Affiliations. Ravindra R Kamble1 Belgur S Sudha1. Department of Chemistry and Food Science, Yuvaraja's College, University of Mysore, Mysore 570 005 ...

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

    DEFF Research Database (Denmark)

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

    2009-01-01

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

  15. Synthesis and characterization of super-microporous material with ...

    Indian Academy of Sciences (India)

    Administrator

    Synthesis and characterization of super-microporous material with enhanced hydrothermal stability. SHUJIE WU, KE SONG, JINGQI GUAN and QIUBIN KAN*. College of Chemistry, Jilin University, Changchun 130023, P.R. China. MS received 9 July 2009; revised 18 November 2009. Abstract. Super-microporouos silicon ...

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

    Indian Academy of Sciences (India)

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

  17. Synthesis and characterization of thermally stable oligomer-metal ...

    African Journals Online (AJOL)

    Synthesis and characterization of thermally stable oligomer-metal complexes of copper(II), nickel(II), zinc(II) and cobalt(II) derived from oligo- p - nitrophenylazomethinephenol. ... The properties of oligomer-metal complexes were studied by elemental, FT-IR and magnetic moments analyses. The thermal stabilities of the ...

  18. SYNTHESIS AND CHARACTERIZATION OF AN OXO-BRIDGED ...

    African Journals Online (AJOL)

    a

    SYNTHESIS AND CHARACTERIZATION OF AN OXO-BRIDGED RHENIUM(V). COMPLEX WITH AN AMINE-PHENOL TETRADENTATE LIGAND. A. Abrahams1, T.I.A. Gerber1* and Peter Mayer2. 1Department of Chemistry, Nelson Mandela Metropolitan University, P.O. Box 77000, 6031. Port Elizabeth, South Africa.

  19. 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.

  20. Synthesis, characterization, sintering and dielectric properties of ...

    Indian Academy of Sciences (India)

    Nanoparticles of barium gadolinium antimonate (Ba2GdSbO6), a complex perovskite-type oxide, has been synthesized using an auto ignition combustion process for the first time. The nanoparticles thus obtained have been characterized by powder X-ray diffraction, thermogravimetric analysis, differential thermal analysis, ...

  1. SYNTHESIS, CHARACTERIZATION OF BIOLOGICALLY ACTIVE N ...

    African Journals Online (AJOL)

    DR. AMINU

    2013-12-02

    Dec 2, 2013 ... complex were characterized by solubility, melting point/decomposition temperature, molar .... allowed to cool in an ice bath and the greenish yellow ... of the cobalt(II) Schiff base complex. Table 1: Physical properties of the Schiff base ligand and its cobalt(II) complex. Compound. Colour. Melting point(oC).

  2. Synthesis, Characterization and Antimicrobial Activities of Some ...

    African Journals Online (AJOL)

    Some transition metal complexes of nicotinamide have been prepared and characterized using melting point, conductivity measurement, infrared, electronic, HNMR and atomic absorption spectroscopic methods. . The antibacterial and antifungal studies of the metal complexes and the ligand have been evaluated against ...

  3. Synthesis, characterization and studies on antioxidant and ...

    Indian Academy of Sciences (India)

    Abstract. In the present study, a new thiourea derivative bearing benzothiazole ligand, 1-(benzo[d]thiazol-2- yl)thiourea (btt) and its ternary metal (Cu(II), Co(II) and Ni(II)) complexes were synthesized. The structural characterization was carried out by micro analysis, IR, 1H-NMR, EPR, UV-Visible spectral analyses, molar.

  4. Synthesis and characterization of multicolour fluorescent ...

    Indian Academy of Sciences (India)

    In this study, we successfully developed Y 2 O 3 nanoparticles doped with Tb 3 + and Eu 3 + ions to generate fluorescent images of latent fingerprints. The optical and structural characterization of the nanoparticles was carried out and the fluorescence mechanisms are discussed. In our studies, the developed nanoparticles ...

  5. Synthesis and Characterization of Pyridine Functionalized ...

    African Journals Online (AJOL)

    MBI

    2013-06-26

    Jun 26, 2013 ... ABSTRACT. Reaction of imidazole with two equivalent of 2-picolyl chloride afforded bis (2-picolyl) imidazolium salts (1). Treatment of the synthesized imidazolium salt with silver(I) oxide resulted in the formation of bis NHC silver(I) complex (2). The compound was characterized spectroscopically (NMR, ...

  6. Synthesis, spectrometric characterization and trypanocidal activity of ...

    African Journals Online (AJOL)

    ... Coupled with High-Performance Liquid Chromatography) and they were characterized using spectrometry IR, NMR 1H and 13C (Nuclear Magnetic Resonance). These compounds were then tested in vitro on Trypanosoma brucei brucei according to the “LILIT, Alamar Blue” method to estimate their trypanocidal activity.

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

    Indian Academy of Sciences (India)

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

  8. Synthesis, characterization and thermal properties of thiosalicylate ...

    Indian Academy of Sciences (India)

    The compounds were characterized by Infra Red (IR), Nuclear Magnetic Resonance (NMR) and mass spectra (ESI-MS). Their glass-transition temperatures, ... Fadwa Babiker Mustafa1. Fundamental and Applied Sciences Department, Universiti Teknologi PETRONAS, Bandar Seri Iskandar, 31750 Tronoh, Perak, Malaysia ...

  9. Synthesis, characterization and applications of nanostructural ...

    Indian Academy of Sciences (India)

    The compounds are characterized by XRD, TG-DTA, SEM, TEM, surface area and porosity measurements. Because of the porous nature having large surface area (107 ... MgO powder as adsorbent [6] for the removal of fluoride content in ground water. Among the available wet chemical processes, combustion technique is ...

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

    African Journals Online (AJOL)

    The nanoporous particles were characterized by UV (ultraviolet (UV) visible spectroscopy and dynamic light scattering (DLS) while a zetasizer was applied to determine their average particle size. Their surface morphology and shape were assessed by transmission electron microscopy (TEM) and scanning election ...

  11. Synthesis, characterization and antimicrobial activity of mixed ...

    African Journals Online (AJOL)

    The present study aimed at synthesizing copper(II) and zinc(II) complexes of mixed ascorbic acid and nicotinamide and physiochemically characterize by solubility test, melting point, conductivity test, infrared, electronic and proton nuclear magnetic resonance techniques. The result of the physiochemical studies indicated ...

  12. Synthesis, characterization and ion exchange properties of ...

    Indian Academy of Sciences (India)

    The material has been characterized on the basis of chemical composition, pH titration, Fourier transform infrared spectroscopy (FTIR) and thermogravimetric analysis. The effect on the exchange capacity of drying the exchanger at different temperatures has been studied. The analytical importance of the material has been ...

  13. Synthesis and characterization of superabsorbent hydrogel based ...

    African Journals Online (AJOL)

    In this work, acrylonitrile (AN) and acrylic acid (AA) monomers were directly grafted onto chitosan using ammonium persulfate (APS) as an initiator and methylenebisacrylamide (MBA) as a crosslinking agent under an inert atmosphere. The hydrogels structure was characterized by Fourier transform infrared (FTIR) ...

  14. Synthesis, physical characterization, antibacterial activity and ...

    African Journals Online (AJOL)

    Some five-coordinated cobalt(III) complexes were synthesized and characterized using elemental analysis, 1H NMR and IR spectra. The formation constants and the thermodynamic parameters were measured spectrophotometrically for the 1:1 adduct formation of [Co(Chel)(PBu3)]ClO4.H2O where Chel = cd3OMesalen, ...

  15. Synthesis, characterization and conductivity studies of polypyrrole ...

    Indian Academy of Sciences (India)

    The polypyrrole–fly ash composites were also characterized by employing X-ray diffractometry (XRD) and infrared spectroscopy (IR). ... Department of Physics, GM Institute of Technology, Davangere 577 006, India; Department of Physics, KBN College of Engineering, Gulbarga 585 104, India; Department of Materials ...

  16. Synthesis and characterization of fluorophore attached silver ...

    Indian Academy of Sciences (India)

    Silver nanoparticles stabilized by soluble starch were synthesized and characterized. in vivo studies in rats showed no toxicity and revealed their distribution in various tissues and permeability across BBB. This starch stabilized silver nanoparticles have good biological characteristics to act as a potential promising vector for ...

  17. Synthesis, characterization and electrochemical performance of ...

    Indian Academy of Sciences (India)

    The crystalstructure of prepared samples of Li 2 Ni x Fe 1 − x SiO 4 was characterized using an X-ray diffractometer. Different crystallographicparameters such as crystallite size and lattice cell parameters have been calculated. Scanning electron microscopy andFourier transform infrared spectroscopy investigations were ...

  18. Synthesis, characterization and antimicrobial screening of hybrid ...

    Indian Academy of Sciences (India)

    chloroquinolin-3-yl)-6-(aryl)pyrimidin-2-yl)-2-morpholinoacetamides (5a-l) were synthesized by multistep reactions. Compounds were characterized by IR, NMR and mass spectra. Antimicrobial screening of title compounds (5a-l) was carried out ...

  19. Synthesis and Characterization of Tolvaptan Impurities

    Directory of Open Access Journals (Sweden)

    Madhuresh Kumar Sethi

    2014-01-01

    Full Text Available Twenty-six possible as well as observed impurities during the preparation of Tolvaptan have been identified, prepared, and characterized by HPLC (high performance liquid chromatography, NMR (nuclear magnetic resonance, and mass spectra. Control of these impurities, formed during various stages of Tolvaptan preparation, has been mentioned in this paper.

  20. Synthesis and Characterization of Tolvaptan Impurities

    OpenAIRE

    Madhuresh Kumar Sethi; Vijendra Singh Rawat; Jayaprakash Thirunavukarasu; Rajakrishna Yerramalla; Anish Kumar

    2014-01-01

    Twenty-six possible as well as observed impurities during the preparation of Tolvaptan have been identified, prepared, and characterized by HPLC (high performance liquid chromatography), NMR (nuclear magnetic resonance), and mass spectra. Control of these impurities, formed during various stages of Tolvaptan preparation, has been mentioned in this paper.

  1. Synthesis, spectral characterization and in vitro antibacterial ...

    African Journals Online (AJOL)

    Shafqat Nadeem

    2015-12-17

    Dec 17, 2015 ... GPCR L = GPCR ligand, ICM = ion channel modulator, KI = kinase inhibitor, NRL = nuclear receptor ligand, PI = protease inhibitor,. EI = enzyme inhibitor. New Palladium(II) iodide complexes ... PSA has been shown to be a very good descriptor characterizing drug absorption, including intestinal absorp-.

  2. Synthesis, characterization and ion exchange properties of ...

    Indian Academy of Sciences (India)

    zirconium(IV) oxychloride. Its ion exchange capacity for Na+ and K+ was found to be 2⋅20 and 2⋅35 meq g–1 dry exchanger, respectively. The material has been characterized on the basis of chemical composition, pH titration, Fourier transform infrared spectroscopy (FTIR) and thermogravimetric analysis. The effect on the.

  3. Biological synthesis and characterization of silver nanoparticles ...

    Indian Academy of Sciences (India)

    The biosynthesis of silver nanoparticles (AgNPs) using plant extracts became one of the potential areas ... Biosynthesized AgNPs were characterized by the help of UV–visible spectroscopy for their stability and physicochemical ... spectroscopy, X-ray diffraction, scanning electron microscopy. The obtained results confirmed ...

  4. 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.

  5. 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.

  6. Synthesis, characterization and performance of bifunctional catalysts for the synthesis of menthol from citronellal

    NARCIS (Netherlands)

    ten Dam, J.; Ramanathan, A; Djanashvili, K.; Kapteijn, F.; Hanefeld, U.

    2017-01-01

    The synthesis of a series of bifunctional catalysts (1 wt% Pt/W-TUD-1 (Technische Universiteit Delft-1) and 1 wt% Pt/WO3/TUD-1) with different tungsten loadings (5-30 wt% WO3) is described. They were characterized using ICP-OES, INAA, N2 physisorption, XRD and

  7. 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.

  8. Carbon nanotubes: synthesis, structure, functionalization, and characterization.

    Science.gov (United States)

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

    2014-01-01

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

  9. Synthesis and characterization of Co nanoparticles

    Science.gov (United States)

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

    2017-05-01

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

  10. Use of two artificial sweeteners, cyclamate and acesulfame, to identify and quantify wastewater contributions in a karst spring.

    Science.gov (United States)

    Zirlewagen, Johannes; Licha, Tobias; Schiperski, Ferry; Nödler, Karsten; Scheytt, Traugott

    2016-03-15

    The identification and differentiation of different sources of contamination are crucial aspects of risk assessment in water resource protection. This is especially challenging in karst environments due to their highly heterogeneous flow fields. We have investigated the use of two artificial sweeteners, cyclamate and acesulfame, as an indicator set for contamination by wastewater within the rural catchment of a karst spring. The catchment was investigated in detail to identify the sources of artificial sweeteners and quantify their impact. Spring water was analysed following two different but typical recharge events: (1) a rain-on-snow event in winter, when no wastewater overflow from the sewer system was observed, and (2) an intense rainfall event in summer triggering an overflow from a stormwater detention basin. Acesulfame, which is known to be persistent, was quantified in all spring water samples. Its concentrations decreased after the winter event with no associated wastewater spillage but increased during the summer event following a recent input of untreated wastewater. Cyclamate, which is known to be degradable, was only detected following the wastewater inflow incident. The cyclamate signal matched very well the breakthrough of faecal indicator bacteria, indicating a common origin. Knowing the input function, cyclamate was used quantitatively as a tracer in transport modelling and the impact of 'combined sewer overflow' on spring water quality was quantified. Signals from artificial sweeteners were compared to those from bulk parameters (discharge, electrical conductivity and turbidity) and also to those from the herbicides atrazine and isoproturon, which indicate 'old' and 'fresh' flow components, respectively, both originating from croplands. High concentration levels of the artificial sweeteners in untreated wastewater (cyclamate and acesulfame) and in treated wastewater (acesulfame only) make them powerful indicators, especially in rural settings

  11. Synthesis and characterization of carboxymethyl tamarind

    Directory of Open Access Journals (Sweden)

    Shunwei WU

    2015-10-01

    Full Text Available Series of carboxymethyl tamarind kernel polysaccharide (CMTKP with different degree of substitution (DS were prepared by the reactions of tamarind kernel polysaccharide (TKP and sodium monochloroacetic acid (SMCA in alkaline aqueous isopropanol. The influence of mole ratio of NaOH to SMCA, SMCA concentration, reaction temperature and time on DS, reaction efficiency (RE as well as the transmittance and apparent viscosity of CMTKP aqueous solution was investigated. The maximum DS of 0.92 and the RE of 77% were obtained. The solubility of CMTKP in cold water and the freeze-thaw stability were apparently improved and the transmittance of the mass fraction of 2% CMTKP aqueous solution could be up to 97%. Thermal stability decreased showed by TGA, and crystalline region reduced with the increasing of DS after carboxymethylation showed by XRD. The structure was characterized by FT-IR and solid-state 13C NMR.

  12. 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,...

  13. 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.

  14. Synthesis and Physicochemical Characterization of Chitin Derivatives

    Directory of Open Access Journals (Sweden)

    İlhan Uzun

    2013-01-01

    Full Text Available Firstly, chitin derivatives were synthesized. For this purpose, chitin was modified via ring-opening reaction with cyclic anhydrides in lithium chloride/N,N-dimethylacetamide. Then, chitin derivatives synthesized were characterized by FTIR, 1H NMR, 13C NMR, and U-Vis spectroscopies and scanning electron microscopy. Thermogravimetric analysis was performed to investigate the thermal stability of chitin derivatives. Thermogravimetric analysis results showed that chitin modified with trimellitic anhydride is thermally more stable than chitin modified with phthalic anhydride. In addition, the electrical conductivity of chitin modified with phthalic anhydride and trimellitic anhydride was also measured. Electrical conductivity measurement results showed that the electrical conductivity of chitin modified with trimellitic anhydride (1.2×10−4 S cm−1 is higher than that of chitin modified with phthalic anhydride (9.2×10−5 S cm−1.

  15. Synthesis and characterization of thermoplastic polyphenoxyquinoxalines

    Science.gov (United States)

    Erdem, Haci Bayram

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

  16. Synthesis and electrochemical characterization of substituted indolizine carboxylates

    Directory of Open Access Journals (Sweden)

    Soare Maria-Laura

    2013-01-01

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

  17. Synthesis and characterization of PbTe micro/nanostructures ...

    Indian Academy of Sciences (India)

    Administrator

    2.1 Materials and characterization. All the reagents for the synthesis of the capping agent and PbTe micro/nanostructures such as 1,8-diamino-3,6- dioxaoctane, 2-hydroxybenzophenone, methanol, Pb(NO3)2,. Te powder, ethylene glycol, hydrazine hydrate (N2H4⋅. H2O) and NaOH were purchased from Merck company.

  18. Open-Framework Germanates and Nickel Germanates : Synthesis and Characterization

    OpenAIRE

    Huang, Shiliang

    2012-01-01

    Microporous materials have a wide range of important applications in separation, gas adsorption, ion-exchange and catalysis. Open-framework germanates are a family of microporous compounds and are of particular interest. This thesis focuses on the synthesis and characterization of new open-framework germanates as well as introducing the transition-metal nickel into germanate structures. One new microporous germanosilicate, SU-78 and four new open-framework germanates, SU-74, SU-75, SU-69 and ...

  19. Synthesis and characterization of copper nanostructures on silicon substrates

    Energy Technology Data Exchange (ETDEWEB)

    Kanitkar, P; Aiyer, R C [Department of Physics, University of Pune, Pune 411 007, Maharashtra (India); Sen, S; Muthe, K P; Gupta, S K [Technical Physics and Prototype Engineering Division(TPPED), BARC, Mumbai 400 085, Maharashtra (India)], E-mail: drgupta@barc.gov.in

    2008-05-01

    Vacuum vapour deposition technique has been utilized for the synthesis of copper nanostructures on Si(111), Si(100) and Si(110) substrates at an optimized substrate temperature of 750 deg. C. The samples are characterized by SEM, AFM and XPS. Their morphology is strongly governed by orientation of substrate. It is possible to realize the growth of triangular, square like and rod shaped geometries by choosing an appropriate orientation. This variation is attributed to the surface reconstruction which occurs at high temperature.

  20. Synthesis and optical characterization of interactive nanosystems

    Science.gov (United States)

    Yasmin, Zannatul

    The use of interactive nanosystems (INSs) has unique advantages in sensing applications. Due to their multivalent interactions and stimuli responsiveness i.e. chemical, optical, pH, these adaptive networks can enhance sensing applications. In this work, two distinct INSs are synthesized and the interparticle interactions are probed optically. One of them is the gold nanoparticles based INS in presence of the biomolecule, glutathione. Their unique optical properties and surface binding affinity to thiol-containing glutathione provide an intriguing opportunity to probe bio-systems. The second one is the rare earth oxides/fluorides conjugated with gold nanoparticles based INS which exhibit tunabilty in their multi-wavelength absorbance and emission through coupling with the surface plasmon resonance of gold nanoparticles. The conjugation of these two interactive particles is uniquely synthesized in the presence of the bio-polymer chitosan. This structure displays tunable optical properties. The two novel INSs presented are characterized through their optical signatures using various spectroscopies including a novel approach developed in this work that comprises an all optical photoacoustic spectroscopy (AOPAS). The AOPAS technique is used to determine the unique characteristics of these INSs in aqueous environments by measuring their optical properties in situ. Additionally, we expect the AOPAS technique will provide unique information about nano-bio interfaces and the usefulness of INS as sensors in biological systems without the artifacts limiting the use of current methods, such as fluorescence-based indicators.

  1. NiO Nanoparticles: Synthesis and Characterization

    Directory of Open Access Journals (Sweden)

    A. Rahdar

    2015-04-01

    Full Text Available In the current paper,Nanostructured Nickel oxide (NiO were synthesized by co-precipitation method using Nickel(II Chloride Hexahydrate (NiCl2.6H2O and sodium hydroxide (NaOH as starting material. Structural, optical and magnetic properties of nanostructures were characterized by X-ray diffraction (XRD, scanning electron microscopy (SEM, Atomic force microscope (AFM, UV–Vis absorption; Fourier transformed infrared (FTIR and vibrating sample magnetometer (VSM technique. The X-ray diffraction pattern studies revealed the NiO have a  face-centered cubic (FCC structure and confirmed the presence of high degree of crystallinity nature NiO nanoparticles that their average size is found to be 26 nm. The composition of nanostructures confirmed by analysis of FTIR spectra. The average size of the NiO nanoparticle observed from scanning electron microscopy images is found to be dimensions about 24 nm. Magnetic measurement confirmed the Nickel Oxide nanostructures superparamagnetic behavior at room temperature (RT after calcinations.

  2. Synthesis and Characterization of Barium Hexafluoridoosmates

    Directory of Open Access Journals (Sweden)

    Sergei I. Ivlev

    2017-12-01

    Full Text Available Two barium hexafluoridoosmates, Ba(OsF62 and BaOsF6, were synthesized and were characterized for the first time using X-ray powder and single crystal diffraction, IR spectroscopy, as well as NMR spectroscopy in anhydrous hydrogen fluoride. Ba(OsF62 crystallizes in the space group type P21/c with the cell parameters a = 6.4599(4, b = 10.7931(8, c = 14.7476(10 Å, β = 115.195(5°, V = 930.42(12 Å3, Z = 4 at 293 K. BaOsF6 crystallizes in the space group type R 3 ¯ with the cell parameters a = 7.3286(10, c = 7.2658(15 Å, V = 337.95(12 Å3, Z = 3 at 100 K. Additionally, we have obtained the compounds Ba(OsF62∙3BrF3, Ba(OsF62∙HF, Ba(OsF62∙6H2O from the respective solvents, and Ba(OsF62.

  3. Synthesis, characterization and magnetic evaluation of praseodymium modified cerium oxide

    Science.gov (United States)

    Cruz Pacheco, A. F.; Gómez Cuaspud, J. A.; Parra Vargas, C. A.

    2017-01-01

    This paper report the synthesis, characterization and magnetic evaluation of Ce0.6Pr0.4O2 system using a chemical route that involves the combustion of citrate species. The precursors were characterized by Fourier transform infrared spectroscopy (FTIR), to identify, the main vibrational bands associated with the organic material after combustion process. The structural analysis by X-ray diffraction (XRD) revealed the obtaining of an Fm-3m (225) cubic phase with a particle size around 10nm. Finally, the measurement of the magnetization as a function of applied magnetic field and of susceptibility showed a perfect paramagnetic behaviour.

  4. Carbon nanotubes: Synthesis, characterization, and applications

    Science.gov (United States)

    Deck, Christian Peter

    Carbon nanotubes (CNTs) possess exceptional material properties, making them desirable for use in a variety of applications. In this work, CNTs were grown using two distinct catalytic chemical vapor deposition (CVD) procedures, floating catalyst CVD and thermal CVD, which differed in the method of catalyst introduction. Reaction conditions were optimized to synthesize nanotubes with desired characteristics, and the effects of varying growth parameters were studied. These parameters included gas composition, temperature, reaction duration, and catalyst and substrate material. The CNT products were then examined using several approaches. For each CVD method, nanotube growth rates were determined and the formation and termination mechanisms were investigated. The effects of reaction parameters on nanotube diameters and morphology were also explored to identify means of controlling these important properties. In addition to investigating the effects of different growth parameters, the material properties of nanotubes were also studied. The floating catalyst CVD method produced thick mats of nanotubes, and the mechanical response of these samples was examined using in-situ compression and tension testing. These results indicated that mat structure is composed of discontinuous nanotubes, and a time-dependent response was also observed. In addition, the electrical resistance of bulk CNT samples was found to increase for tubes grown with higher catalyst concentrations and with bamboo morphologies. The properties of nanotubes synthesized using thermal CVD were also examined. Mechanical testing was performed using the same in-situ compression approach developed for floating catalyst CVD samples. A second characterization method was devised, where an optical approach was used to measure the deflection of patterned nanotubes exposed to an applied fluid flow. This response was also simulated, and comparisons with the experimental data were used to determine the flexural

  5. 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.

  6. 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

  7. Nanoscale Synthesis and Characterization Laboratory Annual Report 2007

    Energy Technology Data Exchange (ETDEWEB)

    Hamza, A V

    2008-04-07

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-09-25

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

  9. Synthesis and Characterization of Thymine-15N2

    Directory of Open Access Journals (Sweden)

    XU Jian-fei

    2016-02-01

    Full Text Available A novel and mild synthesis method of thymine-15N2 was designed. Ethyl formate and ethyl propionate as raw materials, the intermediate ethyl 2-formylpropionate was condensed under sodium metal, the target compound thymine-15N2 was obtained by condensation with isotope urea-15N2 under acid catalysis. Synthesis route had the advantages of simple operation, short process flow and less side product. The yield was more than 80% and isotope 15N abundance did not diluted. The product was characterized by HPLC, IR, MS, 1H NMR and 13C NMR. The chemical purity was more than 99% and 15N enrichment was more than 98 atom%.

  10. Synthesis and Reactive Characterization of Aluminum Iodate Hexahydrate Crystals

    Science.gov (United States)

    Smith, Dylan; Pantoya, Michelle

    A monomolecular aluminum based explosive crystal has been synthesized from aluminum particles dissolved in iodic acid solution. The precipitate from solution is aluminum iodate hexahydrate (Al(IO3)3 (HIO3)2 (H2O)6) , as confirmed by X-ray diffraction (XRD) analysis. The method of synthesis first dissolves iodine oxide in water, creating an IO3- solution with pH synthesis. Reactivity is characterized in terms of flame speed with measurements purposefully designed to capture less than 1% light emission, resulting in speeds as high as 3200 m/s for AIH + Al density of 3.43 g/cc. Army Research Office under award W911NF-14-1-0250, partial support from DTRA under award HDTRA1-15-1-0029.

  11. New Synthesis of TATB. Scaleup and Product Characterization

    Energy Technology Data Exchange (ETDEWEB)

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

    2000-03-15

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

  12. Synthesis and characterization of 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.

  13. Electrochemical synthesis and characterization of zinc oxalate nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Shamsipur, Mojtaba, E-mail: mshamsipur@yahoo.com [Department of Chemistry, Razi University, Kermanshah (Iran, Islamic Republic of); Roushani, Mahmoud [Department of Chemistry, Razi University, Kermanshah (Iran, Islamic Republic of); Department of Chemistry, Ilam University, Ilam (Iran, Islamic Republic of); Pourmortazavi, Seied Mahdi [Faculty of Material and Manufacturing Technologies, Malek Ashtar University of Technology, Tehran (Iran, Islamic Republic of)

    2013-03-15

    Highlights: ► Synthesis of zinc oxalate nanoparticles via electrolysis of a zinc plate anode in sodium oxalate solutions. ► Design of a Taguchi orthogonal array to identify the optimal experimental conditions. ► Controlling the size and shape of particles via applied voltage and oxalate concentration. ► Characterization of zinc oxalate nanoparticles by SEM, UV–vis, FT-IR and TG–DTA. - Abstract: A rapid, clean and simple electrodeposition method was designed for the synthesis of zinc oxalate nanoparticles. Zinc oxalate nanoparticles in different size and shapes were electrodeposited by electrolysis of a zinc plate anode in sodium oxalate aqueous solutions. It was found that the size and shape of the product could be tuned by electrolysis voltage, oxalate ion concentration, and stirring rate of electrolyte solution. A Taguchi orthogonal array design was designed to identify the optimal experimental conditions. The morphological characterization of the product was carried out by scanning electron microscopy. UV–vis and FT-IR spectroscopies were also used to characterize the electrodeposited nanoparticles. The TG–DTA studies of the nanoparticles indicated that the main thermal degradation occurs in two steps over a temperature range of 350–430 °C. In contrast to the existing methods, the present study describes a process which can be easily scaled up for the production of nano-sized zinc oxalate powder.

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

    Directory of Open Access Journals (Sweden)

    K. Basavaiah

    2012-01-01

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

  15. Synthesis and 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

  16. Synthesis, characterization, and antifouling potential of functionalized copper nanoparticles.

    Science.gov (United States)

    Anyaogu, Kelechi C; Fedorov, Andrei V; Neckers, Douglas C

    2008-04-15

    The synthesis, characterization, and antimicrobial properties of functionalized copper nanoparticle/polymer composites are reported. Copper nanoparticles (Cu NPs) are stabilized by surface attachment of the acrylic functionality that can be copolymerized with other acrylic monomers, thus, becoming an integral part of the polymer backbone. Biological experiments show that Cu NP/polymer composites exhibit antimicrobial activity similar to that of conventional copper-based biocides. Atomic absorption spectroscopy shows the smallest amount of copper ions leaching from chemically bound acrylated Cu NPs compared to the nonfunctionalized biocides. These composites have a strong potential for use in antibacterial or marine antifouling coatings.

  17. 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.

  18. Materials Research Society Symposium Proceedings Volume 635. Anisotropic Nanoparticles - Synthesis, Characterization and Applications

    National Research Council Canada - National Science Library

    Lyon, L

    2000-01-01

    This volume contains a series of papers originally presented at Symposium C, "Anisotropic Nanoparticles Synthesis, Characterization and Applications," at the 2000 MRS Fall Meeting in Boston, Massachusetts...

  19. 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.

  20. Synthesis and characterization of five-coordinated indium amidinates

    Energy Technology Data Exchange (ETDEWEB)

    Riahi, Yasaman

    2016-07-29

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

  1. Synthesis, complexation, and coordination oligomerization of 1,8-pyrazine-capped 5,12-dioxocyclams.

    Science.gov (United States)

    Hegedus, Louis S; Sundermann, Michael J; Dorhout, Peter K

    2003-07-14

    (Methyl)(methoxy)-5,12-dioxocyclam 1 was alkylated on the secondary amines (capped) with 2,6-bis(bromomethyl)pyrazine. The resulting macrocycle was complexed to copper(II) to produce a five-coordinate complex 5a which was fully characterized by a range of spectroscopic methods (IR, UV-vis, ESR) as well as by X-ray crystallography. The structure of this complex is similar to the previously reported pyridine complex, with the five-coordinate copper having distorted square pyramidal geometry and a Cu-Pz bond length of 2.125 A. Attempts to prepare this same complex under microwave irradiation instead produced a trinuclear complex 6a having an octahedral copper(II) center complexed to two pyrazine-cyclam copper units through the amide carbonyl oxygen and the methoxyl group oxygen of the cyclam unit. The X-ray crystal structure of the trinuclear complex showed extensive distortion in the cyclam rings. The remote nitrogen of pyrazine-cyclam complex 5a was capable of coordinating an additional metal. Treatment with RuCl(2)(DMSO)(4) or Rh(2)(OAc)(4), respectively, produced trimetallic Cu-Ru-Cu complex 7 or tetrametallic Cu-Rh-Rh-Cu complex 8. The latter was fully characterized, including an X-ray crystal structure, and had two pyrazine-cyclam complexes bridged by a Rh(2)(OAc)(4) unit through the remote pyrazine nitrogens. There was little distortion in the pyrazine-cyclam copper units as compared to complex 5a: the four metals were collinear, and the two cyclam units were eclipsed. All of the copper complexes were subjected to cyclic voltametry measurements, and no reversible redox changes were observed. Magnetic measurements of 6a and 8 showed the copper atoms to be weakly antiferromagnetically coupled.

  2. Piezoelectric nanostructures of zinc oxide: Synthesis, characterization and devices

    Science.gov (United States)

    Gao, Puxian

    In this thesis, a systematic study has been carried out on the synthesis, characterization and device fabrication of piezoelectric ZnO nanstructures. The achieved results are composed of the following four parts. Firstly, through a systematic investigation on the Sn-catalyzed ZnO nanostructure, an improved understanding of the chemical and physical process occurring during the growth of hierarchical nanostructures has been achieved. Decomposed Sn from SnO2 has been successfully demonstrated and proved to be an effective catalyst guiding the growth of not only aligned ZnO nanowires, but also the hierarchical nanowire-nanoribbon junction arrays and nanopropeller arrays. During the vapor-liquid-solid (VLS) catalyzing growth process at high temperature, Sn in the liquid state has been proved to be able to guide the growth of nanowires and nanoribbons in terms of growth directions, side facets, and crystallographic interfaces between Sn and ZnO nanostructures. Secondly, using pure ZnO as the only source material, by precisely tuning and controlling the growth kinetics, a variety of hierarchical polar surface dominated nanostructures have been achieved, such as single crystal nanorings, nanobows, nanosprings and superlattice nanohelices. High yield synthesis of ZnO nanosprings over 50% has been successfully obtained by mainly controlling the pre-pumping level associated with the partial pressure of residual oxygen during the vapor-solid growth process. The rigid superlattice nanohelices of ZnO have been discovered, which is a result of minimization of the electrostatic energy induced by polar surfaces. The formation process of the nanohelix has been systematically characterized. Thirdly, two new strategies have been successfully developed for fabricating ZnO quantum dots and synthesis of ZnO nanodiskettes and nanotubes. The formation process is based on a common concept of self-assembly. Finally, a series of devices and applications studies based on several piezoelectric

  3. Synthesis and characterization of related substances of Azilsartan Kamedoxomil

    Directory of Open Access Journals (Sweden)

    Maddi N. V. D. Harikiran

    2017-03-01

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

  4. Synthesis, characterization and antioxidant capacity of naringenin-oxime

    Science.gov (United States)

    Türkkan, Baki; Özyürek, Mustafa; Bener, Mustafa; Güçlü, Kubilay; Apak, Reşat

    2012-01-01

    The recognition of the benefits of polyphenolic antioxidants is eliciting increasing interest in the search for new polyphenolic derivatives with improved antioxidant activity. Since naringenin (4',5,7-trihydroxyflavanone) (NG) is one of the most abundant citrus and grapefruit polyphenolics and flavanone oximes were used in the synthesis of anticancer and radioprotector compounds having antiradical activity, the corresponding oxime of NG, naringenin oxime (NG-Ox), was synthesized and investigated. The structure of NG-Ox was characterized by FT-IR, 1H NMR, elemental analysis, and the synthesized compound was screened for its antioxidant capacity by using the cupric reducing antioxidant capacity (CUPRAC) method. Trolox equivalent antioxidant capacity (TEAC) of NG-Ox was measured to be higher than that of the parent compound, NG. Other parameters of antioxidant activity (scavenging effects on rad OH, O 2rad -, and H 2O 2) of NG-Ox were also determined.

  5. Synthesis and characterization of silica-coated nanoparticles of magnetite

    Science.gov (United States)

    Ferreira, R. V.; Pereira, I. L. S.; Cavalcante, L. C. D.; Gamarra, L. F.; Carneiro, S. M.; Amaro, E.; Fabris, J. D.; Domingues, R. Z.; Andrade, A. L.

    2010-01-01

    Magnetic nanoparticles coated with silica have been subjected of extensive, and, in many aspects, also intensive investigations because of their potential application in different technological fields, particularly in biomedicine. This work was conceived and is being carried out in two main parts: (1) synthesis of the ferrimagnetic nanoparticles, specifically magnetite, and (2) coating these particles with tetraethyl orthosilicate (TEOS). The nanosized magnetite sample was prepared by the reduction-precipitation and the nanomagnetite particles were coated by the sol-gel method, based on the hydrolysis of tetraethyl orthosilicate (TEOS). The so obtained materials were characterized with powder X-ray diffraction (XRD), FTIR spectroscopy, saturation magnetization measurements, and 57Fe Mössbauer spectroscopy at room temperature.

  6. Synthesis and characterization of silica-coated nanoparticles of magnetite

    Energy Technology Data Exchange (ETDEWEB)

    Ferreira, R. V., E-mail: robertavia@gmail.com; Pereira, I. L. S.; Cavalcante, L. C. D. [Universidade Federal de Minas Gerais, Departamento de Quimica (Brazil); Gamarra, L. F. [Instituto Israelita de Ensino e Pesquisa Albert Einstein, IIEPAE (Brazil); Carneiro, S. M. [Instituto Butantan (Brazil); Amaro, E. [Instituto Israelita de Ensino e Pesquisa Albert Einstein, IIEPAE (Brazil); Fabris, J. D.; Domingues, R. Z. [Universidade Federal de Minas Gerais, Departamento de Quimica (Brazil); Andrade, A. L., E-mail: angelala01@hotmail.com [Universidade Federal de Minas Gerais, Departamento de Quimica/s10 (Brazil)

    2010-01-15

    Magnetic nanoparticles coated with silica have been subjected of extensive, and, in many aspects, also intensive investigations because of their potential application in different technological fields, particularly in biomedicine. This work was conceived and is being carried out in two main parts: (1) synthesis of the ferrimagnetic nanoparticles, specifically magnetite, and (2) coating these particles with tetraethyl orthosilicate (TEOS). The nanosized magnetite sample was prepared by the reduction-precipitation and the nanomagnetite particles were coated by the sol-gel method, based on the hydrolysis of tetraethyl orthosilicate (TEOS). The so obtained materials were characterized with powder X-ray diffraction (XRD), FTIR spectroscopy, saturation magnetization measurements, and {sup 57}Fe Moessbauer spectroscopy at room temperature.

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

    Science.gov (United States)

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

    2013-01-01

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

  8. Template synthesis and characterization of carbon nanomaterials from ferrocene crystals

    Energy Technology Data Exchange (ETDEWEB)

    Cherkasov, Nikolay, E-mail: zdx@gmx.com [Lomonosov Moscow State University, Department of Chemistry, 119991, Moscow (Russian Federation); Savilov, Serguei V.; Ivanov, Anton S.; Egorov, Alex V.; Lunin, Valery V. [Lomonosov Moscow State University, Department of Chemistry, 119991, Moscow (Russian Federation); Ibhadon, Alex O. [School of Biological, Biomedical and Environmental Sciences and Department of Chemistry, University of Hull, Cottingham Road, Hull HU6 7RX (United Kingdom)

    2014-07-01

    Filamentous ribbon-like structures of highly disordered carbon of thickness 10–100 nm built from merged individual carbon nanofibers were synthesised by chemical vapour deposition from saturated ferrocene–benzene solution at 950 K. The materials obtained were characterized by electron microscopy, x-ray and electron diffraction, Raman spectroscopy and a possible growth mechanism for their formation was proposed and discussed. The synthesis demonstrates the possibility of a template growth of carbon nanomaterials and supports the vapour–solid–solid growth model of carbon materials because the catalysing metal particles are solid under the experimental conditions. Due to the large number of structural defects, filamentous structure, submicrometer thickness and low intraparticle diffusion of the nanomaterials, they can find application in catalysis as catalyst supports and sorbents.

  9. Synthesis and Characterization of Hydroxyapatite/Fullerenol Nanocomposites.

    Science.gov (United States)

    Djordjevic, Aleksandar; Ignjatovic, Nenad; Seke, Mariana; Jovic, Danica; Uskokovic, Dragan; Rakocevic, Zlatko

    2015-02-01

    Fullerenols are polyhydroxylated, water soluble derivatives of fullerene C60, with potential application in medicine as diagnostic agents, antioxidants or nano drug carriers. This paper describes synthesis and physical characterization of a new nanocomposite hydroxyapatite/fullerenol. Surface of the nanocomposite hydroxyapatite/fullerenol is inhomogeneous with the diameter of the particles in the range from 100 nm to 350 nm. The ζ potential of this nanocomposite is ten times lower when compared to hydroxyapatite. Surface phosphate groups of hydroxyapatite are prone to forming hydrogen bonds, when in close contact with hydroxyl groups, which could lead to formation of hydrogen bonds between hydroxyapatite and hydroxyl groups of fullerenol. The surface of hydroxyapatite particles (-2.5 mV) was modified by fullerenol particles, as confirmed by the obtained ζ potential value of the nanocomposite biomaterial hydroxyapatite/fullerenol (-25.0 mV). Keywords: Hydroxyapatite, Fullerenol, Nanocomposite, Surface Analysis.

  10. Synthesis and Characterization of SF-PPV-I

    Science.gov (United States)

    Wang, Y.; Fan, Z.; Taft, C.; Sun, S.

    2001-01-01

    Conjugated electro-active polymers find their potential applications in developing variety inexpensive and flexible shaped electronic and photonic devices, such as photovoltaic or photo/electro light emitting devices. In many of these opto-electronic polymeric materials, certain electron rich donors and electron deficient acceptors are needed in order to fine-tune the electronic or photonic properties of the desired materials and structures. While many donor type of conjugated polymers have been widely studied and developed in the past decades, there are relatively fewer acceptor type of conjugated polymers have been developed. Key acceptor type conjugated polymers developed so far include C60 and CN-PPV, and each has its limitations. Due to the complexity and diversity of variety future electronic materials and structural needs, alternative and synthetically amenable acceptor conjugated polymers need to be developed. In this paper, we present the synthesis and characterization of a new acceptor conjugated polymer, a sulfone derivatized polyphenylenevinylene "SF-PPV".

  11. 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.

  12. Graphene-based materials: synthesis, characterization, properties, and applications.

    Science.gov (United States)

    Huang, Xiao; Yin, Zongyou; Wu, Shixin; Qi, Xiaoying; He, Qiyuan; Zhang, Qichun; Yan, Qingyu; Boey, Freddy; Zhang, Hua

    2011-07-18

    Graphene, a two-dimensional, single-layer sheet of sp(2) hybridized carbon atoms, has attracted tremendous attention and research interest, owing to its exceptional physical properties, such as high electronic conductivity, good thermal stability, and excellent mechanical strength. Other forms of graphene-related materials, including graphene oxide, reduced graphene oxide, and exfoliated graphite, have been reliably produced in large scale. The promising properties together with the ease of processibility and functionalization make graphene-based materials ideal candidates for incorporation into a variety of functional materials. Importantly, graphene and its derivatives have been explored in a wide range of applications, such as electronic and photonic devices, clean energy, and sensors. In this review, after a general introduction to graphene and its derivatives, the synthesis, characterization, properties, and applications of graphene-based materials are discussed. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

    Directory of Open Access Journals (Sweden)

    Anish Stephen

    2013-01-01

    Full Text Available This 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 20–40 nm. Optimization of methodology in terms of concentration of reactants and pH of the reaction mixture reduced the reaction time for silver nanoparticle formation to 2 mins. Silver nanoparticles (AgNPs were characterized by UV-Vis spectroscopy and transmission electron microscopy (TEM. UV-vis spectroscopy derived spectrum demonstrated a peak of 430 nm which corresponds to the plasmon absorbance of silver nanoparticles. Transmission electron microscopy revealed spherical shaped silver nanoparticles in the size range of 20–40 nm.

  14. Synthesis, characterization and DNA interaction studies of new triptycene derivatives

    Directory of Open Access Journals (Sweden)

    Sourav Chakraborty

    2014-06-01

    Full Text Available A facile and efficient synthesis of a new series of triptycene-based tripods is being reported. Using 2,6,14- or 2,7,14-triaminotriptycenes as synthons, the corresponding triazidotriptycenes were prepared in high yield. Additionally, we report the transformation of 2,6,14- or 2,7,14-triaminotriptycenes to the corresponding ethynyl-substituted triptycenes via their tribromo derivatives. Subsequently, derivatization of ethynyl-substituted triptycenes was studied to yield the respective propiolic acid and ethynylphosphine derivatives. Characterization of the newly functionalized triptycene derivatives and their regioisomers were carried out using FTIR and multinuclear NMR spectroscopy, mass spectrometry, and elemental analyses techniques. The study of the interaction of these trisubstituted triptycenes with various forms of DNA revealed interesting dependency on the functional groups of the triptycene core to initiate damage or conformational changes in DNA.

  15. Electrochemical Synthesis and Characterization of Zinc Sulfide Nanoparticles

    Directory of Open Access Journals (Sweden)

    M. Rahimi-Nasarabadi

    2014-04-01

    Full Text Available Electrosynthesis process has been used for preparation of zinc sulfide nanoparticles. Zinc sulfide nanoparticles in different size and shapes were electrodeposited by electrolysis of zinc plate as anode in sodium sulfide solution. Effects of several reaction variables, such as electrolysis voltage, sulfide ion concentration as reactant, stirring rate of electrolyte solution and temperature on particle size of prepared zinc sulfide were investigated. The significance of these parameters in tuning the size of zinc sulfide particles was quantitatively evaluated by analysis of variance (ANOVA. Also, optimum conditions for synthesis of zinc sulfide nanoparticles via electrosynthesis reaction were proposed. The structure and composition of prepared nanoparticles under optimum condition was characterized by X-ray diffraction (XRD, scanning electron microscopy (SEM, transmission electron microscopy (TEM, and UV-Vis spectrophotometry techniques.

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

    Directory of Open Access Journals (Sweden)

    Selinay Y. Erişkin

    2014-01-01

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

  17. 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.

  18. Synthesis and characterization of carbon cryogel/zeolite composites

    Directory of Open Access Journals (Sweden)

    Biljana Babić

    2011-06-01

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

  19. Validation of an HPLC-DAD/UV method for the quantification of cyclamate in tabletop sweeteners: risk of exceeding the acceptable daily intake.

    Science.gov (United States)

    Sargaço, B; Serra, C; Vasco, E

    2017-06-01

    Cyclamate is widely used as intense sweetener in the European Union. The absence of a maximum limit for the use of cyclamate in tabletop sweeteners and the growing demand for this type of product highlights the importance of developing robust analytical methods for the determination of its content to understand if the consumption of tabletop sweeteners can have a negative impact on human health. The present work aimed at the optimisation and validation of an high-performance liquid chromatography (HPLC) analytical method for cyclamate determination in tabletop sweeteners based on the procedure of European Standard EN 12857. The validated method was then applied to the determination of this sweetener in different types of tabletop sweeteners (liquid, powder and tablets). Both standards and samples solutions were submitted to a derivatisation procedure which converted cyclamate to N,N-dichlorocyclohexylamine. The derivatised product was separated and quantified using a reversed-phase column, a mobile phase composed of water (20%) and methanol (80%), isocratic flow of 1 ml min(-1), and detection by ultraviolet spectrophotometry at a wavelength of 314 nm. The analytical method was internally validated according to the following validation parameters: working range, linearity, limits of detection and quantification, sensitivity, precision (repeatability and intermediate precision), and uncertainty. This method proved to be specific and selective for the determination of this sweetener, showing repeatability, RSDr ≤ 3%, intermediate precision, RSDR ≤ 3.3%, and recovery rates from 92% to 108% for the different tabletop sweeteners. The method uncertainty was 9.4%. The concentration of cyclamate in the samples varied significantly, from 2.9% to 73.9%, which demonstrated that a possible excessive consumption of one of the analysed sweeteners can lead to exceeding the acceptable daily intake for cyclamate.

  20. Synthesis and Characterization of Gelatin-Based Magnetic Hydrogels.

    Science.gov (United States)

    Helminger, Maria; Wu, Baohu; Kollmann, Tina; Benke, Dominik; Schwahn, Dietmar; Pipich, Vitaliy; Faivre, Damien; Zahn, Dirk; Cölfen, Helmut

    2014-06-01

    A simple preparation of thermoreversible gelatin-based ferrogels in water provides a constant structure defined by the crosslinking degree for gelatin contents between 6 and 18 wt%. The possibility of varying magnetite nanoparticle concentration between 20 and 70 wt% is also reported. Simulation studies hint at the suitability of collagen to bind iron and hydroxide ions, suggesting that collagen acts as a nucleation seed to iron hydroxide aggregation, and thus the intergrowth of collagen and magnetite nanoparticles already at the precursor stage. The detailed structure of the individual ferrogel components is characterized by small-angle neutron scattering (SANS) using contrast matching. The magnetite structure characterization is supplemented by small-angle X-ray scattering and microscopy only visualizing magnetite. SANS shows an unchanged gelatin structure of average mesh size larger than the nanoparticles with respect to gel concentration while the magnetite nanoparticles size of around 10 nm seems to be limited by the gel mesh size. Swelling measurements underline that magnetite acts as additional crosslinker and therefore varying the magnetic and mechanical properties of the ferrogels. Overall, the simple and variable synthesis protocol, the cheap and easy accessibility of the components as well as the biocompatibility of the gelatin-based materials suggest them for a number of applications including actuators.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-01-01

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

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

    Science.gov (United States)

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

    2015-03-16

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

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

    Science.gov (United States)

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

    2017-01-01

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

  4. Genetic and Biochemical Characterization of Peptidoglycan Synthesis in Chlamydia

    National Research Council Canada - National Science Library

    McCoy, Andrea J

    2005-01-01

    .... Unlike other wall-less bacteria, chlamydiae synthesize penicillin-binding proteins, are sensitive to antibiotics that inhibit cell wall synthesis, and encode a nearly complete pathway for the synthesis of peptidoglycan...

  5. Monopicolinate cross-bridged cyclam combining very fast complexation with very high stability and inertness of its copper(II) complex.

    Science.gov (United States)

    Lima, Luís M P; Halime, Zakaria; Marion, Ronan; Camus, Nathalie; Delgado, Rita; Platas-Iglesias, Carlos; Tripier, Raphaël

    2014-05-19

    The synthesis of a new cross-bridged 1,4,8,11-tetraazacyclotetradecane (cb-cyclam) derivative bearing a picolinate arm (Hcb-te1pa) was achieved by taking advantage of the proton sponge properties of the starting constrained macrocycle. The structure of the reinforced ligand as well as its acid-base properties and coordination properties with Cu(2+) and Zn(2+) was investigated. The X-ray structure of the free ligand showed a completely preorganized conformation that lead to very fast copper(II) complexation under mild conditions (instantaneous at pH 7.4) or even in acidic pH (3 min at pH 5) at room temperature and that demonstrated high thermodynamic stability, which was measured by potentiometry (at 25 °C and 0.10 M in KNO3). The results also revealed that the complex exists as a monopositive copper(II) species in the intermediate pH range. A comparative study highlighted the important selectivity for Cu(2+) over Zn(2+). The copper(II) complex was synthesized and investigated in solution using different spectroscopic techniques and DFT calculations. The kinetic inertness of the copper(II) complex in acidic medium was evaluated by spectrophotometry, revealing the very slow dissociation of the complex. The half-life of 96 days, in 5 M HClO4, and 465 min, in 5 M HCl at 25 °C, show the high kinetic stability of the copper(II) chelate compared to that of the corresponding complexes of other macrocyclic ligands. Additionally, cyclic voltammetry experiments underlined the perfect electrochemical inertness of the complex as well as the quasi-reversible Cu(2+)/Cu(+) redox system. The coordination geometry of the copper center in the complex was established in aqueous solution from UV-vis and EPR spectroscopies.

  6. Hydrothermal synthesis and characterization of zirconia based catalysts

    Energy Technology Data Exchange (ETDEWEB)

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

    2013-07-15

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

  7. 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

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

    Science.gov (United States)

    Franus, Wojciech; Wdowin, Magdalena; Franus, Małgorzata

    2014-09-01

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

  9. Synthesis, Characterization and Application of Multiscale Porous Materials

    Energy Technology Data Exchange (ETDEWEB)

    Hussami, Linda

    2010-07-01

    This thesis work brings fresh insights and improved understanding of nano scale materials through introducing new hybrid composites, 2D hexagonal in MCM-41 and 3D random interconnected structures of different materials, and application relevance for developing fields of science, such as fuel cells and solar cells. New types of porous materials and organometallic crystals have been prepared and characterized in detail. The porous materials have been used in several studies: as hosts to encapsulate metal-organic complexes; as catalyst supports and electrode materials in devices for alternative energy production. The utility of the new porous materials arises from their unique structural and surface chemical characteristics as demonstrated here using various experimental and theoretical approaches. New single crystal structures and arene-ligand exchange properties of f-block elements coordinated to ligand arene and halogallates are described in Paper I. These compounds have been incorporated into ordered 2D-hexagonal MCM-41 and polyhedral silica nano foam (PNF-SiO{sub 2}) matrices without significant change to the original porous architectures as described in Paper II and III. The resulting inorganic/organic hybrids exhibited enhanced luminescence activity relative to the pure crystalline complexes. A series of novel polyhedral carbon nano foams (PNF-C's) and inverse foams were prepared by nano casting from PNF-SiO{sub 2}'s. These are discussed in Paper IV. The synthesis conditions of PNF-C's were systematically varied as a function of the filling ratio of carbon precursor and their structures compared using various characterization methods. The carbonaceous porous materials were further tested in Paper V and VI as possible catalysts and catalyst supports in counter- and working electrodes for solar- and fuel cell applications

  10. 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.

  11. Silver Nanoparticles: Synthesis, Characterization, Properties, Applications, and Therapeutic Approaches

    Directory of Open Access Journals (Sweden)

    Xi-Feng Zhang

    2016-09-01

    Full Text Available Recent advances in nanoscience and nanotechnology radically changed the way we diagnose, treat, and prevent various diseases in all aspects of human life. Silver nanoparticles (AgNPs are one of the most vital and fascinating nanomaterials among several metallic nanoparticles that are involved in biomedical applications. AgNPs play an important role in nanoscience and nanotechnology, particularly in nanomedicine. Although several noble metals have been used for various purposes, AgNPs have been focused on potential applications in cancer diagnosis and therapy. In this review, we discuss the synthesis of AgNPs using physical, chemical, and biological methods. We also discuss the properties of AgNPs and methods for their characterization. More importantly, we extensively discuss the multifunctional bio-applications of AgNPs; for example, as antibacterial, antifungal, antiviral, anti-inflammatory, anti-angiogenic, and anti-cancer agents, and the mechanism of the anti-cancer activity of AgNPs. In addition, we discuss therapeutic approaches and challenges for cancer therapy using AgNPs. Finally, we conclude by discussing the future perspective of AgNPs.

  12. Synthesis and characterization of Ce doped MFI zeolite

    Energy Technology Data Exchange (ETDEWEB)

    Kalita, Banani [Department of Chemistry, Gauhati University, Guwahati, Assam 781014 (India); Talukdar, Anup K., E-mail: anup_t@sify.com [Department of Chemistry, Gauhati University, Guwahati, Assam 781014 (India)

    2012-04-16

    Highlights: Black-Right-Pointing-Pointer Cerium was incorporated into the tetrahedral position of MFI zeolite structure. Black-Right-Pointing-Pointer Unit cell volume increases with an increase of Ce content in the framework of MFI. Black-Right-Pointing-Pointer A band at 310 nm in the UV-vis spectra indicates Ce incorporation in MFI structure. Black-Right-Pointing-Pointer The mass loss (%) in the region 373-423 K decreases with increase of Ce in MFI. - Abstract: Ce doped MFI (mobil five) zeolites with different Si to (Ce + Al) and different Ce to Al ratios were synthesized by a hydrothermal synthesis method. All the samples were characterized by different techniques such as X-ray diffraction, Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), UV-vis diffuse reflectance spectroscopy (DRS) and scanning electron microscopy (SEM). The results showed that almost pure MFI phase was obtained in all cases with incorporation of cerium metal into the framework. The increase in unit cell parameters observed with an increase in Ce content is indicative of incorporation of Ce into the framework structure of microporous material MFI. Corroboration of the framework incorporation of Ce into the MFI zeolite structure was also obtained from the UV-vis DRS spectra by the presence of an absorption band at 280 nm. TGA and SEM of the samples provide complementary evidence for Ce incorporation into the framework MFI structure.

  13. Three bilindione isomers: synthesis, characterization and reactivity of biliverdin analogs.

    Science.gov (United States)

    Wang, Jun-Fei; Ma, Fang; Sun, Hao-Ling; Zhang, Jing; Zhang, Jun-Long

    2017-07-01

    Linear tetrapyrrole is the core structure of light-sensitive native cofactors such as phycocyanobilin, phytochromobilin and bile pigments, which attracts increasing attention in biomimetic chemistry, photochemistry and coordination chemistry. To decipher the relationship between structures and functions, in this work, we firstly reported the synthesis, isolation and characterization of three bilindione isomers (ZZZ, syn, syn, syn 1, EZE, syn, syn, anti 2 and EZE, anti, syn, anti 3) bearing meso-pentafluorophenyl groups. The structures were confirmed by X-ray diffraction and 2-D NMR spectroscopes. More importantly, the interconversion between three isomers under heating and light irradiation was investigated, and isomer 3 was found to be transformed to 1 and 2 more easily, which is in line with the results of DFT calculation. This work provides important insights for understanding the relationship between structures and functions and would be important to further construct metal complexes based on linear tetrapyrrole ligands, which are complementary to well-studied the cyclic analogs such as porphyrin and corroles.

  14. L-arginine modified magnetic nanoparticles: green synthesis and characterization

    Science.gov (United States)

    Bagherpour, A. R.; Kashanian, F.; Seyyed Ebrahimi, S. A.; Habibi-Rezaei, M.

    2018-02-01

    In recent years, there has been considerable interest in Arg which is a unique, nontoxic, and biocompatible biomolecule since it can be utilized as an agent for the functionalization and subsequent stabilization of MNPs against oxidation and aggregation, during or after a synthesis procedure. Our studies demonstrate that Arg has great impacts on MNPs with the decreasing size of the particle. Also, saturation magnetization and electrostatic interactions of RMNPs have a direct impact on biological molecules such as proteins and nucleic acids. By controlling the concentration of Arg, it is possible to accurately control the above-mentioned characteristics, which are useful tools for applications such as connecting to antibodies, catalysis, drug loading, and modification of MNP stability. In the current study, three RMNPs with different Arg densities, i.e. 0.42, 1.62, and 2.29 μg per mg were successfully synthesized through a simple co-precipitation method (named p 0.5, p 1, and p 1.5, respectively) and verified by colorimetric determination. Also, the as-synthesized RMNP powders were characterized by XRD, SEM/EDAX, FTIR, VSM, and zeta potential analysis. The presence of a magnetic core was proved by XRD, FTIR, and EDAX. Colorimetric analysis showed the existence of Arg in the synthesized samples. According to the zeta potential and VSM results, increasing the cap of Arg on the MNP surface leads to an increase in the surface charge and decrease in the magnetization of the RMNPs, respectively.

  15. 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.

  16. A new class of pegylated plasmonic liposomes: synthesis and characterization.

    Science.gov (United States)

    Stiufiuc, Rares; Iacovita, Cristian; Stiufiuc, Gabriela; Florea, Adrian; Achim, Marcela; Lucaciu, Constantin M

    2015-01-01

    The multifunctional nanoobjects that can be controlled, manipulated and triggered using external stimuli represent very promising candidates for nanoscale therapeutic and diagnostic applications. In this study we report the successful synthesis and characterization of a new class of very stable multifunctional nanoobjects, containing cationic liposomes decorated with PEGylated gold nanoparticles (PEGAuNPs). The multifunctional hybrid nanoobjects (mHyNp) were prepared by taking advantage of the electrostatic interactions between small unilamelar cationic liposomes and negatively charged gold nanoparticles. The mHyNps have been investigated by UV-VIS absorption spectroscopy, Dynamic Light Scattering (DLS), Zeta Potential Measurements and Transmission Electron Microscopy (TEM). The TEM images clearly revealed the attachment of individual gold nanoparticles onto the spherical outer surface of the cationic liposomes which was also confirmed by DLS and UV-VIS data. Furthermore, the plasmonic properties of the hybrid complexes have been evaluated by using the Surface Enhanced Raman Spectroscopy (SERS) technique. It is shown that PEG mediated interaction between the liposomes and the gold nanoparticles enabled the recording of the SER spectra of the liposomes in aqueous environment, thus demonstrating the plasmonic properties of the hybrids. Copyright © 2014 Elsevier Inc. All rights reserved.

  17. Heterocyclic energetic materials: Synthesis, characterization and computational design

    Science.gov (United States)

    Tsyshevsky, Roman; Pagoria, Philip; Smirnov, Aleksander; Kuklja, Maija

    2017-06-01

    Achievement of the tailored properties (high performance, low sensitivity, etc.) in targeted new energetic materials (EM) remains a great challenge. Recently, attention of researchers has shifted from conventional nitroester-, nitramine-, and nitroaromatic-based explosives to new heterocyclic EM with oxygen- and nitrogenrich molecular structures. They have increased densities and formation enthalpies complemented by attractive performance and high stability to external stimuli. We will demonstrate that oxadiazol-containing heterocycles offer a convenient playground to probe specific chemical functional groups as building blocks for design of EM. We discuss a joint experimental and computational approach for design, characterization, synthesis, and modeling of novel heterocyclic EM. Combinatorically, we comprehensively analyzed how overall stability and performance of each material in the family (BNFF, LLM-172, LLM-175, LLM-191, LLM-192, LLM-200) depends upon their chemical composition and details of the molecular structure (such as a substitution of a nitro group by an amino group and 1,2,5-oxadiazole fragment by 1,2,3- or 1,2,4-oxadiazol ring). We will also discuss proposed new EM with predicted superior chemical and physical properties. P. Pagoria, R. Tsyshevsky, A. Smirnov.

  18. Silver Nanoparticles: Synthesis, Characterization, Properties, Applications, and Therapeutic Approaches

    Science.gov (United States)

    Zhang, Xi-Feng; Liu, Zhi-Guo; Shen, Wei; Gurunathan, Sangiliyandi

    2016-01-01

    Recent advances in nanoscience and nanotechnology radically changed the way we diagnose, treat, and prevent various diseases in all aspects of human life. Silver nanoparticles (AgNPs) are one of the most vital and fascinating nanomaterials among several metallic nanoparticles that are involved in biomedical applications. AgNPs play an important role in nanoscience and nanotechnology, particularly in nanomedicine. Although several noble metals have been used for various purposes, AgNPs have been focused on potential applications in cancer diagnosis and therapy. In this review, we discuss the synthesis of AgNPs using physical, chemical, and biological methods. We also discuss the properties of AgNPs and methods for their characterization. More importantly, we extensively discuss the multifunctional bio-applications of AgNPs; for example, as antibacterial, antifungal, antiviral, anti-inflammatory, anti-angiogenic, and anti-cancer agents, and the mechanism of the anti-cancer activity of AgNPs. In addition, we discuss therapeutic approaches and challenges for cancer therapy using AgNPs. Finally, we conclude by discussing the future perspective of AgNPs. PMID:27649147

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2010-10-01

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

  20. 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

  1. 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.

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

    Directory of Open Access Journals (Sweden)

    Ali A

    2016-08-01

    Full Text Available Attarad Ali,1 Hira Zafar,1 Muhammad Zia,1 Ihsan ul Haq,2 Abdul Rehman Phull,3 Joham Sarfraz Ali,1 Altaf Hussain4 1Department of Biotechnology, 2Department of Pharmacy, Quaid-i-Azam University, Islamabad, Pakistan; 3Department of Biology, Kongju National University, Kongju, South Korea; 4Department of Materials Science and Engineering, Institute of Space Technology, Islamabad, Pakistan Abstract: 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. Keywords: superparamagnetism, iron oxide nanoparticles, surfactants, hyperthermia, biodistribution, bioelimination

  3. Synthesis and characterization of polyvinylpyrrolidone coated cerium oxide nanoparticles.

    Science.gov (United States)

    Merrifield, Ruth C; Wang, Zhi Wei; Palmer, Richard E; Lead, Jamie R

    2013-01-01

    There is a pressing need for the development of standard and reference nanomaterials for environmental nanoscience and nanotoxicology. To that aim, suspensions of polyvinylpyrrolidone (PVP)-coated ceria nanoparticles (NPs) were produced. Four differently sized monodispersed samples were produced by using different PVP chain lengths. The chemical and physical properties of these NPs were characterized as prepared and in different ecotoxicology exposure media. Dynamic light scattering analysis showed that the samples were monodispersed, with an unchanged size when suspended in the different media over a 72 h period. Electron microscopy confirmed this and revealed that the larger (ca. 20 nm) particles were aggregates composed of the smaller individual particles (4-5 nm). Electron energy loss spectroscopy (EELS) showed that the smallest and largest samples were composed almost entirely of cerium(III) oxide, with only small amounts of cerium(IV) present in the largest sample. Dissolved cerium concentrations in media were low and constant, showing that the NPs did not dissolve over time. The simple synthesis of the these NPs and their physical and chemical stability in different environmental conditions make them potentially suitable for use as reference materials for (eco)toxicology and surface water environmental studies.

  4. Silver Nanoparticles: Synthesis, Characterization, Properties, Applications, and Therapeutic Approaches.

    Science.gov (United States)

    Zhang, Xi-Feng; Liu, Zhi-Guo; Shen, Wei; Gurunathan, Sangiliyandi

    2016-09-13

    Recent advances in nanoscience and nanotechnology radically changed the way we diagnose, treat, and prevent various diseases in all aspects of human life. Silver nanoparticles (AgNPs) are one of the most vital and fascinating nanomaterials among several metallic nanoparticles that are involved in biomedical applications. AgNPs play an important role in nanoscience and nanotechnology, particularly in nanomedicine. Although several noble metals have been used for various purposes, AgNPs have been focused on potential applications in cancer diagnosis and therapy. In this review, we discuss the synthesis of AgNPs using physical, chemical, and biological methods. We also discuss the properties of AgNPs and methods for their characterization. More importantly, we extensively discuss the multifunctional bio-applications of AgNPs; for example, as antibacterial, antifungal, antiviral, anti-inflammatory, anti-angiogenic, and anti-cancer agents, and the mechanism of the anti-cancer activity of AgNPs. In addition, we discuss therapeutic approaches and challenges for cancer therapy using AgNPs. Finally, we conclude by discussing the future perspective of AgNPs.

  5. Fluorescent nanosensors for intracellular measurements: synthesis, characterization, calibration, and measurement.

    Science.gov (United States)

    Desai, Arpan S; Chauhan, Veeren M; Johnston, Angus P R; Esler, Tim; Aylott, Jonathan W

    2013-01-01

    Measurement of intracellular acidification is important for understanding fundamental biological pathways as well as developing effective therapeutic strategies. Fluorescent pH nanosensors are an enabling technology for real-time monitoring of intracellular acidification. The physicochemical characteristics of nanosensors can be engineered to target specific cellular compartments and respond to external stimuli. Therefore, nanosensors represent a versatile approach for probing biological pathways inside cells. The fundamental components of nanosensors comprise a pH-sensitive fluorophore (signal transducer) and a pH-insensitive reference fluorophore (internal standard) immobilized in an inert non-toxic matrix. The inert matrix prevents interference of cellular components with the sensing elements as well as minimizing potentially harmful effects of some fluorophores on cell function. Fluorescent nanosensors are synthesized using standard laboratory equipment and are detectable by non-invasive widely accessible imaging techniques. The outcomes of studies employing this technology are dependent on reliable methodology for performing measurements. In particular, special consideration must be given to conditions for sensor calibration, uptake conditions and parameters for image analysis. We describe procedures for: (1) synthesis and characterization of polyacrylamide and silica based nanosensors, (2) nanosensor calibration and (3) performing measurements using fluorescence microscopy.

  6. 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

  7. Preparation and characterization of aminobenzyl cellulose by two step synthesis from native cellulose

    Science.gov (United States)

    Synthesis and structural characterizations of nitro- and amino-benzyl cellulose were carried out. Cellulose derivatives were synthesized by etherification. Nitrobenzylation produced 80% yield by treating a mixture of microcrystalline cellulose, 4-dimethyl aminopyridine and 4-nitrobenzyl chloride at ...

  8. A New Class of Metal-Cyclam-Based Zirconium Metal–Organic Frameworks for CO2 Adsorption and Chemical Fixation

    Energy Technology Data Exchange (ETDEWEB)

    Zhu, Jie [Department; Usov, Pavel M. [Department; Xu, Wenqian [X-ray; Celis-Salazar, Paula J. [Department; Lin, Shaoyang [Department; Kessinger, Matthew C. [Department; Landaverde-Alvarado, Carlos [Department; Macromolecules; Cai, Meng [Department; May, Ann M. [Department; Slebodnick, Carla [Department; Zhu, Dunru [College; Senanayake, Sanjaya D. [Department; Morris, Amanda J. [Department; Macromolecules

    2018-01-08

    Metal-organic frameworks (MOFs) have shown great promise in catalysis, mainly due to their high content of active centers, large internal surface areas, tunable pore size, and versatile chemical functionalities. However, it is a challenge to rationally design and construct MOFs that can serve as highly stable and reusable heterogeneous catalysts. Here two new robust 3D porous metal-cyclam-based zirconium MOFs, denoted VPI-100 (Cu) and VPI-100 (Ni), have been prepared by a modulated synthetic strategy. The frameworks are assembled by eight-connected Zr-6 clusters and metallocyclams as organic linkers. Importantly, the cyclam core has accessible axial coordination sites for guest interactions and maintains the electronic properties exhibited by the parent cyclam ring. The VPI-100 MOFs exhibit excellent chemical stability in various organic and aqueous solvents over a wide pH range and show high CO2 uptake capacity (up to similar to 9.83 wt% adsorption at 273 K under 1 atm). Moreover, VPI-100 MOFs demonstrate some of the highest reported catalytic activity values (turnover frequency and conversion efficiency) among Zr-based MOFs for the chemical fixation of CO2 with epoxides, including sterically hindered epoxides. The MOFs, which bear dual catalytic sites (Zr and Cu/Ni), enable chemistry not possible with the cyclam ligand under the same conditions and can be used as recoverable stable heterogeneous catalysts without losing performance.

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

    OpenAIRE

    Nascimento, Ana Cláudia Lobão do

    2016-01-01

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

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

    Science.gov (United States)

    2016-03-31

    positioning has made high-performance, light-weight power sources of increasing importance to the US military. Polymer electrolyte membranes , which...AFRL-AFOSR-VA-TR-2016-0168 Design, Synthesis, and Characterization of High Performance Polymer Electrolytes for Printed Electronics and Energy...Sep 2015 4. TITLE AND SUBTITLE Design, Synthesis, and Characterization of High Performance Polymer Electrolytes for Printed Electronics and Energy

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1993-10-01

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

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

    Science.gov (United States)

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

    2015-01-01

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

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

    Indian Academy of Sciences (India)

    Administrator

    Abstract. Metathesis synthesis of complex metal fluorides using mechanochemical activation has been reported. The high lattice energy of the byproduct KCl helps the reaction towards product formation in under 20 min. The proposed process, in contrast to the available methods of synthesis, is very rapid, economical and ...

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

    Science.gov (United States)

    Rekulapally, Sujith R.

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

  15. Synthesis, Characterization, and Fabrication of All Inorganic Quantum Dot LEDs

    Science.gov (United States)

    Salman, Haider Baqer

    Quantum Dot LEDs with all inorganic materials are investigated in this thesis. The research was motivated by the potential disruptive technology of core shell quantum dots in lighting and display applications. These devices consisted of three main layers: hole transport layer (HTL), electron transport layer (ETL), and emissive layer where the emission of photons occurs. The latter part was formed of CdSe / ZnS core-shell quantum dots, which were synthesized following hot injection method. The ETL and the HTL were formed of zinc oxide nanocrystals and nickel oxide, respectively. Motivated by the low cost synthesis and deposition, NiO and ZnO were synthesized following sol-gel method and deposited using spin coating. The anode of the device was a commercial slide of indium tin oxide deposited on glass substrate while the cathode was a 100 nm aluminum layer that was deposited using an Auto 306T Edwards thermal evaporator. In this research, Raman spectroscopy, micro-photoluminescence spectroscopy, absorbance spectroscopy, X-ray diffraction (XRD) spectroscopy, and atomic force microscopy, were used to characterize the materials. Three sharp peaks were observed in the XRD measurements of the NiO thin film related to three planes and indicated a proper level of crystallinity. The AFM image of the same material indicated a roughness RMS value of 2 nm which was accepted for a device fabrication. The photoluminescence spectrum exhibited a peak at 515 nm for the quantum dots and a peak at 315 nm for the ZnO nanocrystals. The narrow shape of these spectra proved a limited amount of size variation. The transfer characteristics of the fabricated device indicated that the current density ramped up producing green light when the voltage was higher than 5 V to reach 160 mA cm -2 at 9 V.

  16. Synthesis, characterization and antimicrobial activity of some novel benzimidazole derivatives

    Directory of Open Access Journals (Sweden)

    Immadisetty Sri Krishnanjaneyulu

    2014-01-01

    Full Text Available A series of novel N-((1H-benzoimidazol-1-yl methyl-4-(1-phenyl-5-substituted-4, 5-dihydro-1-benzoimidazol-1-yl methyl-4-(1-phenyl-5-substituted-4, 5-dihydro-1H-pyrazol-3-yl benzenamine were synthesized by treating various 1-(4-((1H-benzoimidazol-1-yl methylamino phenyl-3-substitutedprop-2-en-1-one with phenyl hydrazine in the presence of sodium acetate through a simple ring closure reaction. The starting material, 1-(4-((1H-benzoimidazol-1-yl methylamino phenyl-3-substitutedprop-2-en-1-one,-benzoimidazol-1-yl methylamino phenyl-3-substitutedprop-2-en-1-one, was synthesized from o-phenylenediamine by a multistep synthesis. All the synthesized compounds were characterized by spectroscopic means and elemental analyses. The title compounds were investigated for in vitro antibacterial and antifungal properties against some human pathogenic microorganisms by employing the agar streak dilution method using Ciprofloxacin and Ketoconazole as standard drugs. All title compounds showed activity against the entire strains of microorganism. Structural activity relationship studies reveal that compounds possessing an electron-withdrawing group display better activity than the compounds containing electron-donating groups, whereas the unsubstituted derivatives display moderate activity. Based on the results obtained, N-((1H-benzoimidazol-1-yl methyl-4-(1-phenyl-5-(4-(trifluoromethyl phenyl-4,5-dihydro-1H-pyrazol-3-yl benzenamine 5i was found to be very active compared with the rest of the compounds and standard drugs that were subjected to antimicrobial assay.

  17. Synthesis, characterization and antimicrobial activity of some novel benzimidazole derivatives.

    Science.gov (United States)

    Krishnanjaneyulu, Immadisetty Sri; Saravanan, Govindaraj; Vamsi, Janga; Supriya, Pamidipamula; Bhavana, Jarugula Udaya; Sunil Kumar, Mittineni Venkata

    2014-01-01

    A series of novel N-((1H-benzoimidazol-1-yl) methyl)-4-(1-phenyl-5-substituted-4, 5-dihydro-1-benzoimidazol-1-yl) methyl)-4-(1-phenyl-5-substituted-4, 5-dihydro-1H-pyrazol-3-yl) benzenamine were synthesized by treating various 1-(4-((1H-benzoimidazol-1-yl) methylamino) phenyl)-3-substitutedprop-2-en-1-one with phenyl hydrazine in the presence of sodium acetate through a simple ring closure reaction. The starting material, 1-(4-((1H-benzoimidazol-1-yl) methylamino) phenyl)-3-substitutedprop-2-en-1-one,-benzoimidazol-1-yl) methylamino) phenyl)-3-substitutedprop-2-en-1-one, was synthesized from o-phenylenediamine by a multistep synthesis. All the synthesized compounds were characterized by spectroscopic means and elemental analyses. The title compounds were investigated for in vitro antibacterial and antifungal properties against some human pathogenic microorganisms by employing the agar streak dilution method using Ciprofloxacin and Ketoconazole as standard drugs. All title compounds showed activity against the entire strains of microorganism. Structural activity relationship studies reveal that compounds possessing an electron-withdrawing group display better activity than the compounds containing electron-donating groups, whereas the unsubstituted derivatives display moderate activity. Based on the results obtained, N-((1H-benzoimidazol-1-yl) methyl)-4-(1-phenyl-5-(4-(trifluoromethyl) phenyl)-4,5-dihydro-1H-pyrazol-3-yl) benzenamine 5i was found to be very active compared with the rest of the compounds and standard drugs that were subjected to antimicrobial assay.

  18. Synthesis and characterization of diblock copolymer templated iron oxide nanoparticles

    Science.gov (United States)

    Akcora, Pinar

    2005-07-01

    Templating ordered assemblies of magnetic oxide nanoparticles within self-assembled diblock copolymers of varying morphologies is an important problem with a wide applicability such as in electromagnetics, optical devices, metal catalysts, medicine and biology. In this thesis, the effects of different polymer structures on particle ordering and resultant magnetic properties have been investigated using various microstructure and magnetic characterization tools. Ring-opening metathesis polymerization (ROMP) of norbornene and functionalized norbornene monomers has been used to synthesize diblock copolymers of narrow polydispersities using Grubbs' catalyst. These block copolymers can be used as templates to form inorganic nanoparticles. In this research, the structural and physical understanding of the inorganic-copolymer system was studied by small-angle neutron and x-ray scattering techniques and transmission electron microscopy. Synthesis of gamma-Fe2O3 nanoparticles has been achieved within novel block copolymers of (norbornene)-b-(deuterated norbornene dicarboxylic) acid and (norbornene methanol-(norbornene dicarboxylic acid). The polymer morphologies were controlled by varying the volume fractions of the constituent blocks. The pure norbornene based diblock copolymer morphologies were demonstrated by electron microscopy for the first tune. Spherical, cylindrical and lamellar morphologies of these novel diblock copolymers were reported. The block ratios of the synthesized polymers were determined using gel permeation chromatography-light scattering, elemental analysis and UV-VIS spectroscopy. Solution phase doping and submersion of thin films in metal salt solutions were employed as metal doping methods and the observed nanoparticle structures were compared to those of the undoped copolymer morphologies. This project reports on the types of templating structures and dispersion of the nanoparticles. The effects of particle, interactions on the microphase

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

    Science.gov (United States)

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

    2015-09-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-01-01

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

  1. Synthesis, characterization and biosensing application of photon upconverting nanoparticles

    Science.gov (United States)

    Kumar, Manoj; Zhang, Peng

    2009-02-01

    Phosphor/fluorescent molecules/particles have been widely used in various applications for quite some time. Typically, light with longer wavelength(s) is emitted when excited by shorter wavelength light. The opposite effect also exists, where a phosphor particle is excited with an infrared or red light and emits color(s) of shorter wavelengths, a process called up-conversion. Materials with upconverting properties have narrower absorption and line emission spectra than their down-converting counterparts. Because most non-target materials in a complex mixture do not possess such photon up-conversion properties, a dramatically improved S/N ratio is expected in sensing and luminescence reporting applications. This makes photon upconverting materials ideal for identification of trace amounts of target molecules. Here we report the synthesis, characterization and DNA detection application based on NaYF4:Yb3+, Er3+ photon upconverting nanoparticles. The design of a nucleotide sensor for the detection of point mutation associated with sickle cell disease is described. The underlying principle for the detection is luminescence resonance energy transfer (LRET), with the photon upconverting nanoparticle as the donor and a dye, N,N,N',N'-tetramethyl-6-carboxyrhodamine (TAMRA), as the acceptor. The detection scheme is based on a sandwich-type hybridization format. The presence of the target DNA is indicated by the increase of the normalized acceptor's emission. Based on photon upconverting nanoparticles, which display high S/N ratio and no photobleaching, the DNA sensor demonstrates high sensitivity and specificity. The results demonstrate great potential of such nanomaterials as oligonucleotide sensors.

  2. Synthesis and Characterization of LaTiO2N

    Science.gov (United States)

    Rugen, Evan E.

    Photocatalysts offer an excellent opportunity to shift the global energy landscape from a fossil fuel-dependent paradigm to sustainable and carbon-neutral solar fuels. Oxynitride materials such as LaTiO2N are potential photocatalysts for the water splitting reaction due to their high oxidative stability and their narrow band gaps, which are suitable for visible light absorption. However, facile synthetic routes to metal oxynitrides with controlled morphologies are rare, and the local structures of these materials are under-characterized. Ultrasonic spray synthesis (USS) offers a facile method toward complex metal oxides which can potentially be converted to oxynitrides with preservation of the microsphere structures that typify the products from such aerosol routes. Here, La-Ti-O microspheres were facilely produced by USS and converted by ammonolysis to LaTiO2N microspheres with porous shells and hollow interiors. This particle architecture is accounted for by coupling suitable combustion chemistry with the aerosol technique, producing precursor particles where the La3+ and Ti4+ are well-mixed at small length scales; this feature enables preservation of the microsphere morphology during nitridation despite the crystallographic changes that occur. The LaTiO2N microspheres are comparable oxygen evolving photocatalysts to samples produced by conventional solid state methods. Pair distribution function (PDF) analysis is a local probe designed to examine the structure of disordered crystalline materials, and is an ideal technique for characterizing the ordering of anions in oxynitrides. Preliminary studies using PDF analysis to determine the presence of anion ordering and local structure in LaTiO2N produced by solid state methods are presented here. Future experiments are proposed that will grant detailed insight into the factors driving the degree of anion ordering in these types of materials. These results demonstrate the utility of USS as a facile, potentially

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2017-01-01

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

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

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

  4. Combustion synthesis and characterization of nanocrystalline WO3.

    Science.gov (United States)

    Morales, Walter; Cason, Michael; Aina, Olawunmi; de Tacconi, Norma R; Rajeshwar, Krishnan

    2008-05-21

    The energy payback time associated with the semiconductor active material is an important parameter in a photovoltaic solar cell device. Thus lowering the energy requirements for the semiconductor synthesis step or making it more energy-efficient is critical toward making the overall device economics more competitive relative to other nonpolluting energy options. In this communication, combustion synthesis is demonstrated to be a versatile and energy-efficient method for preparing inorganic oxide semiconductors such as tungsten trioxide (WO3) for photovoltaic or photocatalytic solar energy conversion. The energy efficiency of combustion synthesis accrues from the fact that high process temperatures are self-sustained by the exothermicity of the combustion process, and the only external thermal energy input needed is for dehydration of the fuel/oxidizer precursor mixture and bringing it to ignition. Importantly, we show that, in this approach, it is also possible to tune the optical characteristics of the oxide semiconductor (i.e., shift its response toward the visible range of the electromagnetic spectrum) in situ by doping the host semiconductor during the formative stage itself. As a bonus, the resultant material shows enhanced surface properties such as markedly improved organic dye uptake relative to benchmark samples obtained from commercial sources. Finally, this synthesis approach requires only very simple equipment, a feature that it shares with other "mild" inorganic semiconductor synthesis routes such as sol-gel chemistry, chemical bath deposition, and electrodeposition. The present study constitutes the first use of combustion synthesis for preparing WO3 powder comprising nanosized particles.

  5. Transition metal borides. Synthesis, characterization and superconducting properties

    Energy Technology Data Exchange (ETDEWEB)

    Kayhan, Mehmet

    2013-07-12

    A systematic study was done on the synthesis and superconducting properties of metal rich transition metal borides. Five different binary systems were investigated including the boride systems of niobium, tantalum, molybdenum, tungsten and rhenium. High temperature solid state methods were used in order to synthesize samples of different transition metal borides of the composition M{sub 2}B, MB, M{sub 3}B{sub 2}, MB{sub 2}, and M{sub 2}B{sub 4}. The reactions were carried out in three different furnaces with different sample containers: the electric arc (copper crucible), the high frequency induction furnace (boron nitride, tantalum or glassy carbon crucibles), and the conventional tube furnace (sealed evacuated quartz ampoules). The products obtained were characterized with X-ray powder diffractometry, scanning electron microscopy and energy-dispersive X-ray spectroscopy. Phase analyses and crystal structure refinements using the Rietveld method and based on structure models known from literature were performed. A neutron diffraction measurement was done for W{sub 2}B{sub 4} to allow for a complete crystal structure determination, because of the presence of a heavy element like tungsten and a light element like boron that made it difficult to determine the accurate determination of the boron atom positions and occupancies from X-ray data. A new structure model for W{sub 2}B{sub 4} was proposed. Magnetic measurements in a SQUID magnetometer down to temperatures as low as 1.8 K were performed to several of the products in order to see if the transition metal borides become superconducting at low temperatures, and the results were compared with data from literature. Superconducting properties were found for the following compounds: NbB{sub 2} (T{sub C} = 3.5 K), β-MoB (T{sub C} = 2.4 K), β-WB (T{sub C} = 2.0 K), α-WB (T{sub C} = 4.3 K), W{sub 2}B{sub 4} (T{sub C} = 5.4 K), Re{sub 7}B{sub 3} (T{sub C} = 2.4 K). A relationship between the superconducting properties

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

    Science.gov (United States)

    Haders, Daniel Joseph, II

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-09-03

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2006-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2013-11-15

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

  10. Metal oxide and mercuric sulfide nanoparticles synthesis and characterization

    Science.gov (United States)

    Xu, Xin

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

  11. Synthesis And Characterization Of Gd2O3: Tb 30%

    Science.gov (United States)

    Djebara, Abdelhakim; Halimi, Rachid

    2008-09-01

    Over the past decade, nanotechnology has grown leading to the control of the synthesis and functionalization of nanoparticule for applications in the biological marking. The manufacture of nanoparticule luminescent intrinsically could move towards a single detection. By saving this very small optical signal, we can track the movement of the receptor in the membrane during unprecedented times, reaching overtime. This result is a significant advantage compared to the fluorescent molecules whose average lifespan is more limited. These particles can be detected by both the luminescence of rare earth ions present in the heart and that of organic fluorophore. The results look very encouraging. This work aims to study the development of nanoparticule of rare earth oxide as probes to monitor the dynamics of action unique biological entities. The goal of my work has been improved reproducibility of the synthesis and optimization protocol synthesis.

  12. Synthesis of new fullerides via the "break-and-seal" approach and their characterization

    OpenAIRE

    Kozhemyakina, Nina V.

    2009-01-01

    The present dissertation deals with the synthesis and characterization of fullerides. For the first time the "break-and-seal" technique was applied for fulleride synthesis. The reaction was performed in a completely all-glass apparatus under vacuum, avoiding the use of glass connections and use of grease. Starting from crown-ethers, potassium metal and C60 fullerene, six new fullerides have been synthesized. The modified "temperature difference method" was successfully used for growing single...

  13. Synthesis and characterization of new homologous series of ...

    Indian Academy of Sciences (India)

    isoxazoles, including 1,3-Dipolar Cycloaddition reac- tion,14 and condensation of 1,3-dicarbonyl compounds with hydroxylamine and condensations.15 Our interest in synthesizing isoxazole derivatives comes from the ease of synthesis and their excellent mesomorphic behaviour. The isoxazole ring incorporates a strong. ∗.

  14. short communication synthesis and characterization of two novel ...

    African Journals Online (AJOL)

    Preferred Customer

    spectroscopy and thermogravimetric analysis (TGA). These complexes contain ... are active as homo-generous catalysts for a variety of oxidation reactions [6, 7]. Secondly, in the particular case of ... In this paper, we report synthesis, elemental analysis, IR and UV-Vis data of two new trinuclear complexes containing acrylic ...

  15. The synthesis, characterization and biological evaluation of a stable ...

    African Journals Online (AJOL)

    A convenient one pot synthesis of two novel compounds including a stable phosphorus ylide and an imidazole from electron-poor acetylenes in fairly good yields by the condensation of triphenylphosphine and acetylene derivatives, in the presence of dimethyl thiourea from the 1:1:1 addition reactions is described.

  16. Synthesis and characterization of PbTe micro/nanostructures ...

    Indian Academy of Sciences (India)

    In addition, effect of preparation parameters like reaction time and temperature in hydrothermal synthesis on the morphology of the final products was tested. The products were analysed with the aid of SEM, XRD, FT–IR and EDS. Based on the obtained results, it was found that pure cubic phased PbTe has been obtained ...

  17. A study on the synthesis, characterization and catalytic activity of ...

    Indian Academy of Sciences (India)

    2017-11-23

    Nov 23, 2017 ... K K Shah and A K Talukdar with routes based upon more environment-friendly technolo- gies. Therefore, direct phenol hydroxylation with H2O2 is of contemporary interest. 2. Experimental. 2.1 Synthesis of MFI zeolites. In this work, Ru-incorporated MFI zeolites were synthesized with an Si to Al and Ru ...

  18. Synthesis and characterization of bi-functional magneto-luminescent ...

    Indian Academy of Sciences (India)

    A step-wise synthetic method has been developed for the synthesis of multifunctional, magnetic luminescent nanocomposites with Fe₃O₄ nanospheres as the core encapsulated in silica and europium-doped sodium lutetium fluoride (NaLuF₄ :Eu³⁺) as the shell. X-ray powder diffraction (XRPD), scanning electron ...

  19. Synthesis, characterization, X-ray structure, optical properties and ...

    Indian Academy of Sciences (India)

    ESMA LAMERA

    +. Scheme 1. Synthesis of compounds 1 and 2. mixture of EtOH-H2O as solvents and catalytic quantity of sulfuric acid. Two hours are sufficient for complete conversion of the starting materials. The crude product ..... Phys. Lett. 397. 31. Kleinman, D A 1962 Nonlinear Dielectric Polarization in optical media Phys. Rev. 126 1977.

  20. Synthesis and characterization of mixture of nanozirconia and ...

    Indian Academy of Sciences (India)

    Administrator

    synthesis of multi-component inorganic materials. For example, Nagarajan and Rao (1990) synthesized .... the possible reaction intermediates in the acid dissolution stage. It is well known from the literature (Craigen et ... route and dental restorative polymer composites rein- forced with this nanopowder. Acknowledgements.

  1. SYNTHESIS AND CHARACTERIZATION OF N, N'-BIS-(3 ...

    African Journals Online (AJOL)

    user

    deactivators, separation techniques and environmental chemistry. (Trevin et al., 1997). Perla et al. (2006) reported the synthesis of Ni (II) and Co(II) complexes with N,N'-. Bis(2-benzyl)ethylenediimine as modifying agents to produce chemically modified electrodes used to facilitate the detection of organic pollutants in water.

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

    Science.gov (United States)

    Mahler, Graciela; Davyt, Danilo; Gordon, Sandra; Incerti, Marcelo; Nunez, Ivana; Pezaroglo, Horacio; Scarone, Laura; Serra, Gloria; Silvera, Mauricio; Manta, Eduardo

    2008-01-01

    In this laboratory activity, students are introduced to the synthesis of an albendazole metabolite obtained by a sulfide oxidation reaction. Albendazole as well as its metabolite, albendazole sulfoxide, are used as anthelmintic drugs. The oxidation reagent is H[subscript 2]O[subscript 2] in acetic acid. The reaction is environmental friendly,…

  3. Synthesis and characterization of mesoporous Si-MCM-41 materials ...

    Indian Academy of Sciences (India)

    Administrator

    synthesis of plasticizers, perfumes, fragrance in cosme- tics, flavours in food, diluents in paints and coatings and intermediates in drugs, dye stuffs and fine chemicals. (Otera 2003). The conventional catalyst used in esterifi- cation reactions is sulphuric acid, methanesulfonic acid or p-toluenesulfonic acid that are cited as ...

  4. Combustion synthesis and structural characterization of Li–Ti mixed ...

    Indian Academy of Sciences (India)

    saturation at an applied field of ±10 kOe and the loops are highly symmetric in nature. The cation distribution is known indirectly by using saturation magnetization values. Keywords. Li–Ti mixed ferrites; combustion synthesis; hysteresis. 1. Introduction. Lithium ferrites are low cost materials, which are gene- rally found useful ...

  5. A Study on the Synthesis, Characterization and Catalytic Activity of ...

    Indian Academy of Sciences (India)

    49

    incorporated Mobil Five (MFI) zeolite materials with silicon (Si) to aluminium (Al) ratio. 14 of 100 and with Al .... synthesis procedure were tetrapropylammonium bromide (Lancaster), sodium aluminate. 76. (Kemphasol) ...... Pilot Plant Scale Reactor, Industrial and Engineering Chemistry Research, 37 (1998). 332. 2081. 333.

  6. Synthesis and characterization of nickel/barium hexa-aluminate ...

    Indian Academy of Sciences (India)

    Electrodeposition of nickel/barium hexa-aluminate (Ni/BHA) composite coatings has been carried out from a Watt's bath on mild steel substrate. BHA powders with plate habit were synthesized by solution combustion synthesis followed by heat treatment to ensure complete conversion to the hexa-aluminate phase.

  7. Synthesis and characterization of single-source molecular ...

    Indian Academy of Sciences (India)

    regime. Precursors for palladium chalcogenides, indium sulphides and II–VI materials are presented. Synthesis of a variety of palladium(II)/platinum(II) complexes with internally functionalised chalco- genolate ligands, selenocarboxylates; gallium and indium dithiolate complexes and zinc/cadmium/ mercury complexes with ...

  8. Synthesis and photonic bandgap characterization of polymer inverse opals

    Energy Technology Data Exchange (ETDEWEB)

    Miguez, H.; Meseguer, F.; Lopez, C. [Consejo Superior de Investigaciones Cientificas, Madrid (Spain). Inst. de Ciencia de Materiales; Universidad Politecnica de Valencia (Spain). Centro Tecnologico de Ondas; Lopez-Tejeira, F.; Sanchez-Dehesa, J. [Universidad Autonoma de Madrid (Spain). Dept. de Fisica Teorica de la Materia Condensada

    2001-03-16

    Polymer inverse opals with long-range order have been fabricated and their photonic crystal behavior examined. Good agreement between band structure calculations and experiment is found. It is envisaged that these inverse opals could be used for the modification of the electronic properties of incorporated luminescent materials and as matrices for the synthesis of spherical colloidal particles. (orig.)

  9. Noble silver nanoparticles (AgNPs) synthesis and characterization ...

    African Journals Online (AJOL)

    Nanotechnology is rapidly growing with nanoparticles produced and utilized in a wide range of pharmaceutical and commercial products throughout the world. In this study, fig (Ficus carica) leaf extracts were used for ecofriendly extracellular synthesis of stable silver nanoparticles (AgNPs) by treating an aqueous silver ...

  10. Synthesis and characterization of Polyindole and its catalytic ...

    Indian Academy of Sciences (India)

    The catalytic performance study of polyindole as a heterogeneous catalyst is reported for the synthesis of 3,3'-arylmethylene-bis-1H-Indole derivatives using various substituted aldehydes and indole under reflux reaction condition with good to excellent yield. Polyindole was synthesized by chemical oxidative polymerization ...

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

    Indian Academy of Sciences (India)

    tion of hydrocarbons and as precursors in the synthesis of hydrodesulfurization catalyst,10 sensors,11 scintilla- tor materials,12 and for their electrochemical,13 and photoluminescence14 properties. The molybdate material, NiMoO4 was applied for alkane dehydrogenation.15 Three different phases of nickel molybdate can ...

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

    CSIR Research Space (South Africa)

    Aderibigbe, BA

    2014-01-01

    Full Text Available In this research, aminoquinoline compounds were synthesized, characterized and incorporated into water soluble polymers to form conjugates. The conjugates were characterized by X ray Diffraction (XRD), Thermal Gravimetric Analysis (TGA), Scanning...

  13. 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.

  14. Synthesis and biological characterization of arylomycin B antibiotics.

    Science.gov (United States)

    Roberts, Tucker C; Smith, Peter A; Romesberg, Floyd E

    2011-05-27

    Antibiotics are virtually always isolated as families of related compounds, but the evolutionary forces underlying the observed diversity are generally poorly understood, and it is not even clear whether they are all expected to be biologically active. The arylomycin class of antibiotics is comprised of three related families that are differentiated by nitration, glycosylation, and hydroxylation of a conserved core scaffold. Previously, we reported the total synthesis of an A series member, arylomycin A2, as well as the A series derivative arylomycin C16 and showed that both are active against a broader spectrum of bacteria than previously appreciated. We now report the total synthesis of a B series analogue, arylomycin B-C16, and its aromatic amine derivative. While the aromatic amine loses activity against all bacteria tested, the B series compound shows activities that are similar to the A series compounds, except that it also gains activity against the important pathogen Streptococcus agalactiae.

  15. One Pot Synthesis and Characterization of Alginate Stabilized Semiconductor Nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Sundarrajan, Parani; Eswaran, Prabakaran; Marimuthu, Alexander; Subhadra, Lakshmi Baddireddi; Kannaiyan, Pandian [Univ., of Madras, Chennai (India)

    2012-10-15

    Uniform and well dispersed metal sulfide semiconductor nanoparticles incorporated into matrices of alginate biopolymer are prepared by using a facile in situ method. The reaction was accomplished by impregnation of alginate with divalent metal ions followed by reaction with thioacetamide. XRD analysis showed that the nanoparticles incorporated in the polymer matrix were of cubic structure with the average particle diameter of 1.8 to 4.8 nm. Field emission scanning electron microscopy and high resolution transmission electron microscopy images indicated that the particles were well dispersed and distributed uniformly in the matrices of alginate polymer. FT-IR spectra confirmed the presence of alginate in the nanocomposite. The crystalline nature and thermal stability of the alginate polymer was found to be influenced by the nature of the divalent metal ions used for the synthesis. The proposed method is considered to be a simple and greener approach for large scale synthesis of uniform sized nanoparticles.

  16. Synthesis and Characterization of Two New p-tert-Butylcalix[4]-arene Schiff Bases

    Directory of Open Access Journals (Sweden)

    Saeed Taghvaee Ganjali

    2001-03-01

    Full Text Available Synthesis and characterization of two new Schiff bases of p-tertbuthylcalix[4]arene (H2L1 and HL2 is described. The synthesis of H2L1 and HL2 has been achieved by the condensation of salicylaldehyde with the amine group of upper rim monoamine p-tert-butylcalix[4]arene in ethanol. These compounds have been characterized on the basis of elemental analysis and spectral data. Solvatochromicity and fluorescence properties were observed and measured for H2L1 and HL2. Solvatochromicity of these ligands indicates their potential for NLO applications.

  17. Synthesis, Characterization and Applications in Catalysis of Polyoxometalate/Zeolite Composites

    Directory of Open Access Journals (Sweden)

    Frédéric Lefebvre

    2016-05-01

    Full Text Available An overview of the synthesis, characterization and catalytic applications of polyoxometalates/zeolites composites is given. The solids obtained by direct synthesis of the polyoxometalate in the presence of the zeolite are first described with their applications in catalysis. Those obtained by a direct mixing of the two components are then reviewed. In all cases, special care is taken in the localization of the polyoxometalate, inside the zeolite crystal, in mesopores or at the external surface of the crystals, as deduced from the characterization methods.

  18. Synthesis and characterization of metal/semiconductor nanocomposites for photocatalysis

    OpenAIRE

    Mavrič, Tina

    2017-01-01

    The doctoral dissertation focused on improving photocatalytic activity of nanopowdered ZnO by constructing I) Metal-Semiconductor and II) Semiconductor-Semiconductor heterostructures. Both heterostructure types have been reported to have a beneficial effect on photocatalytic efficiency. For the first part (I) Ag/ZnO nanocomposite was synthesized. Here we investigated an influence of polyvinylpyrrolidone (PVP) addition during the synthesis on the particle properties and their photoactivity. Th...

  19. Synthesis and Characterization of a New Perhalogenated Porphyrin

    Energy Technology Data Exchange (ETDEWEB)

    Jia, Songling; Medforth, Craig J.; Nelson, Nora Y.; Nurco, Daniel J.; Shelnutt, John; Smith, Kevin M.

    1999-05-19

    The first synthesis of an octahalotetraalkylporphyrin [2,3,7,8,12,13,17,18 -octabromo-5,10,15,20- tetrakis(trifluoromethyl)porphinato nickel(II)] is reported; this perhalogenated porphyrin has several novel properties including a very nonplanar ruffled structure with an unusually short Ni- N distance, an extremely red-shifted optical spectrum, and hindered rotation of the trifluoromethyl groups ({Delta}G278K =47 kJ mol-1).

  20. Synthesis, surface characterization and optical properties of 3 ...

    Indian Academy of Sciences (India)

    mizes the solubility difference between CuS and ZnS by coordinating with Cu2+ and thus the possibility of copre- cipitation of ZnS and CuS can be greatly improved during the synthesis and this makes it possible to obtain ZnS:Cu nanoparticles in which Cu2+ ions replace the Zn2+ ions in the lattice. 3.2 Grain size studies.

  1. Synthesis and thermoelectric characterization of Bi2Te3 nanoparticles

    OpenAIRE

    Scheele, Marcus; Oeschler, Niels; Meier, Katrin; Kornowski, Andreas; Klinke, Christian; Weller, Horst

    2010-01-01

    We report a novel synthesis for near monodisperse, sub-10-nm Bi2Te3 nanoparticles. At first, a new reduction route to bismuth nanoparticles is described which are applied as starting materials in the formation of rhombohedral Bi2Te3 nanoparticles. After ligand removal by a novel hydrazine hydrate etching procedure, the nanoparticle powder is spark plasma sintered to a pellet with preserved crystal grain sizes. Unlike previous works on the properties of Bi2Te3 nanoparticles, the full thermoele...

  2. Controlling Magnetic and Ferroelectric Order Through Geometry: Synthesis, Ab Initio Theory, Characterization of New Multi-Ferric Fluoride Materials

    Energy Technology Data Exchange (ETDEWEB)

    Halasyamani, Shiv [Univ. of Houston, TX (United States); Fennie, Craig [Cornell Univ., Ithaca, NY (United States)

    2016-11-03

    We have focused on the synthesis, characterization, and ab initio theory on multi-functional mixed-metal fluorides. With funding from the DOE, we have successfully synthesized and characterized a variety of mixed metal fluoride materials.

  3. Synthesis and characterization of castor oil based polyurethane ...

    Indian Academy of Sciences (India)

    Unknown

    The filled mold was kept in a preheated circulating air oven maintained at 70°C. It was held at this temperature for 24 h and 120°C for 4 h. The sheet thus formed, was cooled slowly and removed from the mold. 3. Characterization and testing. The IPNs were characterized according to the ASTM standard specification.

  4. Synthesis and electrochemical characterization of stabilized nickel nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Dominguez-Crespo, M.A.; Ramirez-Meneses, E.; Torres Huerta, A.M. [Centro de Investigacion en Ciencia Aplicada y Tecnologia Avanzada, CICATA-IPN Unidad Altamira, Carretera Tampico-Puerto Industrial, C.P. 89600 Altamira, Tamaulipas (Mexico); Montiel-Palma, V. [Centro de Investigaciones Quimicas, Universidad Autonoma del Estado de Morelos, Av. Universidad 1001, Colonia Chamilpa, C.P.62201 Cuernavaca, Morelos (Mexico); Dorantes Rosales, H. [Departamento de Metalurgia, Escuela Superior de Ingenieria Quimica e Industrias Extractivas - IPN, C.P. 07300, D.F. (Mexico)

    2009-02-15

    Nickel stabilized nanoparticles produced by an organometallic approach (Chaudret's method) starting from the complex Ni(1,5-COD){sub 2} were used as electrode materials for hydrogen evolution in NaOH at two temperatures (298 and 323 K). The synthesis of the nickel nanoparticles was performed in the presence of two different stabilizers, 1,3-diaminopropane (DAP) and anthranilic acid (AA), by varying the molar ratios (1:1, 1:2 and 1:5 metal:ligand) in order to evaluate their influence on the shape, dispersion, size and electrocatalytic activity of the metallic particles. The presence of an appropriate amount of stabilizer is an effective alternative to the synthesis of small monodispersed metal nanoparticles with diameters around 5 and 8 nm for DAP and AA, respectively. The results are discussed in terms of morphology and the surface state of the nanoparticles. The importance of developing a well-controlled synthetic method which results in higher performances of the resulting nanoparticles is highlighted. Herein we found that the performance with respect to the HER of the Ni electrodes dispersed on a carbon black Vulcan substrate is active and comparable to that reported in the literature for the state-of-the-art electrocatalysts. Appreciable cathodic current densities of {proportional_to}240 mA cm{sup -2} were measured with highly dispersed nickel particles (Ni-5{sub DAP}). This work demonstrates that the aforementioned method can be extended to the preparation of highly active stabilized metal particles without inhibiting the electron transfer for the HER reaction, and it could also be applied to the synthesis of bimetallic nanoparticles. (author)

  5. First synthesis and characterization for the stereoisomers of Ulipristal acetate.

    Science.gov (United States)

    Zhao, Yi; Li, Xiaolong; Liu, Hong; Yu, Yongguo; Hai, Li; Guo, Li; Wu, Yong

    2015-03-01

    The three stereoisomers, 11α,17α-isomer I, 11α,17β-isomer II and 11β,17β-isomer III are related substances of the selective progesterone receptor modulator Ulipristal acetate. Herein, we presented an efficient and practical synthesis approach to deliver these three stereoisomers for the first time, and also confirmed the structure of the key intermediate 5a by single-crystal X-ray analysis. Our research will be of immense help for organic chemists to study the impurity profile of Ulipristal acetate. Copyright © 2014 Elsevier Inc. All rights reserved.

  6. Solution combustion synthesis and characterization of nanosized bismuth ferrite

    Science.gov (United States)

    Sai Kumar, V. Sesha; Rao, K. Venkateswara; Krishnaveni, T.; Kishore Goud, A. Shiva; Reddy, P. Ranjith

    2012-06-01

    The present paper describes a simple method of nanosized BiFeO3 by the solution combustion synthesis using bismuth and iron nitrates as oxidizers and the combination fuel of citric acid and ammonium hydroxide, with fuel to oxidizer ratio (Ψ = 1) one. The X-ray Diffraction results indicated rhombohedral phase (R3m) with JCPDS data card no: 72-2035. The ferroelectric transition of the sample at 8310C was detected by differential thermal analysis. Thermal analysis was done by Thermal gravimetric-Differential thermal analyzer and obtained results were presented in this paper.

  7. Green synthesis and characterization of silver nanoparticle using Aloe barbadensis

    Energy Technology Data Exchange (ETDEWEB)

    Thappily, Praveen, E-mail: pravvmon@gmail.com, E-mail: shiiuvenus@gmail.com; Shiju, K., E-mail: pravvmon@gmail.com, E-mail: shiiuvenus@gmail.com [Laboratory for Molecular Photonics and Electronics (LAMP), Department of Physics, National Institute of Technology, Calicut, Kerala 673601 (India)

    2014-10-15

    Green synthesis of silver nanoparticles was achieved by simple visible light irradiation using aloe barbadensis leaf extract as reducing agent. UV-Vis spectroscopic analysis was used for confirmation of the successful formation of nanoparticles. Investigated the effect of light irradiation time on the light absorption of the nanoparticles. It is observed that upto 25 minutes of light irradiation, the absorption is linearly increasing with time and after that it becomes saturated. Finally, theoretically fitted the time-absorption graph and modeled a relation between them with the help of simulation software.

  8. Green synthesis and characterization of silver nanoparticle using Aloe barbadensis

    Science.gov (United States)

    Thappily, Praveen; Shiju, K.

    2014-10-01

    Green synthesis of silver nanoparticles was achieved by simple visible light irradiation using aloe barbadensis leaf extract as reducing agent. UV-Vis spectroscopic analysis was used for confirmation of the successful formation of nanoparticles. Investigated the effect of light irradiation time on the light absorption of the nanoparticles. It is observed that upto 25 minutes of light irradiation, the absorption is linearly increasing with time and after that it becomes saturated. Finally, theoretically fitted the time-absorption graph and modeled a relation between them with the help of simulation software.

  9. Synthesis and Crystallographic Characterization of a Maleimide Derivative of Tryptamine

    Directory of Open Access Journals (Sweden)

    Jean Dubois

    2016-11-01

    Full Text Available While mechanosynthesis of the target compound, 1-[2-(1H-indol-3-yl-ethyl]-pyrrole-2,5-dione, C14 H12 N2 O2, did not yield the desired product, it instead resulted in an open intermediate. On the other hand, synthesis starting from the activated maleic anhydride yielded the final maleimide compound. The outcome of the mechanosynthesis has been evaluated by powder X-ray diffraction, and structures of both the final product and open intermediate have been confirmed using single-crystal crystallography.

  10. Synthesis and characterization of zwitterionic carbon dioxide fixing reagents

    DEFF Research Database (Denmark)

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

    2010-01-01

    The synthesis of three amine-based carbon dioxide fixing reagents is presented. The reagents were designed so that they would be able to bind CO2 reversibly through the formation of the well known carbamates that was stabilized through forming a zwitterion. CO2 fixing experiments were performed...... with 13CO2 labeling and medium pressure NMR. The experiments showed that two of the three reagents were able to form carbamates and thus bind CO2. In addition we investigated this particular class of molecules for the possible formation of neutrally charged spiro compounds and we show that these did...

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

    OpenAIRE

    Anish Stephen; Sankar Seethalakshmi

    2013-01-01

    This 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 20–40 nm. Optimization of methodology in terms of concentration of reactants and pH of the reaction mixture reduced the reaction time for silver nanoparticle formation to 2 mins. Silve...

  12. The ovalbumin gene. In vitro enzymatic synthesis and characterization.

    Science.gov (United States)

    Monahan, J J; McReynolds, L A; O'Malley, B W

    1976-12-10

    Using purified single-stranded ovalbumin complementary DNA (cDNAov) as a template for avian myeloblastosis (AM) virus reverse transcriptase, we have enzymatically synthesized a complete double-stranded cDNAov sequence. Our data suggests that many single-stranded cDNAov molecules contain short double-stranded sequences (hairpins) at their 3' termini capable of acting as primers for synthesis of complete double-stranded cDNAs. Optimum conditions for synthesis of the double-stranded cDNAov were found to be a high temperature (46 degrees) and a low salt concentration. Nevertheless, in all cases 40% of the initial single-stranded cDNAov molecules fail to prime for synthesis of a complementary double strand. Following synthesis, the second DNA strand is covalently linked to the first cDNAov strand as shown by analysis on alkaline sucrose gradients. The two strands have a high Tm on hydroxylapatite (89 degrees). These intact double-stranded cDNAov structures have a bouyant density in CsCl gradients of 1.700 g/cm3 and rapidly renature after heat denaturation with a C0t1/2 value of less than 2 X 10(-6) mol s liter(-1). All size classes of cDNAs, i.e. partial as well as complete transcripts of the mRNA, are capable of forming double-stranded structures. The closed loop of the double-stranded cDNAov could be opened with S1 nuclease. The denatured complementary strands of the cDNAov then renatured with the appropriate second order kinetics at a C0t1/2 value of 1.89 X 10(-3) mol s liter(-1). Using the enzyme terminal deoxyribonucleotidyltransferase to label to free 3'-terminal end of double-stranded [32P]cDNAov with 3H, we demonstrate a convenient procedure to study the site for restriction endonuclease cleavage within the ovalbumin gene.

  13. Bifunctional cyclam-based ligands with phosphorus acid pendant moieties for radiocopper separation: thermodynamic and kinetic studies.

    Science.gov (United States)

    Paúrová, Monika; Havlíčková, Jana; Pospíšilová, Aneta; Vetrík, Miroslav; Císařová, Ivana; Stephan, Holger; Pietzsch, Hans-Jürgen; Hrubý, Martin; Hermann, Petr; Kotek, Jan

    2015-03-16

    Two macrocyclic ligands based on cyclam with trans-disposed N-methyl and N-(4-aminobenzyl) substituents as well as two methylphosphinic (H2L1) or methylphosphonic (H4L2) acid pendant arms were synthesised and investigated in solution. The ligands form stable complexes with transition metal ions. Both ligands show high thermodynamic selectivity for divalent copper over nickel(II) and zinc(II)-K(CuL) is larger than K(Ni/ZnL) by about seven orders of magnitude. Complexation is significantly faster for the phosphonate ligand H4L2, probably due to the stronger coordination ability of the more basic phosphonate groups, which efficiently bind the metal ion in an "out-of-cage" complex and thus accelerate its "in-cage" binding. The rate of Cu(II) complexation by the phosphinate ligand H2L1 is comparable to that of cyclam itself and its derivatives with non-coordinating substituents. Acid-assisted decomplexation of the copper(II) complexes is relatively fast (τ1/2 = 44 and 42 s in 1 M aq. HClO4 at 25 °C for H2L1 and H4L2, respectively). This combination of properties is convenient for selective copper removal/purification. Thus, the title ligands were employed in the preparation of ion-selective resins for radiocopper(II) separation. Glycidyl methacrylate copolymer beads were modified with the ligands through a diazotisation reaction. The separation ability of the modified polymers was tested with cold copper(II) and non-carrier-added (64)Cu in the presence of a large excess of both nickel(II) and zinc(II). The experiments exhibited high overall separation efficiency leading to 60-70% recovery of radiocopper with high selectivity over the other metal ions, which were originally present in 900-fold molar excess. The results showed that chelating resins with properly tuned selectivity of their complexing moieties can be employed for radiocopper separation. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Synthesis and characterization of semiconductor nanomaterials for thermoelectric applications

    Science.gov (United States)

    Dirmyer, Matthew R.

    In this dissertation, I explore simple chemical means to produce various nanomaterials. In Chapter 2, the synthesis of size-tuned bismuth telluride nanoparticles is discussed. The solution phase synthesis of bismuth telluride nanoparticles has been accomplished in the presence of a library of thiols as the capping ligand. These crystalline nanostructures range in size from ˜20 to ˜100nm with a relatively narrow size dispersity. Size and shape of the resulting nanostructures has been investigated as a function of chain length of the thiol and temperature. An investigation into the thermoelectric properties of the nanostructures shows promising electrical conductivity, thermopower, and thermal conductivity for undoped bismuth telluride. In Chapter 3, a soluble precursor for antimony telluride is described. This precursor was used to fabricate semiconductor nanowires of varying diameter and thin films through simple templating methods. Electrical conductivity and thermoelectric power measurements of these films are only slightly lower than for antimony telluride films fabricated by vacuum deposition. In Chapter 4, the polytetrafluoroethylene (PTFE)/metal nanocomposites are discussed. Palladium and nickel PTFE nanocomposites were made by impregnation of the polymer with metal acetates. Annealing and jet blowing of these materials form PTFE nanofiber/metal nanoparticle composites.

  15. Synthesis and characterization of hydroxyapatite from fish bone waste

    Science.gov (United States)

    Marliana, Ana; Fitriani, Eka; Ramadhan, Fauzan; Suhandono, Steven; Yuliani, Keti; Windarti, Tri

    2015-12-01

    Waste fish bones is a problem stemming from activities in the field of fisheries and it has not been used optimally. Fish bones contain calcium as natural source that used to synthesize hydroxyapatite (HA). In this research, HA synthesized from waste fish bones as local wisdom in Semarang. The goal are to produce HA with cheaper production costs and to reduce the environmental problems caused by waste bones. The novelty of this study was using of local fish bone as a source of calcium and simple method of synthesis. Synthesis process of HA can be done through a maceration process with firing temperatures of 1000°C or followed by a sol-gel method with firing at 550°C. The results are analyzed using FTIR (Fourier Transform Infrared), XRD (X-Ray Diffraction) and SEM-EDX (Scanning Electron Microscopy-Energy Dispersive X-Ray). FTIR spectra showed absorption of phosphate and OH group belonging to HA as evidenced by the results of XRD. The average grain size by maceration and synthesized results are not significant different, which is about 69 nm. The ratio of Ca/P of HA by maceration result is 0.89, then increase after continued in the sol-gel process to 1.41. Morphology of HA by maceration results are regular and uniform particle growth, while the morphology of HA after the sol-gel process are irregular and agglomerated.

  16. Synthesis and characterization of hydroxyapatite from fish bone waste

    Energy Technology Data Exchange (ETDEWEB)

    Marliana, Ana, E-mail: na-cwith22@yahoo.co.id; Fitriani, Eka; Ramadhan, Fauzan; Suhandono, Steven; Yuliani, Keti; Windarti, Tri [Chemistry Department, Faculty of Science and Mathematics, Diponegoro University, Indonesia, 50 275 (Indonesia)

    2015-12-29

    Waste fish bones is a problem stemming from activities in the field of fisheries and it has not been used optimally. Fish bones contain calcium as natural source that used to synthesize hydroxyapatite (HA). In this research, HA synthesized from waste fish bones as local wisdom in Semarang. The goal are to produce HA with cheaper production costs and to reduce the environmental problems caused by waste bones. The novelty of this study was using of local fish bone as a source of calcium and simple method of synthesis. Synthesis process of HA can be done through a maceration process with firing temperatures of 1000°C or followed by a sol-gel method with firing at 550°C. The results are analyzed using FTIR (Fourier Transform Infrared), XRD (X-Ray Diffraction) and SEM-EDX (Scanning Electron Microscopy-Energy Dispersive X-Ray). FTIR spectra showed absorption of phosphate and OH group belonging to HA as evidenced by the results of XRD. The average grain size by maceration and synthesized results are not significant different, which is about 69 nm. The ratio of Ca/P of HA by maceration result is 0.89, then increase after continued in the sol-gel process to 1.41. Morphology of HA by maceration results are regular and uniform particle growth, while the morphology of HA after the sol-gel process are irregular and agglomerated.

  17. SYNTHESIS AND CHARACTERIZATION OF BIODEGRDABLE PLASTIC FROM CASAVA STARCH AND ALOE VERA EXTRACT WITH GLYCEROL PLASTICIZER

    OpenAIRE

    Mery Apriyani; Endaruji Sedyadi

    2016-01-01

    Synthesis and characterizations of Biodegradable Plastic made of Cassava Waste Starch, glycerol, acetic acid and Aloe vera extract has done. The aims of this research are to study the influence of addition of aloe vera extract in plastics mechanics properties, water vapor transmission rate and biodegradation. There are five main steps in this research, extraction of aloe vera, cassava starch preparation from cassava waste, preparations, characterization and biodegradability study of biodegrad...

  18. Synthesis and characterization of implants for bone substitutions made of biomedical apatites containing silicon

    OpenAIRE

    Sprio, Simone

    2008-01-01

    In the last decades the development of bone substitutes characterized by a superior biomimetism has become of particular interest, owing to the increasing economic and societal impact of the bone diseases. In the present work of research the development of bone substitutes characterized by improved biomimetism, has been faced in a chemical, structural and morphological perspective. From a chemical point of view, it has been developed the synthesis of hydroxyapatite powders, exhibiting m...

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

    African Journals Online (AJOL)

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

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

    African Journals Online (AJOL)

    acetohydrazide have been prepared. All the compounds were analytically and spectroscopically characterized by various techniques. The data of molar conductance indicated the prepared complexes are nonelectrolyte in nature except complexes (10) ...

  1. Synthesis, characterization and catalytic performance of a novel ...

    Indian Academy of Sciences (India)

    22 precursor with H2O2 and characterized by various physicochemical techniques (X-ray powder diffraction, transmission electron microscopy, thermogravimetric-differential thermal analyses, Fourier transform infrared spectroscopy and ...

  2. Synthesis and characterization of nanoboron powders prepared with ...

    Indian Academy of Sciences (India)

    % hydrochloric acid (only one) to remove impurities. Boron powders were obtained after centrifuging, decanting, washing and drying operations. Sample was characterized by inductively coupled plasma (ICP), energy-dispersive spectroscopy, ...

  3. Synthesis and characterization of pyrochlore-type yttrium titanate ...

    Indian Academy of Sciences (India)

    , Hunan 410083, P.R. China. 2Key Laboratory of ... East China Institute of Technology, Fuzhou, Jiangxi 344000, P.R. China ... microstructures and average size of as-prepared products were characterized by transmission electron microscopy.

  4. Synthesis and characterization of stable aqueous dispersions of ...

    Indian Academy of Sciences (India)

    The chemically synthesized graphene was characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), UV–visible absorption spectroscopy, Fourier transform infrared (FTIR) and Raman spectroscopy, thermogravimetric analysis (TGA), optical microscopy. The stability of aqueous ...

  5. Extended germa[N]pericyclynes: synthesis and characterization.

    Science.gov (United States)

    Tanimoto, Hiroki; Fujiwara, Taro; Mori, Junta; Nagao, Tomohiko; Nishiyama, Yasuhiro; Morimoto, Tsumoru; Ito, Shunichiro; Tanaka, Kazuo; Chujo, Yoshiki; Kakiuchi, Kiyomi

    2017-02-14

    We herein describe the syntheses and characterization of extended germa[N]pericyclynes, which are macrocycles composed of germanium-butadiyne units. The obtained novel extended germa[4]-[8]pericyclynes were characterized by X-ray crystallography, UV-Vis spectroscopy, fluorescence and phosphorescence emission spectroscopy, and cyclic voltammetry, and exhibited characteristic absorptions and emissions. Density functional theory (DFT) calculations suggested smaller HOMO-LUMO gap energy compared to that of general germapericyclynes.

  6. Synthesis and characterization of novel benzo[d][1,3]dioxole ...

    Indian Academy of Sciences (India)

    Abstract. An expeditious synthesis of novel organoselenium compounds (2–5) incorporating benzo[d]. [1,3]dioxole subunit has been reported. All these newly synthesized compounds have been characterized by elemental analysis and various spectroscopic techniques viz., multinuclear NMR (1H, 13C and 77Se), IR and.

  7. Synthesis and characterization of sol–gel derived ZnS: Mn 2 ...

    Indian Academy of Sciences (India)

    Synthesis and characterization of undoped and Mn2+ doped ZnS nanocrystallites (radius 2–3 nm) embedded in a partially densified silica gel matrix are presented. Optical transmittance, photoluminescence (PL), ellipsometric and electron spin resonance measurements revealed manifestation of quantum size effect.

  8. Synthesis and characterization of hydroxyapatite crystals: a review study on the analytical methods

    NARCIS (Netherlands)

    Koutsopoulos, S.

    2002-01-01

    For the synthesis of hydroxyapatite crystals from aqueous solutions three preparation methods were employed. From the experimental processes and the characterization of the crystals it was concluded that aging and precipitation kinetics are critical for the purity of the product and its

  9. Synthesis, characterization and gas sensing performance of SnO2 ...

    Indian Academy of Sciences (India)

    Synthesis, characterization and gas sensing performance of SnO2 thin films prepared by spray pyrolysis. GANESH E PATIL, D D KAJALE, D N CHAVAN†, N K PAWAR††, P T AHIRE, S D SHINDE#,. V B GAIKWAD# and G H JAIN. ∗. Materials Research Laboratory, Arts, Commerce and Science College, Nandgaon 423 106, ...

  10. Synthesis and characterization of 2-substituted bornane pharmacophores for novel cannabinergic ligands

    OpenAIRE

    Duclos, Richard I.; Lu, Dai; Guo, Jianxin; Makriyannis, Alexandros

    2008-01-01

    Analogously to the fenchyl and adamantyl groups, the bornyl and epimeric isobornyl groups are compact lipophilic substituents that can be incorporated into drug design to improve pharmacological or physicochemical properties. Methods are reported for the synthesis and characterization of 2-substituted norbornanes and bornanes that can serve as novel cannabinergic ligand intermediates.

  11. Synthesis and characterization of 2-substituted bornane pharmacophores for novel cannabinergic ligands.

    Science.gov (United States)

    Duclos, Richard I; Lu, Dai; Guo, Jianxin; Makriyannis, Alexandros

    2008-09-22

    Analogously to the fenchyl and adamantyl groups, the bornyl and epimeric isobornyl groups are compact lipophilic substituents that can be incorporated into drug design to improve pharmacological or physicochemical properties. Methods are reported for the synthesis and characterization of 2-substituted norbornanes and bornanes that can serve as novel cannabinergic ligand intermediates.

  12. Facile synthesis and characterization of rough surface V2O5 ...

    Indian Academy of Sciences (India)

    Home; Journals; Bulletin of Materials Science; Volume 40; Issue 6. Facile synthesis and characterization of rough surface V 2 O 5 nanomaterials for pseudo-supercapacitor electrode material with high capacitance. YIFU ZHANG YUTING HUANG. Volume 40 Issue 6 October 2017 pp 1137-1149 ...

  13. Synthesis and characterization of MoO3–WO3 composite thin films ...

    Indian Academy of Sciences (India)

    Home; Journals; Bulletin of Materials Science; Volume 36; Issue 1. Synthesis and characterization of MoO3–WO3 composite thin films by liquid phase deposition technique: Investigation of its photochromic properties. H M Farveez Ahmed Noor Shahina Begum. Volume 36 Issue 1 February 2013 pp 45-49 ...

  14. Synthesis and Characterization of Multimetallic Fe(II) and Mn(II ...

    African Journals Online (AJOL)

    MBI

    Mustapha and Gani. 56. Synthesis and Characterization of Multimetallic Fe(II) and Mn(II) Using. N4O3 Potentially Heptadentate Ligand. Mustapha, A. and Gani, S. M.. Department of Chemistry, Federal University Dutse, PMB 7156, Jigawa State ... ligands and their complexes with nickel(II) and copper(II) has also been ...

  15. Design, synthesis, and characterization of novel fine-particle, unsupported catalysts for coal liquefaction

    Energy Technology Data Exchange (ETDEWEB)

    Klein, M.T.

    1991-12-30

    The purpose of this work is to investigate the kinetics-assisted design, synthesis and characterization of fme-pardcle, unsupported catalysts for coal liquefaction. The goal is to develop a fundamental understanding of coal catalysis and catalysts that will, in turn, allow for the specification of a novel optimal catalyst for coal liquefaction.

  16. Synthesis and Characterization of Mn 2+ and Fe 2+ Complexes of ...

    African Journals Online (AJOL)

    Tris-2-aminoethylamine was condensed with 5-bromosalicylaldehyde to yield the potentially heptadentate N4O3 ligand, the ligand synthesis was followed by complexation with metal ions (M= Fe2+, Mn2+). The complexes were characterized by infrared and UV visible, while their melting point, solubility and conductivity ...

  17. Design, synthesis and characterization of 1 H-pyridin-4-yl-3, 5 ...

    Indian Academy of Sciences (India)

    Home; Journals; Journal of Chemical Sciences; Volume 127; Issue 3. Design, synthesis and characterization of 1 H-pyridin-4-yl-3, 5-disubstituted indazoles and their anti-inflammatory and analgesic activity. Arava Veera Reddy Surendrareddy Gogireddy P K Dubey Madhava Reddy B Veeresh B. Regular Articles Volume ...

  18. Synthesis and Characterization of SPIO-loaded PEG-b-PS Micelles ...

    Indian Academy of Sciences (India)

    66

    Synthesis and Characterization of SPIO-loaded PEG-b-PS Micelles as Contrast Agent for Long-term Nanoparticle-based MRI phantom. Man Theerasilp1,2, Witaya Sungkarat3 and Norased Nasongkla1,2,*. 1Department of Biomedical Engineering, Faculty of Engineering, Mahidol University,. Puttamonthon Nakorn Pathom ...

  19. Synthesis and characterization of Znq2 and Znq2: CTAB particles for ...

    Indian Academy of Sciences (India)

    Home; Journals; Bulletin of Materials Science; Volume 40; Issue 6. Synthesis and characterization of Znq2 and Znq2:CTAB particles for optical applications ... The crystallinenature of title samples was confirmed by powder X-ray diffraction. Thermo gravimetric analysis and differential thermal analysis were carried out to find ...

  20. Oxidative synthesis of a novel polyphenol having pendant Schiff base group: Synthesis, characterization, non-isothermal decomposition kinetics

    Energy Technology Data Exchange (ETDEWEB)

    Dilek, Deniz [Faculty of Education, Secondary Science and Mathematics Education, Canakkale Onsekiz Mart University, 17100 Canakkale (Turkey); Dogan, Fatih, E-mail: fatihdogan@comu.edu.tr [Faculty of Education, Secondary Science and Mathematics Education, Canakkale Onsekiz Mart University, 17100 Canakkale (Turkey); Bilici, Ali, E-mail: alibilici66@hotmail.com [Control Laboratory of Agricultural and Forestry Ministry, 34153 Istanbul (Turkey); Kaya, Ismet [Department of Chemistry, Faculty of Science and Arts, Canakkale Onsekiz Mart University, Canakkale (Turkey)

    2011-05-10

    Research highlights: {yields} In this study, the synthesis and thermal characterization of a new functional polyphenol are reported. {yields} Non-isothermal methods were used to evaluate the thermal decomposition kinetics of resulting polymer. {yields} Thermal decomposition of polymer follows a diffusion type kinetic model. {yields} It is noted that this kinetic model is quite rare in polymer degradation studies. - Abstract: In here, the facile synthesis and thermal characterization of a novel polyphenol containing Schiff base pendant group, poly(4-{l_brace}[(4-hydroxyphenyl)imino]methyl{r_brace}benzene-1,2,3-triol) [PHPIMB], are reported. UV-vis, FT-IR, {sup 1}H NMR, {sup 13}C NMR, GPC, TG/DTG-DTA, CV (cyclic voltammetry) and solid state conductivity measurements were utilized to characterize the obtained monomer and polymer. The spectral analyses results showed that PHPIMB was composed of polyphenol main chains containing Schiff base pendant side groups. Thermal properties of the polymer were investigated by thermogravimetric analyses under a nitrogen atmosphere. Five methods were used to study the thermal decomposition of PHPIMB at different heating rate and the results obtained by using all the kinetic methods were compared with each other. The thermal decomposition of PHPIMB was found to be a simple process composed of three stages. These investigated methods were those of Flynn-Wall-Ozawa (FWO), Tang, Kissinger-Akahira-Sunose (KAS), Friedman and Kissinger methods.

  1. Chemical Synthesis and Electrochemical Characterization of Nanoporous Gold films

    DEFF Research Database (Denmark)

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

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

  2. 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.

  3. Synthesis and characterization of one-dimensional titanate structure

    Directory of Open Access Journals (Sweden)

    Ljubica M. Nikolić

    2008-12-01

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

  4. Synthesis and characterization of spherical Tb-MCM-41

    Energy Technology Data Exchange (ETDEWEB)

    Pires, Luiza H.O., E-mail: lulenapires@hotmail.co [Universidade Federal do Para, Instituto de Ciencias Exatas e Naturais, Laboratorio de Catalise e Oleoquimica, CP 479, CEP 66075-110, Belem, PA (Brazil); Queiroz, Renan M.; Souza, Ruth P.; Costa, Carlos E.F. da; Zamian, Jose R. [Universidade Federal do Para, Instituto de Ciencias Exatas e Naturais, Laboratorio de Catalise e Oleoquimica, CP 479, CEP 66075-110, Belem, PA (Brazil); Weber, Ingrid T. [Universidade Federal de Pernambuco, Centro de Ciencias Exatas e da Natureza, Av. Prof. Luis Barros Freire, s/n, Cidade Universitaria, 50670-901 Recife, PE (Brazil); Filho, Geraldo N. da Rocha [Universidade Federal do Para, Instituto de Ciencias Exatas e Naturais, Laboratorio de Catalise e Oleoquimica, CP 479, CEP 66075-110, Belem, PA (Brazil)

    2010-02-04

    Spherical MCM-41 was synthesized at room temperature and functionalized by means of direct synthesis method. Evidence for the terbium presence in the silica matrix was obtained by means of EDX. Scanning electron microscopy (SEM) micrographs showed that terbium incorporation did not change significantly MCM-41 morphology. The maintenance of the hexagonal structure was confirmed by X-ray diffraction (XRD) pattern analysis. The cell parameter increase and the surface area decrease, observed by N{sub 2} adsorption-desorption technique, were taken as evidence of terbium introduction inside the MCM-41 framework. By FT-IR spectra it was found that the main features of the silica framework were maintained. The presence of a strong absorption band centered at ca. 220 nm in the diffuse reflectance UV-vis spectra could indicate the presence of tetra-coordinated terbium in the silica network of Tb-MCM-41 samples.

  5. Cobalt-based Magnetic Nanoparticles: Design, Synthesis and Characterization

    Science.gov (United States)

    Zamanpour, Mehdi

    The ever-increasing desire for more energy attainable from a smaller volume of matter has driven researchers to explore advanced materials at the molecular or even atomic size scale. Magnetic materials at the nanometer size scale have been the subject of enormous research effort worldwide for more than half a century. Different magnetic nanoparticles have shown different behavior in the absence and presence of an external magnetic field, which has led them to be categorized as soft (easy to demagnetize) or hard (resistive against demagnetization) magnets. Applications range from medical and biomedical devices to magnetic recording media and magnetic sensing have emphasized the importance of this class of materials. Soft magnetic phases have found application in power generation and magnetic targeted drug delivery, while hard magnets have been subject of extensive research for application as energy storage media. Discovery of the exchange-coupling phenomenon between the spins of two adjacent hard and soft magnetic phases which means taking advantage of both high magnetic moment of the soft phase as well as high coercivity of the hard phase has attracted scientists to develop advanced materials for energy storage with no usage of fossil fuels: clean energy. In this Dissertation, synthesis of pure phase, soft FeCo nanoparticles with high magnetic moment and hard phase CoxC nanoparticles possessing high coercivity is reported. The polyol method (chemical co-precipitating at polyhydric alcohol as reducing agent) is used to make FeCo and Co xC nanoparticles and the effects of important reaction kinetics parameters on the structure and magnetic properties of the products are studied. Careful analysis of correlations between these parameters and the properties of the magnetic particles has made synthesis of FeCo and CoxC nanoparticles with desired properties possible. Fabrication of MnAlC-FeCo heterostructures as a rare earth-free alternative for high-performance permanent

  6. Green Synthesis, Characterization and Uses of Palladium/Platinum Nanoparticles

    Science.gov (United States)

    Siddiqi, Khwaja Salahuddin; Husen, Azamal

    2016-11-01

    Biogenic synthesis of palladium (Pd) and platinum (Pt) nanoparticles from plants and microbes has captured the attention of many researchers because it is economical, sustainable and eco-friendly. Plant and their parts are known to have various kinds of primary and secondary metabolites which reduce the metal salts to metal nanoparticles. Shape, size and stability of Pd and Pt nanoparticles are influenced by pH, temperature, incubation time and concentrations of plant extract and that of the metal salt. Pd and Pt nanoparticles are broadly used as catalyst, as drug, drug carrier and in cancer treatment. They have shown size- and shape-dependent specific and selective therapeutic properties. In this review, we have discussed the biogenic fabrication of Pd/Pt nanoparticles, their potential application as catalyst, medicine, biosensor, medical diagnostic and pharmaceuticals.

  7. Synthesis and Characterization of CDS Nanocrystals with Thermoresponsive Polymer

    Science.gov (United States)

    Alsaleh, Ahmad; Khan, Aslam; Ahamad, Tansir; Alam Khan, M.

    2010-04-01

    This paper reports the synthesis of thermoresponsive colloidal nanocomposites based on CdS and poly(N-isopropylacrylamide) (pNIPAAm). CdS nanocrystals are prepared at room temperature from cadmium chloride and sodium sulfide salts in presence of an organic ligand (3-mercaptopropionic acid) (MPA). As prepared, MPA bound CdS nanocrystals are stable over a month and show good optical properties. The effect of the different ratios of MPA/Cd2+ and H2O/DMF on the resulting particle size of CdS nanocrystals are investigated by UV-Vis absorption measurements. Transmission electron microscopy shows that the particle sizes are about 4 nm, which is in close agreement with the size obtained by UV-Vis spectroscopy.

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

    OpenAIRE

    Franus, Wojciech; Wdowin, Magdalena; Franus, Małgorzata

    2014-01-01

    In this paper, we present the possibility of using fly ash to produce synthetic zeolites. The synthesis class F fly ash from the Stalowa Wola SA heat and power plant was subjected to 24 h hydrothermal reaction with sodium hydroxide. Depending on the reaction conditions, three types of synthetic zeolites were formed: Na-X (20 g fly ash, 0.5 dm3 of 3 mol · dm−3 NaOH, 75 °C), Na-P1 (20 g fly ash, 0.5 dm3 of 3 mol · dm−3 NaOH, 95 °C), and sodalite (20 g fly ash, 0.8 dm3 of 5 mol · dm−3 NaOH + 0.4...

  9. Synthesis and characterization of a nanocrystalline diamond aerogel.

    Science.gov (United States)

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

    2011-05-24

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

  10. Carbon quantum dots: synthesis, characterization, and assessment of cytocompatibility.

    Science.gov (United States)

    Zhang, Zhengwei; Duan, Yu; Yu, Yan; Yan, Zhengyu; Chen, Jianqiu

    2015-07-01

    A simple method for the synthesis of water-soluble carbon quantum dots (CQDs) has been developed by chemical oxidation treatment of the flour. The as-synthesized CQDs were monodispersed sphere particles with the approximate diameter of 5-8 nm, and exhibited strong fluorescence, excitation-dependent photoluminescence behavior and high photostability in a wide range of pH values. We investigated the cytotoxicity of as-prepared CQDs using rat mesangial cells (RMC). Compared with CdTe quantum dots, CQDs show no apparent cytotoxicity and much better biosafety property. The as-synthesized CQDs were also tested to label and image RMC in vitro and demonstrated to be highly promising biological fluorescent probes.

  11. 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.

  12. Stop Flow Lithography Synthesis and Characterization of Structured Microparticles

    Directory of Open Access Journals (Sweden)

    David Baah

    2014-01-01

    Full Text Available In this study, the synthesis of nonspherical composite particles of poly(ethylene glycol diacrylate (PEG-DA/SiO2 and PEG-DA/Al2O3 with single or multiple vias and the corresponding inorganic particles of SiO2 and Al2O3 synthesized using the Stop Flow Lithography (SFL method is reported. Precursor suspensions of PEG-DA, 2-hydroxy-2-methylpropiophenone, and SiO2 or Al2O3 nanoparticles were prepared. The precursor suspension flows through a microfluidic device mounted on an upright microscope and is polymerized in an automated process. A patterned photomask with transparent geometric features masks UV light to synthesize the particles. Composite particles with vias were synthesized and corresponding inorganic SiO2 and Al2O3 particles were obtained through polymer burn-off and sintering of the composites. The synthesis of porous inorganic particles of SiO2 and Al2O3 with vias and overall dimensions in the range of ~35–90 µm was achieved. BET specific surface area measurements for single via inorganic particles were 56–69 m2/g for SiO2 particles and 73–81 m2/g for Al2O3 particles. Surface areas as high as 114 m2/g were measured for multivia cubic SiO2 particles. The findings suggest that, with optimization, the particles should have applications in areas where high surface area is important such as catalysis and sieving.

  13. Hydrothermal synthesis and characterization of the semiconductor material Cu2ZnTiS4

    Science.gov (United States)

    Pérez Bustos, H. G.; Patarroyo-Mesa, M.; Gómez-Cuaspud, J. A.; Pineda-Triana, Y.; Vera-López, E.

    2017-12-01

    This paper describes the results of the synthesis and characterization of a quaternary semiconductor based on Cu2ZnTiS4 (abbreviated CZTiS), using a hydrothermal technique. The results confirm that time (24, 48 and 72 hours) and temperature (250, 275, and 300°C) factors, used in synthesis process, regulate different levels of electrical conductivity in these materials. The results of ultraviolet spectroscopy (UV) analysis, confirm the production of semiconductor solids with Band-gap values around 1.4eV, being coherent with a strong absorption in the ultraviolet region. The X-Ray Diffraction analysis (XRD), confirm that there is an opposite and proportional relationship between the crystal sizes, the reaction times and the synthesis temperature. In all cases, the particle sizes were 50-100nm. The results derived from Scanning Electron Microscopy (SEM), confirm the obtaining of homogenous materials with optimal morphological properties in accordance with synthesis method. Similarly, the composition values derived from the Energy-Dispersion X-ray Spectroscopy analysis (EDS), shown that obtained compositions are in agree with expected values. Finally, the results of electric characterization, confirm that used synthesis parameters show a strong dependence on the conductive behaviour of solids being the most relevant result the shown by the solid obtained at 300°C and 72 hours of reaction in accordance with preliminary works.

  14. Cobalt(II complexes with aromatic carboxylates and N-functionalized cyclam bearing 2-pyridylmethyl pendant arms

    Directory of Open Access Journals (Sweden)

    G. VUCKOVIC

    2005-09-01

    Full Text Available Novel binuclear Co(II complexeswithN-functionalized cyclam, N,N’,N”,N’’’-tetrakis(2-pyridylmethyltetraazacyclotetradecane (tpmc and one of the aromatic monoor dicarboxylato ligands (benzoate, phthalate or isophthalate ions were prepared. They were analyzed and studied by elemental analyses (C, H, N, electrical conductivities, VIS and IR spectroscopy andmagnetic as well as cyclic voltammetric measurements. In [Co2(C6H5COO2tpmc](ClO42.3H2O, the benzoate ligands are most probably coordinated as chelates in the trans-position to each Co(II and the macrocycle adopts a chair conformation. In the complexes [Co2(Ytpmc](ClO42·zH2O, (Y = phthalate or i-phthalate dianizon, z = 2; 4, it is proposed that the isomeric dicarboxylates are bonded combined as bridges and chelates. The composition and the assumed geometries of the complexes are compared with the, earlier reported, corresponding Cu(II complexes. Cyclic voltammetry measurements showed that the compounds are electrochemically stable.

  15. Green synthesis, characterization and antibacterial activity of copper ...

    African Journals Online (AJOL)

    The optical properties of the synthesized Cu nanoparticles were characterized by UV-Vis Spectroscopy while the crystallinity of synthesized Cu nanoparticles was verified with the help of X-ray diffraction analysis. The antimicrobial activity of Cu nanoparticles was determined by Agar disc diffusion method against some ...

  16. Synthesis, Characterization and DNA Cleavage of Copper(II ...

    African Journals Online (AJOL)

    characterization and DNA interactions of copper (II) and nickel (II) complexes with unsymmetrical Schiff base ligands. Indian J Chem 2013; 52A: 845-853. 23. Neves A, Bortoluzzi AJ, Jovito R, Peralta RA, Souza BD,. Szpoganicz B, Joussef AC, Terenzi H, Severino PC,. Fischer FL, Schenk G, Riley MJ, Smith SJ, Gahan LR.

  17. Synthesis, characterization and electrical properties of visible-light ...

    Indian Academy of Sciences (India)

    The synthesized nanocomposite material was characterized by standard analytical techniques like X-ray diffraction (XRD), UV–vis spectroscopy, scanning electron microscopy, transmission electron microscopy and energy-dispersive spectroscopy. The XRD analysis confirms two things; first, synthesized nanocomposite ...

  18. Synthesis, characterization and evaluation of biological activities of ...

    African Journals Online (AJOL)

    Purpose: To synthesize, characterize and investigate the antimicrobial properties of pure and manganese-doped zinc oxide nanoparticles. Method: Un-doped and manganese-doped zinc oxide (Mn-doped ZnO) nanoparticles were prepared using co-precipitation method. The synthesized Mn-doped ZnO nanoparticles were ...

  19. synthesis and characterization of new optically active poly(amide ...

    African Journals Online (AJOL)

    Preferred Customer

    dL/g. The resulting polymers were fully characterized by means of FTIR spectroscopy, elemental analyses, inherent viscosity, and solubility tests. Thermal properties of these polymers were investigated by thermal gravimetric analysis (TGA) and differential thermal gravimetric (DTG). All of the polymers were readily soluble.

  20. Synthesis, characterization and oxide ionic conductivity of β-type ...

    Indian Academy of Sciences (India)

    With the help of XRD, crystal systems and lattice parameters of the solid solutions were obtained and their characterization was carried out. Thermal measurements were made by using a simultaneous DTA/TG system. The total conductivity (T) in the -Bi2O3 doped with Yb2O3 system was measured using four-probe d.c. ...

  1. Synthesis, spectral characterization and redox properties of iron (II ...

    Indian Academy of Sciences (India)

    R', R = H (a), Me (b), Cl (c) and R' = Me (1/3), Et (2/4) have been synthesized and formulated as tris-chelates Fe(RaaiR') 3 2 + . They are characterized by microanalytical, conductance, UV-Vis, IR, magnetic (polycrystalline state) data.

  2. Synthesis and characterization of bimetallic nanocatalysts and their ...

    Indian Academy of Sciences (India)

    TiO2-supported bimetallic nanocatalysts were prepared and reduced at two different temperatures, 375°C and 575°C for selective hydrogenation of citral to corresponding unsaturated alcohols (geraniol (GOL) and nerol (NOL)). The nanocatalysts were characterized by difference techniques of Fourier transform infrared ...

  3. An efficient synthesis, X-ray and spectral characterization of ...

    Indian Academy of Sciences (India)

    Non-insulin-dependent diabetes mellitus (NIDDM) is a metabolic disorder characterized by hyperglycemia as well as insulin resistance and/or impaired insulin secretion.1,2 Therapy for NIDDM has been aimed at improving glycemic control by a combination of diet, exercise, and oral agents.3 These oral agents stimulate.

  4. Synthesis and characterization of super-microporous material with ...

    Indian Academy of Sciences (India)

    Super-microporouos silicon material with high hydrothermal stability denoted as MCM-41-T has been prepared from mesoporous MCM-41 by high temperature treatment. The structural and chemical property of MCM-41-T has been characterized by X-ray diffraction, transmission electron microscopy, N2 ...

  5. Synthesis and characterization of water-soluble carbon nanotubes ...

    Indian Academy of Sciences (India)

    Carbon nanotubes (CNT) has been synthesized by pyrolysing mustard oil using an oil lamp. It was made water-soluble (wsCNT) through oxidative treatment by dilute nitric acid and was characterized by SEM, AFM, XRD, Raman and FTIR spectroscopy. The synthesized wsCNT showed the presence of several junctions and ...

  6. Synthesis and Characterization of Some Mono Chloro-S- Triazine ...

    African Journals Online (AJOL)

    A series of ten bifunctional mono-chloro-s-triazine vinyl sulphone reactive dyes were synthesized based on Hacid with varied substituents coded as (BRD). These dyes were characterized by IR spectroscopy. The results revealed an incorporation of various substituents. The visible absorption spectra of these dyes were ...

  7. Synthesis and spectra characterization of mixed ligand complexes ...

    African Journals Online (AJOL)

    The synthesized ligand and its metal complexes have been characterized by elemental analysis and spectroscopic (i.r. and electronic) methods. An octahedral geometric structure is proposed for the metal complexes. The six coordinate environment of the metals is composed of N5X core with thr ee nitrogen atoms from the ...

  8. Synthesis, characterization, electrical and catalytic studies of some ...

    African Journals Online (AJOL)

    hydroxyacetophenone, 2-hydroxy-5-methyl-3-nitro acetophenone and carbohydrazide and its complexes with VO(IV), Cr(III), Mn(III), Fe(III), MoO2(VI), WO2(VI), Zr(IV) and UO2(VI) have been prepared. They were characterized by elemental analysis, ...

  9. Synthesis, characterization and low frequency ac conduction of ...

    Indian Academy of Sciences (India)

    in situ polymerization of aniline was carried out in the presence of fly ash (FA) to synthesize polyaniline/fly ash (PANI/FA) composites. The PANI/FA composites have been synthesized with various compositions (15, 20, 30 and 40 wt%) of FA in PANI. The composites, thus synthesized have been characterized by infrared ...

  10. Synthesis and characterization of a chiral dimeric copper (II ...

    Indian Academy of Sciences (India)

    Compound 1 crystallizes in the orthorhombic chiral P212121 space group with = 4, = 10.21(2), = 11.574(3), = 25.364(9). Each copper shows square pyramidal geometry with O2NCl2 coordination and the Cu2Cl2 core geometry adopts a butterfly shape. Crystals of 1 were further characterized by elemental analysis, ...

  11. Synthesis, characterization and antibacterial screening of 2,4 ...

    African Journals Online (AJOL)

    seafood

    2012-05-15

    May 15, 2012 ... 1Department of Chemistry, University of Fort Hare, Alice 5700, South Africa. 2Department of ... characterized by elemental analysis, Fourier transform infrared (FTIR) and ultraviolet visible (UV-Vis) spectroscopy, and ..... Nickel(II) complexes of 2-hydrazino-4,6-dimethyl pyrimidine, J. Inorg. Nucleic Chem.

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

    Indian Academy of Sciences (India)

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

  13. Synthesis and characterization of two novel trinuclear oxo-centered ...

    African Journals Online (AJOL)

    Two novel oxo-centered trinuclear compounds, [M2M'O(C3H3O2)6(H2O)3]+ (M = Cr, M' = Cr, Fe) have been synthesized. The complexes were characterized by elemental analysis, infrared and electronic spectroscopy and thermogravimetric analysis (TGA). These complexes contain unsaturated carboxylate bridging ...

  14. Synthesis and characterization of a Schiff base Cobalt (III) complex ...

    African Journals Online (AJOL)

    Cobalt (III) tris(azido)-2-Morpholino-N-(1-(2-pyridyl)ethylidene)ethanamine complex was synthesized, characterized and evaluated for in vitro anticancer activities. The chemical structure of the compound was assessed by elemental analysis, single crystal x-ray crystallography, FT-IR and UV-Visible spectroscopy.

  15. Synthesis and characterization of poly (2, 5-dimethoxyaniline) and ...

    Indian Academy of Sciences (India)

    ... which exhibit remarkably improved solubility in common organic solvents, were obtained by chemical polymerization, and characterized by a host of physical techniques. The lowering of the quinoid absorption in the IR spectra and the upshifting of the 1s envelope in the XPS spectra indicate residual doping in the XPS ...

  16. Synthesis and characterization of bimetallic nanocatalysts and their ...

    Indian Academy of Sciences (India)

    The nanocatalysts were characterized by difference techniques of Fourier trans- form infrared spectroscopy (FT-IR), ... second metal (Ru) also leads to an increase in GOL and NOL selectivity during citral hydrogenation. Partially generated oxidized second ... hols are of considerable interest in the perfumery industry.13,14.

  17. Synthesis, characterization and ion recognition studies of lower rim ...

    Indian Academy of Sciences (India)

    An amido-linked rhodamine conjugate of calix[4]arene, L has been synthesized and characterized. Metal ion recognition properties of L have been studied by emission and absorption techniques with 14 different metal ions including the transition ones. Results show that, L exhibits ratiometric emission intensity towards ...

  18. Synthesis and Characterization of Metal Complexes with Schiff Base Ligands

    Science.gov (United States)

    Wilkinson, Shane M.; Sheedy, Timothy M.; New, Elizabeth J.

    2016-01-01

    In order for undergraduate laboratory experiments to reflect modern research practice, it is essential that they include a range of elements, and that synthetic tasks are accompanied by characterization and analysis. This intermediate general chemistry laboratory exercise runs over 2 weeks, and involves the preparation of a Schiff base ligand and…

  19. SYNTHESIS AND CHARACTERIZATION OF POLY[3-(2\\',5 ...

    African Journals Online (AJOL)

    Poly[3-(2\\',5\\'-diheptyloxyphenyl)thiophene], PDHOPT, has been prepared electrochemically from its monomer for solar cell application. PDHOPT exhibits a band gap of 2.1 eV. The redox properties of PDHOPT were characterized using cyclic voltammetry. The estimated energy levels of the highest occupied molecular ...

  20. Synthesis and characterization of water-soluble carbon nanotubes ...

    Indian Academy of Sciences (India)

    Abstract. Carbon nanotubes (CNT) has been synthesized by pyrolysing mustard oil using an oil lamp. It was made water-soluble (wsCNT) through oxidative treatment by dilute nitric acid and was characterized by SEM, AFM, XRD, Raman and FTIR spec- troscopy. The synthesized wsCNT showed the presence of several ...

  1. Synthesis and characterization of bio-based polyurethane from ...

    Indian Academy of Sciences (India)

    Benzoylated tannin prepared by benzoylation of cashewnut husk tannin, was treated with hexame-thylenediisocyanate in the presence of 1,4-butanediol as an extender to prepare thermosetting polyurethane. The sample was characterized using FT–IR and 13C NMR spectra. Thermal, morphological, physico-chemical and ...

  2. Synthesis, characterization and anti-inflammatory evaluation of ...

    African Journals Online (AJOL)

    In order to explore the novel anti-inflammatory agents, some novel Trolox derivatives were synthesized and characterized by IR, 1H-NMR, 13C-NMR, mass and elemental analysis. The anti-inflammatory activities of the target compounds were evaluated via the croton oil-induced ear oedema test in Swiss mice. According to ...

  3. Synthesis and characterization and antibacterial activity of some ...

    African Journals Online (AJOL)

    Some new transition metal complexes of ciprofloxacin-imine derived from ciprofloxacin and o-phenylenediamine were synthesized and characterized on the basis of melting point, magnetic moment, conductance measurements, elemental analysis, infrared, UV/Vis, nuclear magnetic resonance spectroscopy, mass spectra ...

  4. Synthesis and characterization of new thiourea and urea derivatives ...

    Indian Academy of Sciences (India)

    A new class of antimicrobial and antioxidant agents, based on thiourea and urea derivatives of 6-fluoro-3-(piperidin-4-yl)benzo[] isoxazole were synthesized by adopting a simple and efficient method. Synthesized compounds were characterized by spectral data of IR, 1H, 13C NMR and mass spectra. The compounds ...

  5. SYNTHESIS, CHARACTERIZATION AND BIO-ACTIVITY OF SOME ...

    African Journals Online (AJOL)

    Preferred Customer

    Erturk, O. Biologia 2006, 61, 275. 19. Devendranath Reddy, C.; Reddy, M.S.; Raju, C.N. Ind. J. Chem. 2000, 39B, 426. 20. Quin, L.D.; Verkade, J.G. Phosphorus-31 NMR Spectral Properties Compound. Characterization and Structural Analysis, VCH Publisher: New York; 1994. 21. Sankar, A.U.R.; Kumar, B.S.; Raju, C.N.; ...

  6. Synthesis, characterization, and bioavailability in rats of ferric phosphate nanoparticles

    NARCIS (Netherlands)

    Rohner, F.; Ernst, F.O.; Arnold, M.; Hilbe, M.; Biebinger, R.; Ehrensperger, F.; Pratsinis, S.E.; Langhans, W.; Hurrell, R.F.; Zimmermann, M.B.

    2007-01-01

    Particle size is a determinant of iron (Fe) absorption from poorly soluble Fe compounds. Decreasing the particle size of metallic Fe and ferric pyrophosphate added to foods increases Fe absorption. The aim of this study was to develop and characterize nanoparticles of FePO4 and determine their

  7. Synthesis, characterization and antibacterial activity of aspirin and ...

    African Journals Online (AJOL)

    Dr J. T. Ekanem

    Novel complexes of Co (11), Ni (11) and Fe (111) with aspirin and paracetamol have synthesized and characterized using infrared, electronic and Hnmr spectral, melting point and conductivity measurements. The two ligands have been found to act as bidentate chelating agents. Aspirin complexes coordinate through the ...

  8. Synthesis, characterization and catalytic activity of sulphonated multi ...

    Indian Academy of Sciences (India)

    MWCNTs-SO3H was prepared and characterized by some microscopic and spectroscopic techniques including scanning electron microscopy, transmission electron microscopy, FT-IR spectroscopy and Raman spectroscopy. Acidity of the catalyst was measured by acid-base titration. The catalyst was reused several times ...

  9. Synthesis and nonlinear optical characterization of new 1, 3, 4 ...

    Indian Academy of Sciences (India)

    A new series of 1,3,4-oxadiazole derivatives containing 2-fluoro-4-methoxy phenyl were synthesized by refluxing mixture of acid hydrazide 3 with different aromatic carboxylic acids (a–e) in phosphorous oxychloride. These newly synthesized compounds were characterized by NMR, mass spectral, and IR spectral studies, ...

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

    Indian Academy of Sciences (India)

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

  11. Synthesis and characterization of dihexyldithiocarbamate as a chelating agent in extraction of gold(III)

    Energy Technology Data Exchange (ETDEWEB)

    Fatimah, Soja Siti, E-mail: soja-sf@upi.edu [Departemen Pendidikan Kimia, Universitas Pendidikan Indonesia, Jl. Dr. Setiabudhi No. 229, Bandung 40154 (Indonesia); Department of Chemistry, Faculty of Mathematics and Natural Sciences, Padjadjaran University, Jl. Raya Bandung-Sumedang, Km. 21, Jatinangor (Indonesia); Bahti, Husein H.; Hastiawan, Iwan [Department of Chemistry, Faculty of Mathematics and Natural Sciences, Padjadjaran University, Jl. Raya Bandung-Sumedang, Km. 21, Jatinangor (Indonesia); Permanasari, Anna [Departemen Pendidikan Kimia, Universitas Pendidikan Indonesia, Jl. Dr. Setiabudhi No. 229, Bandung 40154 (Indonesia)

    2016-02-08

    The use of dialkyldithiocarbamates as chelating agents of transition metals have been developing for decades. Many chelating agents have been synthesized and used in the extraction of the metals. Studies on particular aspects of extraction of the metals, such as the effect of increasing hydrophobicity of chelating agents on the effectiveness of the extraction, have been done. However, despite the many studies on the synthesis and applications of this type of chelating agents, interests in the aspect of molecular structure of the synthesized ligands and of their complexes, have been limited. This study aimed at synthesizing and characterizing dihexylthiocarbamate, and using the ligand for the extraction of gold III). Characterization of the ligand and of its metal complex were done by using elemental analysis, DTG, and spectroscopic methods to include NMR, ({sup 1}H, and {sup 13}C), FTIR, and MS-ESI. Data on the synthesis, characterization, and the application of the ligand as a chelating agent are presented.

  12. Synthesis and characterization of boehmites obtained from gibbsite in presence of different environments

    Energy Technology Data Exchange (ETDEWEB)

    Denigres Filho, Ricardo Wilson Nastari; Rocha, Gisele de Araujo; Vieira-Coelho, Antonio Carlos, E-mail: acvcoelh@usp.br [Universidade de Sao Paulo (LPSS/EP/USP), SP (Brazil). Departamento de Engenharia Metalurgica e de Materiais. Laboratorio de Materias-Primas Particuladas; Montes, Celia Regina [Centro de Energia Nuclear na Agricultura (NUPEGEL/CENA/USP), Piracicaba, SP (Brazil). Nucleo de Pesquisas Geoquimicas e Geofisicas da Listosfera

    2016-05-15

    In this study, results related to boehmite synthesis by hydrothermal processes starting from a Bayer commercial gibbsite are reported. The processes have been conducted from aqueous suspensions with initial acidic or alkaline pH, without or with acetate ion, at 160 deg C for 72h to 168h. The final materials were characterized by X-ray diffraction (XRD), thermal methods (DTA and TGA) and scanning electron microscopy (SEM). The influence of the synthesis conditions on the morphology of the boehmite crystals obtained from the gibbsite at different hydrothermal processes are discussed. (author)

  13. Synthesis, Characterization and Properties of Nanoparticles of Intermetallic Compounds

    Energy Technology Data Exchange (ETDEWEB)

    DiSalvo, Francis J. [Cornell Univ., Ithaca, NY (United States)

    2015-03-12

    The research program from 2010 to the end of the grant focused on understanding the factors important to the synthesis of single phase intermetallic nano-particles (NPs), their size, crystalline order, surface properties and electrochemical activity. The synthetic method developed is a co-reduction of mixtures of single metal precursors by strong, soluble reducing agents in a non-protic solvent, tetrahydrofuran (THF). With some exceptions, the particles obtained by room temperature reduction are random alloys that need to be annealed at modest temperatures (200 to 600 °C) in order to develop an ordered structure. To avoid significant particle size growth and agglomeration, the particles must be protected by surface coatings. We developed a novel method of coating the metal nanoparticles with KCl, a by-product of the reduction reaction if the proper reducing agents are employed. In that case, a composite product containing individual metal nanoparticles in a KCl matrix is obtained. The composite can be heated to at least 600 °C without significant agglomeration or growth in particle size. Washing the annealed product in the presence of catalyst supports in ethylene glycol removes the KCl and deposits the particles on the support. Six publications present the method and its application to producing and studying new catalyst/support combinations for fuel cell applications. Three publications concern the use of related methods to explore new lithium-sulfur battery concepts.

  14. Synthesis and characterization of several molybdenum chloride cluster compounds

    Energy Technology Data Exchange (ETDEWEB)

    Beers, W.W.

    1983-06-01

    Investigation into the direct synthesis of Mo/sub 4/Cl/sub 8/(P(C/sub 2/H/sub 5/)/sub 3/)/sub 4/ from Mo/sub 2/(OAc)/sub 4/ led to a synthetic procedure that produces yields greater than 80%. The single-crystal structure disclosed a planar rectangular cluster of molybdenum atoms. Metal-metal bond distances suggest that the long edges of the rectangular cluster should be considered to be single bonds and the short metal-metal bonds to be triple bonds. This view is reinforced by an extended Hueckel calculation. Attempts to add a metal atom to Mo/sub 4/Cl/sub 8/(PR/sub 3/)/sub 4/ to form Mo/sub 5/Cl/sub 10/(PR/sub 3/)/sub 3/ led instead to a compound with the composition Mo/sub 8/Cl/sub 16/(PR/sub 3/)/sub 4/. Solution and reflectance uv-visible spectra and x-ray photoelectron spectra suggest that tetranuclear molybdenum units are present. The facile reaction between Mo/sub 8/Cl/sub 16/(PR/sub 3/)/sub 4/ and PR/sub 3/ imply that the linkage between tetrameric units is weak.

  15. Synthesis and characterization of solid solutions in ABCO 4 system

    Science.gov (United States)

    Novoselov, A.; Zimina, G.; Komissarova, L.; Pajaczkowska, A.

    2006-01-01

    Formation of continuous solid solutions with a tetragonal structure of K 2NiF 4-type was investigated by direct solid-state synthesis, carbonate precipitations, the freeze-drying method and the Czochralski crystal growth technique. In the systems of SrLaAlO 4-CaLaAlO 4, SrNdAlO 4-CaNdAlO 4, SrPrAlO 4-CaPrAlO 4, SrLaAlO 4-SrLaGaO 4 and SrLaAlO 4-SrLaFeO 4 solid solutions are formed in the whole concentration range (0.0⩽ x⩽1.0) and in the systems of SrLaAlO 4-SrLaMnO 4 and SrLaAlO 4-SrLaCrO 4 in the limited compositional interval of (0.0⩽ x⩽0.20) and (0.0⩽ x⩽0.25), respectively, with composition dependency of lattice constants following Vegard's law.

  16. Synthesis, Characterization and Thermal Diffusivity of Holmium and Praseodymium Zirconates

    Directory of Open Access Journals (Sweden)

    Stopyra M.

    2016-06-01

    Full Text Available A2B2O7 oxides with pyrochlore or defected fluorite structure are among the most promising candidates for insulation layer material in thermal barrier coatings. The present paper presents the procedure of synthesis of holmium zirconate Ho2Zr2O7 and praseodymium zirconate Pr2Zr2O7 via Polymerized-Complex Method (PCM. Thermal analysis of precursor revealed that after calcination at relatively low temperature (700°C fine-crystalline, single-phase material is obtained. Thermal diffusivity was measured in temperature range 25-200°C, Ho2Zr2O7 exhibits lower thermal diffusivity than Pr2Zr2O7. Additionally, PrHoZr2O7 was synthesized. The powder in as-calcined condition is single-phase, but during the sintering decomposition of solid solution took place and Ho-rich phase precipitated. This material exhibited the best insulating properties among the tested ones.

  17. Green synthesis of silver nanoparticles and their characterization by XRD

    Science.gov (United States)

    Mehta, B. K.; Chhajlani, Meenal; Shrivastava, B. D.

    2017-05-01

    A cost effective and environment friendly technique for green synthesis of silver nanoparticles has been reported. Silver nanoparticles have been synthesized using ethanol extract of fruits of Santalum album (Family Santalaceae), commonly known as East Indian sandalwood. Fruits of S.album were collected and crushed. Ethanol was added to the crushed fruits and mixture was exposed to microwave for few minutes. Extract was concentrated by Buchi rotavaporator. To this extract, 1mM aqueous solution of silver nitrate (AgNO3) was added. After about 24 hr incubation Ag+ ions in AgNO3 solution were reduced to Ag atoms by the extract. Silver nanoparticles were obtained in powder form. X-ray diffraction (XRD) pattern of the prepared sample of silver nanoparticles was recorded The diffractogram has been compared with the standard powder diffraction card of JCPDS silver file. Four peaks have been identified corresponding to (hkl) values of silver. The XRD study confirms that the resultant particles are silver nanoparticles having FCC structure. The average crystalline size D, the value of the interplanar spacing between the atoms, d, lattice constant and cell volume have been estimated. Thus, silver nanoparticles with well-defined dimensions could be synthesized by reduction of metal ions due to fruit extract of S.album.

  18. Synthesis and morphological characterization of block copolymers for improved biomaterials

    Energy Technology Data Exchange (ETDEWEB)

    Schricker, Scott, E-mail: Schricker.1@osu.edu [Restorative and Prosthetic Dentistry Section, College of Dentistry, The Ohio State University, Columbus, OH 43210 (United States); Palacio, Manuel [Nanoprobe Laboratory for Bio- and Nanotechnology and Biomimetics, The Ohio State University, Columbus, OH 43210 (United States); Thirumamagal, B.T.S. [Restorative and Prosthetic Dentistry Section, College of Dentistry, The Ohio State University, Columbus, OH 43210 (United States); Bhushan, Bharat [Nanoprobe Laboratory for Bio- and Nanotechnology and Biomimetics, The Ohio State University, Columbus, OH 43210 (United States)

    2010-05-15

    Biocompatible polymers are known to act as scaffolds for the regeneration and growth of bone. Block copolymers are of interest as scaffold materials because a number of the blocks are biocompatible, and their nanostructure is easily tunable with synthetic techniques. In this paper, we report the synthesis of a novel class of biomaterials from block copolymers containing a hydrophobic block of methyl methacrylate and a hydrophilic block of either acrylic acid, dimethyl acrylamide, or 2-hydroxyethyl methacrylate. The block copolymers were synthesized using a combination of reversible addition-fragmentation chain transfer (RAFT) polymerization and click chemistry. Since the surface morphology is critical for successful cell growth, atomic force microscopy (AFM) studies were conducted for selected block copolymers. The topography, phase angle and friction maps were obtained in dry and physiological buffer environments to study the morphology. Results of AFM imaging identified the presence of polymer domains corresponding to the copolymer components. The distribution of nanoscale features in these block copolymers is comparable to those found on other surfaces that exhibit favorable cell adhesion and growth. In physiological buffer medium, the hydrophilic component of the block copolymer (acrylic acid or hydroxyethyl methacrylate) appears to be present in greater amounts on the surface as a consequence of water absorption and swelling.

  19. Synthesis and characterization of polyaniline as emeraldine salt

    Energy Technology Data Exchange (ETDEWEB)

    Gawri, Isha; Khatta, Swati; Singh, K. P.; Tripathi, S. K., E-mail: surya@pu.ac.in, E-mail: surya-tr@yahoo.com [Department of Physics, Center of Advanced Study in Physics, Panjab University, Chandigarh-160 014 (India)

    2016-05-06

    Polyaniline in emeraldine salt (PANI-ES) form was successfully synthesized by oxidative polymerization of aniline using ammonium peroxidisulphate as oxidant in the presence of hydrochloric acid as catalyst under ice bath condition. The as prepared powdered sample was characterized using X-Ray Diffraction (XRD) and Fourier Transform Infrared (FTIR) spectroscopy. Using XRD, the average crystalline size was found to be 5.63 nm and d-spacing corresponding to crystalline peak 2θ = 25.08° had come out to be 4.2 Å. Also FTIR absorption spectra showed all the characteristics bands of PANI –ES. The ohmic contact between the PANI-ES film and the substrate was confirmed by Current-Voltage (I-V) characterization.

  20. Second harmonic chalcone crystal: Synthesis, growth and characterization

    Energy Technology Data Exchange (ETDEWEB)

    D' Silva, E.D., E-mail: deepak.dsilva@gmail.co [Department of studies in Physics, Mangalore University, Mangalagangotri, Mangalore 574199 (India); Narayan Rao, D. [School of Physics, University of Hyderabad, Hyderabad 500046 (India); Philip, Reji [Light and Matter Physics Group, Raman Research Institute, Bangalore 560080 (India); Butcher, Ray J. [Department of Chemistry, Howard University, Washington, DC 20059 (United States); Rajnikant [Department of Physics and Electronics, University of Jammu, Jammu Tawi 180006 (India); Dharmaprakash, S.M. [Department of studies in Physics, Mangalore University, Mangalagangotri, Mangalore 574199 (India)

    2011-05-15

    The novel nonlinear optical chalcone derivative (2E)-3-[4-(methylsulfanyl)phenyl]-1-(3-bromophenyl)prop-2-en-1-one (3Br4MSP) crystals have been grown by slow evaporation technique at ambient temperature. The crystal was subjected to different types of characterization method in order to study its possible application in nonlinear optics. The structure determination of the grown crystal was done by single crystal X-ray diffraction study. The morphology of the crystal is studied. The crystal was subjected to thermal analysis to find its thermal stability. The grown crystals were characterized for their optical transmission and mechanical hardness. The second harmonic generation (SHG) efficiency of the crystal is obtained by classical powdered technique. The laser damage threshold for 3Br4MSP crystal was determined using Q-switched Nd:YAG laser.

  1. Synthesis, characterization, and properties of reduced europium molybdates and tungstates

    Science.gov (United States)

    Abeysinghe, Dileka; Gerke, Birgit; Morrison, Gregory; Hsieh, Chun H.; Smith, Mark D.; Pöttgen, Rainer; Makris, Thomas M.; zur Loye, Hans-Conrad

    2015-09-01

    Single crystals of K0.094Eu0.906MoO4, K0.097Eu0.903WO4, EuWO4, and EuMoO4 were grown from molten chloride fluxes contained in vacuum-sealed fused silica and structurally characterized via single crystal X-ray diffraction. The in situ reduction of Eu3+ to Eu2+ was carried out using Mo, W, and Zn as metal reducing agents. All four compounds crystallize in the tetragonal space group of I41/a and adopt the scheelite (CaWO4) structure type. The magnetic susceptibility of the reported compounds shows paramagnetic behavior down to 2 K. 151Eu Mössbauer spectroscopy was used to analyze the relative Eu2+ and Eu3+ content of the samples. All the compounds were further characterized by EPR, and UV-vis spectroscopy.

  2. Synthesis and characterization of europium doped LiF phosphor

    Energy Technology Data Exchange (ETDEWEB)

    Villalobos, M. L.; Vallejo, M. A.; Sosa A, M. [Universidad de Guanajuato, Division de Ciencias e Ingenierias, Loma del Bosque No. 103, Lomas del Campestre, 37150 Leon, Guanajuato (Mexico); Diaz T, L. A., E-mail: villaloboscm2010@licifug.ugto.mx [Centro de Investigaciones en Optica, A. C., Loma del Bosque No. 115, Lomas del Campestre, 37150 Leon, Guanajuato (Mexico)

    2015-10-15

    LiF with different dopants has been one of the most investigated materials to use as thermoluminescent dosimeter. In this paper, we present the preparation method, the characterization and the thermoluminescent response of Eu doped LiF irradiated with X-rays. Pure and Eu doped LiF samples with different dopant concentration (0, 0.25, 0.5, 0.75 and 1 % mol) were synthesized using the precipitation method. The samples were structurally characterized by X-ray diffraction (XRD), the diffraction patterns showed a main cubic crystalline structure and a secondary hexagonal structure. The photoluminescence spectrum exhibited four well defined peaks characteristic of the Eu{sup 3+} ion. Thermoluminescent (Tl) glow curves of x-ray irradiated samples showed a well-defined single peak around 200 degrees C, except for the pure and 0.25% Eu doped samples. (Author)

  3. Synthesis and Characterization of Novel Epoxy Geopolymer Hybrid Composites

    Directory of Open Access Journals (Sweden)

    Oreste Tarallo

    2013-09-01

    Full Text Available The preparation and the characterization of novel geopolymer-based hybrid composites are reported. These materials have been prepared through an innovative synthetic approach, based on a co-reticulation in mild conditions of commercial epoxy based organic resins and a metakaolin-based geopolymer inorganic matrix. This synthetic strategy allows the obtainment of a homogeneous dispersion of the organic particles in the inorganic matrix, up to 25% in weight of the resin. The materials obtained present significantly enhanced compressive strengths and toughness with respect to the neat geopolymer, suggesting their wide utilization for structural applications. A preliminary characterization of the porous materials obtained by removing the organic phase from the hybrid composites by means of heat treatments is also reported. Possible applications of these materials in the field of water purification, filtration, or as lightweight insulating materials are envisaged.

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

    Science.gov (United States)

    Aderibigbe, B A; Neuse, E W; Sadiku, E R; Ray, S Shina; Smith, P J

    2014-06-01

    In this research, aminoquinoline compounds were synthesized, characterized, and incorporated into water-soluble polymers to form conjugates. The conjugates were characterized by X-ray diffraction, thermal gravimetric analysis, scanning electron microscope, Fourier transform infrared spectroscopy, and nuclear magnetic resonance spectroscopy to confirm the successful incorporation of the aminoquinoline compound on to the polymer. The synthesized conjugates were screened for in vitro antiplasmodial activity in triplet test against chloroquine-sensitive strain of Plasmodium falciparum and chloroquine drug was used as a reference drug in all the experiments. A full dose-response was performed to determine the concentration inhibiting 50% of parasite growth (IC50 value). Polymeric conjugates containing 3-diethylamino-1-propylamine solubilizing units were found to be most active against the chloroquine-sensitive strain of P. falciparum. © 2013 Wiley Periodicals, Inc.

  5. Synthesis and Characterization of Novel Epoxy Geopolymer Hybrid Composites.

    Science.gov (United States)

    Roviello, Giuseppina; Ricciotti, Laura; Ferone, Claudio; Colangelo, Francesco; Cioffi, Raffaele; Tarallo, Oreste

    2013-09-09

    The preparation and the characterization of novel geopolymer-based hybrid composites are reported. These materials have been prepared through an innovative synthetic approach, based on a co-reticulation in mild conditions of commercial epoxy based organic resins and a metakaolin-based geopolymer inorganic matrix. This synthetic strategy allows the obtainment of a homogeneous dispersion of the organic particles in the inorganic matrix, up to 25% in weight of the resin. The materials obtained present significantly enhanced compressive strengths and toughness with respect to the neat geopolymer, suggesting their wide utilization for structural applications. A preliminary characterization of the porous materials obtained by removing the organic phase from the hybrid composites by means of heat treatments is also reported. Possible applications of these materials in the field of water purification, filtration, or as lightweight insulating materials are envisaged.

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

    Energy Technology Data Exchange (ETDEWEB)

    Asha, E-mail: arana5752@gmail.com [Department of Basic and Applied Sciences, Bhagat Phool Singh Mahilla Vishwavidyalaya, Khanpur Kalan, Sonipat-131305 (India); Goyal, Sneh Lata; Kishore, Nawal [Department of Applied Physics, Guru Jambheshwar University of Science and Technology, Hisar-125001 (India)

    2016-05-23

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

  7. Synthesis and characterization of HDA/NaMMT organoclay

    Indian Academy of Sciences (India)

    In this study, the rheologic and colloidal characterizations of sodium montmorillonite (NaMMT) were examined. Hexadecylamine (CH3(CH2)15NH2, HDA) was added to the bentonite water dispersion (2%, w/w) in different concentrations in the range 5.6 × 10-4–9.4 × 10-3 m mol/l. The rheological and electrokinetic ...

  8. Synthesis, characterization and investigation of catalytic activity of ...

    Indian Academy of Sciences (India)

    xCoxFe2O4 nanoparticles were prepared via a hy- drothermal ... 3.1 Characterization of Cu1−xCoxFe2O4 nanoparticles. Figure 1 shows the indexed x-ray diffraction (XRD) patterns of Cu1−xCoxFe2O4 (x = 0.0, 0.5 and 1.0). Cu-rich catalyst (x = 0) ...

  9. Synthesis and characterization of antiseptic soap from neem oil and ...

    African Journals Online (AJOL)

    In this work, neem oil and shea butter oil were mixed in various proportions and used in preparing soaps which were subsequently characterized. The combination of Neem oil to Shea butter oil considered were 100:0, 80:20, 60:40, 50:50, 40:60, 20:80 and 0:100 (wt:wt). The physical properties of the prepared soap ...

  10. Synthesis, Characterization and Biological Activity Studies of Mixed ...

    African Journals Online (AJOL)

    ADOWIE PERE

    ABSTRACT: Mixed ligand-metal complexes of Paracetamol and Ascorbic acid were synthesized using FeCl2.4H2O,. CuCl2.2H2O, NiCl2.6H2O, CoCl2.6H2O and ZnSO4 salts based on two concentrations (3mmol and 5mmol). The complexes were characterized using some physical techniques such as melting point, ...

  11. Synthesis and Characterization of Copper (II) Complex of Glycine ...

    African Journals Online (AJOL)

    Copper(II)Complex of amino acid was synthesized by refluxing the mixtures of ethanolic solutions of glycine and copper(II)chloride. The complex compound was characterized by melting point (225oC), PH 5.78 at 28oC, moisture content of 5% with a yield of 68%. The compound is insoluble in water but readily soluble in ...

  12. Synthesis and Characterization of PEGylated Toll Like Receptor 7 Ligands

    OpenAIRE

    Chan, Michael; Hayashi, Tomoko; Mathewson, Richard D.; Yao, Shiyin; Gray, Christine; Tawatao, Rommel; Kalenian, Kevin; Zhang, Yanmei; Hayashi, Yuki; Lao, Fitzgerald S.; Cottam, Howard B.; Carson, Dennis A.

    2011-01-01

    Toll like receptor 7 (TLR7) is located in the endosomal compartment of immune cells. Signaling through TLR7, mediated by the adaptor protein MyD88, stimulates the innate immune system and shapes adaptive immune responses. Previously, we characterized TLR7 ligands conjugated to protein, lipid or polyethylene glycol (PEG). Among the TLR7 ligand conjugates, the addition of PEG chains reduced the agonistic potency. PEGs are safe in humans and widely used for improvement of pharmacokinetics in exi...

  13. Synthesis and characterization of antiseptic soap from neem oil and ...

    African Journals Online (AJOL)

    GWANDI

    2013-07-17

    Jul 17, 2013 ... In this work, neem oil and shea butter oil were mixed in various proportions and used in preparing soaps which were subsequently characterized. The combination of Neem oil to Shea butter oil considered were 100:0, 80:20, 60:40, 50:50, 40:60, 20:80 and 0:100 (wt:wt). The physical properties of the.

  14. Synthesis and spectroscopic characterization of chiral biphenyl-cholesterol gels.

    Science.gov (United States)

    Geiger, H Cristina; Lamson, Melissa; Galka, Daniel J

    2014-11-25

    The synthesis of 4-(3-cholesteroxycarbonylpropyloxy)biphenyl (BO4-chol), 4-(7-cholesteroxycarbonylheptyloxy)biphenyl (BO8-chol), and 4,4'-bis(7-cholesteroxycarbonyl heptyloxy)biphenyl (BBO8-chol) is reported. These gelators form 1% and 2% (w/w) stable gels in n-octanol. The gels formed from single cholesterol gelators (BO4-chol and BO8-chol) exhibit lower phase transition temperatures (Tg) (62-65, 68-69 °C) than the gel obtained from the bischolesterol gelator BBO8-chol (96-98 °C). All three gelators form chiral gels in n-octanol as observed by induced circular dichroism (ICD) spectroscopy. The effect of two cholesterol moieties versus one cholesterol unit linked to a biphenyl molecule by a flexible chain, and the effect of the chain length on the gelation ability of these three novel gelators was investigated by circular dichroism (CD), absorption, and fluorescence spectroscopies. The gels obtained from BO4-chol and BO8-chol exhibit biphasic circular dichroism spectra with opposite chirality. The ICD spectra of both BO8-chol and BBO8-chol gels show a positive ICD band followed by a negative band at room temperature. However, while BO8-chol gel ICD absorptions decrease equally as temperature increases, BBO8-chol gel shows an inversion of the Cotton effect bands between 50 and 60 °C until completely disappearing above the phase transition temperature. SEM was used for the investigation of the morphology of the xerogels. On the basis of XRD data and molecular modeling, we propose packing modes for the formation of the organogelator aggregates.

  15. Synthesis and characterization of pHLIP® coated gold nanoparticles

    Directory of Open Access Journals (Sweden)

    Jennifer L. Daniels

    2017-07-01

    Full Text Available Novel approaches in synthesis of spherical and multispiked gold nanoparticles coated with polyethylene glycol (PEG and pH Low Insertion Peptide (pHLIP® were introduced. The presence of a tumor-targeting pHLIP® peptide in the nanoparticle coating enhances the stability of particles in solution and promotes a pH-dependent cellular uptake. The spherical particles were prepared with sodium citrate as a gold reducing agent to form particles of 7.0±2.5 nm in mean metallic core diameter and ∼43 nm in mean hydrodynamic diameter. The particles that were injected into tumors in mice (21 µg of gold were homogeneously distributed within a tumor mass with no staining of the muscle tissue adjacent to the tumor. Up to 30% of the injected gold dose remained within the tumor one hour post-injection. The multispiked gold nanoparticles with a mean metallic core diameter of 146.0±50.4 nm and a mean hydrodynamic size of ~161 nm were prepared using ascorbic acid as a reducing agent and disk-like bicelles as a template. Only the presence of a soft template, like bicelles, ensured the appearance of spiked nanoparticles with resonance in the near infrared region. The irradiation of spiked gold nanoparticles by an 805 nm laser led to the time- and concentration-dependent increase of temperature. Both pHLIP® and PEG coated gold spherical and multispiked nanoparticles might find application in radiation and thermal therapies of tumors.

  16. Synthesis, deposition and characterization of ferroelectric films for electrooptic devices

    Science.gov (United States)

    Tunaboylu, Bahadir

    The use of integrable ferroelectric electro-optic thin films is a revolutionary approach in the development of high-speed, low-voltage and high-contrast ratio integrated electro-optic spatial light modulators (SLM) for free-space optoelectronic interconnects. Thin films offer improved performance over bulk ferroelectric (FE) materials because of their lower modulator capacitance and operation at high speeds with low switching energies. Integration of ferroelectric thin films with silicon technology will also impact both the uncooled infrared sensor and dynamic and nonvolatile memory technologies. Ferroelectrics such as lead lanthanum zirconate titanate (PLZT) and patassium tantalate niobate (KTN) present great potential for SLMs due to their large electro-optic (EO) effect in the bulk form. The development of thin-film SLMs require electro-optic films of high optical quality with good dielectric and EO properties. High quality thin films of PLZT and KTN were deposited using RF magnetron sputtering on r-plane sapphire substrates which offer integration capability with semiconductor devices. PLZT films with extremely large peak dielectric constant, 2800 at the Curie temperature of 180sp°C, were achieved with remarkably low dissipation loss factor leap forward for the FE-SLM technology with respect to the goal of fully integrated thin film electrooptic light modulators. Microstructural development and phase transformation kinetics in PLZT films were also analyzed for the first time and are presented here. Energy required for the formation of desirable perovskite phase was determined to be 322 kJ/mol. Single-phase PLZT films with larger average grain size showed higher dielectric constants and better EO properties as compared to films with smaller grain size. Furthermore, a method of sol-gel synthesis of KTN with reproducible characteristics was developed for fabrication of both thin films and homogeneous sputtering targets. Also for the first time, a stoichiometric

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-11-15

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

  18. A novel vanadium n-propylamino phosphate catalyst: synthesis, characterization and applications

    Directory of Open Access Journals (Sweden)

    Rajini Anumula

    2013-02-01

    Full Text Available A novel, lamellar type Vanadium n-propylamino phosphate catalyst is synthesized and characterized by using various physicochemical techniques such as Powder X-ray diffraction, Scanning electron microscopy/Energy dispersive X-ray analysis, Thermogravimetry/Differential thermal analysis, Fourier transform Infrared analysis, Electron spin resonance spectroscopy, Ultraviolet - Visible Diffuse reflectance spectroscopy, X-ray Photoelectron spectroscopy, 31P Magic angle spinning Nuclear Magnetic Resonance spectroscopy and Catalytic applications toward Octahydroquinazolinone synthesis. It is found that the n-propylamine is present as sandwich between Vanadyl phosphate layers. Most of the Vanadium is present as V4+ ions in tetrahedral co-ordination. Vanadium n-propylamino phosphate catalyses Octahydroquinazolinone synthesis more effeciently and the optimum conditions required for Octahydroquinazolinone synthesis are, Benzaldehyde (2 mmol, Dimedone (2 mmol, Urea (4 mmol, Methanol + Water (1:1, 5 mL and Catalyst (0.05 g. A plausible mechanism is also proposed.

  19. Refined Synthesis and Characterization of Controlled Diameter, Narrow Size Distribution Microparticles for Aerospace Research Applications

    Science.gov (United States)

    Tiemsin, Pacita I.; Wohl, Christopher J.

    2012-01-01

    Flow visualization using polystyrene microspheres (PSL)s has enabled researchers to learn a tremendous amount of information via particle based diagnostic techniques. To better accommodate wind tunnel researchers needs, PSL synthesis via dispersion polymerization has been carried out at NASA Langley Research Center since the late 1980s. When utilizing seed material for flow visualization, size and size distribution are of paramount importance. Therefore, the work described here focused on further refinement of PSL synthesis and characterization. Through controlled variation of synthetic conditions (chemical concentrations, solution stirring speed, temperature, etc.) a robust, controllable procedure was developed. The relationship between particle size and salt concentration, MgSO4, was identified enabling the determination of PSL diameters a priori. Suggestions of future topics related to PSL synthesis, stability, and size variation are also described.

  20. A novel vanadium n-propylamino phosphate catalyst: synthesis, characterization and applications

    Directory of Open Access Journals (Sweden)

    Rajini Anumula

    2012-01-01

    Full Text Available A novel, lamellar type Vanadium n-propylamino phosphate catalyst is synthesized and characterized by using various physicochemical techniques such as Powder X-ray diffraction, Scanning electron microscopy/Energy dispersive X-ray analysis, Thermogravimetry/Differential thermal analysis, Fourier transform Infrared analysis, Electron spin resonance spectroscopy, Ultraviolet - Visible Diffuse reflectance spectroscopy, X-ray Photoelectron spectroscopy, 31P Magic angle spinning Nuclear Magnetic Resonance spectroscopy and Catalytic applications toward Octahydroquinazolinone synthesis. It is found that the n-propylamine is present as sandwich between Vanadyl phosphate layers. Most of the Vanadium is present as V4+ ions in tetrahedral co-ordination. Vanadium n-propylamino phosphate catalyses Octahydroquinazolinone synthesis more effeciently and the optimum conditions required for Octahydroquinazolinone synthesis are, Benzaldehyde (2 mmol, Dimedone (2 mmol, Urea (4 mmol, Methanol + Water (1:1, 5 mL and Catalyst (0.05 g. A plausible mechanism is also proposed.

  1. Synthesis and Characterization of a Mg2+-Selective Fluorescent Probe

    Directory of Open Access Journals (Sweden)

    Chunwei Yu

    2014-07-01

    Full Text Available A new Mg2+-selective fluorescent probe P was synthesized and characterized. With optimal conditions, the proposed probe P showed good selectivity to Mg2+ compared to other common metal ions, and worked in a wide linear range of 5.0 × 10−7–6.0 × 10−6 M with a detection limit of 1.7 × 10−7 M Mg2+ in ethanol-water solution (9:1, v/v, 20 mM HEPES, pH = 10.0.

  2. Conjugated polymer light-emitting diodes: Synthesis, fabrication and characterization

    Science.gov (United States)

    Kasim, Ramesh Kumar

    A new conjugated polymer, poly(2,6-quinoline vinylene) was synthesized by direct polymerization and via a precursor route. The optical band gap of the polymer was determined to be 2.39 eV. Precursor polymer, with xanthate as the leaving group, was prepared and electroluminescent properties of the con ugated polymer were characterized. A copolymer namely, poly(1,4-phenylene vinylene-co-2,6-quinoline vinylene), PPVQV, containing p-type and n-type segments, was prepared via a precursor route and characterized. The EL spectrum of the copolymer is blue shifted with respect to both PPV and PQV. Bilayer devices with PPV and PPVQV yielded improved emission efficiency. Further improvement in emission efficiency was achieved by using blends of copolymer and PPV homopolymer to construct devices with 'graded' composition. EL properties of poly(4,4'-dinonyl-2,2' -bithiazol-5,5'-diyl) (PNBT) and its methylated derivative (MPNBT) were characterized. PNBT showed orange emission and intensity decreased very rapidly. Continued operation at higher voltages caused a red shift in the emission spectrum. MPNBT showed orange EL with broader emission spectrum. Bilayer and blend devices consisting of MPNBT and PPV showed lower onset field. EL properties of electron withdrawing group substituted thiophene-based polymers with regioregular and regiorandom structures were characterized. Regioregular polymers showed lower EL efficiency than respective regiorandom polymers. A non-catalytic chemical reduction method to deposit silver on polymer films was developed. It yielded shiny films with good polymer/metal interface. The deposition was carried out on a lab bench without special precautions. Strong reduction conditions gave gray or brown spongy films, while mild reduction conditions yielded good quality films. LEDs that work under both forward and reverse dc bias were fabricated using PPV as emission layer. The reverse bias EL in LEDs on heat-treated ITO substrates is attributed to the

  3. Synthesis and Characterization of Organotin Containing Copolymers: Reactivity Ratio Studies

    Directory of Open Access Journals (Sweden)

    Mohamed H. El-Newehy

    2010-03-01

    Full Text Available Organotin monomers containing dibutyltin groups – dibutyltin citraconate (DBTC as a new monomer and dibutyltin maleate (DBTM – were synthesized. Free radical copolymerizations of the organotin monomers with styrene (ST and butyl acrylate (BA were performed. The overall conversion was kept low (≤15% wt/wt for all studied samples and the copolymers composition was determined from tin analysis using the Gillman and Rosenberg method. The reactivity ratios were calculated from the copolymer composition using the Fineman-Ross (FR method. The synthesized monomers were characterized by elemental analysis, 1H-, 13C-NMR and FTIR spectroscopy.

  4. Synthesis and Characterization of Cotton Fiber-based Nanocellulose.

    Science.gov (United States)

    Theivasanthi, T; Anne Christma, F L; Toyin, Adeleke Joshua; Gopinath, Subash C B; Ravichandran, Ramanibai

    2017-11-10

    Nanocellulose prepared from the natural material has a promising wide range of opportunities to obtain the superior material properties towards various end-products. In this research, commercially available natural cotton was treated with aqueous sodium hydroxide solution to eliminate the hemicellulose and lignin, then cellulose was collected. The collected cellulose was subjected to acid hydrolysis using sulfuric acid to obtain nanocellulose. The prepared nanocellulose was further characterized with the aid of Fourier transform infrared spectroscopy, X-ray diffraction and Scanning Electron Microscopy to elucidate the chemical structure, crystallinity and the morphology. Copyright © 2017 Elsevier B.V. All rights reserved.

  5. Microwave assisted combustion synthesis and characterization of nickel ferrite nanoplatelets

    Directory of Open Access Journals (Sweden)

    M. Venkatesh

    2016-09-01

    Full Text Available Nickel ferrite nanoplatelets have been successfully synthesized by a simple microwave assisted combustion method using trisodium citrate as a fuel. The prepared sample was chemically and structurally characterized by different techniques and the magnetic behaviour was studied by field dependent magnetization measurement. The obtained results indicate that the prepared sample is phase pure nickel ferrite nanoplatelets having size in the range of 40–50 nm and it exhibits a soft ferromagnetic nature with saturation magnetization of 49 emu/g and coercivity of 167 G. Hence proposed method is a facile approach to obtain nickel ferrite nanoplatelets for broad spectrum of applications.

  6. Synthesis, Characterization, and Flocculation Properties of Branched Cationic Polyacrylamide

    Directory of Open Access Journals (Sweden)

    Weimin Sun

    2013-01-01

    Full Text Available A water soluble branched cationic polyacrylamide (BCPAM was synthesized using solution polymerization. The polymerization was initiated using potassium diperiodatocuprate, K5[Cu(HIO62](Cu(III, initiating the self-condensing vinyl copolymerization of acrylamide and acryloxyethyltrimethyl ammonium chloride (DAC monomer. The resulting copolymer was characterized by the use of Fourier-transform infrared (FTIR spectroscopy and nuclear magnetic resonance (NMR spectroscopy. Its flocculation properties were evaluated with standard jar tests of sewage. The effects of initiator concentration, monomer concentration, reaction temperature, and the mass ratio of monomers on intrinsic viscosity and flocculation properties of the product were determined using single-factor experiments and orthogonal experiment.

  7. Synthesis, Characterization and Copolymerization of N-(phenylaminomaleimide with MMA

    Directory of Open Access Journals (Sweden)

    B. L. Hiran

    2007-01-01

    Full Text Available The free radical copolymerization of N-(phenylaminomaleimide (N-PAMI was carried. The copolymerization with methyl methacrylate (MMA was performed at 65°C with AIBN as the initiator in THF solvent. Resulting copolymer was characterized by density measurement, intrinsic viscosity, solubility, FT-IR & 1H NMR spectroscopy. Effect of the solvent and time on copolymer yield was also investigated. The molecular weight of copolymer was determined by gel permeation chromatography (GPC. The thermal stability of copolymer was determined by Thermogravimetric analysis (TGA.

  8. Synthesis and characterization of In(OH)3 nanocubes

    Science.gov (United States)

    Lu, Xifeng; Wang, Tao; Zhang, Xizhou; Qiu, Aiguo; Cui, Deliang

    2009-09-01

    In this work, In(OH)3 nanocubes were successfully synthesized in large quantities with InCl3·4H2O as indium source in the presence of sodium hydroxide by a hydrothermal process at 240 °C for 12 h. The structure and the morphology of the In(OH)3 samples were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The results revealed that the resultant In(OH)3 nanocubes were nearly uniform in size. Photoluminescence (PL) measurement was carried out.

  9. Synthesis and characterization of lamellar aragonite with hydrophobic property

    Energy Technology Data Exchange (ETDEWEB)

    Wang Chengyu, E-mail: wangcy@nefu.edu.cn [College of Materials Science and Engineering, Northeast Forestry University, 150040 (China); Xu Yang [China Nation Center for Quality Supervision and Test of Woodworking Machinery, Northeast Forestry University, 150040 (China); Liu Yalan; Li Jian [College of Materials Science and Engineering, Northeast Forestry University, 150040 (China)

    2009-04-30

    A novel and simple synthetic method for the preparation of hydrophobic lamellar aragonite has been developed. The crystallization of aragonite was conducted by the reaction of sodium carbonate with calcium chloride in the presence of sodium stearate. The resulting products were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR) and the contact angle. The results revealed that sodium stearate plays an important role in determining the structure and morphology of the sample. Besides, we have succeeded in surface modification of particles in situ at the same time. The contact angle of the modified aragonite reached 108.59 deg.

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

    Directory of Open Access Journals (Sweden)

    Rios Sarah P.O.

    2002-01-01

    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

  11. Synthesis and structural characterization of boron nitride thin films

    Energy Technology Data Exchange (ETDEWEB)

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

    1994-12-15

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

  12. Synthesis and Characterization of Carbon Metal Nano Tubes

    Science.gov (United States)

    Tiwari, B.; Tripathi, I. P.; Saxena, Sanjay; Singh, Sudhanshu; Haribhushan

    2010-11-01

    Nano technology is emerging as the latest technology these days. It is proving its importance in every sphere of life. Metal carbon nano tube due to their vast applications is being used very frequently. So to prepare CNTs a new method is developed. In this methods Complexes of transition metal Ni(II) with amino acids present in egg albumin have been synthesized. The complex is analyzed on the basis of spectroscopic methods of UV, IR, and NMR Spectroscopy. The amino acid metal Complex is decomposed at higher temperature to obtain metal carbon nano tubes. These metal carbon nano tubes are characterized using scanning probe instruments like DLS.

  13. Single crystal: Urea bisthiourea sodium acetate synthesis, growth and characterization

    Science.gov (United States)

    Manickam, R.; Srinivasan, G.

    2017-05-01

    Crystals of urea bisthiourea sodium acetate (UBTSA) were successfully grown from an aqueous solution by slow evaporation method at room temperature. Recrystallization process was used to increase the purity of the grown crystal. The grown crystals were characterized by single crystal XRD, FT-Raman, UV and TGA/DTA analysis. Structure and unit cell parameters were determined by single crystal XRD. Functional groups of grown crystal and their modes of vibration were identified using FT-Raman spectral analysis. Absorbance percentage of the grown crystal was studied using UV analysis. Thermo gravimetric analysis and differential thermal analysis reveal that the good thermal stability of the material.

  14. Synthesis and characterization of MCM-41-supported nano zirconia catalysts

    Directory of Open Access Journals (Sweden)

    Mohamed S. Abdel Salam

    2015-03-01

    Full Text Available Series of MCM-41 supported sulfated Zirconia (SZ catalysts with different loadings (2.5–7.5% wt. were prepared using direct impregnation method. The acquired solid catalysts were characterized structurally and chemically using X-RD, HRTEM, BET, FT-IR, Raman spectroscopy and TPD analysis. The acidity of the solid catalysts was investigated through cumene cracking and isopropanol dehydration at different temperatures. As the SZ loading increases, the surface acidity of the mesoporous catalysts was enhanced, this was reflected by the higher catalytic activity toward cumene cracking and isopropanol dehydration.

  15. Eco-Friendly Synthesis and Characterization of Reduced Graphene Oxide

    Science.gov (United States)

    Ickecan, D.; Zan, R.; Nezir, S.

    2017-09-01

    Graphene is a single sheet of sp2 bonded carbon having a two-dimensional (2D) layer. It has remarkable electronic, mechanical and thermal properties. In this paper, the graphene oxide (GO) was reduced by reducing chemicals such as ascorbic acid and hydrazine and then characterized by transmission electron microscopy (TEM), Raman spectroscopy and Fourier transform infrared spectroscopy. TEM results of the chemically reduced graphene were showed that the structure consists of a mixture of single and few layers of reduced graphene oxide (rGO).

  16. Hydrothermal synthesis of siderite nano-particles and characterizations

    Science.gov (United States)

    Oza, Mahatta; Joshi, M. J.

    2017-05-01

    Siderite is an iron ore in the form of ferrous carbonate (FeCO3). It finds applications in ceramics, in pig iron production, pigments in paints and in petroleum drilling fluids as a scavenger for H2S. An attempt was made to synthesize FeCO3 nano-particles by hydrothermal treatment of aqueous solution of iron sulphate, ascorbic acid, and ammonium carbonate with a molar ratio of 1:1:3, respectively, at 140˚C for 1.5 h. The synthesized powder was further characterized by different characterization techniques like powder XRD, FT-IR and TGA. The powder XRD analysis suggested the nano-crystalline nature of the sample with Hexagonal crystal system having unit cell parameters as: a = 4.691Ǻ, b = 4.691 Ǻ and c = 15.37Ǻ. The average crystallite size was found to be ̴ 10.70 nm from Scherrer's formula. FT-IR spectrum confirmed the presence of O-H, and C-O functional groups. The TGA results suggested that the material started decomposing from the beginning and showed weight loss of 32.4% at 358°C temperature. Thereafter, the sample very slowly decomposed and at the end of process sample showed weight loss of 39.5% at 900°C after giving up carbon dioxide.

  17. Synthesis, characterization, and reactivity of alkyldisulfanido zinc complexes.

    Science.gov (United States)

    Galardon, Erwan; Tomas, Alain; Selkti, Mohamed; Roussel, Pascal; Artaud, Isabelle

    2009-07-06

    The alkyldisulfanido zinc complexes Tp(iPr,iPr)Zn(SSR) and Tp(Ph,Me)Zn(SSR) where Tp(iPr,iPr) is hydridotris-((3,5-isopropyl)pyrazolyl)borate, Tp(Ph,Me) is hydridotris-((3-phenyl,5-methyl)pyrazolyl)borate, and (SSR) is tert-butyldisulfanido or triphenylmethanedisulfanido were synthesized by reaction between the corresponding hydroxo complexes TpZn(OH) and the synthetic persulfide RSSH. All the complexes were characterized by elemental analysis and (1)H NMR spectroscopy, and representative members of the class were also structurally characterized. The reactivity of the alkyldisulfanido TpZn(SSR) complexes with thiols was studied. In the absence of base, a simple exchange reaction between the alkyldisulfanido ligand and the thiol was observed in dichloromethane; when in the presence of base, the corresponding hydrogen(sulfido) complexes TpZn(SH) were obtained. The mechanism of the latter reaction has been studied and does not involve the coordinated alkyldisulfanido group. Reaction of the hydrogen(sulfido) complexes Tp(iPr,iPr)Zn(SH) with the thiosulfonate PhCH(2)S-SO(2)CF(3) did not yield the expected alkyldisulfanido complex but benzyltrisulfide and a new complex tentatively assigned as Tp(iPr,iPr)Zn(O(2)SCF(3)).

  18. Synthesis and characterization of partially biodegradable and thermosensitive hydrogel.

    Science.gov (United States)

    Zhang, Xian-Zheng; Sun, Guo-Ming; Wu, Da-Qing; Chu, Chih-Chang

    2004-08-01

    A partially biodegradable and thermosensitive hybrid hydrogel network (DAN series) based on dextran-allylisocyanate (Dex-AI) and poly(N-isopropylacrylamide) (PNIPAAm) was synthesized via UV photocrosslinking. These hybrid hydrogels were characterized in terms of their chemical structure, thermal, mechanical, morphological and temperature-induced swelling properties. The effect of the composition ratio of Dex-AI to PNIPAAm on such properties were examined. The differential scanning calorimetry data show that this Dex-AI/PNIPAAm hybrid network has an increased lower critical solution temperature (LCST) and glass transition temperature (Tg) with an increase in the Dex-AI content. The interior morphology of these hybrid hydrogels revealed a decreased porous microstructure with an increase in the Dex-AI content in the hybrid network. Furthermore, if the Dex-AI composition became too high, a distinctive network structure with two different microporous structures appeared. The mechanical properties of these hybrid hydrogels also increased with an increase in the Dex-AI content. The temperature dependence of the swelling ratio, the deswelling kinetics as well as the reswelling kinetics was also characterized by gravimetric method. When comparing with a normal PNIPAAm hydrogel, these Dex-AI/PNIPAAm hybrid networks, due to the presence of Dex-AI moiety, also show improved temperature-induced intelligent properties, such as the faster and controllable response dynamics, which may find promising applications in a wide variety of fields, such as biomedical and bioengineering fields.

  19. CHARACTERIZATION OF IMMOBILIZED LIPASE IN ALUMINOSILICATE FOR LACTOSYL PALMITATE SYNTHESIS

    Directory of Open Access Journals (Sweden)

    Anna Roosdiana

    2010-06-01

    Full Text Available Whey lactose can be esterified enzymatically by using immobilized lipase. The lipase can be isolated from Rhizopus oryzae, purified and immobilized in mesoporous aluminosilica. The use of immobilized lipase has advantages, there are longer shelf life and repeatable use. It is necessary to characterize the immobilized lipase dan ester product. The aim of the research was to characterize immobilized lipase, including determination lipase adsorption type in mesoporous aluminosilicate, immobilized lipase stability during storage time, efficiency of repetitive use of immobilized lipase. The result showed that lipase adsorption in mesoporous aluminosilicate was physical adsorption type through hydrogen bound and electrostatic interaction. Immobilized lipase stability was relatively constant at storage temperature 5 °C for 25 days resulting in 98.16% of initial activity. The repetitive use of immobilized lipase showed efficient until 5 uses within activity of 50.22%. The IR spectra of lactosyl palmitate from both whey and pure lactose result showed bands at wavelength number of 3462 cm-1(OH bond, 1739 cm-1 and 1747 (C=O ester bond 1295 cm-1 dan 1242 cm-1 (C-O ester bond. In addition, the HLB value for lactosyl palmitate (whey 4.708 and lactosyl palmitate (pure lactose 4.715, therefore both lactosyl palmitate is appropriate as emulgator in W/O.   Keywords: immobilized lipase, aluminosilica, lactose, whey, lactosyl palmitate

  20. SYNTHESIS AND CHARACTERIZATION OF POLYIMIDE-ZEOLITE MIXED MATRIX MEMBRANE

    Directory of Open Access Journals (Sweden)

    Budiyono Budiyono

    2012-02-01

    Full Text Available Biogas has become an attractive alternative energy source due to the limitation of energy from fossil. In this study, a new type of mixed matrix membrane (MMM consisting of polyimide-zeolite was synthesized and characterized for biogas purification. The MMM consists of medium concentration of polymer (20% wt polyimide, 80% N-Methyl-2-pyrrolidone (NMP and 25% zeolite 4A in total solid were prepared by a dry/wet phase inversion technique.  The fabricated MMM was characterized using SEM, DSC, TGA and gas permeation. Post treatment coating procedure was also conducted. The research showed that surface coating by 3% silicone rubber toward MMM PI 20% gave the significant effect to improve membrane selectivity. The ideal selectivity for CO2/CH4 separation increased from 0.99 for before coating to 7.9 after coating for PI-Zeolite MMM, respectively. The results suggest that PI-Zeolite MMM with good post treatment procedure will increase the membrane selectivity and permeability with more saver polymer requirement as well as energy saving due to low energy for mixing.

  1. Cobalt hexacyanoferrate-poly(methyl methacrylate) composite: Synthesis and characterization

    Energy Technology Data Exchange (ETDEWEB)

    Zanotto, Antonio, E-mail: zanotto.antonio@gmail.com [Dipartimento di Chimica Fisica ' F. Accascina' , Universita di Palermo, and INSTM UdR Palermo, Parco d' Orleans II, Viale delle Scienze pad. 17, Palermo 90128 (Italy); Matassa, Roberto [Centro Grandi Apparecchiature, UniNetLab, Universita di Palermo, Via Marini 14, Palermo 90128 (Italy); Saladino, Maria Luisa [Dipartimento di Chimica Fisica ' F. Accascina' , Universita di Palermo, and INSTM UdR Palermo, Parco d' Orleans II, Viale delle Scienze pad. 17, Palermo 90128 (Italy); Berrettoni, Mario; Giorgetti, Marco [Department of Physical and Inorganic Chemistry, University of Bologna and Unita di Ricerca INSTM di Bologna, Viale del Risorgimento 4, 40136 Bologna (Italy); Zamponi, Silvia [Dipartimento di Scienze Chimiche, Universita di Camerino Via S. Agostino 1, Camerino 62032 (Italy); Caponetti, Eugenio [Dipartimento di Chimica Fisica ' F. Accascina' , Universita di Palermo, and INSTM UdR Palermo, Parco d' Orleans II, Viale delle Scienze pad. 17, Palermo 90128 (Italy); Centro Grandi Apparecchiature, UniNetLab, Universita di Palermo, Via Marini 14, Palermo 90128 (Italy)

    2010-03-15

    Graphical abstract: The preparation of cobalt hexacyanoferrate nanoparticles-poly(methyl methacrylate) (CoHCF-PMMA) composites are described together with their characterization and thermochromic properties. CoHCF nanoparticles - investigated by dynamic light scattering - were prepared by optimizing solvent composition and temperature to obtain nanoparticles with a reduced degree of aggregation. The nanoparticles were embedded in a PMMA matrix to obtain a transparent coloured composite which was studied by transmission electron microscopy. The nanoparticle chromic features, enhanced by their reduced sizes, were investigated by UV-vis and FT-IR spectroscopy. - Abstract: The preparation of cobalt hexacyanoferrate nanoparticles-poly(methyl methacrylate) (CoHCF-PMMA) composites are described together with their characterization and thermochromic properties. CoHCF nanoparticles - investigated by dynamic light scattering - were prepared by optimizing solvent composition and temperature to obtain nanoparticles with a reduced degree of aggregation. The nanoparticles were embedded in a PMMA matrix to obtain a transparent coloured composite which was studied by transmission electron microscopy. The nanoparticle chromic features, enhanced by their reduced sizes, were investigated by UV-vis and FT-IR spectroscopy.

  2. Characterization of protein synthesis factors from rabbit reticulocytes.

    Science.gov (United States)

    Merrick, W C; Dever, T E; Kinzy, T G; Conroy, S C; Cavallius, J; Owens, C L

    1990-08-27

    As part of our efforts to characterize eukaryotic translation factors, we have sequenced a number of them chemically and inferred sequences from cDNA clones. To our surprise, there appears to be extensive identity of amino acid sequence in most factors characterized to date in that within mammalian species, usually greater than 99% identity is observed. Extreme examples are rabbit EF-1 alpha which is 100% identical to human EF-1 alpha and rabbit eIF-4AI and eIF-4AII which are 100% identical to mouse eIF-4AI and eIF-4AII for those amino acids sequenced (398/406 and 156/407, respectively). An extended analysis has been made of EF-1 alpha which in rabbit has three different post-translational modifications, dimethyllysine, trimethyllysine and glycerylphosphorylethanolamine. A comparison of the primary structure of EF-1 alpha to E. coli EF-Tu indicates an overall sequence identity of 33%. However, within the amino terminal 180 amino acids (the GTP-binding domain), there are found regions of much greater identity (50/85 = 59%).

  3. Synthesis and characterization of novel ternary and quaternary reduced molybdenum oxides

    Energy Technology Data Exchange (ETDEWEB)

    Schimek, George L. [Iowa State Univ., Ames, IA (United States)

    1993-07-01

    This thesis is divided into 8 sections: synthesis and characterization (char.) of Ba3Mo18O28 (an oligomer with four traps edge-sharing Mo octahedra); synthesis and char. of KxMyMo14O22 (M=Sn, Pb, Sr) (oligomers with three traps edge-sharing Mo octahedra); synthesis and char. of K0.19Ba3.81Mo22O34 (an oligomer with five traps edge-sharing Mo octahedra); synthesis and char. of Ti0.31Fe1.69Mo4O7 (a material containing closest-packing of infinite chains of octahedral Mo clusters); synthesis and char. of KxM2-xMo10O16 (M=Ca, Sr, Gd) (oligomers with two traps edge-sharing Mo octahedra); synthesis and char. of the RE4Mo4O11 series; synthesis and char. of Pb0.31WO3 (a tetragonal tungsten bronze containing lead); and examination of superstructure in Fe1.89Mo4.11O7, Sn0.9Mo4O6, InMo4O6, and Mn1.5Mo8O11 by electron microscopy.

  4. Lipid-hydrogel nanoparticles: Synthesis methods and characterization

    Science.gov (United States)

    Hong, Jennifer S.

    vesicles with encapsulated hydrogel precursor. The encapsulated hydrogel precursor is polymerized off-chip and the resultant hybrid nanoparticle size distributions are highly monodisperse and precisely controlled across a broad range relevant to the targeted delivery and controlled release of encapsulated therapeutic agents. Given the ability to modify liposome size and surface properties by altering the lipid components and the many polymers of current interest for nanoparticle synthesis, this approach could be adapted for a variety of hybrid nanoparticle systems.

  5. Synthesis and characterization of fluorinated polyaminoquinones and fluorinated polyimides

    Science.gov (United States)

    Vaccaro, Eleonora

    Phenolic and quinonoid compounds are widely studied in biological sciences because of their ability to chelate heavy metals like iron and copper and recently have found new applications in synthetic macromolecules. Amino- p-benzoquinone polymers, poly[(2,5-hexamethylenediamino)-1,4-benzoquinone] and poly {[2,5-(2,2'-bistrifluoromethyl)-4,4' -biphenylenediamino]1,4-benzoquinone}, were synthesized and evaluated as adhesion promoters for steel/epoxy joints. An improvement in the torsional shear strength of these joints was observed when these polymers were used as adhesion promoters. The durability of the adhesive bond was also improved after boiling water treatment, relative to untreated and silane treated joints. The improvement in adhesion could be attributed to the formation of a chelate between the polyaminoquinone (PAQ) and the iron surface and a chemical reaction between the PAQ and the epoxy resin. A low molecular weight model compound, bis[2,5-(4-methylanilido)]-1,4-benzoquinone was also used to study coupling between the epoxy adhesive and the steel surface. Electron spin resonance (ESR), atomic absorption spectroscopy and infrared spectroscopy were used to document the epoxy-coupling agent reaction and the chelate formation. Polyimides have acquired importance in the last twenty years as the most promising macromolecules for high technology applications in new materials. Their good thermo-oxidative stability is well known, as well as their high glass transition temperature. Polyimides are versatile polymers, which can be utilized for a wide range of applications: i.e., as matrices for high performance advanced composite materials, as thin films in electronic applications, as structural adhesives and sealants and as membranes for gas separation. A novel anhydride, 1,1,1-trifluoromethyl-1-pentafluorophenylethylidene-2,2-diphthalic anhydride, 8FDA, was synthesized. Five diamines were used in the synthesis of polyimides, namely p-phenylene diamine, 3

  6. Prediction, synthesis and characterization of new topological materials

    Science.gov (United States)

    Gibson, Quinn Davis

    Over the past few years, a rediscovery of the concept of topology as it applies to the electronic structure of materials has created an explosion of research and discovery of new materials properties. While this field has been mainly of interest to the condensed matter physics community, this work explores it from a materials chemistry perspective, to both develop new materials, via a combination of computation, synthesis and measurement, to understand how the electronic topology can relate to structure and bonding. As such, adding chemical complexity to existing topological materials has been a focus of this study. In order to expand upon the archetypal topological insulator family of Bi2X3 (X=Se,Te), the super lattice materials, which contain alternating layers of Bi2 or Sb2 and Bi 2X3 or Sb2Te3, were investigated, revealing novel properties. The compound Bi4Se3 was shown to have termination dependent surface states, revealing a relationship between the nature of the surface states and the chemical nature of the surface, as well as novel mirror symmetry protected surface states. The 2:1 family (in the Sb2Te structure) were shown to be new topological insulators, with a novel Sb/Bi ordering when Bi is substituted for Sb in Sb2Te. Finally the 1:1 family was shown to, unexpectedly, be strong topological insulators, despite the theoretical prediction that they are weak topological insulators. Furthermore, other materials families were investigated as topological insulators, such as the chimney ladder family. Ir4Ge5 is identified as a likely candidate, and Ru2Sn3 was shown to have novel, quasi one-dimensional surface states. The exact reason for the existence of these states is not known and is under investigation. Finally, possible 3D Dirac and Weyl semi-metals were investigated. A set of rules to predict 3D Dirac semi-metals were developed, and Cd3 As2 was experimentally verified as the first of this kind of material. Studies towards Weyl semi-metals involved the

  7. Green Synthesis, Characterization, and Application of Metal-based Nanomaterials

    Science.gov (United States)

    Lewis, Crystal Shenandoa

    Metal-based nanomaterials have attracted significant research interest due to their unique size-dependent optical, magnetic, electronic, thermal, mechanical, and chemical properties as compared with their bulk counterparts. These advantageous and tailorable properties render these materials as ideal candidates for catalysis, photovoltaics, and even biomedical applications. However, nanomaterials are typically synthesized via chemical or physical processes, which are continuing to rise in cost, complexity, and toxicity. As a result, 'milder' and more environmentally benign nanoscale synthetic methodologies, particularly U-tube double diffusion, molten salt, and hydrothermal techniques, have been utilized to mitigate for these drawbacks. Moreover, these efficient and facile techniques coupled with the unique attributes of nanomaterials will aid in a more practical translation from the lab scale to industry with potential applications spanning from electronics, energy, to medicine. In this thesis, we will discuss the sustainable synthesis of crystalline elemental copper (Cu), nickel (Ni), magnetic spinel ferrites (MFe2O 4 wherein M is Co, Ni, or Zn), rare earth ion doped-calcium titanate (RE-CaTiO3), and hematite (alpha-Fe2O3) as well as our ability to tailor the size and/or morphology and hence tune their properties for potential applications in solar cells and biomedicine. Specifically, for the Cu and Ni nanowires (NWs), the diameters have been dictated by the various template diameters used in the U-tube double diffusion technique. Subsequently, their photocatalytic properties were observed when coupled with TiO2 NPs. For MFe2O4, RE-CaTiO3, and alpha-Fe2O3 nanostructures, the hydrothermal method was employed wherein various parameters such as reaction temperature, concentration, and addition of surfactant were varied to influence their morphology and/or composition. For example, as the reaction temperature was increased, ultrasmall MFe2O4 particles transformed from

  8. Synthesis and photophysical characterization of stable indium bacteriochlorins.

    Science.gov (United States)

    Krayer, Michael; Yang, Eunkyung; Kim, Han-Je; Kee, Hooi Ling; Deans, Richard M; Sluder, Camille E; Diers, James R; Kirmaier, Christine; Bocian, David F; Holten, Dewey; Lindsey, Jonathan S

    2011-05-16

    Bacteriochlorins have wide potential in photochemistry because of their strong absorption of near-infrared light, yet metallobacteriochlorins traditionally have been accessed with difficulty. Established acid-catalysis conditions [BF(3)·OEt(2) in CH(3)CN or TMSOTf/2,6-di-tert-butylpyridine in CH(2)Cl(2)] for the self-condensation of dihydrodipyrrin-acetals (bearing a geminal dimethyl group in the pyrroline ring) afford stable free base bacteriochlorins. Here, InBr(3) in CH(3)CN at room temperature was found to give directly the corresponding indium bacteriochlorin. Application of the new acid catalysis conditions has afforded four indium bacteriochlorins bearing aryl, alkyl/ester, or no substituents at the β-pyrrolic positions. The indium bacteriochlorins exhibit (i) a long-wavelength absorption band in the 741-782 nm range, which is shifted bathochromically by 22-32 nm versus the analogous free base species, (ii) fluorescence quantum yields (0.011-0.026) and average singlet lifetime (270 ps) diminished by an order of magnitude versus that (0.13-0.25; 4.0 ns) for the free base analogues, and (iii) higher average yield (0.9 versus 0.5) yet shorter average lifetime (30 vs 105 μs) of the lowest triplet excited state compared to the free base compounds. The differences in the excited-state properties of the indium chelates versus free base bacteriochlorins derive primarily from a 30-fold greater rate constant for S(1) → T(1) intersystem crossing, which stems from the heavy-atom effect on spin-orbit coupling. The trends in optical properties of the indium bacteriochlorins versus free base analogues, and the effects of 5-OMe versus 5-H substituents, correlate well with frontier molecular-orbital energies and energy gaps derived from density functional theory calculations. Collectively the synthesis, photophysical properties, and electronic characteristics of the indium bacteriochlorins and free base analogues reported herein should aid in the further design of such

  9. Synthesis, Characterization, and Enhanced Magnetic Properties of Iron Carbide Nanomaterials

    Science.gov (United States)

    Williams, Brent M.

    Permanent magnets are classified as hard magnetic materials with the main purpose of generating flux for applications such as electric motors, turbines, and hard drives. High coercivity, magnetic remanence, and saturation values with high stability are some of the requirements for permanent magnets. Rare-earth magnets including neodymium and samarium based magnets are known to have superior magnetic properties due to their high magnetocrystalline anisotropy. However, due to the price of rare-earth materials development of alternate permanent magnets composed of inexpensive materials is an ongoing process. Previously cobalt carbide (CoxC) have shown promise as a potential rare-earth free magnet alternative with magnetic properties comparable to that of hexaferrite materials. Unfortunately, CoxC magnets have a low magnetic saturation (50 emu g-1) which drastically lowers its energy product. Alternatively, iron carbide has a rather high bulk magnetization value of 140 emu g-1 and is composed of naturally abundant materials. The sole issue of iron carbide is that it is considered an intermediate magnet with properties between those of a hard and a soft magnetic material. The main focus of this work is the enhancement of the hard magnetic properties of iron carbide through size effect, shape anisotropy, magnetocrystalline anisotropy and exchange anisotropy. First a wet synthesis method was developed which utilized hexadecyltrimethylammonium chloride to control particle size, shape, and crystal structure to manipulate the magnetic properties of iron carbide. With this method a semi-hard 50 nm orthorhombic Fe3C phase and a magnetically soft single crystal hexagonal Fe7C3 structure with texture-induced magnetic properties were developed. The properties for both materials were further enhanced through formation of exchange bias Fe3C/CoO nanoaggregates and spring exchange coupling of the ferromagnetically hard and soft phases of Fe7C3/SrFe 12O19. A 33% increase in coercivity

  10. Nanomanufacturing of silica nanowires: Synthesis, characterization and applications

    Science.gov (United States)

    Sekhar, Praveen Kumar

    In this research, selective and bottom-up manufacturing of silica nanowires on silicon (Si) and its applications has been investigated. Localized synthesis of these nanowires on Si was achieved by metal thin film catalysis and metal ion implantation based seeding approach. The growth mechanism of the nanowires followed a vapor-liquid-solid (VLS) mechanism. Mass manufacturing aspects such as growth rate, re-usability of the substrate and experimental growth model were also investigated. Further, silica nanowires were explored as surface enhanced Raman (SER) substrate and immunoassay templates towards optical and electrochemical detection of cancer biomarkers respectively. Investigating their use in photonic applications, optically active silica nanowires were synthesized by erbium implantation after nanowire growth and implantation of erbium as a metal catalyst in Si to seed the nanowires. Ion implantation of Pd in Si and subsequent annealing in Ar at 1100 0 C for 60 mins in an open tube furnace resulted in silica nanowires of diameters ranging from 15 to 90 nm. Similarly, Pt was sputtered on to Si and further annealed to obtain silica nanowires of diameters ranging from 50 to 500 nm. Transmission electron microscopy studies revealed the amorphous nature of the wires. In addition, nano-sized Pd catalyst was found along the body of the nanowires seeded by Pd implantation into Si. After functionalization of the wires with 3 - AminoPropylTriMethoxySilane (APTMS), the Pd decorated silica nanowires served as an SER substrate exhibiting a sensitivity of 10 7 towards the detection of interleukin-10 (IL-10, a cancer biomarker) with higher spatial resolution. Voltammetric detection of IL-10 involved silica nanowires synthesized by Pd thin film catalysis on Si as an immunoassay template. Using the electrochemical scheme, the presence of IL-10 was detected down to 1fg/mL in ideal pure solution and 1 pg/mL in clinically relevant samples. Time resolved photoluminescence (PL

  11. Synthesis, characterization, and properties of reduced europium molybdates and tungstates

    Energy Technology Data Exchange (ETDEWEB)

    Abeysinghe, Dileka [Department of Chemistry and Biochemistry, University of South Carolina, Columbia, SC 29208 (United States); Gerke, Birgit [Institut für Anorganische und Analytische Chemie, Universität Münster , Corrensstrasse 30, Münster D-48149 (Germany); Morrison, Gregory; Hsieh, Chun H.; Smith, Mark D. [Department of Chemistry and Biochemistry, University of South Carolina, Columbia, SC 29208 (United States); Pöttgen, Rainer [Institut für Anorganische und Analytische Chemie, Universität Münster , Corrensstrasse 30, Münster D-48149 (Germany); Makris, Thomas M. [Department of Chemistry and Biochemistry, University of South Carolina, Columbia, SC 29208 (United States); Loye, Hans-Conrad zur, E-mail: zurloye@mailbox.sc.edu [Department of Chemistry and Biochemistry, University of South Carolina, Columbia, SC 29208 (United States)

    2015-09-15

    Single crystals of K{sub 0.094}Eu{sub 0.906}MoO{sub 4}, K{sub 0.097}Eu{sub 0.903}WO{sub 4}, EuWO{sub 4}, and EuMoO{sub 4} were grown from molten chloride fluxes contained in vacuum-sealed fused silica and structurally characterized via single crystal X-ray diffraction. The in situ reduction of Eu{sup 3+} to Eu{sup 2+} was carried out using Mo, W, and Zn as metal reducing agents. All four compounds crystallize in the tetragonal space group of I4{sub 1}/a and adopt the scheelite (CaWO{sub 4}) structure type. The magnetic susceptibility of the reported compounds shows paramagnetic behavior down to 2 K. {sup 151}Eu Mössbauer spectroscopy was used to analyze the relative Eu{sup 2+} and Eu{sup 3+} content of the samples. All the compounds were further characterized by EPR, and UV-vis spectroscopy. - Graphical abstract: TOC Caption Two new reduced europium containing quaternary oxides, K{sub 0.094}Eu{sub 0.906}MoO{sub 4} and K{sub 0.097}Eu{sub 0.903}WO{sub 4}, and two previously reported ternary reduced oxides, EuWO{sub 4} and EuMoO{sub 4}, were synthesized via an in situ reduction of Eu{sup 3+} to Eu{sup 2+} under flux method using Mo, W, and Zn as metal reducing agents. {sup 151}Eu Mössbauer spectroscopy was used to analyze the relative Eu{sup 2+} and Eu{sup 3+} content of the samples. - Highlights: • K{sub 0.094}Eu{sub 0.906}MoO{sub 4}, K{sub 0.097}Eu{sub 0.903}WO{sub 4}, EuWO{sub 4}, and EuMoO{sub 4} have been synthesized and characterized. • The in situ reduction of Eu{sup 3+} to Eu{sup 2+} was carried out using Mo, W, and Zn as metal reducing agents. • Magnetic susceptibility data were collected. • {sup 151}Eu Mössbauer spectroscopy was used to analyze Eu{sup 2+} and Eu{sup 3+} content.

  12. Synthesis, characterization and properties of hollow nickel phosphide nanospheres

    Energy Technology Data Exchange (ETDEWEB)

    Ni Yonghong; Tao Ali; Hu Guangzhi; Cao Xiaofeng; Wei Xianwen; Yang Zhousheng [College of Chemistry and Materials Science, Anhui Key Laboratory of Functional Molecular Solids, Anhui Normal University, Wuhu 241000 (China)

    2006-10-14

    Nickel phosphide (Ni{sub 12}P{sub 5}) hollow nanospheres with a mean diameter of 100 nm and a shell thickness of 15-20 nm have been successfully prepared by a hydrothermal-microemulsion route, using NaH{sub 2}PO{sub 2} as a phosphorus source. XRD, EDS (HR)TEM, SEM and the SAED pattern were used to characterize the final product. Experiments showed that the as-prepared nickel phosphide hollow nanospheres could selectively catalytically degrade some organic dyes such as methyl red and Safranine T under 254 nm UV light irradiation. At the same time, the nickel phosphide hollow nanospheres showed a stronger ability to promote electron transfer between the glass-carbon electrode and adrenalin than nickel phosphide honeycomb-like particles prepared by a simple hydrothermal route. A possible formation process for nickel phosphide hollow nanospheres was suggested based on the experimental results.

  13. Synthesis and preliminary characterization of octakis (chloropropyldimethylsiloxy octasilsesquioxane

    Directory of Open Access Journals (Sweden)

    Devaney Ribeiro do Carmo

    2004-09-01

    Full Text Available Octakis (hydridodimethylsiloxy octasilsesquioxane was hydrosilated with allyl chloride using Spiers catalyst (H2PtCl6. This reaction was monitored using FT-IR spectroscopy. The synthesized product was characterized by 13C, 29Si NMR (MAS, SEM, FT-IR, Thermogravimetric techniques. The three propyl groups alpha, beta, gamma, (to the terminal silicon atom, associated of an allyl chloride, were clearly seen in the 13C NMR (alpha-CH2 at 31.8; beta-CH2 at 37.7; gamma-CH2 at 50.1 ppm. In addition, the 29Si NMR spectrum of the final product, exhibits three Q signals for Q type silicon attributed to Q² (-90.1 Q³ (-100.2 and Q4 (-111.3ppm. The presence of allyl chloride substitutes in octameric cube confers a relative porosity and thermal stability to the material.

  14. SYNTHESIS, CHARACTERIZATION AND CRYSTAL STRUCTURE OF BIS-(2-HYDROXYBENZALDEHYDEDIAMINOGUANIZONE

    Directory of Open Access Journals (Sweden)

    Diana Dragancea, Vladimir B. Arion, Sergiu Shova

    2008-12-01

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

  15. Synthesis and characterization of copper(II) complexes of semicarbazones

    Science.gov (United States)

    Chandra, Usha; Chandra, Sulekh

    1992-08-01

    Copper(II) complexes of the general composition Cu(ligand) 2X 2 (where X=CI -, Br -, NO -3, ClO -4 and 1/2 SO 2-4) and Cu(ligand) (CH 3COO) 2 have been synthesized with methyl n-pentyl ketone and methyl n-hexyl ketone semicarbazones. All the complexes prepared have been characterized by elemental analysis, magnetic moment, molar conductance, IR, electronic and electron spin resonance spectral studies. The complexes Cu(ligand) 2X 2 (X = Cl -, Br -, NO -3) and Cu(ligand) (CH 3COO) 2 may have tetragonal geometry, while the complexes Cu(ligand) 2X 2 (X = ClO -4 and 1/2 SO 2-4) may be assigned a five-coordinated trigonally distorted square pyramidal geometry.

  16. Superparamagnetic bimetallic iron-palladium nanoalloy: synthesis and characterization

    Energy Technology Data Exchange (ETDEWEB)

    Nazir, Rabia; Mazhar, Muhammad [Department of Chemistry, Quaid-i-Azam University, Islamabad 45320 (Pakistan); Akhtar, M Javed; Nadeem, M; Siddique, Muhammad [Physics Division, PINSTECH, PO Nilore, Islamabad 44000 (Pakistan); Shah, M Raza [HEJ Research Institute of Chemistry, University of Karachi, Karachi 75270 (Pakistan); Khan, Nawazish A [Material Science Laboratory, Department of Physics, Quaid-i-Azam University, Islamabad 45320 (Pakistan); Mehmood, Mazhar [National Centre for Nanotechnology, PIEAS, Islamabad 45650 (Pakistan); Butt, N M [Pakistan Science Foundation, Islamabad 44000 (Pakistan)], E-mail: mazhar42pk@yahoo.com

    2008-05-07

    Iron-palladium nanoalloy in the particle size range of 15-30 nm is synthesized by the relatively low temperature thermal decomposition of coprecipitated [Fe(Bipy){sub 3}]Cl{sub 2} and [Pd(Bipy){sub 3}]Cl{sub 2} in an inert ambient of dry argon gas. The silvery black Fe-Pd alloy nanoparticles are air-stable and have been characterized by EDX-RF, XRD, AFM, TEM, magnetometry, {sup 57}Fe Moessbauer and impedance spectroscopy. This Fe-Pd nanoalloy is in single phase and contains iron sites having up to 11 nearest-neighboring atoms. It is superparamagnetic in nature with high magnetic susceptibility, low coercivity and hyperfine field.

  17. Synthesis and characterization of barium fluoride substituted zinc tellurite glasses

    Science.gov (United States)

    Aishwarya, K.; Vinitha, G.; Varma, G. Sreevidya; Asokan, S.; Manikandan, N.

    2017-12-01

    Glasses in the TeO2-ZnO-BaF2 system were prepared by standard melt quenching technique and were characterized for their thermal, optical and structural properties. Samples were found to show good thermal stability with values ranging above 100 °C for all the compositions. Optical bandgap and refractive index values were calculated from linear optical measurements using UV-Vis spectroscopy. Infrared spectra showed the presence of hydroxyl groups in the glasses indicating that the effect of fluorine was negligible in removing the hydroxyl impurities for the experimental conditions and compositions used. Raman measurements showed the modification occurring in the glass network due to addition of barium fluoride in terms of increase in the formation of non-bridging oxygen atoms compared to strong Te-O-Te linkages in the glass matrix.

  18. ZnO nanofluids: Green synthesis, characterization, and antibacterial activity

    Energy Technology Data Exchange (ETDEWEB)

    Jalal, Razieh [Dept. of Chemistry, Ferdowsi University of Mashhad, Mashhad 91779 Mashhad (Iran, Islamic Republic of); Goharshadi, Elaheh K., E-mail: gohari@ferdowsi.um.ac.ir [Dept. of Chemistry, Ferdowsi University of Mashhad, Mashhad 91779 Mashhad (Iran, Islamic Republic of); Center of Nano Research, Ferdowsi University of Mashhad (Iran, Islamic Republic of); Abareshi, Maryam [Dept. of Chemistry, Ferdowsi University of Mashhad, Mashhad 91779 Mashhad (Iran, Islamic Republic of); Moosavi, Majid [Dept. of Chemistry, Faculty of Sciences, University of Isfahan, Isfahan 81746-73441 (Iran, Islamic Republic of); Yousefi, Abbas [Pare-Tavous Research Institute, Mashhad (Iran, Islamic Republic of); Nancarrow, Paul [QUILL Research Centre and School of Chemistry and Chemical Engineering, Queen' s University Belfast (United Kingdom)

    2010-05-15

    Zinc oxide nanoparticles have been synthesized by microwave decomposition of zinc acetate precursor using an ionic liquid, 1-butyl-3-methylimidazolium bis(trifluoromethylsulfonyl) imide, [bmim][NTf{sub 2}] as a green solvent. The structure and morphology of ZnO nanoparticles have been characterized using X-ray diffraction and transmission electron microscopy. The ZnO nanofluids have been prepared by dispersing ZnO nanoparticles in glycerol as a base fluid in the presence of ammonium citrate as a dispersant. The antibacterial activity of suspensions of ZnO nanofluids against (E. coli) has been evaluated by estimating the reduction ratio of the bacteria treated with ZnO. Survival ratio of bacteria decreases with increasing the concentrations of ZnO nanofluids and time. The results show that an increase in the concentrations of ZnO nanofluids produces strong antibacterial activity toward E. coli.

  19. Synthesis and characterization of lanthanum doped zinc oxide nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Kumar, Vinod; Sonia,; Suman,; Kumar, Sacheen, E-mail: sacheen3@gmail.com; Kumar, Dinesh [Department of Electronics science, Kurukshetra University, Kurukshetra, Haryana, India-136119 (India)

    2016-05-06

    La doped ZnO (Zn{sub 1-x}La{sub x}O, 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–Visible spectrophotometer. 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.

  20. Synthesis and characterization of electrical conducting chitosan-graft-polyaniline

    Directory of Open Access Journals (Sweden)

    2007-05-01

    Full Text Available A mucopolysaccharide, chitosan was grafted with polyaniline through oxidative-radical copolymerization using ammonium persulfate in acidic medium. The grafting conditions were extensively studied by varying grafting parameters. All the findings have been discussed and proposed a plausible mechanism for the graft copolymerization. The representative chitosan-graft-polyaniline (Ch-g-PANI was characterized using UV-vis, FTIR, TGA, X-ray diffraction and Scanning electron microscopy taking chitosan as reference. Ch-g-PANI exhibited electrical conductivity, which increases with the extent of grafting onto chitosan backbone. Its electrical conductivity is further influenced by pH and showed pH switching electrical conduction behavior when exposed to NN3/HCl vapors. The application of conducting biomaterial such as Ch-g-PANI in the electronic devices especially for the fabrication of sensor devices would be attractive not only in terms of product cost and environmental safety but also from a materials science point of view.

  1. Synthesis and characterization of gold nanoparticles using Ficus religiosa extract

    Directory of Open Access Journals (Sweden)

    Kirtee Wani

    2013-03-01

    Full Text Available We report a cost effective and eco-friendly biosynthesis of gold nanoparticles (F-AuNPs using aqueous extract of Ficus religiosa as the reducing and stabilizing agent. These nanoparticles were characterized by various techniques such as UV-Vis, XRD, TEM and FTIR. The characteristic surface plasmon peak was observed at 540 nm while XRD analysis suggested it to be a face-centered cubic (fcc structure with peaks at 38.06, 44.46, 64.75 and 77.56. FTIR studies indicated the capping of the nanoparticles with polyphenols, amines and carboxylates present in the extract of Ficus religiosa whereas TEM analysis showed spherical morphology with other shapes such as triangles and hexagons. The F-AuNPs were found to be non-toxic to HEK 293 cells, thereby suggesting their potential application in the field of nanobiotechnology.

  2. Synthesis, Characterization and Photophysical Studies of Tricoumarin-Pyridines.

    Science.gov (United States)

    Naik, Nirmala S; Shastri, Lokesh A; Bathula, Chinna; Chougala, Bahubali; Shastri, Samundeeswari; Holiyachi, Megharaja; Sunagar, Vinay

    2017-03-01

    A series of novel tricoumarin-pyridines have been synthesized by the reaction of 4-formyl coumarins and substituted 3-acetylcoumarin with ammonium acetate for the application in organic electronics as well as fluorescent dyes. The structures of all new compounds were confirmed and characterized by IR, (1)H NMR and ESI-Mass analysis. All the important photo physical prerequisites for organic electronic application such as strong and broad optical absorption, thermal stability were determined for the synthesized molecules. Optical properties were studied by UV-Vis absorption and fluorescence spectroscopy. Optical band gaps of the tricoumarin-pyridines were found to be 2.72-3.10 eV as calculated from their onset absorption edge. The tricoumarin-pyridines were thermally stable up to 290-370 °C as determined by thermogravimetric analysis (TGA). Photophysical studies indicate the synthesized materials are promising candidates for organic electronic applications.

  3. Green Synthesis and Characterization of Carbon Nanotubes/Polyaniline Nanocomposites

    Directory of Open Access Journals (Sweden)

    Van Hoa Nguyen

    2015-01-01

    Full Text Available Carbon nanotubes/polyaniline (CNT/PANI nanocomposites were synthesized by the interfacial polymerization of aniline in the presence of CNTs using two green solvents, water and an ionic liquid (1-butyl-3-methylimidazolium tetrafluoroborate, [bmim][BF4], as the two phases. The formation and incorporation of PANI on the surface of the CNTs were confirmed by scanning electron microscopy, transmission electron microscopy, X-ray diffraction, Fourier transform infrared spectroscopy ultraviolet-visible spectroscopy, and X-ray photoelectron spectroscopy. The analyses showed that the surface of the CNTs was coated with different morphologies of thin PANI layers depending on whether a HCl or HNO3 solution was used. The thermal stability of the composites was much better than that of the bare CNTs and pure PANI. The as-prepared composites were also used to modify the nickel foam electrodes for characterization of the electrochemical properties.

  4. Synthesis, characterization and photoinduced curing of polysulfones with (methacrylate functionalities

    Directory of Open Access Journals (Sweden)

    Cemil Dizman

    2010-06-01

    Full Text Available The UV-curable telechelic polysulfones with (methacrylate functionalities were synthesized by condensation polymerization and subsequent esterification. The final polymers and intermediates at various stages were characterized by 1H NMR, FT-ATR, and GPC. The oligomeric films prepared from the appropriate solutions containing these telechelics and 2,2-dimethoxy-2-phenylacetophenone (DMPA as the photoinitiator undergo rapid polymerization upon irradiation forming insoluble networks. The photo-curing behavior was investigated by photo-DSC and the effects of the molecular weight of the polysulfone precursor and type of functionality on the rate of polymerization and conversion were evaluated. Thermal properties of the photochemically cured films were studied by differential scanning calorimeter (DSC and thermal gravimetric analysis (TGA.

  5. Synthesis and characterization of new soluble polyamides from Acenaphtohydrazinomercaptotriazole diamine

    Directory of Open Access Journals (Sweden)

    Hossein Mighani

    2015-08-01

    Full Text Available AbstractA diamine Acenaphtohydrazinomercaptotriazole (AHTD was synthesized in one step from acenaphthoqinone and 4-amino-3-hydrazino-5-mercapto-1,2,4-triazole. The diamin was characterized by FTIR, 1HNMR, 13CNMR and melting point. Diamin was used to prepare novel polyamides. The low temperature solution polycondensation of diamin with tow aromatic and tow aliphatic diacid chlorides afforded diamin-containing polyamides with inherent viscosities of 0.38–0.47 dl/g in DMF at 25 °C. The polyamides were generally soluble in a wide range of solvents such as dimethylformamide(DMF, N-Methylpyrolidone(NMP, tetrachloroethane (TCE, dimethylsulfoxide(DMSO and H2SO4. Thermal analysis showed that these polyamides were practically crustily and with Tg under 100 °C.

  6. Al-doped ZnO nanofilms: Synthesis and characterization

    Energy Technology Data Exchange (ETDEWEB)

    Huczko, A.; Dabrowska, A. [Department of Chemistry, Warsaw University, Warsaw (Poland); Madhup, D.K. [Department of Physics, Kathmandu University, Dhulikhel (Nepal); College of Biomedical Engineering and Applied Sciences, Hadigaun, Kathmandu (Nepal); Subedi, D.P.; Chimouriya, S.P. [Department of Physics, Kathmandu University, Dhulikhel (Nepal)

    2010-12-15

    Al-doped and un-doped ZnO nanofilms on quartz substrate were obtained by ultrasonic spray pyrolysis of salt solutions (mole concentration of Al within 0-10%). The films were characterized by Scanning electron microscopy (SEM), X-ray diffraction (XRD), Atomic force microscopy (AFM) and UV spectroscopy to study the morphology and optical properties. The optical studies showed that the increase in Al within ZnO thin layer increases its band gap energy. The obtained value of band gap energy is very close to the determined oscillation energy. However, the dispersion energy is nearly half of band gap energy value. (Copyright copyright 2010 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  7. Synthesis and Characterization of the Actinium Aquo Ion.

    Science.gov (United States)

    Ferrier, Maryline G; Stein, Benjamin W; Batista, Enrique R; Berg, John M; Birnbaum, Eva R; Engle, Jonathan W; John, Kevin D; Kozimor, Stosh A; Lezama Pacheco, Juan S; Redman, Lindsay N

    2017-03-22

    Metal aquo ions occupy central roles in all equilibria that define metal complexation in natural environments. These complexes are used to establish thermodynamic metrics (i.e., stability constants) for predicting metal binding, which are essential for defining critical parameters associated with aqueous speciation, metal chelation, in vivo transport, and so on. As such, establishing the fundamental chemistry of the actinium(III) aquo ion (Ac-aquo ion, Ac(H 2 O) x 3+ ) is critical for current efforts to develop 225 Ac [ t 1/2 = 10.0(1) d] as a targeted anticancer therapeutic agent. However, given the limited amount of actinium available for study and its high radioactivity, many aspects of actinium chemistry remain poorly defined. We overcame these challenges using the longer-lived 227 Ac [ t 1/2 = 21.772(3) y] isotope and report the first characterization of this fundamentally important Ac-aquo coordination complex. Our X-ray absorption fine structure study revealed 10.9 ± 0.5 water molecules directly coordinated to the Ac III cation with an Ac-O H2O distance of 2.63(1) Å. This experimentally determined distance was consistent with molecular dynamics density functional theory results that showed (over the course of 8 ps) that Ac III was coordinated by 9 water molecules with Ac-O H2O distances ranging from 2.61 to 2.76 Å. The data is presented in the context of other actinide(III) and lanthanide(III) aquo ions characterized by XAFS and highlights the uniqueness of the large Ac III coordination numbers and long Ac-O H2O bond distances.

  8. 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.

  9. Synthesis and characterization of agar-based silver nanoparticles and nanocomposite film with antibacterial applications.

    Science.gov (United States)

    Shukla, Mahendra K; Singh, Ravindra Pal; Reddy, C R K; Jha, Bhavanath

    2012-03-01

    This study describes the synthesis and characterization of silver nanoparticles and nanocomposite material using agar extracted from the red alga Gracilaria dura. Characterization of silver nanoparticles was carried out based on UV-Vis spectroscopy (421 nm), transmission electron microscopy, EDX, SAED and XRD analysis. The thermal stability of agar/silver nanocomposite film determined by TGA and DSC analysis showed distinct patterns when compared with their raw material (agar and AgNO(3)). The TEM findings revealed that the silver nanoparticles synthesized were spherical in shape, 6 nm in size with uniform dispersal. The synthesized nanoparticles had the great bactericidal activity with reduction of 99.9% of bacteria over the control value. The time required for synthesis of silver nanoparticles was found to be temperature dependent and higher the temperature less the time for nanoparticles formation. DSC and XRD showed approximately the same crystalline index (CI(DSC) 0.73). Copyright © 2011 Elsevier Ltd. All rights reserved.

  10. Synthesis and Characterization of New Photoluminescent Oxadiazole/Carbazole-Containing Polymers

    OpenAIRE

    Simona Concilio; Valeria Bugatti; Pio Iannelli; Stefano Piotto Piotto

    2010-01-01

    We report on the synthesis and the characterization of a new class of segmented polyethers POC containing the oxadiazole and carbazole units. The polymers exhibit a high thermal stability, high glass transition temperatures, and good solubility in common organic solvents, despite the extended aromatic portion in the main polymer chain. The synthetic procedures are simple, and no acid side-products are obtained. According to previous reports on oxadiazole/carbazole-containing materials, POCs s...

  11. Silicon to Nickel Silicide Longitudinal Nanowire Heterostructures: Synthesis, Electrical Characterization and Novel Devices

    OpenAIRE

    Weber, Walter Michael

    2009-01-01

    The scope of this thesis is the synthesis and electrical characterization of Si to Ni silicide nanowire heterostructures with the focus on investigating their electronic transport properties and conceiving a novel type of transistor. Intrinsic Si nanowires (SiNW) were grown employing the vapor-liquid-solid mechanism. A central part of this thesis is the development of the longitudinal intrusion of Ni silicide into the SiNWs resulting in interfaces with a sharpness of at most a couple of n...

  12. SYNTHESIS AND CHARACTERIZATION OF METALLIC COPPER NANOPARTICLES VIA THERMAL DECOMPOSITION METHOD

    OpenAIRE

    A. Dinesh Karthik; Dr. K. Geetha

    2017-01-01

    Copper (II) fumarate was used as a precursor to prepare metallic copper nanoparticles by thermal decomposition. Synthesis of inorganic nanoparticles by thermal decomposition is one of the methods to produce stable nanodisperse suspensions with the ability of self assembly. Copper (II) fumarate precursor was treated with oleylamine which is used as both the medium and the Stabilizing reagent. The precursor and copper nanoparticles were characterized by UV-Vis Spectroscopy, FT - IR, XRD, CV, AF...

  13. Bio-Nano Interactions : Synthesis, Functionalization and Characterization of Biomaterial Interfaces

    OpenAIRE

    Cai, Yixiao

    2016-01-01

    Current strategies for designing biomaterials involve creating materials and interfaces that interact with biomolecules, cells and tissues.  This thesis aims to investigate several bioactive surfaces, such as nanocrystalline diamond (NCD), hydroxyapatite (HA) and single crystalline titanium dioxide, in terms of material synthesis, surface functionalization and characterization. Although cochlear implants (CIs) have been proven to be clinically successful, the efficiency of these implants stil...

  14. Synthesis, Characterization, and Biological Activity of Nickel (II) and Palladium (II) Complex with Pyrrolidine Dithiocarbamate (PDTC)

    OpenAIRE

    Sk Imadul Islam; Suvendu Bikash Das; Sutapa Chakrabarty; Sudeshna Hazra; Akhil Pandey; Animesh Patra

    2016-01-01

    The synthesis of square planar Ni(II) and Pd(II) complexes with pyrrolidine dithiocarbamate (PDTC) was characterized by elemental, physiochemical, and spectroscopic methods. Two complexes were prepared by the reaction of nickel acetate and palladium acetate with pyrrolidine dithiocarbamate (PDTC) in 1 : 2 molar ratio. The bovine serum albumin (BSA) interaction with complexes was examined by absorption and fluorescence spectroscopic techniques at pH 7.4. All the spectral data suggest that coor...

  15. Synthesis And Characterization Of Zinc Oxide Nanoparticles-based Dental Cement

    OpenAIRE

    Nofrizal; Prihantini, Ardini; Nugroho, Dwi Wahyu; R., Tito Prastyo; Ikono, Radyum; W., Wahyu Bambang; Sukarto, Agus; Siswanto; Rochman, Nurul Taufiqu

    2012-01-01

    Dental cement-based mixture of zinc oxide and eugenol is one of the commonly used dental cement. One of the major shortcomings that limit its application is dental cement zinc oxide and eugenol has detrimental mechanical properties. This study aims to carry out the synthesis and characterization of nano-based dental cement of zinc oxide mixed with eugenol with the hypothesis that zinc oxide nanoparticles will provide better mechanical properties. Physical and mechanical properties of cement-b...

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

    DEFF Research Database (Denmark)

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

    2014-01-01

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

  17. Synthesis and Characterization of Thin Film Lithium-Ion Batteries Using Polymer Electrolytes

    Science.gov (United States)

    Maranchi, Jeffrey P.; Kumta, Prashant N.; Hepp, Aloysius F.; Raffaelle, Ryne P.

    2002-01-01

    The present paper describes the integration of thin film electrodes with polymer electrolytes to form a complete thin film lithium-ion battery. Thin film batteries of the type, LiCoO2 [PAN, EC, PC, LiN(CF3SO2)2] SnO2 have been fabricated. The results of the synthesis and characterization studies will be presented and discussed.

  18. Ultrafine Magnetite Nanopowder: Synthesis, Characterization, and Preliminary Use as Filler of Polymethylmethacrylate Nanocomposites

    OpenAIRE

    Pietro Russo; Domenico Acierno; Mariano Palomba; Gianfranco Carotenuto; Roberto Rosa; Antonino Rizzuti; Cristina Leonelli

    2012-01-01

    Magnetite (Fe3O4) nanoparticles prepared by microwave-assisted hydrothermal synthesis have been characterized in terms of morphological and structural features. Electron micrographs collected in both scanning (SEM) and transmission (TEM) modes and evaluations of X-ray powder diffraction (XRD) patterns have indicated the achievement of a monodispersed crystallite structure with particles having an average size around 15–20 nm. Structural investigations by Micro-Raman spectroscopy highlighted t...

  19. Synthesis and Characterization of Rhenium(V) Oxo Complexes Bearing PNP-Pincer Ligands

    NARCIS (Netherlands)

    Korstanje, Ties J.; Lutz, Martin; Jastrzebski, Johann T. B. H.; Klein Gebbink, Bert

    2014-01-01

    The synthesis of a series of pyridine-based PNP-pincer rhenium-oxo complexes, with phenyl (1, 3), tertbutyl (2), or cyclohexyl (4) groups on the phosphorus atoms and either a ReO2X (1, 2) or a ReCl2O (3, 4) core is reported. The structures of these compounds were characterized using H-1, C-13, and

  20. Studies on n-butyl nitroxyethylnitramine (n-buNENA): Synthesis, characterization and propellant evaluations

    Energy Technology Data Exchange (ETDEWEB)

    Rao, Kala P.C.; Sikder, Aarun K.; Kulkarni, Mahadev A.; Bhalerao, Melind M.; Gandhe, Balkrishna R. [High Energy Materials Research Laboratory, Pune 411 021 (India)

    2004-04-01

    The laboratory synthesis of the energetic plasticizer n-buNENA was scaled up to one kg batch size and the compound was fully characterized by spectral data and elemental analysis. N-buNENA was formulated with CMDB and EDB propellant compositions. The results showed an improvement in mechanical properties and burning rate over a wide range of pressure along with acceptable limits of hazard and thermal stability as compared to DEP based propellant systems. (Abstract Copyright [2004], Wiley Periodicals, Inc.)

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

    OpenAIRE

    M. Jannathul Firdhouse; P. Lalitha

    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...

  2. Lewis-acid-promoted stoichiometric and catalytic oxidations by manganese complexes having cross-bridged cyclam ligand: a comprehensive study.

    Science.gov (United States)

    Dong, Lei; Wang, Yujuan; Lv, Yanzong; Chen, Zhuqi; Mei, Fuming; Xiong, Hui; Yin, Guochuan

    2013-05-06

    Redox-inactive metal ions have been recognized to be able to participate in redox metal-ion-mediated biological and chemical oxidative events; however, their roles are still elusive. This work presents how the redox-inactive metal ions affect the oxidative reactivity of a well-investigated manganese(II) with its corresponding manganese(IV) complexes having cross-bridged cyclam ligand. In dry acetone, the presence of these metal ions can greatly accelerate stoichiometric oxidations of triphenylphosphine and sulfides by the manganese(IV) complexes through electron transfer or catalytic sulfoxidations by the corresponding manganese(II) complexes with PhIO. Significantly, the rate enhancements are highly Lewis-acid strength dependent on added metal ions. These metal ions like Al(3+) can also promote the thermodynamic driving force of the Mn(IV)-OH moiety to facilitate its hydrogen abstraction from ethylbenzene having a BDE(CH) value of 85 kcal/mol, while it is experimentally limited to 80 kcal/mol for Mn(IV)-OH alone. Adding Al(3+) may also improve the manganese(II)-catalyzed olefin epoxidation with PhIO. However, compared with those in electron transfer, improvements in hydrogen abstraction and electron transfer are minor. The existence of the interaction between Lewis acid and the manganese(IV) species was evidenced by the blue shift of the characteristic absorbance of the manganese(IV) species from 554 to 537 nm and by converting its EPR signal at g = 2.01 into a hyperfine 6-line signal upon adding Al(3+) (I = 5/2). Cyclic voltammograms of the manganese(IV) complexes reveal that adding Lewis acid would substantially shift its potential to the positive direction, thus enhancing its oxidizing capability.

  3. Synthesis and characterization of carbon-coated cobalt ferrite nanoparticles

    Science.gov (United States)

    Bakhshi, Hamed; Shokuhfar, Ali; Vahdati, Nima

    2016-09-01

    Cobalt ferrite nanoparticles (CFNPs) were prepared via a reverse micelle method. The CFNPs were subsequently coated with carbon shells by means of thermal chemical vapor deposition (TCVD). In this process, acetylene gas (C2H2) was used as a carbon source and the coating was carried out for 1, 2, or 3 h at 750°C. The Ar/C2H2 ratio was 10:1. Heating during the TCVD process resulted in a NP core size that approached 30 nm; the thickness of the shell was less than 10 nm. The composition, structure, and morphology of the fabricated composites were characterized using X-ray diffraction, simultaneous thermal analysis, transmission electron microscopy, high-resolution transmission electron microscopy, and selected-area diffraction. A vibrating sample magnetometer was used to survey the samples' magnetic properties. The deposited carbon shell substantially affected the growth and magnetic properties of the CFNPs. Micro-Raman spectroscopy was used to study the carbon coating and revealed that the deposited carbon comprised graphite, multiwalled carbon nanotubes, and diamond- like carbon. With an increase in coating time, the intensity ratio between the amorphous and ordered peaks in the Raman spectra decreased, which indicated an increase in crystallite size.

  4. Sol-Gel Synthesis and Characterization of Nanoparticles

    Directory of Open Access Journals (Sweden)

    S. Ramesh

    2013-01-01

    Full Text Available The nanoparticles have been synthesized by sol-gel technique. X-ray diffraction, scanning electron microscopy, optical absorption spectroscopy, and electron paramagnetic resonance spectroscopy were used to characterize the sample. The X-ray diffraction results indicate the formation of nanocrystalline materials in tetragonal lattice with P42/nnm space group. The identical distribution of elements were confirmed by scanning electron microscopy with energy dispersive X-ray spectrometry and X-ray mapping. Electron paramagnetic resonance lineshapes of the samples are obtained at various (13 K, 77 K, and 300 K temperatures. The isotropic lineshapes of the sample B1 are attributed to dipole-dipole interaction of Ti3+ ions. The incorporation of Al3+ ions into the sample B2–B5 the isotropic nature of the lineshapes are collapsed due to the distraction in crystal field. Optical absorption spectra results reveal the presence of Ag-TiO2 nanoparticles.

  5. Synthesis, characterization and antimicrobial activity of important heterocyclic acrylic copolymers

    Directory of Open Access Journals (Sweden)

    2008-10-01

    Full Text Available The acrylate monomer, 7-acryloyloxy-4-methyl coumarin (AMC has been synthesized by reacting 7-hydroxy-4-methyl coumarin, with acryloyl chloride in the presence of NaOH at 0–5°C. Copolymers of 7-acryloyloxy-4-methyl coumarin (AMC with vinyl acetate (VAc were synthesized in DMF (dimethyl formamide solution at 70±1°C using 2,2′-azobisisobutyronitrile (AIBN as an initiator with different monomer-to-monomer ratios in the feed. The copolymers were characterized by Fourier transform infra red (FTIR spectroscopy. The copolymer composition was evaluated by 1H-NMR (proton nuclear magnetic resonance and was further used to determine reactivity ratios. The monomer reactivity ratios for AMC (M1-VAc (M2 pair were determined by the application of conventional linearization methods such as Fineman-Ross (r1 = 0.6924; r2 = 0.6431, Kelen-Tüdõs (r1 = 0.6776; r2 = 0.6374 and extended Kelen-Tüdõs (r1 = 0.6657; r2 = 0.6256. Thermo gravimetric analysis showed that thermal decomposition of the copolymers occurred in single stage in the temperature range of 263–458°C. The molecular weights of the polymers were determined using gel permeation chromatography. The homo and copolymers were tested for their antimicrobial properties against selected microorganisms.

  6. Synthesis and characterization of PIL/pNIPAAm hybrid hydrogels

    Directory of Open Access Journals (Sweden)

    Pfensig Sylvia

    2016-09-01

    Full Text Available In this study, varying amounts of NIPAAm and an ionic liquid (IL, namely 1-vinyl-3-isopropylimidazolium bromide ([ViPrIm]+[Br]−, have been used to synthesize hybrid hydrogels by radical emulsion polymerization. Amounts of 70/30%, 50/50%, 30/70%, 15/85% and 5/95% (wt/wt of PIL/pNIPAAm were used to produce hybrid hydrogels as well as the parental hydrogels. The adhesive strength was investigated and evaluated for mechanical characterization. Thermal properties of resulting hydrogels have been investigated using differential scanning calorimetry (DSC in a default heating temperature range (heating rate 10 K min−1. The presence of poly ionic liquids (PIL in the polymer matrix leads to a moved LCST (lower critical solution temperature to a higher temperature range for certain hybrid hydrogels PIL/pNIPAAm. While pNIPAAm exhibits an LCST at 33.9 ± 0.3°C, PIL/pNIPAAm 5/95% and PIL/pNIPAAm 15/85% were found to have LCSTs at 37.6 ± 0.9°C and 52 ± 2°C, respectively. This could be used for controlled drug release that goes along with increasing body temperature in response to an implantation caused infection.

  7. Synthesis, Characterization, and Anticancer Activity of New Benzofuran Substituted Chalcones

    Directory of Open Access Journals (Sweden)

    Demet Coşkun

    2016-01-01

    Full Text Available Benzofuran derivatives are of great interest in medicinal chemistry and have drawn considerable attention due to their diverse pharmacological profiles including anticancer activity. Similarly, chalcones, which are common substructures of numerous natural products belonging to the flavonoid class, feature strong anticancer properties. A novel series of chalcones, 3-aryl-1-(5-bromo-1-benzofuran-2-yl-2-propanones propenones (3a–f, were designed, synthesized, and characterized. In vitro antitumor activities of the newly synthesized (3a–f and previously synthesized (3g–j chalcone compounds were determined by using human breast (MCF-7 and prostate (PC-3 cancer cell lines. Antitumor properties of all compounds were determined by 3-(4,5-dimethylthiazol-2-yl-2,5-diphenyltetrazolium bromide (MTT assay. Cell viability assay for the tested chalcone compounds was performed and the log⁡IC50 values of the compounds were calculated after 24-hour treatment. Our results indicate that the tested chalcone compounds show antitumor activity against MCF-7 and PC-3 cell lines (p<0.05.

  8. Synthesis and characterization of redox-active ferric nontronite

    Energy Technology Data Exchange (ETDEWEB)

    Ilgen, A. G.; Kukkadapu, R. K.; Dunphy, D. R.; Artyushkova, K.; Cerrato, J. M.; Kruichak, J. N.; Janish, M. T.; Sun, C. J.; Argo, J. M.; Washington, R. E.

    2017-10-01

    Heterogeneous redox reactions on clay mineral surfaces control mobility and bioavailability of redox-sensitive nutrients and contaminants. Iron (Fe) residing in clay mineral structures can either catalyze or directly participate in redox reactions; however, chemical controls over its reactivity are not fully understood. In our previous work we demonstrated that converting a minor portion of Fe(III) to Fe(II) (partial reduction) in the octahedral sheet of natural Fe-rich clay mineral nontronite (NAu-1) activates its surface, making it redox-active. In this study we produced and characterized synthetic ferric nontronite (SIP), highlighting structural and chemical similarities and differences between this synthetic nontronite and its natural counterpart NAu-1, and probed whether mineral surface is redox-active by reacting it with arsenic As(III) under oxic and anoxic conditions. We demonstrate that synthetic nontronite SIP undergoes the same activation as natural nontronite NAu-1 following the partial reduction treatment. Similar to NAu-1, SIP oxidized As(III) to As(V) under both oxic (catalytic pathway) and anoxic (direct oxidation) conditions. The similar reactivity trends observed for synthetic nontronite and its natural counterpart make SIP an appropriate analog for laboratory studies. The development of chemically pure analogs for ubiquitous soil minerals will allow for systematic research of the fundamental properties of these minerals.

  9. Synthesis and characterization in AuCu–Si nanostructures

    Energy Technology Data Exchange (ETDEWEB)

    Novelo, T.E., E-mail: tenovelo@hotmail.com [Centro de Investigación en Materiales Avanzados, S.C., Laboratorio Nacional de Nanotecnología, Av. Miguel de Cervantes 120, Complejo Industrial Chihuahua, 31109 Chihuahua, Chihuahua Mexico (Mexico); Amézaga-Madrid, P. [Centro de Investigación en Materiales Avanzados, S.C., Laboratorio Nacional de Nanotecnología, Av. Miguel de Cervantes 120, Complejo Industrial Chihuahua, 31109 Chihuahua, Chihuahua Mexico (Mexico); Maldonado, R.D. [Universidad Anáhuac-Mayab, Carretera Mérida-Progreso Km. 15.5 A.P. 96-Cordemex, CP. 97310 Mérida, Yucatán Mexico (Mexico); Oliva, A.I. [Centro de Investigación y de Estudios Avanzados el IPN Unidad Mérida, Departamento de Física Aplicada, Km 6 Antigua Carretera a Progreso, A.P. 73-Cordemex, 97310 Mérida, Yucatán Mexico (Mexico); Alonzo-Medina, G.M. [Universidad Anáhuac-Mayab, Carretera Mérida-Progreso Km. 15.5 A.P. 96-Cordemex, CP. 97310 Mérida, Yucatán Mexico (Mexico)

    2015-03-15

    Au/Cu bilayers with different Au:Cu concentrations (25:75, 50:50 and 75:25 at.%) were deposited on Si(100) substrates by thermal evaporation. The thicknesses of all Au/Cu bilayers were 150 nm. The alloys were prepared by thermal diffusion into a vacuum oven with argon atmosphere at 690 K during 1 h. X-ray diffraction analysis revealed different phases of AuCu and CuSi alloys in the samples after annealing process. CuSi alloys were mainly obtained for 25:75 at.% samples, meanwhile the AuCuII phase dominates for samples prepared with 50:50 at.%. Additionally, the Au:Cu alloys with 75:25 at.%, produce Au{sub 2}Cu{sub 3} and Au{sub 3}Cu phases. The formed alloys were characterized by scanning electron microscopy (SEM), atomic force microscopy (AFM), transmission electron microscopy (TEM) and energy dispersive spectroscopy (EDS) to study the morphology and the elemental concentration of the formed alloys. - Highlights: • AuCu/Si alloy thin films were prepared by thermal diffusion. • Alloys prepared with 50 at.% of Au produce the AuCuII phase. • Alloys prepared with 75 at.% of Au produce Au{sub 3}Cu and Au{sub 2}Cu{sub 3} phases. • All alloys present diffusion of Si and Cu through the CuSi alloy formation.

  10. Synthesis, structure characterization, and enzyme screening of clenbuterol glucuronides.

    Science.gov (United States)

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

    2009-07-12

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

  11. Cobalt-doped nanohydroxyapatite: synthesis, characterization, antimicrobial and hemolytic studies

    Energy Technology Data Exchange (ETDEWEB)

    Tank, Kashmira P., E-mail: kashmira_physics@yahoo.co.in [Saurashtra University, Crystal Growth Laboratory, Physics Department (India); Chudasama, Kiran S.; Thaker, Vrinda S. [Saurashtra University, Bioscience Department (India); Joshi, Mihir J., E-mail: mshilp24@rediffmail.com [Saurashtra University, Crystal Growth Laboratory, Physics Department (India)

    2013-05-15

    Hydroxyapatite (Ca{sub 10}(PO{sub 4}){sub 6}(OH){sub 2}; HAP) is a major mineral component of the calcified tissues, and it has various applications in medicine and dentistry. In the present investigation, cobalt-doped hydroxyapatite (Co-HAP) nanoparticles were synthesized by surfactant-mediated approach and characterized by different techniques. The EDAX was carried out to estimate the amount of doping in Co-HAP. The transmission electron microscopy result suggested the transformation of morphology from needle shaped to spherical type on increasing the doping concentration. The powder XRD study indicated the formation of a new phase of brushite for higher concentration of cobalt. The average particle size and strain were calculated using Williamson-Hall analysis. The average particle size was found to be 30-60 nm. The FTIR study confirmed the presence of various functional groups in the samples. The antimicrobial activity was evaluated against four organisms Pseudomonas aeruginosa and Shigella flexneri as Gram negative as well as Micrococcus luteus and Staphylococcus aureus as Gram positive. The hemolytic test result suggested that all samples were non-hemolytic. The photoluminescence study was carried out to identify its possible applicability as a fluorescent probe.

  12. Synthesis, characterization and photoluminescence of tin oxide nanoribbons and nanowires

    Energy Technology Data Exchange (ETDEWEB)

    Duraia, El-Shazly M.A., E-mail: duraia_physics@yahoo.co [Suez Canal University, Faculty of Science, Physics Department, Ismailia (Egypt); Al-Farabi Kazakh National University, Almaty (Kazakhstan); Institute of Physics and Technology, 11 Ibragimov Street, 050032 Almaty (Kazakhstan); Mansorov, Z.A. [Al-Farabi Kazakh National University, Almaty (Kazakhstan); Tokmolden, S. [Institute of Physics and Technology, 11 Ibragimov Street, 050032 Almaty (Kazakhstan)

    2009-11-15

    In this work we report the successful formation of tin oxide nanowires and tin oxide nanoribbons with high yield and by using simple cheap method. We also report the formation of curved nanoribbon, wedge-like tin oxide nanowires and star-like nanowires. The growth mechanism of these structures has been studied. Scanning electron microscope was used in the analysis and the EDX analysis showed that our samples is purely Sn and O with ratio 1:2. X-ray analysis was also used in the characterization of the tin oxide nanowire and showed the high crystallinity of our nanowires. The mechanism of the growth of our1D nanostructures is closely related to the vapor-liquid-solid (VLS) process. The photoluminescence PL measurements for the tin oxide nanowires indicated that there are three stable emission peaks centered at wavelengths 630, 565 and 395 nm. The nature of the transition may be attributed to nanocrystals inside the nanobelts or to Sn or O vacancies occurring during the growth which can induce trapped states in the band gap.

  13. Synthesis and characterization of ammonium phosphate fertilizers with boron

    Directory of Open Access Journals (Sweden)

    ANGELA MAGDA

    2010-07-01

    Full Text Available The concentration of boron, an essential micronutrient for plants, presents a narrow range between deficiency and toxicity. In order to provide the boron requirement for plants, and to avoid toxicity problems, boron compounds are mixed with basic fertilizers. Sodium borate pentahydrate was used as a boron source. Ammonium orthophosphates fertilizers with boron were prepared by neutralizing phosphoric acid with ammonia and addition of variable amounts of sodium tetraborate pentahydrate to the reaction mixture at a NH3:H3PO4 molar ratio of 1.5. The fertilizers obtained with boron contents ranging from 0.05 to 1 % (w/w were fully characterized by chemical analysis, thermal analysis, X-ray diffraction and infrared spectrophotometry. The studies showed that up to 500 °C, regardless of the boron content, no significant changes concerning thermal stability and nutritional properties occurred. Above 500 °C, an increase of thermal stability with an increase of the boron content was observed. X-Ray diffraction of a heat-treated sample containing 5 % (w/w boron indicated the appearance of boron orthophosphate, BPO4, as a new crystalline phase, and the disappearance of the previous structures above 500 °C, which explains the increase in thermal stability.

  14. [Synthesis, characterization and study on vibration spectra of potassium triborate].

    Science.gov (United States)

    Zhang, Jin-Ping; Sun, Yong; Yang, Gang; Li, Zuo-Hu

    2007-07-01

    Potassium triborate was synthesized with potassium carbonate and boric acid by controlling suitable feed mixture ratio, reaction temperature and dehydration temperature in the self-designed boiling reactor. According to chemical analysis, the formula of the synthetics was monohydrate potassium triborate (KB3O5 x H2O). It's structure was characterized by XRD, FTIR, Raman and TG, and it was found by XRD analysis that the synthetics was amorphous solid. FTIR and Raman spectroscopy anal-ysis show that three coordination B(3) -O bond, four coordination B(4) -O bond, and hydroxy and triborate anions existed in the formula of the synthetics. Thermogravimetric (TG) analysis show that the groups which can lose mono-water existed in the formula of the synthetics, and structural formula of the synthetics was deduced as K[B3O4 (OH)2]. Vibration spectra of the synthetics were studied, including FTIR and Raman spectroscopy. Vibration absorption peaks of some main groups of the synthetics were investigated, including three coordination B(3) -O bond and four coordination B(4) -O bond that are the main existing forms of boron atoms in the synthetics as well as other groups, and each vibration absorption peak was assigned.

  15. Synthesis, Characterization and Optical Constants of Silicon Oxycarbide

    Directory of Open Access Journals (Sweden)

    Memon Faisal Ahmed

    2017-01-01

    Full Text Available High refractive index glasses are preferred in integrated photonics applications to realize higher integration scale of passive devices. With a refractive index that can be tuned between SiO2 (1.45 and a-SiC (3.2, silicon oxycarbide SiOC offers this flexibility. In the present work, silicon oxycarbide thin films from 0.1 – 2.0 μm thickness are synthesized by reactive radio frequency magnetron sputtering a silicon carbide SiC target in a controlled argon and oxygen environment. The refractive index n and material extinction coefficient k of the silicon oxycarbide films are acquired with variable angle spectroscopic ellipsometry over the UV-Vis-NIR wavelength range. Keeping argon and oxygen gases in the constant ratio, the refractive index n is found in the range from 1.41 to 1.93 at 600 nm which is almost linearly dependent on RF power of sputtering. The material extinction coefficient k has been estimated to be less than 10-4 for the deposited silicon oxycarbide films in the visible and near-infrared wavelength regions. Morphological and structural characterizations with SEM and XRD confirms the amorphous phase of the SiOC films.

  16. Synthesis and characterization of bismuth alkaline titanate powders

    Energy Technology Data Exchange (ETDEWEB)

    Torres-Huerta, A.M., E-mail: atorresh@ipn.mx [CICATA-Altamira, Instituto Politecnico Nacional, Km. 14.5 Carretera Tampico Puerto Industrial Altamira, Altamira, Tamps. 89600 (Mexico); Dominguez-Crespo, M.A. [CICATA-Altamira, Instituto Politecnico Nacional, Km. 14.5 Carretera Tampico Puerto Industrial Altamira, Altamira, Tamps. 89600 (Mexico); Hernandez-Perez, M.A. [ESIQIE, Metalurgia, Instituto Politecnico Nacional, Mexico, D. F (Mexico); Garcia-Zaleta, D.S. [CICATA-Altamira, Instituto Politecnico Nacional, Km. 14.5 Carretera Tampico Puerto Industrial Altamira, Altamira, Tamps. 89600 (Mexico); Brachetti-Sibaja, S.B. [CICATA-Altamira, Instituto Politecnico Nacional, Km. 14.5 Carretera Tampico Puerto Industrial Altamira, Altamira, Tamps. 89600 (Mexico); Instituto Tecnologico de Ciudad Madero, Av. 1o. de Mayo esq. Sor Juana Ines de la Cruz s/n Col. Los Mangos C.P.89440 Cd. Madero Tamaulipas (Mexico)

    2011-06-15

    In this work, samples of bismuth alkaline titanate, (K{sub 0.5}Na{sub 0.5}){sub (2-x/2)}Bi{sub (x/6)}TiO{sub 3}, (x = 0.05-0.75) have been prepared by conventional ceramic technique and molten salts. Metal oxides or carbonates powders were used as starting raw materials. The crystalline phase of the synthesized powders was identified by the X-ray diffraction (XRD) and particle morphology was characterized by scanning electron microscopy (SEM). Solid state reaction method was unsuccessful to obtain pellets. From XRD results, a rhombohedral structure was detected and the parameter lattice were estimated to be a = 5.5478 A and {alpha} = 59.48{sup o}. These parameters were used to refine the structure by Rietveld analysis. SEM results showed several morphologies. Apparently, bismuth is promoting the grain growth whose sizes vary from 30 nm to 180 nm It is expected that these materials can be utilized in practical applications as substitutes for lead zirconatetitanate (PZT)-based ceramics.

  17. ZnS-Graphene nanocomposite: Synthesis, characterization and optical properties

    Energy Technology Data Exchange (ETDEWEB)

    Pan Shugang [Key Laboratory for Soft Chemistry and Functional Materials, Nanjing University of Science and Technology, Ministry of Education, Nanjing 210094 (China); Liu Xiaoheng, E-mail: xhliu@mail.njust.edu.cn [Key Laboratory for Soft Chemistry and Functional Materials, Nanjing University of Science and Technology, Ministry of Education, Nanjing 210094 (China)

    2012-07-15

    A ZnS-Graphene nanocomposite was prepared by a facile one-step hydrothermal method using zinc nitrate hexahydrate, ethylenediamine and carbon disulfide as precursors, graphene oxide as a template. The composite was characterized by X-ray power diffraction, X-ray photoelectron spectroscopy, transmission electron microscopy, Fourier transform infrared, Raman spectra and fluorescence spectroscopy. The results show that graphene oxide was reduced to graphene in the hydrothermal reaction process. Simultaneously, the graphene sheets in the composite are exfoliated and decorated with ZnS nanoparticles. Furthermore, Raman and fluorescence properties of the composite were observed. ZnS-Graphene nanocomposite displays surface-enhanced Raman scattering activity for graphene oxide, and fluorescence enhancement property compared with pure ZnS sample. - Graphical abstract: Approach of reaction makes the reduction of grapheme oxide and the deposition of Zns on the grapheme sheets occur simultaneously and overcomes the aggregation of the grapheme sheets and Zns. Highlights: Black-Right-Pointing-Pointer Graphene oxide is reduced to graphene in the hydrothermal reaction process. Black-Right-Pointing-Pointer ZnS nanoparticles are attached onto the almost transparent graphene sheets. Black-Right-Pointing-Pointer ZnS-Graphene system shows surface-enhanced Raman scattering (SERS) activity. Black-Right-Pointing-Pointer ZnS-Graphene system displays relatively better fluorescence property than pure ZnS.

  18. Synthesis, characterization and catalytic activity of nanosized Ni complexed aminoclay

    Science.gov (United States)

    Ranchani, A. Amala Jeya; Parthasarathy, V.; Devi, A. Anitha; Meenarathi, B.; Anbarasan, R.

    2017-11-01

    A novel Ni complexed aminoclay (AC) catalyst was prepared by complexation method followed by reduction reaction. Various analytical techniques such as FTIR spectroscopy, UV-visible spectroscopy, DSC, TGA, SEM, HRTEM, EDX, XPS and WCA measurement are used to characterize the synthesized material. The AC-Ni catalyst system exhibited improved thermal stability and fiber-like morphology. The XPS results declared the formation of Ni nanoparticles. Thus, synthesized catalyst was tested towards the Schiff base formation reaction between various bio-medical polymers and aniline under air atmosphere at 85 °C for 24 h. The catalytic activity of the catalyst was studied by varying the % weight loading of the AC-Ni system towards the Schiff base formation. The Schiff base formation was quantitatively calculated by the 1H-NMR spectroscopy. While increasing the % weight loading of the AC-Ni catalyst, the % yield of Schiff base was also increased. The k app and Ti values were determined for the reduction of indole and α-terpineol in the presence of AC-Ni catalyst system. The experimental results were compared with the literature report.

  19. Synthesis and Characterization of Zirconium Tungstate Ultra-Thin Fibers

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Lifeng [South Dakota School of Mines and Technology; Howe, Jane Y [ORNL; Fong, Hao [South Dakota School of Mines and Technology; Zhang, Yan [Anhui Normal University, People' s Republic of China

    2009-01-01

    This study reports an innovative method of electrospinning followed by pyrolysis to synthesize zirconium tungstate (ZrW2O8), a material with negative coefficient of thermal expansion (CTE), in ultra-thin fiber form. Morphologies and microstructures of the as-electrospun precursor fibers, the heat-treated intermediate fibers, and the final ZrW2O8 ultra-thin fibers were characterized by SEM, XRD, and TEM. The ZrW2O8 ultra-thin fibers had diameters in the sub-micrometer range with aspect ratios larger than 100; these fibers were polycrystalline, and consisted of single crystalline ZrW2O8 crystallites with sizes of 30-50 nm and surface roughness of several nanometers. The ZrW2O8 ultra-thin fibers are expected to outperform spherically, cylindrically, and/or irregularly shaped polycrystalline ZrW2O8 particles for the development of composites with precisely controlled CTEs. Additionally, this reported method could be utilized as a general approach to convert nano-scaled inorganic particles into fibers.

  20. Synthesis, Characterization, and Pharmacological Evaluation of Selected Aromatic Amines

    Directory of Open Access Journals (Sweden)

    Hammad Ismail

    2015-01-01

    Full Text Available Aromatic amines 1-amino-4-phenoxybenzene (A-1A, 2-(4-aminophenoxy naphthalene (A-2A, and 1-(4-aminophenoxy naphthalene (A-3A were synthesized by the reduction of corresponding nitroaromatics with hydrazine monohydrate and Pd/C 5% (w/w. The newly synthesized compounds were characterized by FTIR, 1H NMR, 13C NMR, UV-visible spectrophotometer, and mass spectrometry and their biological activities were investigated along with structurally similar 4-(4-aminophenyloxy biphenyl (A-A. Results of brine shrimp cytotoxicity assay showed that almost all of the compounds had LD50 values <1 μg/mL. The compounds also showed significant antitumor activity with IC50 values ranging from 67.45 to 12.2 µgmL−1. The cytotoxicity and antitumor studies correlate the results which suggests the anticancerous nature of compounds. During the interaction study of these compounds with DNA, all of the compounds showed hyperchromic effect indicating strong interaction through binding with the grooves of DNA. Moreover, A-3A also showed decrease in λmax confirming higher propensity for DNA groove binding. In DPPH free radical scavenging assay, all the compounds showed potential antioxidant capability. The compounds were highly active in protecting DNA against hydroxyl free radicals. DNA interaction and antioxidant results back up each other indicating that these compounds have potential to be used as cancer chemopreventive agents. Additionally, one compound (A-1A showed significant antibacterial and antifungal activity as well.

  1. Synthesis and Characterization of Cluster-Derived Supported Bimetallic Catalysts

    Energy Technology Data Exchange (ETDEWEB)

    Adams, Richard D; Amiridis, Michael D

    2008-10-10

    New procedures have been developed for synthesizing di- and tri-metallic cluster complexes. The chemical properties of the new complexes have been investigated, particularly toward the activation of molecular hydrogen. These complexes were then converted into bi- and tri-metallic nanoparticles on silica and alumina supports. These nanoparticles were characterized by electron microscopy and were then tested for their ability to produce catalytic hydrogenation of unsaturated hydrocarbons and for the preferential oxidation of CO in the presence of hydrogen. The bi- and tri-metallic nanoparticles exhibited far superior activity and selectivity as hydrogenation catalysts when compared to the individual metallic components. It was found that the addition of tin greatly improved the selectivity of the catalysts for the hydrogenation of polyolefins. The addition of iron improves the catalysts for the selective oxidation of CO by platinum in the presence of hydrogen. The observations should lead to the development of lower cost routes to molecules that can be used to produce polymers and plastics for use by the general public and for procedures to purify hydrogen for use as an alternative energy in the hydrogen economy of the future.

  2. Novel 4-Methylumbelliferone Amide Derivatives: Synthesis, Characterization and Pesticidal Activities

    Directory of Open Access Journals (Sweden)

    Yan Wei

    2018-01-01

    Full Text Available A series of novel 4-methylumbelliferone amide derivatives were designed, synthesized and characterized by 1H NMR, 13C NMR and HR-ESI-MS. The structures of compounds 4bd and 4be (compounds named by authors were further confirmed by X-ray single crystal diffraction. The acaricidal, herbicidal and antifungal activities of the synthesized compounds were assayed for their potential use as pesticide. The results indicated that compounds 4bi, 4ac and 4bd were strong acaricidals against Tetranychus cinnabarinus, with 72h corrected mortalities of greater than 80% at 1000 mg/L. Meanwhile, compounds 4bh and 4bf exhibit the strongest inhibition against the taproot development of Digitaria sanguinalis and Chenopodium glaucum, and were even more potent than the commercial herbicide Acetochlor against D. sanguinalis. In addition, compounds 4bk, 4bh and 4bp showed the highest antifungal activity against the mycelium growth of Valsa mali, which makes them more effective than commercial fungicide Carbendazim.

  3. Synthesis and characterization of polyaniline coated gold nanocomposites

    Energy Technology Data Exchange (ETDEWEB)

    Zuber, Siti Nurzulaiha Mohd; Kamarun, Dzaraini; Zaki, Hamizah; Kamarudin, Mohamad Shukri [Faculty of Applied Sciences, Universiti Teknologi MARA (UiTM), Shah Alam, 40450 Selangor Darul Ehsan (Malaysia); Thomas, Sabu; Kalarikkal, Nandakumar [International and Inter University Centre of Nanoscience and Nanotechnoogy, Mahatma Ghandi University, Priyadarsini Hills Kottayam, Kerala India-686560 (India)

    2015-08-28

    Considerable attention has been drawn during the last two decades to prepare nanocomposites consists of conducting polymer and noble metal due to their potential ability to generate a new class of material with novel optical, chemical, electronic or mechanical properties for various applications. In this work, an attempt has been made to synthesize nanocomposite of polyaniline (PANI) coated with gold nanoparticles (AuNPs) chemically with various types of surfactants such as polyvinylpyrrolidone (PVP), and sodium dodecyl sulphate (SDS) which act as stabilizing agents to help in stabilization of the PANI/Gold nanocomposites system. The synthesized nanocomposites were characterized by UV-Visible, field emission scanning electron microscope (FESEM) and particle size analyzer (PSA). The formation of finger like structure can be seen in the FESEM images when the AuNPs were incorporated into the polymer matrix. The EDX data showed that 18.66% and 12.67% of AuNPs atoms were present in the composite system thus proved the incorporation of AuNPs into the polymer matrix. A small red shift of the absorption peak in the UV-Vis of both PANI/AuNPs composites system may be due to the incorporation of AuNPs in the PANI matrix.

  4. Synthesis and characterization of cadmium-calcium hydroxyapatite solid solutions

    Science.gov (United States)

    Zhao, Xin; Zhu, Yi-nian; Dai, Liu-qin

    2014-06-01

    A series of cadmium-calcium hydroxyapatite solid solutions was prepared by an aqueous precipitation method. By various means, the characterizations confirmed the formation of continuous solid solutions over all ranges of Cd/(Cd+Ca) atomic ratio. In the results, both lattice parameters a and c display slight deviations from Vegard's rule when the Cd/(Cd+Ca) atomic ratio is greater than 0.6. The particles change from smaller acicular to larger hexagonal columnar crystals as the Cd/(Cd+Ca) atomic ratio increases from 0-0.60 to 0.60-1.00. The area of the phosphate peak for symmetric P-O stretching decreases with the increase in Cd/(Cd+Ca) atomic ratio, and the peak disappears when the Cd/(Cd+Ca) atomic ratio is greater than 0.6; the two phosphate peaks of P-O stretching gradually merge together for the Cd/(Cd+Ca) atomic ratio near 0.60. These variations can be explained by a slight tendency of larger Cd ions to occupy M(2) sites and smaller Ca ions to prefer M(1) sites in the structure.

  5. Solid state synthesis and structural characterization of zinc titanates

    Energy Technology Data Exchange (ETDEWEB)

    Ayed, Sarra, E-mail: ayedsarra1@gmail.com [Laboratory of Composite Ceramic and Polymer Materials, Scientific Faculty of Sfax (Tunisia); Abdelkefi, Helmi; Khemakhem, Hamadi [Laboratory of Ferroelectric Materials, Scientific Faculty of Sfax (Tunisia); Matoussi, Adel [Laboratory of Composite Ceramic and Polymer Materials, Scientific Faculty of Sfax (Tunisia)

    2016-08-25

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

  6. Green synthesis and characterization of polymer-stabilized silver nanoparticles.

    Science.gov (United States)

    Medina-Ramirez, Iliana; Bashir, Sajid; Luo, Zhiping; Liu, Jingbo Louise

    2009-10-15

    Silver nanoparticles (Ag-NPs) were synthesized using a facile green chemistry synthetic route. The reaction occurred at ambient temperature with four reducing agents introduced to obtain nanoscale Ag-NPs. The variables of the green synthetic route, such as acidity, concentration of starting materials, and molar ratio of reactants were optimized. Dispersing agents were employed to prevent Ag-NPs from aggregating. Advanced instrumentation techniques, such as X-ray powder diffraction (XRD), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), ultraviolet-visible spectroscopy (UV-vis), and phase analysis light scattering technique (ZetaPALS) were applied to characterize the morphology, particle size distribution, elemental composition, and electrokinetic behavior of the Ag-NPs. UV-vis spectra detected the characteristic plasmon at approximately 395-410 nm; and XRD results were indicative of face-centered cubic phase structure of Ag. These particles were found to be monodispersed and highly crystalline, displaying near-spherical appearance, with average particle size of 10.2 nm using citrate or 13.7 nm using ascorbic acid as reductants from particle size analysis by ZetaPALS, respectively. The rapid electrokinetic behavior of the Ag was evaluated using zetapotential (from -40 to -42 mV), which was highly dependant on nanoparticle acidity and particle size. The current research opens a new avenue for the green fabrication of nanomaterials (including variables optimization and aggregation prevention), and functionalization in the field of nanocatalysis, disinfection, and electronics.

  7. 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.

  8. Synthesis and characterization of hydrophobically modified polymeric betaines

    Directory of Open Access Journals (Sweden)

    Alexey Shakhvorostov

    2015-09-01

    Full Text Available Polymeric betaines containing long alkyl chains C12H25, C14H29, C16H33 and C18H37 were synthesized by Michael addition reaction of alkylaminocrotonates and methacrylic acid (MAA. They were characterized by FTIR, 13C NMR, DSC, DLS, GPC, cryo-TEM, viscometry and zeta-potential measurements. The polymers were fully soluble in DMF, THF and DMSO, partially dissolved in aromatic hydrocarbons (benzene, toluene, o-xylene and formed colloid solutions in aqueous KOH. In aqueous KOH and DMSO solutions, hydrophobically modified polymeric betaines behaved as polyelectrolytes. The average hydrodynamic size and zeta potential of diluted aqueous solutions of hydrophobic polybetainess containing dodecyl-, tetradecyl-, hexadecyl-, and octadecyl groups were studied as a function of pH. Anomalous low values of the isoelectric point (IEP of amphoteric macromolecules were found to be in the range of pH 2.7-3.4. According to DLS data, the average size of macromolecules tends to decrease with dilution. Zeta-potential of amphoteric macromolecules in aqueous solution is much higher than that in DMSO. The cryo-TEM results revealed that in both aqueous KOH and DMSO media, the micron- and nanosized vesicles existed. The structural organization of vesicles in water and DMSO is discussed. The wax inhibition effect of hydrophobic polybetaines at a decrease of the pour point temperatures of high paraffinic oils was better in comparison with commercial available ethylene-vinylacetate copolymers (EVA.

  9. Physicochemical characterization of pulverized phyllite rocks to geopolymer resin synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Melo, L.G.A. [Instituto Militar de Enegenharia (IME), Rio de Janeiro, RJ (Brazil); Pires, E.F.C. [Universidade Federal Fluminense (UFF), Niteroi, RJ (Brazil); Pereira, R.A.; Silva, F.J. [Instituto Federal de Educacao, Ciencia e Tecnologia do Rio de Raneiro (IFRJ), RJ (Brazil)

    2016-07-01

    Full text: Geopolymeric materials have common properties considered unique, such as: early-high compressive strength, durability, high chemical resistance to acids and sulfates attacks, ability to immobilize toxic and radioactive compounds, low porosity, low permeability, and resistance to high temperatures. Together with its environmental benefits, such as low energy consumption and low carbon dioxide emissions during production, these inorganic polymers are strategic materials for sustainable development and a good alternative to Portland cement. The main objective for introducing alternative materials is to lower the associated costs of its industrial process. Thus, the use of phyllite as the geopolymer precursor, is encouraged by its abundance, low cost, and the fact that it already is applied to the ceramic industries as kaolin substitute. This paper presents a physical characterization using TEM, SEM, XRD and XRF techniques of two pulverized phyllite rocks used as geopolymer precursors for refractory applications. It was found that both phyllite rocks studied have a high quartz content of approximately 50% that can be explored as 'filler' function in the microstructure, which stabilizes residual tensions after curing. Kaolinite and muscovite minerals are present up to 40% and are responsible for the high strengths in the geopolymer resins, as determined by compressive strength tests. (author)

  10. Biodirected synthesis and nanostructural characterization of anisotropic gold nanoparticles.

    Science.gov (United States)

    Plascencia-Villa, Germán; Torrente, Daniel; Marucho, Marcelo; José-Yacamán, Miguel

    2015-03-24

    Gold nanoparticles with anisotropic structures have tunable absorption properties and diverse bioapplications as image contrast agents, plasmonics, and therapeutic-diagnostic materials. Amino acids with electrostatically charged side chains possess inner affinity for metal ions. Lysine (Lys) efficiently controlled the growing into star-shape nanoparticles with controlled narrow sizes (30-100 nm) and produced in high yields (85-95%). Anisotropic nanostructures showed tunable absorbance from UV to NIR range, with extraordinary colloidal stability (-26 to -42 mV) and surface-enhanced Raman scattering properties. Advanced electron microscopy characterization through ultra-high-resolution SEM, STEM, and HR-TEM confirmed the size, nanostructure, crystalline structure, and chemical composition. Molecular dynamics simulations revealed that Lys interacted preferentially with Au(I) through the -COOH group instead of their positive side chains with a binding free energy (BFE) of 3.4 kcal mol(-1). These highly monodisperse and colloidal stable anisotropic particles prepared with biocompatible compounds may be employed in biomedical applications.

  11. Synthesis and characterization of polyaniline coated gold nanocomposites

    Science.gov (United States)

    Zuber, Siti Nurzulaiha Mohd; Kamarun, Dzaraini; Zaki, Hamizah; Kamarudin, Mohamad Shukri; Thomas, Sabu; Kalarikkal, Nandakumar

    2015-08-01

    Considerable attention has been drawn during the last two decades to prepare nanocomposites consists of conducting polymer and noble metal due to their potential ability to generate a new class of material with novel optical, chemical, electronic or mechanical properties for various applications. In this work, an attempt has been made to synthesize nanocomposite of polyaniline (PANI) coated with gold nanoparticles (AuNPs) chemically with various types of surfactants such as polyvinylpyrrolidone (PVP), and sodium dodecyl sulphate (SDS) which act as stabilizing agents to help in stabilization of the PANI/Gold nanocomposites system. The synthesized nanocomposites were characterized by UV-Visible, field emission scanning electron microscope (FESEM) and particle size analyzer (PSA). The formation of finger like structure can be seen in the FESEM images when the AuNPs were incorporated into the polymer matrix. The EDX data showed that 18.66% and 12.67% of AuNPs atoms were present in the composite system thus proved the incorporation of AuNPs into the polymer matrix. A small red shift of the absorption peak in the UV-Vis of both PANI/AuNPs composites system may be due to the incorporation of AuNPs in the PANI matrix.

  12. Synthesis and Characterization of Nanosized Fe2O3 Pigments

    Directory of Open Access Journals (Sweden)

    M. F. R. Fouda

    2012-01-01

    Full Text Available The work in this paper was devoted to investigating some nanosized iron oxide pigments prepared by microemulsion technique. The role of concentration of iron salt and surfactant (cetyltrimethylammonium bromide on the produced iron oxide was studied. The techniques employed to characterize the samples were thermogravimetric analysis, X-ray diffractometry, transmission electron microscope, infrared spectroscopy, and diffuse reflectance spectroscopy. The results revealed that the particle size of the prepared sample using 0.2 M iron sulfate and 3.2 wt% of surfactant was in the range 7–9 nm. Increasing the concentration of either iron salt or the surfactant increased the particle size of the obtained ferric oxide. The diffuse reflectance measurements showed that the charge transfer/electron pair transition absorption peak, which is closely related to the reddish color of the oxide, was shifted to a longer wavelength (blue shift by decreasing the dimension of the particles. The samples were tested as pigments. They showed different tints of red color and were found to be promising for applications as pigments in the field of paint manufacturing.

  13. Synthesis and Characterization of Polyelectrolyte Grafted Charged Colloidal Particles

    Science.gov (United States)

    Mohanty, Priti Sundar; Harada, Tamotsu; Matsumoto, Kozo; Matsuoka, Hideki

    2006-05-01

    Novel polyelectrolyte grafted charged colloidal particles have been synthesized via emulsion polymerization method using block copolymer as an emulsifier and have been characterized by determining the surface charge number (Z), chain density (σ) using conductometric titration, the size distribution, hydrodynamic (Rh) radius by dynamic light scattering and the core radius (Rc) by atomic force microscopy. The structural ordering and dynamics have been investigated in a very dilute concentration and the effect of salt concentration (Cs) on hydrodynamic radius have also been studied using dynamic light scattering. The conductivity titration curve was found to show two equivalence points and the potentiometric titration curves are found to sensitive only after a critical salt concentrations. The corresponding measured hydrodynamic radius is also found to decrease after a critical salt concentration. At high salt concentration, the hydrodynamic radius shows a close agreement with that of the core radius measured by the atomic force microscope. These experimental results are in agreement with the recent theoretical prediction and experimental observation that most of the counterions are confined inside the brush region which led to stretching of the chains at low salt concentration.

  14. Synthesis and characterization of Supeparamagnetics Microspheres (PMMA via suspension polymerization

    Directory of Open Access Journals (Sweden)

    Paulo Emilio Feuser

    2014-02-01

    Full Text Available Magnetics nanoparticles (NPMs has found many applications in biomedical and technological areas. The objective of this work is the preparation and characterization of PMMA microspheres containing NPMs coated with oleic acid (NPMs-AO. For the preparation of MNPs-AO was used the coprecipitation method in an aqueous medium. For the preparation of the superparamagnetic microspheres used in suspension polymerization technique. The microspheres showed a size distribution particles of approximately 150um and a spherical morphology. From the analysis of gel permeation chromatography (GPC determined the number average molecular weight (Mw of the magnetics microspheres and there was a variation in the Mw depending on the concentration of MNPs-AO in this reaction. To analyze the magnetic properties used the vibrating sample magnetometer (MAV. The microspheres showed superparamagnetic properties and a value of saturation magnetization (Ms of about 8 emu/g MNPs. Therefore you can conclude that it is possible to obtain superparamagnetics microspheres for a particular application, either, biomedical or technological.

  15. Synthesis and Characterization of Bis(4-methylbenzylammonium Tetrachloridocadmate(II

    Directory of Open Access Journals (Sweden)

    R. Kefi

    2011-01-01

    Full Text Available The crystal structure of the new inorganic-organic hybrid compound [4-CH3C6H4CH2NH3]2[CdCl4] has been determined by single crystal X-ray diffraction. The compound crystallizes in the orthorhombic space group Pnma with lattice parameters a=10.721(2, b=33.986(6, c=5.326(1 Å, β=97.222(1°, V=1940.8(7 Å3, and Z=4. The framework of the title compound is built upon layers parallel to (010 made up from corner-sharing CdCl6 octahedra. 4-Methylbenzylammonium cations are situated between the layers and connect them via an N–H⋯Cl hydrogen bonding network. The Cd atom is located on an inversion centre, and the coordination environment is described as distorted octahedral. Solid state 13C CP-MAS NMR spectroscopy is in agreement with the X-ray structure. DFT calculations allow the attribution of the carbon peaks to the independent crystallographic sites. Thermal analysis and infrared spectroscopy were also used to characterize the complex.

  16. The first organocopper tetrazole derivative: synthesis and characterization.

    Science.gov (United States)

    Voitekhovich, Sergei V; Grigoriev, Yuri V; Lyakhov, Alexander S; Ivashkevich, Ludmila S; Ivashkevich, Oleg A

    2016-09-14

    1-(5-Amino-3-azapentyl)tetrazole dihydrochloride (HL·2HCl) was prepared by heterocyclization of diethylenetriamine with triethyl orthoformate and sodium azide followed by treatment with potassium carbonate and hydrochloric acid. The reaction of CuCl2, HL·2HCl and triethylamine (NEt3) in a molar ratio of 1 : 1 : 3 in water was found to generate a novel organometallic tetrazole derivative Cu2L2Cl2. This compound is present as a binuclear centrosymmetric molecular complex, in which C-deprotonated tetrazole L acts as a chelating ligand via the two amino N and tetrazole ring C coordination sites and the two copper atoms are linked together through two tetrazole ring N(4)-C(5) bridges. This complex is the first organocopper tetrazole derivative. When the molar ratio of the reagents in the abovementioned reaction was changed to 1 : 2 : 2, the complex Cu(HL)2Cl2 was formed along with Cu2L2Cl2. Pure Cu(HL)2Cl2 was isolated after reaction of the reagents in a molar ratio of 1 : 3 : 6. The complex Cu(HL)2Cl2 is present as a mononuclear molecular complex, with a chelating coordination mode of HL via the two amino N atoms only. Both complexes as well as HL·2HCl were characterized by single-crystal X-ray analysis.

  17. Synthesis and characterization of (Ba,Yb doped ceria nanopowders

    Directory of Open Access Journals (Sweden)

    Branko Matović

    2011-06-01

    Full Text Available Nanometric size (Ba, Yb doped ceria powders with fluorite-type structure were obtained by applying selfpropagating room temperature methods. Tailored composition was: Ce0.95−xBa0.05YbxO2−δ with fixed amount of Ba − 0.05 and varying Yb content “x” from 0.05 to 0.2. Powder properties such as crystallite and particle size and lattice parameters have been studied. Röntgen diffraction analyses (XRD were used to characterize the samples at room temperature. Also, high temperature treatment (up to 1550°C was used to follow stability of solid solutions. The mean diameters of the nanocrystals are determined from the full width at half maxima (FWHM of the XRD peaks. It was found that average diameter of crystallites is less than 3 nm. WilliamsonHall plots were used to separate the effect of the size and strain in the nanocrystals.

  18. Synthesis, characterization and antimicrobial studies of Schiff base complexes

    Science.gov (United States)

    Zafar, Hina; Ahmad, Anis; Khan, Asad U.; Khan, Tahir Ali

    2015-10-01

    The Schiff base complexes, MLCl2 [M = Fe(II), Co(II), Ni(II), Cu(II) and Zn(II)] have been synthesized by the template reaction of respective metal ions with 2-acetylpyrrole and 1,3-diaminopropane in 1:2:1 M ratio. The complexes have been characterized by elemental analyses, ESI - mass, NMR (1H and 13C), IR, XRD, electronic and EPR spectral studies, magnetic susceptibility and molar conductance measurements. These studies show that all the complexes have octahedral arrangement around the metal ions. The molar conductance measurements of all the complexes in DMSO indicate their non-electrolytic nature. The complexes were screened for their antibacterial activity in vitro against Gram-positive (Streptococcus pyogenes) and Gram-negative (Klebsiella pneumoniae) bacteria. Among the metal complexes studied the copper complex [CuLCl2], showed highest antibacterial activity nearly equal to standard drug ciprofloxacin. Other complexes also showed considerable antibacterial activity. The relative order of activity against S. Pyogenes is as Cu(II) > Zn(II) > Co(II) = Fe(II) > Ni(II) and with K. Pneumonia is as Cu(II) > Co(II) > Zn(II) > Fe(II) > Ni(II).

  19. Synthesis and characterizations of melamine-based epoxy resins.

    Science.gov (United States)

    Ricciotti, Laura; Roviello, Giuseppina; Tarallo, Oreste; Borbone, Fabio; Ferone, Claudio; Colangelo, Francesco; Catauro, Michelina; Cioffi, Raffaele

    2013-09-05

    A new, easy and cost-effective synthetic procedure for the preparation of thermosetting melamine-based epoxy resins is reported. By this innovative synthetic method, different kinds of resins can be obtained just by mixing the reagents in the presence of a catalyst without solvent and with mild curing conditions. Two types of resins were synthesized using melamine and a glycidyl derivative (resins I) or by adding a silane derivative (resin II). The resins were characterized by means of chemical-physical and thermal techniques. Experimental results show that all the prepared resins have a good thermal stability, but differ for their mechanical properties: resin I exhibits remarkable stiffness with a storage modulus value up to 830 MPa at room temperature, while lower storage moduli were found for resin II, indicating that the presence of silane groups could enhance the flexibility of these materials. The resins show a pot life higher than 30 min, which makes these resins good candidates for practical applications. The functionalization with silane terminations can be exploited in the formulation of hybrid organic-inorganic composite materials.

  20. Synthesis, characterization and pharmacological evaluation of amide prodrugs of Flurbiprofen

    Energy Technology Data Exchange (ETDEWEB)

    Mishra, Ashutosh; Veerasamy, Ravichandran; Jain, Prateek Kumar; Dixit, Vinod Kumar; Agrawal, Ram Kishor [Dr. H. S. Gour Vishwavidyalaya, Sagar (India). Dept. of Pharmaceutical Sciences. Pharmaceutical Chemistry Research Lab.]. E-mail: dragrawal2001@yahoo.co.in

    2008-07-01

    Flurbiprofen (FB) suffers from the general side effects of NSAIDs, owing to presence of free carboxylic acid group. The study was aimed to retard the adverse effects of gastrointestinal origin. Ten prodrugs of FB were synthesized by amidation with ethyl esters of amino acids, namely, glycine, L-phenylalanine, L-tryptophan, L-valine, L-isoleucine, L-alanine, L-leucine, L-glutamic acid, L-aspartic acid and {beta} alanine. Purified synthesized prodrugs were characterized by m.p., TLC, solubility, partition coefficients, elemental analyses, UV, FTIR, NMR and MS. Synthesized prodrugs were subjected for bioavailability studies, analgesic, anti-inflammatory activities and ulcerogenic index. Marked reduction of ulcerogenic index and comparable analgesic, antiinflammatory activities were obtained in all cases as compared to FB. Among synthesized prodrugs AR-9, AR-10 and AR-2 showing excellent pharmacological response and encouraging hydrolysis rate both in (Simulated Intestinal Fluid) SIF and in 80% human plasma. Prodrugs with increased aliphatic side chain length or introduction of aromatic substituent resulted in enhanced partition coefficient but diminished dissolution and hydrolysis rate. Such prodrugs can be considered for sustained release purpose. (author)