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Sample records for synthesis spectroscopic characterization

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

    Science.gov (United States)

    Brahma, Sanjaya; Shivashankar, S. A.

    2015-12-01

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

  2. Synthesis, characterization, spectroscopic properties and DFT study of a new pyridazinone family

    Science.gov (United States)

    Arrue, Lily; Rey, Marina; Rubilar-Hernandez, Carlos; Correa, Sebastian; Molins, Elies; Norambuena, Lorena; Zarate, Ximena; Schott, Eduardo

    2017-11-01

    Nitrogen compounds are widely investigated due to their pharmacological properties such as antihypertensive, antinociceptive, antibacterial, antifungal, analgesic, anticancer and inhibition activities and lately even as pesticide. In this context, we present the synthesis of new compounds: (E)-6-(3,4-dimethoxyphenyl)-3-(3-(3,4-dimethoxyphenyl)acryloyl)-1-(4-R-phenyl)- 5,6-dihydropyridazin-4(1H)-one (with R = sbnd H(1), -Cl(2), -Br(3), sbnd I(4) and sbnd COOH(5)) that was carried out by reaction of (1E, 6E)-1,7-bis(3,4-dimethoxyphenyl)hepta-1,6-diene-3,5-dione with a substituted phenylamine with general formula p-R-C6H4sbnd NH2 (R = sbnd H (1), sbnd Cl (2), -Br(3), sbnd I(4) and sbnd COOH(5)). This is the first synthesis report of a pyridazinone using as precursors a curcuminoid derivative and a diazonium salt formed in situ. All compounds were characterized by EA, FT-IR, UV-Vis, Emission,1H- and13C-NMR spectroscopy and the crystalline and molecular structure of 4 was solved by X-rays diffraction method. DFT and TD-DFT quantum chemical calculations were also employed to characterize the compounds and provide a rational explanation to the spectroscopic properties. To assess the biological activity of the systems, we focused on pesticide tests on compound 2, which showed an inhibitory effect in plant growth of Agrostis tenuis Higland.

  3. Synthesis, Spectroscopic and DFT Characterization of 4â-(4-tert ...

    African Journals Online (AJOL)

    In this work the synthesis, spectral characterization and non-linear optical properties of metal-free .... following literature methods23–26 The advantage of this method ..... Synthesis of phthalocyanine conjugates with gold nanoparticles and.

  4. Synthesis, characterization, and application of novel biodegradable self-assembled 2-(N-phthalimido) ethyl-palmitate nanoparticles for cancer therapy

    Science.gov (United States)

    Kasoju, Naresh; Bora, Debajeet K.; Bhonde, Ramesh R.; Bora, Utpal

    2010-03-01

    We report the synthesis of novel biodegradable nanoparticles (NPs) which can kill the cancer cells without any additional drug loading. The NP was a self-assembled form of a phthalimide based conjugate, in which the phthalimide moiety was responsible for the anticancer activity. We describe the synthesis of a novel 2-(N-phthalimido) ethyl palmitate (PHEP-Pal) conjugate and subsequent preparation of NPs by a simple self assembly process. The successful synthesis of conjugate was confirmed by various characterization studies including nuclear magnetic resonance spectroscope, Fourier transform infrared spectroscope, TOF-liquid chromatography mass spectroscope, differential scanning calorimetry, and X-ray diffraction unit. The synthesis, shape, size, and size distribution of PHEP-Pal NPs were determined by transmission electron microscope, atomic force microscope, and dynamic light scattering technique. Finally, cell culture studies using A549 and HeLa cells were done to evaluate the anticancer effect of PHEP-Pal NPs, which demonstrated the potency of these NPs for use in cancer chemotherapy.

  5. Synthesis of Zinc Diethyldithiocarbamate (ZDEC) and Structure Characterization using Decoupling 1H NMR

    International Nuclear Information System (INIS)

    Sujarit, Jenjira; Phutdhawong, Weerachai

    2003-10-01

    A synthesis of zinc diethyldithiocarbamate (ZDEC) has been studied. The optimization mole ratio of the synthetic process was 2: 2: 2: 1 of diethylamine, carbondisulfide, sodium hydroxide, and zinc chloride. Characterization was carried out mainly by analyzing its spectroscopic properties especially decoupling 1 H NMR technique. ZDEC was obtained in 48.5% yield

  6. Boronate esters: Synthesis, characterization and molecular base receptor analysis

    Science.gov (United States)

    Gómez-Jaimes, Gelen; Barba, Victor

    2014-10-01

    The synthesis of three boronate esters obtained by reacting 4-fluorophenylboronic (1), 4-iodophenylboronic (2) and 3,4-chlorophenylboronic (3) acids with 2,4,5-trihidroxybenzaldehyde is reported. The structural characterization was determined by spectroscopic and spectrometric techniques. The boron atom was evaluated to acts as Lewis acid center in the reaction with pyridine (Py), triethylamine (TEA) and fluoride anion (F-). The titration method was followed by UV-Vis and 11B NMR spectroscopy; results indicate the good interaction with the fluoride ion but poor coordination towards pyridine in solution.

  7. 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.

  8. Spectroscopic characterization of low dose rate brachytherapy sources

    Science.gov (United States)

    Beach, Stephen M.

    The low dose rate (LDR) brachytherapy seeds employed in permanent radioactive-source implant treatments usually use one of two radionuclides, 125I or 103Pd. The theoretically expected source spectroscopic output from these sources can be obtained via Monte Carlo calculation based upon seed dimensions and materials as well as the bare-source photon emissions for that specific radionuclide. However the discrepancies resulting from inconsistent manufacturing of sources in comparison to each other within model groups and simplified Monte Carlo calculational geometries ultimately result in undesirably large uncertainties in the Monte Carlo calculated values. This dissertation describes experimentally attained spectroscopic outputs of the clinically used brachytherapy sources in air and in liquid water. Such knowledge can then be applied to characterize these sources by a more fundamental and metro logically-pure classification, that of energy-based dosimetry. The spectroscopic results contained within this dissertation can be utilized in the verification and benchmarking of Monte Carlo calculational models of these brachytherapy sources. This body of work was undertaken to establish a usable spectroscopy system and analysis methods for the meaningful study of LDR brachytherapy seeds. The development of a correction algorithm and the analysis of the resultant spectroscopic measurements are presented. The characterization of the spectrometer and the subsequent deconvolution of the measured spectrum to obtain the true spectrum free of any perturbations caused by the spectrometer itself is an important contribution of this work. The approach of spectroscopic deconvolution that was applied in this work is derived in detail and it is applied to the physical measurements. In addition, the spectroscopically based analogs to the LDR dosimetry parameters that are currently employed are detailed, as well as the development of the theory and measurement methods to arrive at these

  9. 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.

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

    Science.gov (United States)

    Fatimah, Soja Siti; Bahti, Husein H.; Hastiawan, Iwan; Permanasari, Anna

    2016-02-01

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

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

    International Nuclear Information System (INIS)

    Salaha, A.; Abdel-Bary, E.M.; Kandilea, N.G.

    2005-01-01

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

  12. Identification and Spectroscopic Characterization of Nonheme Iron(III) Hypochlorite Intermediates**

    Science.gov (United States)

    Draksharapu, Apparao; Angelone, Davide; Quesne, Matthew G; Padamati, Sandeep K; Gómez, Laura; Hage, Ronald; Costas, Miquel; Browne, Wesley R; de Visser, Sam P

    2015-01-01

    FeIII–hypohalite complexes have been implicated in a wide range of important enzyme-catalyzed halogenation reactions including the biosynthesis of natural products and antibiotics and post-translational modification of proteins. The absence of spectroscopic data on such species precludes their identification. Herein, we report the generation and spectroscopic characterization of nonheme FeIII–hypohalite intermediates of possible relevance to iron halogenases. We show that FeIII-OCl polypyridylamine complexes can be sufficiently stable at room temperature to be characterized by UV/Vis absorption, resonance Raman and EPR spectroscopies, and cryo-ESIMS. DFT methods rationalize the pathways to the formation of the FeIII-OCl, and ultimately FeIV=O, species and provide indirect evidence for a short-lived FeII-OCl intermediate. The species observed and the pathways involved offer insight into and, importantly, a spectroscopic database for the investigation of iron halogenases. PMID:25663379

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

    International Nuclear Information System (INIS)

    Cendrowski, K.; Chen, X.; Zielinska, B.; Kalenczuk, R. J.; Rümmeli, M. H.; Büchner, B.; Klingeler, R.; Borowiak-Palen, E.

    2011-01-01

    The facile bulk synthesis of silica nanospheres makes them an attractive support for the transport of chemical compounds such as nanocrystalline titanium dioxide. In this contribution we present a promising route for the synthesis of mesoporous silica nanospheres (m-SiO 2 ) with diameter in range 200 nm, which are ideal supports for nanocrystalline titanium dioxide (TiO 2 ). The detailed microscopic and spectroscopic characterizations of core/shell structure (m-SiO 2 /TiO 2 ) were conducted. Moreover, the photocatalytic potential of the nanostructures was investigated via phenol decomposition and hydrogen generation. A clear enhancement of photoactivity in both reactions as compared to commercial TiO 2 -Degussa P25 catalyst is detected.

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

    Science.gov (United States)

    Cendrowski, K.; Chen, X.; Zielinska, B.; Kalenczuk, R. J.; Rümmeli, M. H.; Büchner, B.; Klingeler, R.; Borowiak-Palen, E.

    2011-11-01

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

  15. Synthesis and characterization ligand tris-(2-thiosalicylamidoethyl)amine and its iron complexes and indium

    International Nuclear Information System (INIS)

    Guerra-Garcia, Pedro Pablo; Valle Bourrouet, Grettel

    2006-01-01

    The synthesis of coordination chemistry ligand tris-(2-tiosalicilamidoetil)amine is presented within the framework of study of tripod ligands, the corresponding complexes of iron and indium. Also, its spectroscopic characterization by proton magnetic resonance is showed; so the influence of ligand on a redox active metal and an inactive is compared. Electrochemical methods have been used. The presence of sulfur atoms modifies the redox and magnetic behavior of iron ion (III), as has been found in other similar ligands [es

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

    Indian Academy of Sciences (India)

    were characterized by infrared, electronic, electron paramagnetic resonance ... The catalytic oxidation property of ruthenium(III) complexes were also ... cies at room temperature. ..... aldehyde part of Schiff base ligands, catalytic activ- ity of new ...

  17. Electrochemical synthesis and spectroscopic characterization of ...

    African Journals Online (AJOL)

    phenylpyrrole) coatings in an organic medium on iron and platinum electrodes. ... XPS measurements, infrared (FT-IR) and electronic absorption (UV-vis) spectroscopies were used to characterize the iron and platinum-coated electrodes. Finally the ...

  18. Synthesis, spectroscopic, biological activity and thermal characterization of ceftazidime with transition metals

    Science.gov (United States)

    Masoud, Mamdouh S.; Ali, Alaa E.; Elasala, Gehan S.; Kolkaila, Sherif A.

    2018-03-01

    Synthesis, physicochemical characterization and thermal analysis of ceftazidime complexes with transition metals (Cr(III), Mn(II), Fe(III), Co(II), Ni(II), Cu(II), Zn(II), Cd(II) and Hg(II)) were discussed. It's obtained that ceftazidime act as bidentate ligand. From magnetic measurement and spectral data, octahedral structures were proposed for all complexes except for cobalt, nickel and mercury had tetrahedral structural. Hyper chemistry program confirmed binding sites of ceftazidime. Ceftazidime complexes show higher activity than ceftazidime for some strains. From TG and DTA curves the thermal decomposition mechanisms of ceftazidime and their metal complexes were suggested. The thermal decomposition of the complexes ended with the formation of metal oxides as a final product except in case of Hg complex.

  19. Synthesis and characterization of semi-IPNs based on PVP and PLLA

    International Nuclear Information System (INIS)

    Camilo, A.P.R.; Mano, V.; Felisberti, M.I.

    2010-01-01

    The specific interest in the synthesis of semi-IPNs based on PLLA and PVP homopolymers due to the fact these are biodegradable and biocompatible, which allows us to infer applications in the medical field as sutures, implants, matrices for controlled release of drugs etc. The objective was to prepare a multicomponent material amphiphile in the form of semi-interpenetrating polymer networks, based on poly (L-lactide), PLLA, hydrophobic homopolymer, and poly (vinylpyrrolidone), PVP, hydrophilic component. The preparation of semi-IPN combined the polymerization and crosslinking of N-vinylpyrrolidone in the presence of poly (L-lactide). The products were characterized by spectroscopic and thermal methods. (author)

  20. Synthesis, characterization and biological activity studies of mixed ...

    African Journals Online (AJOL)

    The complexes were characterized using some physical techniques such as melting point, solubility, conductivity measurement and spectroscopic analyses such as UV-Visible spectroscopy, Atomic absorption spectroscopy, and Infrared spectroscopy. Based on the physical and spectroscopic results, the coordination of the ...

  1. Synthesis, Characterization, and Biological Activity of Nickel (II and Palladium (II Complex with Pyrrolidine Dithiocarbamate (PDTC

    Directory of Open Access Journals (Sweden)

    Sk Imadul Islam

    2016-01-01

    Full Text Available 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 coordination of the pyrrolidine dithiocarbamate (PDTC takes place through the two sulphur atoms in a symmetrical bidentate fashion. All the synthesized compounds were screened for their antimicrobial activity against some species of pathogenic bacteria (Escherichia coli, Vibrio cholerae, Streptococcus pneumonia, and Bacillus cereus. It has been observed that complexes have higher activity than the free ligand.

  2. Synthesis and spectroscopic characterization of a fluorescent pyrrole derivative containing electron acceptor and donor groups

    Science.gov (United States)

    Almeida, A. K. A.; Monteiro, M. P.; Dias, J. M. M.; Omena, L.; da Silva, A. J. C.; Tonholo, J.; Mortimer, R. J.; Navarro, M.; Jacinto, C.; Ribeiro, A. S.; de Oliveira, I. N.

    2014-07-01

    The synthesis and fluorescence characterization of a new pyrrole derivative (PyPDG) containing the electron donor-acceptor dansyl substituent is reported. The effects of temperature and solvent polarity on the steady-state fluorescence of this compound are investigated. Our results show that PyPDG exhibits desirable fluorescent properties which makes it a promising candidate to be used as the photoactive material in optical thermometry and thermography applications. Further, the electrochemical and emission properties of polymeric films obtained from the oxidation polymerization of PyPDG are also analyzed.

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

    African Journals Online (AJOL)

    a

    to characterize the iron and platinum-coated electrodes. Finally the ... their derivatives, is easily anodically performed on inert substrates such as platinum, gold, glassy carbon and .... because the electrode is more significantly protected. After 5 ...

  4. Mg-doped hydroxyapatite nanoplates for biomedical applications: A surfactant assisted microwave synthesis and spectroscopic investigations

    International Nuclear Information System (INIS)

    Mishra, Vijay Kumar; Bhattacharjee, Birendra Nath; Parkash, Om; Kumar, Devendra; Rai, Shyam Bahadur

    2014-01-01

    Highlights: • Microwave irradiation technique: employed for the synthesis of Mg-HAp nanoplates. • Surfactant (EDTA) assisted synthesis of Mg-HAp. • FT-IR and Raman analysis of functional groups of Mg-HAp. - Abstract: Nanoplates of Mg doped hydroxyapatite (Mg-HAp) were derived successfully and rapidly via microwave irradiation technique. Hydroxyapatite (HAp) is the hard tissues and main inorganic component in mammals. Different nanostructures of HAp exist in different parts of human bone but nanorods are very common due to its intrinsic nature to grow in rode-like structure under physiological as well as under applied ambient conditions in laboratory. On the addition of Mg at very low level (0.06 mol%) in pure HAp results the formation of 2-D plate-like nanostructures rather than rod-like which is the matter of interest. In this attempt our efforts have been focused on the study of effect of Mg incorporation on structural and spectroscopic properties of HAp prepared via microwave irradiation technique. This technique is preferred due to several advantages viz. very fast as well as homogeneous heating, time/energy saving and eco-friendliness. The calcium nitrate tetrahydrate (Ca(NO 3 ) 2 ⋅4H 2 O)) as a source of calcium, magnesium nitrate hexahydrate (Mg(NO 3 ) 2 ⋅6H 2 O) as a source of magnesium, disodium hydrogen phosphate dihydrate (NaH 2 PO 4 ⋅2H 2 O) as a source of phosphorous and sodium ethylene diamine tetra acetate (NaEDTA) as a surfactant were used as starting reagents. Sodium hydroxide (NaOH) pellets were employed to adjust the pH value of final solution. The solution of fixed pH value was kept into the microwave oven generating waves of frequency 2.45 GHz (water absorption frequency) and power 750 W for 8 min. The precipitate thus obtained was washed, centrifuged and then dried at 100 °C for 2 h. Dried powder was then calcined at 700 °C for 2 h. The bright white powder thus obtained was characterized structurally using X-ray diffraction and

  5. Mg-doped hydroxyapatite nanoplates for biomedical applications: A surfactant assisted microwave synthesis and spectroscopic investigations

    Energy Technology Data Exchange (ETDEWEB)

    Mishra, Vijay Kumar [Department of Physics, Faculty of Science, Banaras Hindu University, Varanasi 221005 (India); Bhattacharjee, Birendra Nath; Parkash, Om [Department of Ceramic Engineering, Indian Institute of Technology, Banaras Hindu University, Varanasi 221005 (India); Kumar, Devendra, E-mail: devendra.cer@iitbhu.ac.in [Department of Ceramic Engineering, Indian Institute of Technology, Banaras Hindu University, Varanasi 221005 (India); Rai, Shyam Bahadur, E-mail: sbrai49@yahoo.co.in [Department of Physics, Faculty of Science, Banaras Hindu University, Varanasi 221005 (India)

    2014-11-25

    Highlights: • Microwave irradiation technique: employed for the synthesis of Mg-HAp nanoplates. • Surfactant (EDTA) assisted synthesis of Mg-HAp. • FT-IR and Raman analysis of functional groups of Mg-HAp. - Abstract: Nanoplates of Mg doped hydroxyapatite (Mg-HAp) were derived successfully and rapidly via microwave irradiation technique. Hydroxyapatite (HAp) is the hard tissues and main inorganic component in mammals. Different nanostructures of HAp exist in different parts of human bone but nanorods are very common due to its intrinsic nature to grow in rode-like structure under physiological as well as under applied ambient conditions in laboratory. On the addition of Mg at very low level (0.06 mol%) in pure HAp results the formation of 2-D plate-like nanostructures rather than rod-like which is the matter of interest. In this attempt our efforts have been focused on the study of effect of Mg incorporation on structural and spectroscopic properties of HAp prepared via microwave irradiation technique. This technique is preferred due to several advantages viz. very fast as well as homogeneous heating, time/energy saving and eco-friendliness. The calcium nitrate tetrahydrate (Ca(NO{sub 3}){sub 2}⋅4H{sub 2}O)) as a source of calcium, magnesium nitrate hexahydrate (Mg(NO{sub 3}){sub 2}⋅6H{sub 2}O) as a source of magnesium, disodium hydrogen phosphate dihydrate (NaH{sub 2}PO{sub 4}⋅2H{sub 2}O) as a source of phosphorous and sodium ethylene diamine tetra acetate (NaEDTA) as a surfactant were used as starting reagents. Sodium hydroxide (NaOH) pellets were employed to adjust the pH value of final solution. The solution of fixed pH value was kept into the microwave oven generating waves of frequency 2.45 GHz (water absorption frequency) and power 750 W for 8 min. The precipitate thus obtained was washed, centrifuged and then dried at 100 °C for 2 h. Dried powder was then calcined at 700 °C for 2 h. The bright white powder thus obtained was characterized

  6. Synthesis of New Benzocoumaryl Oxadiazolyls as Strong Blue ...

    African Journals Online (AJOL)

    NICO

    complexes in DSSCs.5 Beside this, in support of our investiga- ... synthesis and fluorescent studies on benzocoumarins12 and development of new heterocyclic ..... characterized by elemental analysis and spectroscopic data. 3.1. UV-visible ...

  7. Characterization of ion-implanted aluminum and iron by spectroscopic ellipsometry

    International Nuclear Information System (INIS)

    Brodkin, J.S.; Franzen, W.; Culbertson, R.J.

    1990-01-01

    The change in the optical constants of aluminum alloy and iron samples caused by implantation with nitrogen and chromium ions has been investigated by spectroscopic ellipsometry. The objective is to develop a method for simple, non-destructive characterization of ion-implanted metals. 5 refs., 6 figs

  8. Total synthesis of sannanine and analogues thereof

    Indian Academy of Sciences (India)

    BADHER NAVEEN

    2018-03-02

    Mar 2, 2018 ... further characterized HRMS and IR spectral analysis. For all the newly synthesized by solid ..... Burst in a Model of Gouty Arthritis J. Nat. Prod. 70. 936. 3. ... Synthesis, Spectroscopic Characterisation, X-ray Struc- ture and DFT ...

  9. Sub-THz spectroscopic characterization of vibrational modes in artificially designed DNA monocrystal

    International Nuclear Information System (INIS)

    Sizov, Igor; Rahman, Masudur; Gelmont, Boris; Norton, Michael L.; Globus, Tatiana

    2013-01-01

    Highlights: • Sub-THz spectroscopy is used to characterize artificially designed DNA monocrystal. • Results are obtained using a novel near field, RT, frequency domain spectrometer. • Narrow resonances of 0.1 cm −1 width in absorption spectra of crystal are observed. • Signature measured between 310 and 490 GHz is reproducible and well resolved. • Absorption pattern is explained in part by simulation results from dsDNA fragment. - Abstract: Sub-terahertz (sub-THz) vibrational spectroscopy is a new spectroscopic branch for characterizing biological macromolecules. In this work, highly resolved sub-THz resonance spectroscopy is used for characterizing engineered molecular structures, an artificially designed DNA monocrystal, built from a short DNA sequence. Using a recently developed frequency domain spectroscopic instrument operating at room temperature with high spectral and spatial resolution, we demonstrated very intense and specific spectral lines from a DNA crystal in general agreement with a computational molecular dynamics (MD) simulation of a short double stranded DNA fragment. The spectroscopic signature measured in the frequency range between 310 and 490 GHz is rich in well resolved and reproducible spectral features thus demonstrating the capability of THz resonance spectroscopy to be used for characterizing custom macromolecules and structures designed and implemented via nanotechnology for a wide variety of application domains. Analysis of MD simulation indicates that intense and narrow vibrational modes with atomic movements perpendicular (transverse) and parallel (longitudinal) to the long DNA axis coexist in dsDNA, with much higher contribution from longitudinal vibrations

  10. Synthesis and molecular characterization of chitosan based polyurethane elastomers using aromatic diisocyanate.

    Science.gov (United States)

    Zia, Khalid Mahmood; Anjum, Sohail; Zuber, Mohammad; Mujahid, Muhammad; Jamil, Tahir

    2014-05-01

    The present research work was performed to synthesize a new series of chitosan based polyurethane elastomers (PUEs) using poly(ɛ-caprolactone) (PCL). The chitosan based PUEs were prepared by step-growth polymerization technique using poly(ɛ-caprolactone) (PCL) and 2,4-toluene diisocyanate (TDI). In the second step the PU prepolymer was extended with different mole ratios of chitosan and 1,4-butane diol (BDO). Molecular engineering was carried out during the synthesis. The conventional spectroscopic characterization of the synthesized samples using FT-IR confirms the existence of the proposed chitosan based PUEs structure. Internal morphology of the prepared PUEs was studied using SEM analysis. The SEM images confirmed the incorporation of chitosan molecules into the PU backbone. Copyright © 2014 Elsevier B.V. All rights reserved.

  11. Synthesis, spectroscopic characterization and acoustic, volumetric, transport and thermal properties of hydroxyl ammonium based ionic liquids

    International Nuclear Information System (INIS)

    Losetty, Venkatramana; Chennuri, Bharath Kumar; Gardas, Ramesh L.

    2016-01-01

    Graphical abstract: Density, ρ (■) in kg · m"−"3, speed of sound, u (●) in m · s"−"1, dynamic viscosity, η (▴) in mPa · s, electrical conductivity, σ (♦) in S · cm"−"1of [BHEA][TFA] as the function of temperature and at 0.1 MPa pressure. - Highlights: • N-butyl-(N-hydroxyethyl) ammonium based protic ionic liquids (PILs) were synthesized. • Density, speed of sound, electrical conductivity and viscosity were measured for studied PILs. • Transport property data were fitted to Vogel–Tammann–Fulcher (VTF) equation. • FT-IR spectrum was helpful to explain the hydrogen bonding between ions. • Measured and derived properties were analyzed in terms of chemical structure of PILs. - Abstract: In the present work, solvent-free synthesis of two hydroxyethyl ammonium-based ionic liquids (ILs) at room temperature was carried out namely, N-butyl-(N-hydroxyethyl) ammonium trifluoroacetate ([BHEA][TFA]) and N-butyl-(N-hydroxyethyl) ammonium nitrate ([BHEA][NO_3]). The synthesized ionic liquids were characterized by various spectroscopic techniques such as "1H-NMR, "1"3C-NMR and FTIR. Furthermore, density (ρ), speed of sound (u), electrical conductivity (σ) and viscosity (η) have been measured within the temperature range from T = (303.15 to 343.15) K and at 0.1 MPa pressure. The measured density and viscosity values were fitted to the linear and Vogel–Tammann–Fulcher (VTF) equation, respectively. The temperature dependence conductivity of the measured ILs was fitted to a similar equation type of viscosity (VTF). Furthermore, the refractive index was measured at T = 303.15 K, in turn molar refraction (R_m) and free volume (f_V) were calculated using the Lorentz–Lorenz equation. The thermodynamic properties such as thermal expansion coefficient (α), isentropic compressibility (β_S) and intermolecular free length (L_f) were calculated by using the experimental values of density and speed of sound. The thermal decomposition temperature (T

  12. Synthesis and characterization of CdS/PVA nanocomposite films

    Science.gov (United States)

    Wang, Hongmei; Fang, Pengfei; Chen, Zhe; Wang, Shaojie

    2007-08-01

    A series CdS/PVA nanocomposite films with different amount of Cd salt have been prepared by means of the in situ synthesis method via the reaction of Cd 2+-dispersed poly vinyl-alcohol (PVA) with H 2S. The as-prepared films were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), ultraviolet-visible (UV-vis) absorption, photoluminescence (PL) spectra, Fourier transform infrared spectroscope (FTIR) and thermogravimetric analysis (TGA). The XRD results indicated the formation of CdS nanoparticles with hexagonal phase in the PVA matrix. The primary FTIR spectra of CdS/PVA nanocomposite in different processing stages have been discussed. The vibrational absorption peak of Cd sbnd S bond at 405 cm -1 was observed, which further testified the generation of CdS nanoparticles. The TGA results showed incorporation of CdS nanoparticles significantly altered the thermal properties of PVA matrix. The photoluminescence and UV-vis spectroscopy revealed that the CdS/PVA films showed quantum confinement effect.

  13. Synthesis and characterization of CdS/PVA nanocomposite films

    International Nuclear Information System (INIS)

    Wang Hongmei; Fang Pengfei; Chen Zhe; Wang Shaojie

    2007-01-01

    A series CdS/PVA nanocomposite films with different amount of Cd salt have been prepared by means of the in situ synthesis method via the reaction of Cd 2+ -dispersed poly vinyl-alcohol (PVA) with H 2 S. The as-prepared films were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), ultraviolet-visible (UV-vis) absorption, photoluminescence (PL) spectra, Fourier transform infrared spectroscope (FTIR) and thermogravimetric analysis (TGA). The XRD results indicated the formation of CdS nanoparticles with hexagonal phase in the PVA matrix. The primary FTIR spectra of CdS/PVA nanocomposite in different processing stages have been discussed. The vibrational absorption peak of Cd-S bond at 405 cm -1 was observed, which further testified the generation of CdS nanoparticles. The TGA results showed incorporation of CdS nanoparticles significantly altered the thermal properties of PVA matrix. The photoluminescence and UV-vis spectroscopy revealed that the CdS/PVA films showed quantum confinement effect

  14. Synthesis and characterization of a new porphyrin-polyoxometalate hybrid material and investigation of its catalytic activity.

    Science.gov (United States)

    Araghi, Mehdi; Mirkhani, Valiollah; Moghadam, Majid; Tangestaninejad, Shahram; Mohammdpoor-Baltork, Iraj

    2012-03-14

    In the present work, the preparation of a new organic-inorganic hybrid material in which tetrakis(p-aminophenylporphyrin) is covalently linked to a Lindqvist structure of polyoxometalate, is reported. This new porphyrin-polyoxometalate hybrid material was characterized by (1)H NMR, FT-IR and UV-Vis spectroscopic methods and cyclic voltammetry. These spectro- and electrochemical studies provided spectral data of the synthesis of this compound. Cyclic voltammetry showed the influence of the porphyrin on the redox process of the polyoxometalate. The catalytic activity of this hybrid material was investigated in the alkene epoxidation with NaIO(4).

  15. Synthesis, spectroscopic, structural and thermal characterizations of vanadyl(IV) adenine complex prospective as antidiabetic drug agent

    Science.gov (United States)

    El-Megharbel, Samy M.; Hamza, Reham Z.; Refat, Moamen S.

    2015-01-01

    The vanadyl(IV) adenine complex; [VO(Adn)2]ṡSO4; was synthesized and characterized. The molar conductivity of this complex was measured in DMSO solution that showed an electrolyte nature. Spectroscopic investigation of the green solid complex studied here indicate that the adenine acts as a bidentate ligand, coordinated to vanadyl(IV) ions through the nitrogen atoms N7 and nitrogen atom of amino group. Thus, from the results presented the vanadyl(IV) complex has square pyramid geometry. Further characterizations using thermal analyses and scanning electron techniques was useful. The aim of this paper was to introduce a new drug model for the diabetic complications by synthesized a novel mononuclear vanadyl(IV) adenine complex to mimic insulin action and reducing blood sugar level. The antidiabetic ability of this complex was investigated in STZ-induced diabetic mice. The results suggested that VO(IV)/adenine complex has antidiabetic activity, it improved the lipid profile, it improved liver and kidney functions, also it ameliorated insulin hormone and blood glucose levels. The vanadyl(IV) complex possesses an antioxidant activity and this was clear through studying SOD, CAT, MDA, GSH and methionine synthase. The current results support the therapeutic potentiality of vanadyl(IV)/adenine complex for the management and treatment of diabetes.

  16. Synthesis-on” and “synthesis-off” modes of carbon arc operation during synthesis of carbon nanotubes

    International Nuclear Information System (INIS)

    Yatom, Shurik; Selinsky, Rachel S.

    2017-01-01

    Arc discharge synthesis of single-walled carbon nanotubes (SWCNTs) remains largely uncontrollable, due to incomplete understanding of the synthetic process itself. Here, we show that synthesis of SWCNTs by a carbon arc may not constitute a single continuous process, but may instead consist of two distinct modes. One of these, a “synthesis-on” mode, produces the majority of the nanomaterials. During the synthesis-on mode, proportionally more carbon nanotubes are collected than in another mode, a “synthesis-off” mode. Both synthesis-on and synthesis-off modes for a typical arc configuration, employing a hollow anode filled with a mixture of powdered metal catalyst and graphite, were characterized by using in situ electrical, imaging, and spectroscopic diagnostics, along with ex situ imaging and spectroscopy. The synthesis-on mode duration is rare compared to the total arc run-time, helping to explain the poor selectivity found in the final collected products, a known inadequacy of arc synthesis. Finally, the rarity of the synthesis on mode occurence may be due to the synthesis off mode being more favorable energetically.

  17. Synthesis, characterization, photophysical, and photochemical properties of novel zinc(II) and indium(III) phthalocyanines containing 2-phenylphenoxy units

    Energy Technology Data Exchange (ETDEWEB)

    Ali, Haytham Elzien Alamin [Department of Chemistry, Marmara University, Istanbul 34722 (Turkey); University of Khartoum, Department of Chemistry, Faculty of Science, P.O. Box 321, Khartoum, 11115 (Sudan); Pişkin, Mehmet [Çanakkale Onsekiz Mart University, Vocational School of Technical Sciences, Department of Food Technology, Çanakkale 17100 (Turkey); Altun, Selçuk [Department of Chemistry, Marmara University, Istanbul 34722 (Turkey); Durmuş, Mahmut [Gebze Technical University, Department of Chemistry, P.O. Box 141, Gebze, Kocaeli 41400 (Turkey); Odabaş, Zafer, E-mail: zodabas@marmara.edu.tr [Department of Chemistry, Marmara University, Istanbul 34722 (Turkey)

    2016-05-15

    The synthesis of highly soluble and non-aggregated peripherally/non-peripherally Zn and In(OAc) phthalocyanines was achieved by 3-/ and 4-(2-phenylphenoxy)phthalonitrile as starting materials. The novel compounds were characterized by elemental analyses, FT-IR, {sup 1}H-NMR (for phthalonitriles), UV–vis and MALDI-TOF mass (for Pcs) spectroscopic techniques. Additionally, photophysical, photochemical and spectral properties of the phthalocyanines were reported. Especially, the indium(OAc) phthalocyanines showed good singlet oxygen quantum yields in DMSO and they can be appropriate candidates as Type II photosensitizers in photodynamic therapy (PDT) applications.

  18. Synthesis, characterization, photophysical, and photochemical properties of novel zinc(II) and indium(III) phthalocyanines containing 2-phenylphenoxy units

    International Nuclear Information System (INIS)

    Ali, Haytham Elzien Alamin; Pişkin, Mehmet; Altun, Selçuk; Durmuş, Mahmut; Odabaş, Zafer

    2016-01-01

    The synthesis of highly soluble and non-aggregated peripherally/non-peripherally Zn and In(OAc) phthalocyanines was achieved by 3-/ and 4-(2-phenylphenoxy)phthalonitrile as starting materials. The novel compounds were characterized by elemental analyses, FT-IR, 1 H-NMR (for phthalonitriles), UV–vis and MALDI-TOF mass (for Pcs) spectroscopic techniques. Additionally, photophysical, photochemical and spectral properties of the phthalocyanines were reported. Especially, the indium(OAc) phthalocyanines showed good singlet oxygen quantum yields in DMSO and they can be appropriate candidates as Type II photosensitizers in photodynamic therapy (PDT) applications.

  19. Radiation Synthesis of Functional Nanoparticles for Imaging, Sensing and Drug Delivery Applications

    International Nuclear Information System (INIS)

    Grasselli, M.; Soto Espinoza, S.; Risso, V.; Pawlak, E.; Smolko, E.E.

    2010-01-01

    In the present report we describe nanoparticle synthesis by ionizing radiation from globular proteins and methacrylate monomers. Dynamic light scattering and other spectroscopic methods were performed to characterize this new material

  20. Radiation Synthesis of Functional Nanoparticles for Imaging, Sensing and Drug Delivery Applications

    Energy Technology Data Exchange (ETDEWEB)

    Grasselli, M.; Soto Espinoza, S.; Risso, V.; Pawlak, E.; Smolko, E.E., E-mail: mgrasse@unq.edu.ar, E-mail: mariano.grasselli@gmail.com [Quesada 2422, piso 11, dpto. C, C1429 Buenos Aires (Argentina)

    2010-07-01

    In the present report we describe nanoparticle synthesis by ionizing radiation from globular proteins and methacrylate monomers. Dynamic light scattering and other spectroscopic methods were performed to characterize this new material.

  1. Synthesis, spectroscopic characterization, crystallographic studies and antibacterial assays of new copper(II) complexes with sulfathiazole and nimesulide

    Science.gov (United States)

    Nunes, Julia Helena Bormio; de Paiva, Raphael Enoque Ferraz; Cuin, Alexandre; da Costa Ferreira, Ana Maria; Lustri, Wilton Rogério; Corbi, Pedro Paulo

    2016-05-01

    New ternary copper(II) complexes of sulfathiazole (SFT, C9H8N3O2S2) or nimesulide (NMS, C13H11N2O5S) and 2,2‧-bipyridine (bipy) were synthesized, and characterized by chemical and spectroscopic techniques. Elemental analyses indicated a 2:1:1 sulfonamide/copper/bipy composition for both complexes. Mass spectrometric measurements permitted identifying the molecular ions [Cu(SFT)2(bipy)+H]+ and [Cu(NMS)2(bipy)+H]+ at m/z 728 and 835, respectively, confirming the proposed compositions. Crystal structure of the [Cu(SFT)2(bipy)] complex was solved by powder X-ray diffraction analysis (PXRD), attesting that the Cu(II) ion is hexacoordinated in a distorted octahedral geometry. Each SFT molecule coordinates to the metal ion by the nitrogen atoms of the SO2-N group and of the heterocyclic ring. The coordination sphere is completed by a bipyridine. Electronic paramagnetic resonance (EPR) studies were carried out for the [Cu(NMS)2(bipy)] complex, indicating a tetragonal environment around the metal ion. It was suggested that NMS coordinates to Cu(II) by the nitrogen and oxygen atoms of the SO2-N group, which was confirmed by infrared spectroscopic studies. Biological studies showed the antibacterial activity of both Cu-SFT and Cu-NMS complexes, with the minimum inhibitory concentration (MIC) values ranging from 0.10 to 0.84 mmol L-1 against Gram-negative bacteria for [Cu(SFT)2(bipy)], and from 1.50 to 3.00 mmol L-1 against Gram-positive and -negative bacteria for [Cu(NMS)2(bipy)].

  2. The synthesis of [14C] C I pigment violet 19

    International Nuclear Information System (INIS)

    Filer, C.N.; Kelly, T.P.

    1990-01-01

    For the custom synthesis of radiolabeled compounds in the authors laboratory, aside from spectroscopic examination, their identity and radiochemical purity is routinely corroborated by demonstration of cochromatography with an authentic cold standard. In the synthesis of [ 14 C] red pigment 1 for the Cosmetic Toiletry and Fragrance Association, its insolubility precluded this. The preparation as well as characterization of 1 is described

  3. Synthesis and structural characterization of lithium

    Indian Academy of Sciences (India)

    synthesis and characterization of two new iminophos- phonamine ligands ... structures. 2.3 General synthetic method for ligands (1 and 2) ... 2.3b General method for the Synthesis of ligands ...... studies are currently underway in our laboratory.

  4. Novel biosynthesis of Ag-hydroxyapatite: Structural and spectroscopic characterization

    Directory of Open Access Journals (Sweden)

    Álvaro de Jesús Ruíz-Baltazar

    2018-06-01

    Full Text Available Silver-doped hydroxyapatite (Ag-HAP was obtained by green synthesis route. The dopant silver nanoparticles (AgNPs were obtained by biosynthesis based on Melissa officinalis extract. This research is focused on the characterization and the use of the nontoxic and environment-friendly Ag-HAP nanocomposite. The structural and morphological characterization of Ag-HAP nanocomposite was carried out by scanning electron microscopy (SEM, X-ray diffraction, Fourier-transform infrared (FT-IR and Raman spectroscopy. The obtained nanoparticles exhibited a great interaction with the HAP matrix, performing an Ag-HAP nanocomposite. Changes in the structure of the Ag-HAP nanocomposite were corroborated by the different characterization techniques. Additionally, a homogeneous distribution of the AgNPs on the HAP structure was observed. The heterogeneous nucleation process employed to doping the HAP, offer a functional route to obtain a green composite with potentials applications in multiple fields, such as tissue engineering, bone repair as well as protein. These properties can be evaluated in subsequent studies. Keywords: Green synthesis, Ag nanoparticles, Hydroxyapatite, Structural characterization, Spectroscopy

  5. Spectroscopic characterization of uranium in evaporation basin sediments

    Science.gov (United States)

    Duff, M. C.; Morris, D. E.; Hunter, D. B.; Bertsch, P. M.

    2000-05-01

    Evaporation ponds in the San Joaquin Valley (SJV), CA, used for the containment of irrigation drainage waters contain elevated levels of uranium (U) resulting from the extensive leaching by carbonate-rich irrigation waters of the local agricultural soils that contain low levels of naturally-occurring U. The SJV ponds are subjected to changes in redox chemistry with cycles of drying and flooding. Our past studies have shown that U in the SJV Pond 14 surface sediments is present as mostly the oxidized and soluble form, U(VI). However, we were uncertain whether the U in the soil was only present as a U oxide of mixed stoichiometry, such as U 3O 8(s) (pitchblende) or other species. Here we present characterization information, which includes wet chemical and in situ spectroscopic techniques (X-ray absorption near-edge structure (XANES) and low temperature time-resolved luminescence spectroscopies) for samples from two SJV Pond sediments. Surface sediments from SJV Pond 16 were characterized for average oxidation state of U with XANES spectroscopy. The fraction of U(VI) to U(IV) in the Pond 16 sediments decreased with depth with U(IV) being the dominant oxidation state in the 5 cm to 15 cm depth. Two luminescent U(VI) species were identified in the surface sediments from Pond 14; a U(VI)-tricarbonate phase and another phase likely comprised of U(VI)-hydroxide or hydroxycarbonate. The luminescent U(VI) population in the Pond 16 sediments is dominated by species with comparable spectral characteristics to the U(VI)-hydroxide or hydroxycarbonate species found in the Pond 14 sediments. The luminescence spectroscopic results were complemented by wet chemical U leaching methods, which involved the use of carbonate and sulfuric acid solutions and oxidizing solutions of peroxide, hypochlorite and Mn(IV). Leaching was shown to decrease the total U concentration in the sediments in all cases. However, results from luminescence studies of the residual fraction in the leached

  6. SYNTHESIS, CHARACTERIZATION AND PHOTOCATALYTIC ...

    African Journals Online (AJOL)

    ISSN 1011-3924. © 2018 Chemical Society of Ethiopia and The Authors. Printed in Ethiopia ... SYNTHESIS, CHARACTERIZATION AND PHOTOCATALYTIC ACTIVITY OF .... cm−1 to determine the surface functional groups. 10 mg of sample ...

  7. Synthesis, spectroscopic characterization, biological screenings, DNA binding study and POM analyses of transition metal carboxylates

    Science.gov (United States)

    Uddin, Noor; Sirajuddin, Muhammad; Uddin, Nizam; Tariq, Muhammad; Ullah, Hameed; Ali, Saqib; Tirmizi, Syed Ahmed; Khan, Abdur Rehman

    2015-04-01

    This article contains the synthesis of a novel carboxylic acid derivative, its transition metal complexes and evaluation of biological applications. Six carboxylate complexes of transition metals, Zn(II) and Hg(II), have been successfully synthesized and characterized by FT-IR and NMR (1H, 13C). The ligand, HL, (4-[(2,6-Diethylphenyl)amino]-4-oxobutanoic acid) was also characterized by single crystal X-ray analysis. The complexation occurs via oxygen atoms of the carboxylate moiety. FT-IR date show the bidentate nature of the carboxylate moiety of the ligand as the Δν value in all complexes is less than that of the free ligand. The ligand and its complexes were screened for antifungal and antileishmanial activities. The results showed that the ligand and its complexes are active with few exceptions. UV-visible spectroscopy and viscometry results reveal that the ligand and its complexes interact with the DNA via intercalative mode of interaction. A new and efficient strategy to identify the pharmacophores and anti-pharmacophores sites in carboxylate derivatives for the antibacterial/antifungal activity using Petra, Osiris and Molinspiration (POM) analyses was also carried out.

  8. Biomimetic synthesis and characterization of semiconducting hybrid

    Indian Academy of Sciences (India)

    Triple hybrid materials based on polyaniline-polyethylene glycol and cadmium sulphide have been prepared by the duffusion–limited biomimetic route and characterized by a number of spectroscopic, XRD, SEM, thermal and electrical measurements. These hybrid materials have been prepared by controlled precipitation of ...

  9. Synthesis, characterization and spectroscopic properties of a new Nd{sup 3+}-doped Co-picromerite-type Tutton salt

    Energy Technology Data Exchange (ETDEWEB)

    Souamti, A., E-mail: souamtiahmed88@gmail.com [Laboratoire d' Application de la Chimie aux Ressources et Substances Naturelles et à l' Environnement, Département de Chimie, Université de Carthage, Faculté des Sciences de Bizerte, Zarzouna, Bizerte 7021 (Tunisia); Martín, I.R. [Departamento de Física, Universidad de La Laguna, 38206 La Laguna (Spain); Zayani, L. [Laboratoire d' Application de la Chimie aux Ressources et Substances Naturelles et à l' Environnement, Département de Chimie, Université de Carthage, Faculté des Sciences de Bizerte, Zarzouna, Bizerte 7021 (Tunisia); Hernández-Rodríguez, M.A.; Soler-Carracedo, K.; Lozano-Gorrín, A.D. [Departamento de Física, Universidad de La Laguna, 38206 La Laguna (Spain); Lalla, E. [Extreme Light Infrastructure – Nuclear Physics (ELI-NP), Horia Hulubei, National Institute of Physics and Nuclear Engineering (IFIN HH), 30, Reactorului Street, P.O. Box MG-6, 077125 Magurele, jud. Ilfov (Romania); Chehimi, D. Ben Hassen [Laboratoire d' Application de la Chimie aux Ressources et Substances Naturelles et à l' Environnement, Département de Chimie, Université de Carthage, Faculté des Sciences de Bizerte, Zarzouna, Bizerte 7021 (Tunisia)

    2016-09-15

    Single crystals of Nd{sup 3+}-doped Co-picromerite has been synthesized by the slow evaporation method. After two weeks on hold, the crystals obtained were characterized by different techniques, indeed X-ray powder diffraction (XRPD) shows that these compounds crystallize in the monoclinic system with space group P21/a. Complete dehydration of the double salt was obtained before reaching 200 °C with a phase transition of KS around 570 °C. The IR spectroscopic study confirms the vibrational modes of the sulfate groups and water molecules. Exciting at 473 nm, the emission peaks associated with the 4F{sub 5/2}→4I{sub 9/2}, 4F{sub 3/2}→4I{sub 9/2} and 4F{sub 3/2}→4I{sub 11/2} transitions were observed. The luminescence decay curve was analyzed in the frame of the Inokuti-Hirayama model in order to obtain the intrinsic lifetime and the energy transfer parameter among Nd{sup 3+}ions.

  10. Synthesis, characterization and sup 23 Na NMR shift studies of a novel dysprosium(III) crown ether texaphyrin

    Energy Technology Data Exchange (ETDEWEB)

    Sessler, J.L.; Mody, T.D. (Texas Univ., Austin, TX (United States). Dept. of Chemistry); Ramasamy, R.; Sherry, A.D. (Texas Univ., Dallas, TX (United States))

    1992-05-01

    The synthesis and characterization of a novel dysprosium(III) crown-ether texaphyrin (Dy(BCTxp)){sup 2+} is reported. This complex was designed to serve as a ditopic chelate for both dysprosium(III) and sodium cations. {sup 23}Sodium NMR spectroscopic studies indicates that titration of Na{sup +} with increasing concentrations of (Dy(BCTxp)){sup 2+} results in a shift toward higher frequency and gives a net hyperfine shift of 0.86 ppm. Sodium complexation is taking place into the crown subunit in (Dy(BCTxp)){sup 2+} and the degree of complexation is not reduced substantially by the positive charge on the dysprosium(III) portion of this binucleating system.

  11. New porphyrin-polyoxometalate hybrid materials: synthesis, characterization and investigation of catalytic activity in acetylation reactions.

    Science.gov (United States)

    Araghi, Mehdi; Mirkhani, Valiollah; Moghadam, Majid; Tangestaninejad, Shahram; Mohammdpoor-Baltork, Iraj

    2012-10-14

    New hybrid complexes based on covalent interaction between 5,10,15,20-tetrakis(4-aminophenyl)porphyrinatozinc(II) and 5,10,15,20-tetrakis(4-aminophenyl)porphyrinatotin(IV) chloride, and a Lindqvist-type polyoxometalate, Mo(6)O(19)(2-), were prepared. These new porphyrin-polyoxometalate hybrid materials were characterized by (1)H NMR, FT IR and UV-Vis spectroscopic methods and cyclic voltammetry. These spectro- and electrochemical studies provided several spectral data for synthesis of these compounds. Cyclic voltammetry showed the influence of the polyoxometalate on the redox process of the porphyrin ring. The catalytic activity of tin(IV)porphyrin-hexamolybdate hybrid material was investigated in the acetylation of alcohols and phenols with acetic anhydride. The reusability of this catalyst was also investigated.

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

    Indian Academy of Sciences (India)

    0013167

    SUPPORTING INFORMATION. REGULAR ARTICLE. Synthesis and characterization of six-membered pincer nickelacycles and application in alkylation of benzothiazole. †. HANUMANPRASAD PANDIRI,a DIPESH M SHARMA,a RAJESH G GONNADEb and. BENUDHAR PUNJI*,a. aOrganometallic Synthesis and Catalysis ...

  13. Spectroscopic studies of 2-thenoyltrifluoro acetonate of uranyl salts doped with europium

    International Nuclear Information System (INIS)

    Nakagawa, F.T.; Luiz, J.E.M. de Sa; Felinto, M.C.F.C.; Brito, H.F.; Teotonio, E.E.S.

    2006-01-01

    Uranyl compounds present a great potential as luminescence materials. Some examples of applications are: in laser technology, cathode ray tube, X-rays diagnostic. In this work it was studied the synthesis, characterization and spectroscopic properties study of uranyl 2-thenoyl trifluoroacetonate and uranyl 2- thenoyl trifluoroacetonate doped with europium. The compounds were synthesized and characterized by infrared absorption spectroscopy, thermal analysis, scanning electronic microscopy, and electronic spectroscopy of emission and excitation. The Eu 3+ ion acted as an effective luminescent probe, however the process of energy transfer from UO 2 2+ to Eu 3+ ion has not been efficient. (author)

  14. X-Ray powder diffraction analysis: Synthesis and spectroscopic studies on the stoichiometric elpasolite Cs2NaTmCl6

    International Nuclear Information System (INIS)

    Acevedo, R.; Poblete, V.; Elgueta, R.; Pozo, J.

    2000-01-01

    The elpasolite Cs 2 NaTmCl 6 belonging to the spatial group Fm3m, has been synthesized and characterized by powder DRX and spectroscopic studies. The synthesis was carried out by means of a solid state reaction at 802.9 o C, for two hours, with a temperature gradient of 4 o C/min. and 2 o C/min, at the beginning and end of the reaction, respectively. The optimum crystallization temperature occurs between 764.5 o C and 838.5 o C. The following crystallographic parameters were obtained: a 0 = 10,6866 o A, V =1220,45( o A) 3 , Z = 4, M = 802.90, D x =3,65 y D exp =3,67. The 32 experimental lines that were analyzed show great accuracy considering that R exp less than R wp . The Raman spectrums allowed for precise identification and assignation so that we can make progress in calculating the crystal dynamics and mechanistic aspects, still unexplored in the literature (C.W)

  15. Enzymatic synthesis of tRNA-peptide conjugates and spectroscopic studies of fluorine-modified RNA

    International Nuclear Information System (INIS)

    Graber, D.

    2010-01-01

    The research presented in this thesis concerns the enzymatic synthesis of artificially modified tRNA, in particular the preparation of non-hydrolysable tRNA-peptide conjugates. Another focus is on NMR-spectroscopic investigations of fluorine-modified RNA. In both projects, chemical methods were developed to address specific RNA-biological research questions. In the first part of this thesis the preparation of tRNA-peptide conjugates with a non-hydrolysable 3'-amide linkage is presented. These molecules are of high relevance for the characterization of ribosomal processes that occur in the peptidyl transferase center (such as peptide bond formation, peptide release, or translocation) using X-ray crystallography and biochemical methods. First, a novel concept to prepare chemically modified ('labeled') tRNA was elaborated based on the combination of solid-phase synthesis and enzymatic ligation. Thereby, a variety of differently labeled tRNAs was achieved. Moreover, the most successful high-yield ligation sites were identified to be situated within the TΨ C-loop. Optimization of the synthesis and the corresponding HPLC-purification of the conjugates were initially conducted with puromycin derivatized tRNA. In the course of this project, also two tRNAs with a ribose 3'-amino group at the terminal adenosine A76 were synthesized. For that purpose a protection group pattern had to be developed to obtain a functionalized solid-support bound to 3'-amino-3'-deoxyadenosine which was appropriate for RNA solid-phase synthesis. The successful preparation of tRNA-peptide conjugates was accomplished in cooperation with Holger Moroder and Jessica Steger (Micura group) who contributed short synthetic RNA-peptide conjugates. These fragments represented the tRNA 3'-termini that were required for exploring the new ligation strategies for non-hydrolisable tRNA - a main aim of this thesis. If the 5'-fragments are synthesized by solid-phase synthesis or in vitro transcription they do not

  16. Simple and Efficient One-Pot Synthesis, Spectroscopic Characterization and Crystal Structure of Methyl 5-(4-Chlorobenzoyloxy-1-phenyl-1H-pyrazole-3-carboxylate

    Directory of Open Access Journals (Sweden)

    Imtiaz Khan

    2012-07-01

    Full Text Available A facile one-pot synthesis of methyl 5-(4-chlorobenzoyloxy-1-phenyl-1H-pyrazole-3-carboxylate (4 is described. The title compound was efficiently synthesized by the reaction of phenyl hydrazine, dimethyl acetylenedicarboxylate and 4-chlorobenzoyl chloride in dichloromethane under reflux in good yield. The structure of the target compound was deduced by modern spectroscopic and analytical techniques and unequivocally confirmed by a single crystal X-ray diffraction analysis. The crystal of the title compound belongs to orthorhombic system, space group P 21 21 21 with cell parameters a = 6.6491(3 Å, b = 7.9627(6 Å, c = 30.621(5 Å, α = β = γ = 90° and Z = 4. The crystal packing of the compound (4 is stabilized by an offset π-stacking between the planar benzoyl-substituted diazole moieties.

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

    African Journals Online (AJOL)

    A new series of Mn(II), Fe(II), Co(II), Cu(II) and Zn(II) mixed ligands-metal complexes derived from salicylic acid (SA) and 1,10-phenanthroline (PHEN) have been synthesized and characterized by spectroscopic studies. The coordination of the two ligands towards central metal ions has been proposed in the light of ...

  18. Synthesis and characterization of Tin / Titanium mixed oxide nanoparticles doped with lanthanide for biomarking

    International Nuclear Information System (INIS)

    Paganini, Paula Pinheiro

    2012-01-01

    This work presents the synthesis, characterization and photo luminescent study of tin and titanium mixed oxide nanoparticles doped with europium, terbium and neodymium to be used with luminescent markers on biological systems. The syntheses were done by co-precipitation, protein sol-gel and Pechini methods and the nanoparticles were characterized by infrared spectroscopy, thermogravimetric analysis, scanning electron microscopy, X-ray diffraction and X-ray absorption spectroscopy. The photo luminescent properties studies were conducted for luminophores doped with europium, terbium and neodymium synthesized by coprecipitation method. For luminophore doped with europium it was possible to calculate the intensity parameters and quantum yield and it showed satisfactory results. In the case of biological system marking it was necessary the functionalization of these particles to allow them to bind to the biological part to be studied. So the nanoparticles were functionalized by microwave and Stöber methods and characterized by infrared spectroscopy, scanning electron microscopy, energy dispersive X-ray spectroscopy and X-ray diffraction obtaining qualitative response of functionalization efficacy. The ninhydrin spectroscopic method was used for quantification of luminophores functionalization. The photo luminescent studies of functionalized particles demonstrate the potential applying of these luminophores as luminescent markers. (author)

  19. Synthesis and characterization of iron cobalt (FECO) nanorods ...

    African Journals Online (AJOL)

    Synthesis and characterization of iron cobalt (FECO) nanorods prepared by simple ... shaped by increasing annealing temperature from room temperature to 800 ... Keywords: FeCo nanoparticles, sodium borohydrid, CTAB, chemical synthesis ...

  20. Spectroscopic characterization of alkaline earth uranyl carbonates

    International Nuclear Information System (INIS)

    Amayri, Samer; Reich, Tobias; Arnold, Thuro; Geipel, Gerhard; Bernhard, Gert

    2005-01-01

    A series of alkaline uranyl carbonates, M[UO 2 (CO 3 ) 3 ].nH 2 O (M=Mg 2 , Ca 2 , Sr 2 , Ba 2 , Na 2 Ca, and CaMg) was synthesized and characterized by inductively coupled plasma mass spectrometry (ICP-MS) and atomic absorption spectrometry (AAS) after nitric acid digestion, X-ray powder diffraction (XRD), and thermal analysis (TGA/DTA). The molecular structure of these compounds was characterized by extended X-ray absorption fine-structure (EXAFS) spectroscopy and X-ray photoelectron spectroscopy (XPS). Crystalline Ba 2 [UO 2 (CO 3 ) 3 ].6H 2 O was obtained for the first time. The EXAFS analysis showed that this compound consists of (UO 2 )(CO 3 ) 3 clusters similar to the other alkaline earth uranyl carbonates. The average U-Ba distance is 3.90+/-0.02A.Fluorescence wavelengths and life times were measured using time-resolved laser-induced fluorescence spectroscopy (TRLFS). The U-O bond distances determined by EXAFS, TRLFS, XPS, and Raman spectroscopy agree within the experimental uncertainties. The spectroscopic signatures observed could be useful for identifying uranyl carbonate species adsorbed on mineral surfaces

  1. Accurate spectroscopic characterization of protonated oxirane: a potential prebiotic species in Titan's atmosphere

    International Nuclear Information System (INIS)

    Giacomo Ciamician, Università di Bologna, Via Selmi 2, I-40126 Bologna (Italy))" data-affiliation=" (Dipartimento di Chimica Giacomo Ciamician, Università di Bologna, Via Selmi 2, I-40126 Bologna (Italy))" >Puzzarini, Cristina; Ali, Ashraf; Biczysko, Malgorzata; Barone, Vincenzo

    2014-01-01

    An accurate spectroscopic characterization of protonated oxirane has been carried out by means of state-of-the-art computational methods and approaches. The calculated spectroscopic parameters from our recent computational investigation of oxirane together with the corresponding experimental data available were used to assess the accuracy of our predicted rotational and IR spectra of protonated oxirane. We found an accuracy of about 10 cm –1 for vibrational transitions (fundamentals as well as overtones and combination bands) and, in relative terms, of 0.1% for rotational transitions. We are therefore confident that the spectroscopic data provided herein are a valuable support for the detection of protonated oxirane not only in Titan's atmosphere but also in the interstellar medium.

  2. Accurate spectroscopic characterization of protonated oxirane: a potential prebiotic species in Titan's atmosphere

    Energy Technology Data Exchange (ETDEWEB)

    Puzzarini, Cristina [Dipartimento di Chimica " Giacomo Ciamician," Università di Bologna, Via Selmi 2, I-40126 Bologna (Italy); Ali, Ashraf [NASA Goddard Space Flight Center, Greenbelt, MD 20771 (United States); Biczysko, Malgorzata; Barone, Vincenzo, E-mail: cristina.puzzarini@unibo.it [Scuola Normale Superiore, Piazza dei Cavalieri 7, I-56126 Pisa (Italy)

    2014-09-10

    An accurate spectroscopic characterization of protonated oxirane has been carried out by means of state-of-the-art computational methods and approaches. The calculated spectroscopic parameters from our recent computational investigation of oxirane together with the corresponding experimental data available were used to assess the accuracy of our predicted rotational and IR spectra of protonated oxirane. We found an accuracy of about 10 cm{sup –1} for vibrational transitions (fundamentals as well as overtones and combination bands) and, in relative terms, of 0.1% for rotational transitions. We are therefore confident that the spectroscopic data provided herein are a valuable support for the detection of protonated oxirane not only in Titan's atmosphere but also in the interstellar medium.

  3. Synthesis of unstable cyclic peroxides for chemiluminescence studies

    Energy Technology Data Exchange (ETDEWEB)

    Bartoloni, Fernando H.; Oliveira, Marcelo A. de; Augusto, Felipe A.; Ciscato, Luiz Francisco M.L.; Bastos, Erick L.; Baader, Wilhelm J., E-mail: wjbaader@iq.usp.br [Universidade de Sao Paulo (USP), SP (Brazil). Inst. de Quimica. Dept. de Quimica Fundamental

    2012-11-15

    Cyclic four-membered ring peroxides are important high-energy intermediates in a variety of chemi and bioluminescence transformations. Specifically, a-peroxy lactones (1,2-dioxetanones) have been considered as model systems for efficient firefly bioluminescence. However, the preparation of such highly unstable compounds is extremely difficult and, therefore, only few research groups have been able to study the properties of these substances. In this study, the synthesis, purification and characterization of three 1,2-dioxetanones are reported and a detailed procedure for the known synthesis of diphenoyl peroxide, another important model compound for the chemical generation of electronically excited states, is provided. For most of these peroxides, the complete spectroscopic characterization is reported here for the first time. (author)

  4. Hydrothermal synthesis, characterization and luminescent ...

    Indian Academy of Sciences (India)

    Home; Journals; Bulletin of Materials Science; Volume 39; Issue 4. Hydrothermal synthesis, characterization and luminescent properties of lanthanide-doped NaLaF 4 nanoparticles. JIGMET LADOL HEENA KHAJURIA SONIKA KHAJURIA ... Keywords. Citric acid; X-ray diffraction; down-conversion emission; energy transfer.

  5. Spectroscopic characterization approach to study surfactants effect on ZnO 2 nanoparticles synthesis by laser ablation process

    Science.gov (United States)

    Drmosh, Q. A.; Gondal, M. A.; Yamani, Z. H.; Saleh, T. A.

    2010-05-01

    Zinc peroxide nanoparticles having grain size less than 5 nm were synthesized using pulsed laser ablation in aqueous solution in the presence of different surfactants and solid zinc target in 3% H 2O 2. The effect of surfactants on the optical and structure of ZnO 2 was studied by applying different spectroscopic techniques. Structural properties and grain size of the synthesized nanoparticles were studied using XRD method. The presence of the cubic phase of zinc peroxide in all samples was confirmed with XRD, and the grain sizes were 4.7, 3.7, 3.3 and 2.8 nm in pure H 2O 2, and H 2O 2 mixed with SDS, CTAB and OGM respectively. For optical characterization, FTIR transmittance spectra of ZnO 2 nanoparticles prepared with and without surfactants show a characteristic ZnO 2 absorption at 435-445 cm -1. FTIR spectrum revealed that the adsorbed surfactants on zinc peroxide disappeared in case of CTAB and OGM while it appears in case of SDS. This could be due to high critical micelles SDS concentration comparing with others which is attributed to the adsorption anionic nature of this surfactant. Both FTIR and UV-vis spectra show a red shift in the presence of SDS and blue shift in the presence of CTAB and OGM. The blue shift in the absorption edge indicates the quantum confinement property of nanoparticles. The zinc peroxide nanoparticles prepared in additives-free media was also characterized by Raman spectra which show the characteristic peaks at 830-840 and 420-440 cm -1.

  6. Spectroscopic characterization approach to study surfactants effect on ZnO2 nanoparticles synthesis by laser ablation process

    International Nuclear Information System (INIS)

    Drmosh, Q.A.; Gondal, M.A.; Yamani, Z.H.; Saleh, T.A.

    2010-01-01

    Zinc peroxide nanoparticles having grain size less than 5 nm were synthesized using pulsed laser ablation in aqueous solution in the presence of different surfactants and solid zinc target in 3% H 2 O 2 . The effect of surfactants on the optical and structure of ZnO 2 was studied by applying different spectroscopic techniques. Structural properties and grain size of the synthesized nanoparticles were studied using XRD method. The presence of the cubic phase of zinc peroxide in all samples was confirmed with XRD, and the grain sizes were 4.7, 3.7, 3.3 and 2.8 nm in pure H 2 O 2 , and H 2 O 2 mixed with SDS, CTAB and OGM respectively. For optical characterization, FTIR transmittance spectra of ZnO 2 nanoparticles prepared with and without surfactants show a characteristic ZnO 2 absorption at 435-445 cm -1 . FTIR spectrum revealed that the adsorbed surfactants on zinc peroxide disappeared in case of CTAB and OGM while it appears in case of SDS. This could be due to high critical micelles SDS concentration comparing with others which is attributed to the adsorption anionic nature of this surfactant. Both FTIR and UV-vis spectra show a red shift in the presence of SDS and blue shift in the presence of CTAB and OGM. The blue shift in the absorption edge indicates the quantum confinement property of nanoparticles. The zinc peroxide nanoparticles prepared in additives-free media was also characterized by Raman spectra which show the characteristic peaks at 830-840 and 420-440 cm -1 .

  7. Synthesis of hydrogels of alginate for system controlled release of progesterone

    International Nuclear Information System (INIS)

    Abreu, Marlon de F.; Rodriguez, Ruben J.S.; Silva, Ester C.C. da; Barreto, Gabriela N.S.

    2015-01-01

    The chemical modifications of natural polymers like alginate, has allowed the development of new formulations for controlled release systems. In this work we report the synthesis of a derivative of the amidic alginate with alkyl chain. The polymer was characterized by spectroscopic techniques: Nuclear Magnetic Resonance and Fourier Transform Infrared. (author)

  8. Synthesis, characterization and antimicrobial activities of a Schiff ...

    African Journals Online (AJOL)

    Complexes of Cu(II), Ni(II) and Mn(II) with a Schiff base derived from condensation reaction of phenylalanine and acetylacetone have been synthesized and characterized analytically and spectroscopically. Melting point of the Schiff base was 188oC and the complexes decompose within a temperature range of 210-242oC.

  9. Spectroscopic Characterization of Key Aromatic Molecules: A Route toward The Origin of Life.

    Science.gov (United States)

    Puzzarini, Cristina; Baiardi, Alberto; Bloino, Julien; Barone, Vincenzo; Murphy, Thomas E; Drew, Dennis; Ali, Ashraf

    2017-08-04

    To gain information on the abiotic synthesis of the building blocks of life from simple molecules, and their subsequent chemical evolution to biological systems, the starting point is the identification of target species in Titan-like planets, i.e., planets that resemble the primitive Earth, as well as in Earth-like planets in the habitable zone of their star, namely planets where life can be already originated. In this scenario, molecular spectroscopy plays a crucial role because spectroscopic signatures are at the basis of an unequivocal proof for the presence of these target molecules. Thanks to the advances in many different techniques and to the NASA successful Kepler exoplanet transit mission, thousands of diverse planets outside of our solar system have been discovered. The James Webb Space Telescope (JWST), scheduled to be launched in 2018, will be very helpful in the identification of biosignature gases in Earth-like planets' atmospheres and of prebiotic molecule signatures in Titan-like atmospheres by observing their absorption during transits. While the search for key-target molecules in exoplanet atmospheres can be carried out by the JWST Transit Spectroscopy in the infrared (IR) region (0.6 - 29 µm wavelength range), opportunities for their detection in protostellar cores, protoplanetary disks and on Titan are also offered by the interferometric high spectral and spatial resolution observations using the Atacama Large Millimeter/submillimeter Array (ALMA). In the present work, target molecules have been selected and their spectroscopic characterization presented in view of supporting their infrared and complementary millimeter/submillimeter-wave spectral observations. In detail, the selected target molecules include: (1) the three-membered oxygen-containing heterocycles: oxirane and protonated oxirane, (2) the cyclopropenyl cation and its methyl derivative, (3) two examples of ortho- and peri-fused tri-cyclic aromatic rings, i.e., the phenalenyl

  10. The effect of synthesis temperature on the formation of hydrotalcites in Bayer liquor: a vibrational spectroscopic analysis.

    Science.gov (United States)

    Palmer, Sara J; Frost, Ray L

    2009-07-01

    The seawater neutralization process is currently used in the alumina industry to reduce the pH and dissolved metal concentrations in bauxite refinery residues through the precipitation of Mg, Al, and Ca hydroxide and carbonate minerals. This neutralization method is very similar to the co-precipitation method used to synthesize hydrotalcite (Mg6Al2(OH)16CO3.4H2O). This study looks at the effect of temperature on the type of precipitates that form from the seawater neutralization process of Bayer liquor. The Bayer precipitates have been characterized by a variety of techniques, including X-ray diffraction (XRD), Raman spectroscopy, and infrared spectroscopy. The mineralogical composition of Bayer precipitates largely includes hydrotalcite, hydromagnesite, and calcium carbonate species. Analysis with XRD determined that Bayer hydrotalcites that are synthesized at 55 degrees C have a larger interlayer distance, indicating that more anions are removed from Bayer liquor. Vibrational spectroscopic techniques have identified an increase in hydrogen bond strength for precipitates formed at 55 degrees C, suggesting the formation of a more stable Bayer hydrotalcite. Raman spectroscopy identified the intercalation of sulfate and carbonate anions into Bayer hydrotalcites using these synthesis conditions.

  11. Synthesis and characterization of tunable coumarin- linked glasses as new class of organic/inorganic phosphors

    Energy Technology Data Exchange (ETDEWEB)

    Luridiana, Alberto; Pretta, Gianluca; Secci, Francesco; Frongia, Angelo [Dipartimento di Scienze Chimiche e Geologiche, Università degli Studi di Cagliari, Complesso universitario di Monserrato, SS 554, bivio per Sestu, Monserrato (Canada) (Italy); Chiriu, Daniele; Carbonaro, Carlo Maria; Corpino, Riccardo [Dipartimento di Fisica, Università degli Studi di Cagliari, Complesso universitario di Monserrato, SS 554, bivio per Sestu, Monserrato (Canada) (Italy); Ricci, Pier Carlo, E-mail: carlo.ricci@dsf.unica.it [Dipartimento di Fisica, Universitá degli Studi di Cagliari, S.P. Monserrato-Sestu Km 0,700, 09042 Monserrato (Canada) (Italy)

    2014-10-21

    It is well known that stilbene with a trans conformation is highly fluorescent. From the viewpoint of molecular structure, coumarins bear a carbon-carbon double bond which is fixed as trans conformation as in trans-stilbene through a lactone structure. This can help to avoid the trans-cis transformation of the double bond under ultraviolet (UV) irradiation as observed in stilbene compounds and results in strong fluorescence and high fluorescence quantum yield and photostability in most of coumarin derivatives. Herein we report some preliminary results about the synthesis and spectroscopic characterization of tunable coumarins and the development of a new linkage protocol for the obtainment of monolayer coumarin-covalently linked glasses. The resulting organic/inorganic coumarin/silica based Self-Assembled Monolayer (SMA) film is proposed as new phosphors for the substituting of critical raw materials, like rare earths, in photonics applications.

  12. An Efficient Catalyst for the Synthesis of Schiff Bases

    International Nuclear Information System (INIS)

    Fareed, G.; Afza, N.; Kalhoro, M.A.

    2013-01-01

    An efficient high yielding synthesis of Schiff bases (1-17) is derived from condensation of 2-fluorenamine and 4-amino phenol with a variety of aldehydes catalyzed by dodecatungstosilicic acid P/sub 2/O/sub 5/ under solvent free conditions at room temperature. The catayst is found to be more efficient in terms of ease of reaction workup and high yields. This methodology contributes to an energy efficient, facile and environamental friendly synthesis for the preparation of Schiff bases. The structures of afforded Schiff bases were characterized by spectroscopic data and elemental analysis. (author)

  13. Synthesis, spectroscopic, and molecular structure characterizations of some azo derivatives of 2-hydroxyacetophenone

    Science.gov (United States)

    Albayrak, Çiğdem; Gümrükçüoğlu, İsmail E.; Odabaşoğlu, Mustafa; İskeleli, Nazan Ocak; Ağar, Erbil

    2009-08-01

    Some novel azo compounds were prepared by the reaction of 2-hydroxyacetophenone with aniline and its substituted derivatives. The structures of synthesized azo compounds were determined by IR, UV-Vis, 1H NMR and 13C NMR spectroscopic techniques and the structures of some of these compounds were also determined by X-ray diffraction studies. Structural analysis using IR in solid state shows that the azo form is favoured in the azo compounds whereas UV-Vis analysis of the azo compounds in solution has shown that there is a azo and ionic form. The azo compounds in the basic solvents dimethylformamide (DMF) and dimethylsulfoxide (DMSO) are both azo and ionic form while these compounds in ethyl alcohol (EtOH) and chloroform (CHCl 3) are only azo form.

  14. Electroactive chain-like compounds constructed from trimetallic clusters and 4,4'-bipyridine spacers: one-pot synthesis, characterization and surface binding.

    Science.gov (United States)

    Abe, Masaaki; Inatomi, Atsushi; Hisaeda, Yoshio

    2011-03-14

    This paper reports the synthesis and characterization of a novel series of chain-like compounds where oxo-centered triruthenium cluster moieties are bridged by 4,4'-bipyridine (4,4'-bpy) spacers. A reaction of solvent-coordinated triruthenium "monomer" precursor [Ru(3)O(CH(3)CO(2))(6)(CO)(CH(3)OH)(2)] with a 0.1 equimolar amount of 4,4'-bpy in CH(3)OH gave mixture of chain-like compounds containing "dimers" to "tetramers" which were cleanly separated by column chromatography and characterized by spectroscopic and electrochemical methods. Cyclic voltammetry revealed that all chain-like compounds exhibit reversible and stepwise redox processes in solution with very weak intramolecular coupling between the triruthenium components across the 4,4'-bpy bridge. Photo-induced dissociation of CO from the compounds and electrode surface binding were also investigated.

  15. Synthesis, characterization and comparison of polythiophene ...

    Indian Academy of Sciences (India)

    38

    Synthesis, characterization and comparison of polythiophene-carbon ... b Nanotechnology Research Institute, School of Chemical Engineering, Babol University of Technology, Babol, ..... The scan range was from −0.24 to 1.2 V in reference to.

  16. Absorption and emission spectroscopic characterization of 10-phenyl-isoalloxazine derivatives

    International Nuclear Information System (INIS)

    Shirdel, J.; Penzkofer, A.; Prochazka, R.; Daub, J.; Hochmuth, E.; Deutzmann, R.

    2006-01-01

    The flavoquinone dyes 10-phenyl-isoalloxazine-3-acetic acid ethyl ester (1) and 10-(4-bromo-phenyl)-3-methyl-isoalloxazine (2) in dichloromethane, acetonitrile, and methanol are characterized by absorption and emission spectroscopy. Absorption cross-section spectra, stimulated emission cross-section spectra, fluorescence quantum distributions, quantum yields, lifetimes, and degrees of fluorescence polarization are determined. The blue-light photo-degradation of the dyes is studied. Mass spectroscopic measurements reveal the formation of phenyl-benzo-pteridine (isoalloxazine) derivatives, tetraaza-benzo-aceanthrylene derivatives, dihydro-quinooxaline derivatives, and pyrazino-carbazole derivatives. An enhancement of photo-degradation is observed by the formed photo-fragments

  17. An efficient synthesis and spectroscopic characterization of Schiff bases containing 9,10-anthracenedione moiety

    Directory of Open Access Journals (Sweden)

    Fareed Ghulam

    2013-01-01

    Full Text Available A new method has been developed for the synthesis of novel Schiff bases containg anthraquinone moiety using dodeca-Tungstosilicic acid/P2O5 under solvent free conditions at room temperature. The reaction was completed in 1-3 minutes with excellent yields. This method was found to be more efficient, easy and hazardous free for the synthesis of azomethines. The development of these type of methadologies in synthetic chemistry may contribute to green chemistry. The structures of synthesized novel Schiff bases was elucidated using 1H-NMR, 13C-NMR, LCMS, FTIR and CHN analysis.

  18. SYNTHESIS, SPECTROSCOPIC CHARACTERIZATION AND ...

    African Journals Online (AJOL)

    userpc

    ABSTRACT. A tridendatate Schiff base,L, 2-((2-hydroxynaphthalen-1-yl) methyleneamino)benzoic acid was prepared by condensation of 2-aminobenzoic acid with 2-hydroxy-1-naphthaldehyde.The prepared ligand was used to synthesize Sm(III) and Dy(III) complexes [LnL(NO3)2]NO3.2H2O,. (Ln=Sm(III) and Dy(III)).

  19. Synthesis and characterization of nano silicon and titanium nitride ...

    Indian Academy of Sciences (India)

    The characterization techniques indicated ... Scalable synthesis; microwave plasma; chemical synthesis; nanoparticles. 1. Introduction ... used but very few methods are available to produce silicon and titanium ... current (A). (m3/h). 1. Si. 2.1.

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

    African Journals Online (AJOL)

    Synthesis, characterization, antimicrobial activity and molecular docking studies of combined pyrazol-barbituric acid pharmacophores. Assem Barakat, Bandar M. Al-Qahtani, Abdullah M. Al-Majid, M. Ali Mohammed Rafi Shaik, Mohamed H.M. Al-Agamy, Abdul Wadood ...

  1. Synthesis, structural analysis, Hirshfeld surface, spectroscopic characterization and, in vitro, antioxidant activity of a novel organic cyclohexaphosphate

    Science.gov (United States)

    Fezai, Ramzi; Mezni, Ali; Rzaigui, Mohamed

    2018-02-01

    The new hybrid [4-Cl-2-(CH3)C6H3NH3]6P6O18·2H2O was synthesized under normal conditions of temperature and pressure. Single crystal X-ray diffraction study was used to identify its structure. It revealed that this organic cyclohexaphosphate crystallized in the P 1 bar triclinic space group with a = 10.41 (10) Å b = 10.94 (7) Å, c = 15.45 (10) Å, α = 77.37 (8), β = 89.75 (8)°, γ = 61.69 (7)°, V = 1501 (2) Å3 and Z = 1. In the crystal framework, the assembling of the three dimensional (3D) structure is formed by intermolecular hydrogen bonds and Van Der Waals interactions. A spectroscopic characterization was carried out to elucidate the structure (UV-Vis, FTIR, 31P MAS-NMR and fluorescent properties). The thermal stability was studied by TG-DTA diagrams under argon atmosphere. Furthermore, 3-D Hirshfeld surfaces in combination with 2-D fingerprint plots were carried out. This compound was also evaluated for its antioxidant activity; four tests were done, in vitro, 1,1-diphenyl-2-picrylhydrazyl (DPPH•), hydroxyl scavenging ability (OH•), ferric reducing power (FRP) and ferrous ion chelating (FIC) ability, using ascorbic acid as a control.

  2. synthesis and optical characterization of acid-doped polyaniline thin

    African Journals Online (AJOL)

    HOD

    SYNTHESIS AND OPTICAL CHARACTERIZATION OF ACID-DOPED. POLYANILINE THIN .... MATERIALS AND METHODS .... Characterization of Se Doped Polyaniline”,Current. Applied ... with Silver Nanoparticles”, Advances in Materials.

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

    African Journals Online (AJOL)

    MBI

    2015-12-08

    Dec 8, 2015 ... Synthesis, Characterization, Antimicrobial Activity and Antioxidant. Studies of ... Transition metal complexes of Co(II) and Ni(II) with Schiff base ligand (HL) derived from condensation of 2- ..... 2-((5mercapto-1,3,4-thiadiazol-2-.

  4. 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.

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

    International Nuclear Information System (INIS)

    Thappily, Praveen; Shiju, K.

    2014-01-01

    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

  6. Spectroscopic detection, characterization and dynamics of free radicals relevant to combustion processes

    Energy Technology Data Exchange (ETDEWEB)

    Miller, Terry [The Ohio State Univ., Columbus, OH (United States)

    2015-06-04

    Combustion chemistry is enormously complex. The chemical mechanisms involve a multitude of elementary reaction steps and a comparable number of reactive intermediates, many of which are free radicals. Computer simulations based upon these mechanisms are limited by the validity of the mechanisms and the parameters characterizing the properties of the intermediates and their reactivity. Spectroscopy can provide data for sensitive and selective diagnostics to follow their reactions. Spectroscopic analysis also provides detailed parameters characterizing the properties of these intermediates. These parameters serve as experimental gold standards to benchmark predictions of these properties from large-scale, electronic structure calculations. This work has demonstrated the unique capabilities of near-infrared cavity ringdown spectroscopy (NIR CRDS) to identify, characterize and monitor intermediates of key importance in complex chemical reactions. Our studies have focussed on the large family of organic peroxy radicals which are arguably themost important intermediates in combustion chemistry and many other reactions involving the oxidation of organic compounds. Our spectroscopic studies have shown that the NIR Ã - ˜X electronic spectra of the peroxy radicals allows one to differentiate among chemical species in the organic peroxy family and also determine their isomeric and conformic structure in many cases. We have clearly demonstrated this capability on saturated and unsaturated peroxy radicals and β-hydroxy peroxy radicals. In addition we have developed a unique dual wavelength CRDS apparatus specifically for the purpose of measuring absolute absorption cross section and following the reaction of chemical intermediates. The utility of the apparatus has been demonstrated by measuring the cross-section and self-reaction rate constant for ethyl peroxy.

  7. Electrochemical synthesis and characterization of stable colloidal suspension of graphene using two-electrode cell system

    Energy Technology Data Exchange (ETDEWEB)

    Danial, Wan Hazman, E-mail: hazmandanial@gmail.com; Majid, Zaiton Abdul, E-mail: zaiton@kimia.fs.utm.my; Aziz, Madzlan [Department of Chemistry, Faculty of Science, Universiti Teknologi Malaysia (UTM), 81310 Skudai, Johor (Malaysia); Chutia, Arunabhiram [Institute of Fluid Sciences, Tohoku University, Sendai 980-8577 (Japan); Sahnoun, Riadh [Ibnu Sina Institute for Fundamental Science Studies, Universiti Teknologi Malaysia (UTM), 81310 Skudai, Johor (Malaysia)

    2015-07-22

    The present work reports the synthesis and characterization of graphene via electrochemical exfoliation of graphite rod using two-electrode system assisted by Sodium Dodecyl Sulphate (SDS) as a surfactant. The electrochemical process was carried out with sequence of intercalation of SDS onto the graphite anode followed by exfoliation of the SDS-intercalated graphite electrode when the anode was treated as cathode. The effect of intercalation potential from 5 V to 9 V and concentration of the SDS surfactant of 0.1 M and 0.01 M were investigated. UV-vis Spectroscopic analysis indicated an increase in the graphene production with higher intercalation potential. Transmission Electron Microscopy (TEM) analysis showed a well-ordered hexagonal lattice of graphene image and indicated an angle of 60° between two zigzag directions within the honeycomb crystal lattice. Raman spectroscopy analysis shows the graphitic information effects after the exfoliation process.

  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. Spectroscopic characterization of D-003 obtained from the sugar cane (Saccharum officinarum L.) wax

    International Nuclear Information System (INIS)

    Marrero Delange, David; Cora Medina, Miriam; Laguna Granja, Abilio; Gonzalez Canavaciolo Victor L

    2013-01-01

    D-003, an active pharmaceutical ingredient (API) purified from sugar cane (Saccharum officinarum L.) wax with cholesterol-lowering and antioxidant effects, is composed of a mixture of free saturated very long chain fatty acids (VLCFAs), each within specific relative concentration ranges as determined by the gas chromatography (GC). However, the spectroscopic characterization of D-003 had not been previously reported

  10. Electrochemical synthesis and spectroscopic characterization of poly(N-phenylpyrrole coatings in an organic medium on iron and platinum electrodes

    Directory of Open Access Journals (Sweden)

    A.K.D. Diaw

    2008-12-01

    Full Text Available The electrochemical synthesis of poly(N-phenylpyrrole film was achieved on pretreated iron and platinum electrodes in acetonitrile solutions containing 0.1 M N-phenylpyrrole as the monomer and 0.1 M tetrabutylammonium trifluoromethane sulfonate (Bu4NCF3SO3 as the supporting-salt. The results showed that a surface treatment by 10 % aqueous nitric acid inhibits iron dissolution without preventing the N-phenylpyrrole oxidation. Very strongly adherent films were obtained at constant-potential, constant-current and cyclic voltammetry. XPS measurements, infrared (FT-IR and electronic absorption (UV-vis spectroscopies were used to characterize the iron and platinum-coated electrodes. Finally the anticorrosion properties of the PΦP film were evidenced.

  11. Spectroscopic characterization approach to study surfactants effect on ZnO{sub 2} nanoparticles synthesis by laser ablation process

    Energy Technology Data Exchange (ETDEWEB)

    Drmosh, Q.A. [Laser Research Group, Physics Department, King Fahd University of Petroleum and Minerals, Dhahran 31261 (Saudi Arabia); Center of Excellence in Nanotechnology (CENT), King Fahd University of Petroleum and Minerals, Dhahran 31261 (Saudi Arabia); Gondal, M.A., E-mail: magondal@kfupm.edu.sa [Laser Research Group, Physics Department, King Fahd University of Petroleum and Minerals, Dhahran 31261 (Saudi Arabia); Center of Excellence in Nanotechnology (CENT), King Fahd University of Petroleum and Minerals, Dhahran 31261 (Saudi Arabia); Yamani, Z.H. [Laser Research Group, Physics Department, King Fahd University of Petroleum and Minerals, Dhahran 31261 (Saudi Arabia); Center of Excellence in Nanotechnology (CENT), King Fahd University of Petroleum and Minerals, Dhahran 31261 (Saudi Arabia); Saleh, T.A. [Center of Excellence in Nanotechnology (CENT), King Fahd University of Petroleum and Minerals, Dhahran 31261 (Saudi Arabia); Chemistry Department, King Fahd University of Petroleum and Minerals, Dhahran 31261 (Saudi Arabia)

    2010-05-01

    Zinc peroxide nanoparticles having grain size less than 5 nm were synthesized using pulsed laser ablation in aqueous solution in the presence of different surfactants and solid zinc target in 3% H{sub 2}O{sub 2}. The effect of surfactants on the optical and structure of ZnO{sub 2} was studied by applying different spectroscopic techniques. Structural properties and grain size of the synthesized nanoparticles were studied using XRD method. The presence of the cubic phase of zinc peroxide in all samples was confirmed with XRD, and the grain sizes were 4.7, 3.7, 3.3 and 2.8 nm in pure H{sub 2}O{sub 2}, and H{sub 2}O{sub 2} mixed with SDS, CTAB and OGM respectively. For optical characterization, FTIR transmittance spectra of ZnO{sub 2} nanoparticles prepared with and without surfactants show a characteristic ZnO{sub 2} absorption at 435-445 cm{sup -1}. FTIR spectrum revealed that the adsorbed surfactants on zinc peroxide disappeared in case of CTAB and OGM while it appears in case of SDS. This could be due to high critical micelles SDS concentration comparing with others which is attributed to the adsorption anionic nature of this surfactant. Both FTIR and UV-vis spectra show a red shift in the presence of SDS and blue shift in the presence of CTAB and OGM. The blue shift in the absorption edge indicates the quantum confinement property of nanoparticles. The zinc peroxide nanoparticles prepared in additives-free media was also characterized by Raman spectra which show the characteristic peaks at 830-840 and 420-440 cm{sup -1}.

  12. Synthesis and characterization of semi-IPNs based on PVP and PLLA; Sintese e caracterizacao de semi-IPNs envolvendo os homopolimeros PVP e PLLA

    Energy Technology Data Exchange (ETDEWEB)

    Camilo, A.P.R.; Mano, V., E-mail: mano@ufsj.edu.b [Universidade Federal de Sao Joao del Rei (UFSJ), MG (Brazil). Dept. de Ciencias Naturais; Felisberti, M.I. [Universidade Estadual de Campinas (IQ/UNICAMP), SP (Brazil). Inst. de Quimica

    2010-07-01

    The specific interest in the synthesis of semi-IPNs based on PLLA and PVP homopolymers due to the fact these are biodegradable and biocompatible, which allows us to infer applications in the medical field as sutures, implants, matrices for controlled release of drugs etc. The objective was to prepare a multicomponent material amphiphile in the form of semi-interpenetrating polymer networks, based on poly (L-lactide), PLLA, hydrophobic homopolymer, and poly (vinylpyrrolidone), PVP, hydrophilic component. The preparation of semi-IPN combined the polymerization and crosslinking of N-vinylpyrrolidone in the presence of poly (L-lactide). The products were characterized by spectroscopic and thermal methods. (author)

  13. Synthesis, characterization and spectroscopic studies of the dihydrobis(1,2,3-benzotriazolylborate anion and its complexes with MCl2·py2

    Directory of Open Access Journals (Sweden)

    KHWAJA S. SIDDIQI

    2006-11-01

    Full Text Available The preparation of sodium dihydrobis(1,2,3-benzotriazolylborate was realised by refluxing one mole of sodium borohydride with two moles of 1,2,3-benzotriazole in toluene over a period of 12 h. Its complexes with MCl2·py2 [whereM=Mn(II, Fe(II, Co(II, Ni(II, Cu(II and py=pyridine] were characterized by elemental analysis as well as magnetic, spectroscopic and conductivity measurements. On the basis of these studies, it is proposed that the geometry of all the complexes is octahedral. The ligand field parameters 10 Dq, B and b show extensive overlap between the M–L orbital. The molar conductance of 10-3 M solutions of the complexes in DMSO suggest them to be non-ionic in nature.

  14. Synthesis and characterization of a novel laser ablation sensitive triazene incorporated epoxy resin

    KAUST Repository

    Patole, Archana S.

    2014-01-01

    New triazene monomer was synthesized and further employed as a crosslinking agent partner with epoxy matrix using ethyl methyl imidazole as a curing agent in order to investigate the effect of triazene moieties on polymeric properties for laser ablation application. The synthesized triazene monomer was characterized by analytical and spectroscopic methods, while the surface morphology of resist after laser ablation was visualized by optical laser scanning images and scanning electron microscopy. Thermogravimetrical investigations indicate the loss of nitrogen being the initial thermal decomposition step and exhibit sufficient stabilities for the requirements for laser ablation application. Fourier transform infra-red, nuclear magnetic resonance, and gas chromatography analyses showed the successful synthesis of triazene. The ablation results from the optical laser scanning images revealed that the etching depth could be controlled by varying the concentration of triazene monomer in the formulation of epoxy. The shear strength analysis revealed that that the shear strength increased with increasing the amount of triazene in the formulation of direct ablation sensitive resist. © 2014 The Korean Institute of Metals and Materials and Springer Science+Business Media Dordrecht.

  15. Variable angle spectroscopic ellipsometric characterization of HfO2 thin film

    Science.gov (United States)

    Kumar, M.; Kumari, N.; Karar, V.; Sharma, A. L.

    2018-02-01

    Hafnium Oxide film was deposited on BK7 glass substrate using reactive oxygenated E-Beam deposition technique. The film was deposited using in-situ quartz crystal thickness monitoring to control the film thickness and rate of evaporation. The thin film was grown with a rate of deposition of 0.3 nm/s. The coated substrate was optically characterized using spectrophotometer to determine its transmission spectra. The optical constants as well as film thickness of the hafnia film were extracted by variable angle spectroscopic ellipsometry with Cauchy fitting at incidence angles of 65˚, 70˚ and 75˚.

  16. Characterization of cytochrome c as marker for retinal cell degeneration by uv/vis spectroscopic imaging

    Science.gov (United States)

    Hollmach, Julia; Schweizer, Julia; Steiner, Gerald; Knels, Lilla; Funk, Richard H. W.; Thalheim, Silko; Koch, Edmund

    2011-07-01

    Retinal diseases like age-related macular degeneration have become an important cause of visual loss depending on increasing life expectancy and lifestyle habits. Due to the fact that no satisfying treatment exists, early diagnosis and prevention are the only possibilities to stop the degeneration. The protein cytochrome c (cyt c) is a suitable marker for degeneration processes and apoptosis because it is a part of the respiratory chain and involved in the apoptotic pathway. The determination of the local distribution and oxidative state of cyt c in living cells allows the characterization of cell degeneration processes. Since cyt c exhibits characteristic absorption bands between 400 and 650 nm wavelength, uv/vis in situ spectroscopic imaging was used for its characterization in retinal ganglion cells. The large amount of data, consisting of spatial and spectral information, was processed by multivariate data analysis. The challenge consists in the identification of the molecular information of cyt c. Baseline correction, principle component analysis (PCA) and cluster analysis (CA) were performed in order to identify cyt c within the spectral dataset. The combination of PCA and CA reveals cyt c and its oxidative state. The results demonstrate that uv/vis spectroscopic imaging in conjunction with sophisticated multivariate methods is a suitable tool to characterize cyt c under in situ conditions.

  17. Synthesis and characterization of a new composite based on copper (II) and octa (aminopropil)silsesquioxane

    International Nuclear Information System (INIS)

    Magossi, M.S. de; Carmo, D.R. do

    2014-01-01

    In this work, a new compound based silsesquioxane and nitroprusside of copper was prepared starting from octa (aminopropyl)silsesquioxane following a new route of synthesis. The composite prepared as described ACCuN was preliminarily characterized by spectroscopic techniques, such as Infrared Spectroscopy in the Region of the Fourier transform (FTIR), Energy Dispersive X-ray (EDX), Scanning Electron Microscopy (SEM) and cyclic voltammetry (VC). The FTIR spectra showed absorption bands at 1106 cm"-"1 due to stretching Si-O-Si_(_ν_S_i_-_O_-_S_i_) characteristic of the structure of octa(aminopropylsilsesquioxane and absorption bands at 2063 cm"-"1 ascribed to the stretching NO_(_ν_N_-_O) and 2192 cm"-"1 attributed to the stretching C≡N_(_ν_≡N_). SEM and EDX observed cluster of cubic particles with an average size of approximately 241 nm, containing Si, O, N, Cu and Fe. Cyclic voltammogram of the material (ACCuN) showed a redox couple with average potential Eθ '= 0.73 V. (author)

  18. Synthesis and spectroscopic and structural characterization of the monomeric diborylphosphine and diphosphinoborane compounds PhP(BMes2)2 and MesB(PPh2)2 (Mes = 2,4,6-Me3C6H2)

    International Nuclear Information System (INIS)

    Bartlett, R.A.; Dias, H.V.R.; Power, P.P.

    1988-01-01

    The synthesis and spectroscopic and first x-ray structural characterization of a diborylphosphine, PhP(BMes 2 ) 2 (1), and a diphosphinoborane, MesB(PPh 2 ) 2 (2), are described. The structure of 1 has a planar core that involves the phosphorus and two boron atoms and also the five substituent carbons. In addition, the B-P bond lengths are shortened, which suggests a close structural analogy between 1 and the allyl cation. In the case of 2, although the boron remains planar, both phosphorus centers are pyramidal with slightly longer B-P bonds than in 1. Both 1 and 2 are the first examples of their respective classes of compound to be well characterized. Crystal data with Mo Kα radiation (λ = 0.71069 /angstrom/) at 130 K are as follows. 1: a = 14.302 (4) /angstrom/, b = 15.701 (3) /angstrom/, c = 16.601 (6) /angstrom/, β = 109.61 (2)/degrees/; monoclinic, space group C2/c, Z = 4, R = 0.059. 2: a = 7.815 (2) /angstrom/, b = 8.723 (2) /angstrom/, c = 40.147 (10) /angstrom/, β = 94.90 (2)/degrees/; monoclinic, space group P2 1 /n, Z = 4, R = 0.041. A listing of available 11 B and 31 P NMR data on compounds involving triply connected boron and phosphorus centers is also provided and discussed in the context of the data for 1 and 2. 25 references, 2 figures, 4 tables

  19. Synthesis and characterization of dextran-coated iron oxide nanoparticles

    Science.gov (United States)

    Predescu, Andra Mihaela; Matei, Ecaterina; Berbecaru, Andrei Constantin; Pantilimon, Cristian; Drăgan, Claudia; Vidu, Ruxandra; Predescu, Cristian; Kuncser, Victor

    2018-03-01

    Synthesis and characterization of iron oxide nanoparticles coated with a large molar weight dextran for environmental applications are reported. The first experiments involved the synthesis of iron oxide nanoparticles which were coated with dextran at different concentrations. The synthesis was performed by a co-precipitation technique, while the coating of iron oxide nanoparticles was carried out in solution. The obtained nanoparticles were characterized by using scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction spectrometry, Fourier transform infrared spectroscopy and superconducting quantum interference device magnetometry. The results demonstrated a successful coating of iron oxide nanoparticles with large molar weight dextran, of which agglomeration tendency depended on the amount of dextran in the coating solution. SEM and TEM observations have shown that the iron oxide nanoparticles are of about 7 nm in size.

  20. MnWO{sub 4} nanocapsules: Synthesis, characterization and its electrochemical sensing property

    Energy Technology Data Exchange (ETDEWEB)

    Muthamizh, Selvamani; Suresh, Ranganathan; Giribabu, Krishnamoorthy; Manigandan, Ramadoss; Praveen Kumar, Sivakumar; Munusamy, Settu; Narayanan, Vengidusamy, E-mail: vnnara@yahoo.co.in

    2015-01-15

    Highlights: • Synthesis of MnWO{sub 4} nanocapsules without use of any other external reagent. • High crystalline MnWO{sub 4} was obtained with phase purity. • Electrochemical sensing platform based on MnWO{sub 4} for sensing quercetin. • Micromolar detection ability of MnWO{sub 4} modified GCE. - Abstract: Manganese tungstate (MnWO{sub 4}) was synthesized by surfactant free precipitation method. MnWO{sub 4} was characterized by using various spectroscopic techniques. The phase, crystalline nature and the morphological analysis were carried out using XRD, scanning electron microscopy (SEM), and high resolution transmission electron microscopy (HR-TEM). Further, FT-IR, Raman, and DRS-UV–Vis spectral analysis were carried out in order to ascertain the optical property and the presence of functional groups. From the analysis, the morphology of the MnWO{sub 4} was observed to be in capsules with breadth and thickness were in nm range. The oxidation state of tungsten (W), and manganese (Mn) were investigated using X-ray photo electron spectroscopy (XPS) and electron paramagnetic resonance spectroscopy (EPR). The synthesized MnWO{sub 4} nanocapsules were used to modify glassy carbon electrode (GCE) to detect quercetin.

  1. Spectroscopic methods for characterization of nuclear fuels

    International Nuclear Information System (INIS)

    Sastry, M.D.

    1999-01-01

    Spectroscopic techniques have contributed immensely in the characterisation and speciation of materials relevant to a variety of applications. These techniques have time tested credentials and continue to expand into newer areas. In the field of nuclear fuel fabrication, atomic spectroscopic methods are used for monitoring the trace metallic constituents in the starting materials and end product, and for monitoring process pick up. The current status of atomic spectroscopic methods for the determination of trace metallic constituents in nuclear fuel materials will be briefly reviewed and new approaches will be described with a special emphasis on inductively coupled plasma techniques and ETV-ICP-AES hyphenated techniques. Special emphasis will also be given in highlighting the importance of chemical separation procedures for the optimum utilization of potential of ICP. The presentation will also include newer techniques like Photo Acoustic Spectroscopy, and Electron Paramagnetic Resonance (EPR) Imaging. PAS results on uranium and plutonium oxides will be described with a reference to the determination of U 4+ /U 6+ concentration in U 3 O 8 . EPR imaging techniques for speciation and their spatial distribution in solids will be described and its potential use for Gd 3+ containing UO 2 pellets (used for flux flattening) will be highlighted. (author)

  2. 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.

  3. Synthesis and characterization of rare-earth-doped calcium tungstate nanocrystals

    Science.gov (United States)

    Suneeta, P.; Rajesh, Ch.; Ramana, M. V.

    2018-02-01

    In this paper, we report synthesis and characterization of rare-earth-ion-doped calcium tungstate (CaWO4) nanocrystals (NCs). Rare-earth ions, such as gadolinium (Gd), neodymium (Nd), praseodymium (Pr), samarium (Sm) and holmium (Ho), were successfully doped in the CaWO4 NCs by changing the synthesis conditions. The adopted synthesis route was found to be fast and eco-friendly. Structural characterizations, such as X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and compositional analysis, were performed using energy dispersive analysis of X-rays (EDAX) on as-synthesized NCs. The results indicate the size of the NCs ranging between 47 to 68nm and incorporation of rare-earth ions in CaWO4 NCs.

  4. Synthesis of selectively 13C-labelled benzoic acid for nuclear magnetic resonance spectroscopic measurement of glycine conjugation activity

    International Nuclear Information System (INIS)

    Akira, Kazuki; Hasegawa, Hiroshi; Baba, Shigeo

    1995-01-01

    The synthesis of [4- 13 C]benzoic acid (BA) labelled in a single protonated carbon, for use as a probe to measure glycine conjugation activity by nuclear magnetic resonance (NMR) spectroscopy, has been reported. The labelled compound was prepared by a seven-step synthetic scheme on a relatively small scale using [2- 13 C] acetone as the source of label in overall yield of 16%. The usefulness of [4- 13 C]BA was demonstrated by the NMR spectroscopic monitoring of urinary excretion of [4- 13 C]hippuric acid in the rat administered with the labelled BA. (Author)

  5. Novel biosynthesis of Ag-hydroxyapatite: Structural and spectroscopic characterization

    Science.gov (United States)

    Ruíz-Baltazar, Álvaro de Jesús; Reyes-López, Simón Yobanny; Silva-Holguin, Pamela Nair; Larrañaga, Daniel; Estévez, Miriam; Pérez, Ramiro

    2018-06-01

    Silver-doped hydroxyapatite (Ag-HAP) was obtained by green synthesis route. The dopant silver nanoparticles (AgNPs) were obtained by biosynthesis based on Melissa officinalis extract. This research is focused on the characterization and the use of the nontoxic and environment-friendly Ag-HAP nanocomposite. The structural and morphological characterization of Ag-HAP nanocomposite was carried out by scanning electron microscopy (SEM), X-ray diffraction, Fourier-transform infrared (FT-IR) and Raman spectroscopy. The obtained nanoparticles exhibited a great interaction with the HAP matrix, performing an Ag-HAP nanocomposite. Changes in the structure of the Ag-HAP nanocomposite were corroborated by the different characterization techniques. Additionally, a homogeneous distribution of the AgNPs on the HAP structure was observed. The heterogeneous nucleation process employed to doping the HAP, offer a functional route to obtain a green composite with potentials applications in multiple fields, such as tissue engineering, bone repair as well as protein. These properties can be evaluated in subsequent studies.

  6. Synthesis, characterization, thermal

    Directory of Open Access Journals (Sweden)

    Selma Bal

    2017-09-01

    Full Text Available This work explains the synthesis of a new azo-Schiff base compound, derived from condensation between N-ethylcarbazole-3-carbaldehyde and 1,3-diaminopropane, followed by azo coupling reaction with the diazonium salt of 2-amino-4-methyl phenol. The newly synthesized azo-Schiff base was further reacted with the acetate salts of Copper, Cobalt and Nickel to give three coordination compounds. All synthesized compounds have been characterized through spectral analysis. The coordination compounds have been examined for their thermal and catalytic features. Good and moderate yields were obtained for the oxidation of styrene and cyclohexene. Thermal features of the ligand and its complexes have been explained and the results obtained have supported the proposed structures.

  7. Spectroscopic characterization of schiff base-copper complexes immobilized in smectite clays

    Directory of Open Access Journals (Sweden)

    Patrícia M. Dias

    2010-01-01

    Full Text Available Herein, the immobilization of some Schiff base-copper(II complexes in smectite clays is described as a strategy for the heterogenization of homogeneous catalysts. The obtained materials were characterized by spectroscopic techniques, mostly UV/Vis, EPR, XANES and luminescence spectroscopy. SWy-2 and synthetic Laponite clays were used for the immobilization of two different complexes that have previously shown catalytic activity in the dismutation of superoxide radicals, and disproportionation of hydrogen peroxide. The obtained results indicated the occurrence of an intriguing intramolecular redox process involving copper and the imine ligand at the surface of the clays. These studies are supported by computational calculations.

  8. Spectroscopic characterization of Simultaneous determination of Albendazol from the sugar cane (Saccharum officinarum L.) wax

    International Nuclear Information System (INIS)

    Marrero Delange, David; Cora Medina, Miriam; Laguna Granja, Abilio; Gonzalez Canavaciolo, Victor L

    2013-01-01

    D-003, an active pharmaceutical ingredient (API) purified from sugar cane (Saccharum officinarum L.) wax with cholesterol-lowering and antioxidant effects, is composed of a mixture of free saturated very long chain fatty acids (VLCFAs), each within specific relative concentration ranges as determined by the gas chromatography (GC). However, the spectroscopic characterization of D-003 had not been previously reported

  9. Spectroscopic Characterization of Omeprazole and Its Salts

    Directory of Open Access Journals (Sweden)

    Tomislav Vrbanec

    2017-01-01

    Full Text Available During drug development, it is important to have a suitable crystalline form of the active pharmaceutical ingredient (API. Mostly, the basic options originate in the form of free base, acid, or salt. Substances that are stable only within a certain pH range are a challenge for the formulation. For the prazoles, which are known to be sensitive to degradation in an acid environment, the formulation is stabilized with alkaline additives or with the application of API formulated as basic salts. Therefore, preparation and characterization of basic salts are needed to monitor any possible salinization of free molecules. We synthesized salts of omeprazole from the group of alkali metals (Li, Na, and K and alkaline earth metals (Mg, Ca. The purpose of the presented work is to demonstrate the applicability of vibrational spectroscopy to discriminate between the OMP and OMP-salt molecules. For this reason, the physicochemical properties of 5 salts were probed using infrared and Raman spectroscopy, NMR, TG, DSC, and theoretical calculation of vibrational frequencies. We found out that vibrational spectroscopy serves as an applicable spectroscopic tool which enables an accurate, quick, and nondestructive way to determine the characteristic of OMP and its salts.

  10. Efficient synthesis and physicochemical characterization of natural danshensu, its S isomer and intermediates thereof

    Science.gov (United States)

    Sidoryk, Katarzyna; Filip, Katarzyna; Cmoch, Piotr; Łaszcz, Marta; Cybulski, Marcin

    2018-02-01

    The synthesis and molecular structure details of R- 3,4-dihydroxyphenyl lactic acid (danshensu) and related compounds, i.e. S isomer and the key intermediates have been described. Danshensu is an important water soluble phenolic acid of Salvia miltiorrhiza herb (danshen or red sag) with numerous applications in traditional Chinese medicine (TCM). Our synthetic approach was based on the Knoevenagel condensation of the protected 3,4-dihydroxybenzaldehyd and Meldrum acid derivative, followed by asymmetric Sharples dihydroxylation, reductive mono dehydroxylation and final deprotection. All compounds were characterized by various spectroscopic techniques: 1H-, 13C- magnetic resonance (NMR); Fourier-transformed infrared (FTIR); Raman, HR mass spectroscopy. For the determination of compound optical purities original HPLC methods were developed which allowed for the efficient resolution of danshensu R and S enantiomers as well as its intermediate enantiomers, using commercially available chiral stationary phases. Furthermore, in order to better understand danshensu specificity as a potential API in drug formulation, the physicochemical properties of the compounds were studied by thermal analysis, including differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA).

  11. 2.2.1. Synthesis, spectroscopic characterization and crystal structure of [ReV(O2(pyz4][ReII(NOBr4(pyz] (pyz = pyrazine

    Directory of Open Access Journals (Sweden)

    Mario Pacheco, Alicia Cuevas, Javier González-Platas, Carlos Kremer*

    2015-03-01

    Full Text Available Abstract: A novel Re(V-Re(II nitrosyl complex, [Re(O2(pyz 4][Re(NOBr4(pyz] (pyz = pyrazine was prepared and characterized by X-ray diffraction, elemental analysis, infrared and ultraviolet-visible absorption spectra. This product is obtained in the initial steps of the reaction of (NBu4[Re(NOBr4(EtOH] with pyrazine. Both, the cation and the anion are mononuclear complexes. The Re(V atom in the cation is six-coordinate with four nitrogen atoms from pyrazine ligands, and two oxo ligands. The Re(II anion is also six-coordinate, with four bromide ligands, a linear nitrosyl group and one nitrogen from pyrazine. The spectroscopic studies are discussed and compared with those already reported separately for the cation and the anion. Supporting information: X-Ray (CIF file

  12. Spectroscopic characterization of the on-surface induced (cyclo) dehydrogenation of a N-heteroaromatic compound on noble metal surfaces

    Czech Academy of Sciences Publication Activity Database

    Palacio, I.; Pinardi, A. L.; Martínez, J. I.; Preobrajenski, A.; Cossaro, A.; Jančařík, Andrej; Stará, Irena G.; Starý, Ivo; Méndez, J.; Martín-Gago, J.A.; López, M.F.

    2017-01-01

    Roč. 19, č. 33 (2017), s. 22454-22461 ISSN 1463-9076 Institutional support: RVO:61388963 Keywords : dibenzohelicene * on-surface (cyclo)dehydrogenation * spectroscopic characterization Subject RIV: CC - Organic Chemistry OBOR OECD: Organic chemistry Impact factor: 4.123, year: 2016

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

    African Journals Online (AJOL)

    Synthesis, characterization and antimicrobial activity of mixed ascorbic acid - nicotinamide metal complexes. ... The result of the antimicrobial studies showed that the mixed complexes have higher inhibitory activity than the original ligands against the tested bacteria and fungi species. KEY WORDS: Ascorbic acid, ...

  14. Synthesis, characterization and thermal properties of the silsesquioxane organically modified with 4,5-diphenyl-2-Imidazoltiol

    International Nuclear Information System (INIS)

    Silvestrini, D.R.; Carmo, D.R. do

    2014-01-01

    The present paper describes the preparation of a nanostructured silsesquioxane, the octa-(3-chloropropyl)-octasilsesquioxane (S) that was organofunctionalised with the 4,5-Diphenyl-2-imidazolethiol (DIT). The modification of silsesquioxane with DIT proposed in this paper follows two steps. The composite prepared after functionalization was ascribed as SDIT. The composite SDIT and precursors were characterized by infrared (FTIR), "1"3C and "2"9Si Nuclear Resonance Magnetic (NMR) in solid state, Scanning Electron microscopy (SEM); X-Ray Diffraction (XRD); Energy-Dispersive X-ray spectroscopy (EDS) and Thermogravimetry. By spectroscopic analysis using above techniques, we conclude with that the SDIT synthesis was conducted with success. It was observed a cluster of particles containing cavities in an orderly fashion. The thermogravimetry analyzes performed in two different atmospheres, concluding that the materials (S, DIT and SDIT) when in air atmosphere has a slower degradation process in relation to nitrogen atmosphere. The thermogravimetry of SDIT indicate a greater thermal stability in nitrogen atmosphere. (author)

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

    African Journals Online (AJOL)

    Green synthesis, characterization and antibacterial activity of copper nanoparticles using L -ascorbic ... Journal Home > Vol 10, No 3 (2017) > ... In this study, simple, economical, convenient and environmentally-friendly chemical reduction ...

  16. 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.

  17. Synthesis, Spectroscopic Properties and DFT Calculation of Novel ...

    Indian Academy of Sciences (India)

    L1) identifies its molecular structure and reveals π-π stacking. The synthetic mechanisms for L2, L3 were studied by density functional theory calculations. And a comprehensive study of spectroscopic properties involving experimental data and ...

  18. Surface spectroscopic characterization of a model methane-activation catalyst

    International Nuclear Information System (INIS)

    Chen, J.G.; Weisel, M.D.; Hoffmann, F.M.; Hall, R.B.

    1992-01-01

    In an effort to understand the details concerning the alkali-promoted selectivity for the oxidative coupling of methane, the authors have carried out a detailed characterization of a model K/NiO/Ni(100) catalyst under well-controlled, ultrahigh vacuum conditions. The authors' systematic approach involved the following procedures: detailed investigation of the formation and structure of NiO on a clean Ni(100) surface; spectroscopic characterization of K-doped NiO by in situ deposition of potassium onto well-characterized NiO/Ni(100) substrate; and determination of the reactivities of NiO/Ni(100) and K/NiO/Ni(100) towards H 2 and CH 4 . In this paper, the authors will use the model K/NiO/Ni(100) system as an example to demonstrate that a detailed, complementary characterization of the model catalyst could best be achieved by using a combination of a variety of surface techniques: The methods of HREELS, LEED, XPS and AES could be applied to obtain properties on and near the surface regions; the technique of FYNES, being a photon-in/photon-out method could be utilized to investigate the bulk properties up to 2000 Angstrom below the surface; the method of FTIR using CO as a probing molecule is, on the other hand, sensitive only to the properties of the top-most surface layer. The result is to be presented in this paper will be mainly those obtained by using the two vibrational spectroscopies (HREELS and FTIR). Results from other surface techniques will also be discussed or presented when they provide additional information to the vibrational data

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

    International Nuclear Information System (INIS)

    Pereira, A.B.

    1984-01-01

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

  20. Synthesis and characterization of organically linked ZnO nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-11-15

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

  1. Synthesis and characterization of organically linked ZnO nanoparticles

    International Nuclear Information System (INIS)

    Chory, Christine; Riedel, Ingo; Parisi, Juergen; Kruska, Carsten; Heimbrodt, Wolfram; Feser, Clemens; Beenken, Wichard J.D.; Hoppe, Harald

    2012-01-01

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

  2. Synthesis and characterization of core-shell gold nanoparticles with poly(vinyl pyrrolidone) from a new precursor salt

    Science.gov (United States)

    Behera, M.; Ram, S.

    2013-02-01

    In this article, we report a facile one-step chemical synthesis of gold (Au) nanoparticles (GNPs) from a new precursor salt i.e., gold hydroxide in the presence of poly(vinyl pyrrolidone) (PVP) polymer. The non-aqueous dispersion of GNPs was comprehensively characterized by UV-Visible, FTIR, zeta potential, and transmission electron microscope (TEM). A strong surface plasmon resonance band at 529 nm in the UV-Visible spectrum confirms the formation of GNPs in the Au colloid. The FTIR spectroscopic results showed that PVP molecules get chemisorbed onto the surface of GNP via O-atom of carbonyl group. A negative zeta potential of (-)16 mV reveals accumulation of nonbonding electrons of O-atom of carbonyl group of PVP molecules on the nanosurface of GNP. TEM images demonstrate a core-shell nanostructure with an Au-crystalline core covered by a thin amorphous PVP-shell. PVP-capped GNPs could be a potential candidate for bio-sensing, catalysis, and other applications.

  3. Expression, purification and spectroscopic characterization of the Regulator complex

    Energy Technology Data Exchange (ETDEWEB)

    Nogueira, M.L.C.; Silva, A.L.S.; Camilotti, D.; Silva, C.A.; Sforca, M.L.; Smetana, J.H.C.; Zeri, A.C. [Laboratorio Nacional de Biociencias - LNBIO, Campinas, SP (Brazil); Ospina-Bedoya, M. [Universidad de Antioquia, Medellin (Colombia)

    2012-07-01

    Full text: The mammalian target of rapamycin (mTOR) signaling pathway integrates both intracellular and extracellular signals, serves as a central regulator of cell metabolism in humans and its deregulation is linked to diseases like cancer and diabetes. The small GTPases Rag are mediators of signaling by amino acid (leucine). These GT-Pases are anchored on the surface of the lysosome through an interaction with a complex of three proteins, p18, MP1 and p14, called Ragulator. The p18 protein is responsible for interaction with the lysosomal membrane through its N terminal post translational modification. The objective of this project is to study the interaction of p18 and other components of the Ragulator complex. The p18 protein was expressed in inclusion bodies, which were isolated and solubilized in urea. p18 was renatured with its partners MP1/p14 and this complex, the Ragulator, was subjected to spectroscopic characterization using circular dichroism and dynamic light scattering. (author)

  4. Expression, purification and spectroscopic characterization of the Regulator complex

    International Nuclear Information System (INIS)

    Nogueira, M.L.C.; Silva, A.L.S.; Camilotti, D.; Silva, C.A.; Sforca, M.L.; Smetana, J.H.C.; Zeri, A.C.; Ospina-Bedoya, M.

    2012-01-01

    Full text: The mammalian target of rapamycin (mTOR) signaling pathway integrates both intracellular and extracellular signals, serves as a central regulator of cell metabolism in humans and its deregulation is linked to diseases like cancer and diabetes. The small GTPases Rag are mediators of signaling by amino acid (leucine). These GT-Pases are anchored on the surface of the lysosome through an interaction with a complex of three proteins, p18, MP1 and p14, called Ragulator. The p18 protein is responsible for interaction with the lysosomal membrane through its N terminal post translational modification. The objective of this project is to study the interaction of p18 and other components of the Ragulator complex. The p18 protein was expressed in inclusion bodies, which were isolated and solubilized in urea. p18 was renatured with its partners MP1/p14 and this complex, the Ragulator, was subjected to spectroscopic characterization using circular dichroism and dynamic light scattering. (author)

  5. 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.

  6. Spectroscopic and thermal characterization of carbon nanotubes functionalized through diazonium salt reduction

    International Nuclear Information System (INIS)

    Pandurangappa, Malingappa; Ramakrishnappa, Thippeswamy

    2010-01-01

    Chemical reduction of anthraquinone diazonium chloride (Fast Red AL salt) in presence of hypophosphorous acid and carbon nanotubes results in anthraquinonyl functionalized carbon nanotubes. The surface functionalized moieties have been examined electrochemically by immobilizing them onto the surface of basal plane pyrolytic graphite electrode and studying its voltammetric behaviour. The effect of pH, and scan rate has revealed that the modified species are confined on the electrode surface. The spectroscopic characterization of the modified single walled carbon nanotubes using Fourier transform infrared spectroscopy, X-ray photoemission spectroscopy, thermogravimetric analysis and transmission electron microscopy have revealed that the modifier molecules are covalently bonded on the surface of carbon nanotubes.

  7. Spectroscopic and thermal characterization of carbon nanotubes functionalized through diazonium salt reduction

    Energy Technology Data Exchange (ETDEWEB)

    Pandurangappa, Malingappa, E-mail: mprangachem@gmail.com [Department of Chemistry, Bangalore University, Central College Campus, Dr Ambedkar Veedhi, Bangalore 560 001 (India); Ramakrishnappa, Thippeswamy [Department of Chemistry, Bangalore University, Central College Campus, Dr Ambedkar Veedhi, Bangalore 560 001 (India)

    2010-08-01

    Chemical reduction of anthraquinone diazonium chloride (Fast Red AL salt) in presence of hypophosphorous acid and carbon nanotubes results in anthraquinonyl functionalized carbon nanotubes. The surface functionalized moieties have been examined electrochemically by immobilizing them onto the surface of basal plane pyrolytic graphite electrode and studying its voltammetric behaviour. The effect of pH, and scan rate has revealed that the modified species are confined on the electrode surface. The spectroscopic characterization of the modified single walled carbon nanotubes using Fourier transform infrared spectroscopy, X-ray photoemission spectroscopy, thermogravimetric analysis and transmission electron microscopy have revealed that the modifier molecules are covalently bonded on the surface of carbon nanotubes.

  8. Spectroscopic characterization of manganese-doped alkaline earth

    Indian Academy of Sciences (India)

    The intensity and frequency variations for the characteristic phosphate group vibrations have been correlated with the changes of the structural units present in these glasses. Depolymerization of the phosphate chains in all the glasses is observed with replacement of alkaline earth content by spectroscopic studies.

  9. 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 ...

  10. L-shaped benzimidazole fluorophores: synthesis, characterization and optical response to bases, acids and anions.

    Science.gov (United States)

    Lirag, Rio Carlo; Le, Ha T M; Miljanić, Ognjen Š

    2013-05-14

    Nine L-shaped benzimidazole fluorophores have been synthesized, computationally evaluated and spectroscopically characterized. These "half-cruciform" fluorophores respond to bases, acids and anions through changes in fluorescence that vary from moderate to dramatic.

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

    Indian Academy of Sciences (India)

    Synthesis and structural characterization of a calcium coordination polymer based on a μ3-bridging. tetradentate binding mode of glycine. SUBRAMANIAN NATARAJAN*a, BIKSHANDARKOIL R. SRINIVASANb , J. KALYANA SUNDARa, K. RAVIKUMARc , R.V. KRISHNAKUMARd , J. SURESHe,. aSchool of Physics, ...

  12. Synthesis, structure, morphology and stoichiometry characterization of cluster and nano magnetite

    Energy Technology Data Exchange (ETDEWEB)

    Singh, L. Herojit; Pati, S.S. [Institute of Physics, University of Brasilia, 70919-970, Brasilia, DF (Brazil); Guimarães, Edi M. [Institute of Geoscience, University of Brasilia, 70910-900, Brasilia, DF (Brazil); Rodrigues, P.A.M.; Oliveira, Aderbal C. [Institute of Physics, University of Brasilia, 70919-970, Brasilia, DF (Brazil); Garg, V.K., E-mail: vijgarg@gmail.com [Institute of Physics, University of Brasilia, 70919-970, Brasilia, DF (Brazil)

    2016-08-01

    We have studied the stoichiometry of magnetite nanoparticles using three spectroscopic techniques: Mössbauer, photoacoustic and ferromagnetic resonance (FMR). By varying the weight ratio of the Fe precursor to the reducing agent (sodium acetate) and a post-synthesis annealing, we were able to synthesize samples with different amounts of Fe vacancies, from stoichiometric Fe{sub 3}O{sub 4} to γ-Fe{sub 2}O{sub 3}. By synthesizing magnetite in the presence of zeolite we obtained nanoparticles within the 3–10 nm diameter range. The spectroscopic results show that there is a correlation between the amount of Fe vacancies and (i) the optical absorption and (ii) the g-values from the Electron paramagnetic resonance EPR spectra of the nanoparticles. - Highlights: • Magnetite nanoparticles and cluster synthesized. • Photoacoustic spectroscopy is effective in determining the stoichiometry. • Particles with 9 nm size has 0 < δ < 0.14. • Less than 9 nm gives 0.14 < δ < 0.3 and size <3 nm have δ = 0.33 (i.e. γ-Fe{sub 2}O{sub 3}).

  13. Polypyrrole-silver Nanocomposite: Synthesis and Characterization

    OpenAIRE

    D. M. Nerkar; S. V. Panse; S. P. Patil; S. E. Jaware; G. G. Padhye

    2016-01-01

    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. P...

  14. Synthesis and characterization of activated lithium fluoride with silver

    International Nuclear Information System (INIS)

    Encarnacion E, E. K.; Guerrero S, Z.; Reyes A, J.

    2017-10-01

    The present work shows part of the results obtained in the development of the research that has been carried out since 2015 entitled -Synthesis and characterization of new thermoluminescent materials for the radiation dosimetry and its applications in health-. In the development of this research, the synthesis of crystals of pure lithium fluoride (LiF) and activated with different concentrations of silver (LiF:Ag); synthesized samples are also presented using different temperatures, as well as varying the concentration of the solvent (water-ethanol). The synthesized materials were characterized through different techniques: scanning electron microscopy and X-ray diffraction. Specifically, the results of the calculation of the size of the LiF crystals are presented using the Scherrer equation. Within the results, a dependence on the size of the crystals is highlighted by means of the following factors: the amount of activator in the sample, the temperature at which the sample was synthesized, as well as the amount of solvent in the synthesis. The samples have a simple cubic crystalline phase. (Author)

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

    African Journals Online (AJOL)

    user

    base complexes derived from Salicylaldehyde and histidine with some divalent transition metal ions. Furthermore, Syed (1993) reported the synthesis, characterization and biological evaluation of some. Schiff base metal complexes derived from Anthranilic acid-sugar and naturally occurring amino acid-sugar. Schiff bases ...

  16. Synthesis, structural characterization, Hirshfeld surface analysis and spectroscopic studies of cadmium (II) chloride complex with 4-hydroxy-1-methylpiperidine

    Energy Technology Data Exchange (ETDEWEB)

    Soudani, S. [Université de Carthage, Laboratoire de Chimie des Matériaux, Faculté des Sciences de Bizerte, 7021 Zarzouna (Tunisia); Ferretti, V. [Department of Chemical and Pharmaceutical Sciences and Center for Structural Diffractometry, via Fossato di Mortara 17, I-44121 Ferrara (Italy); Jelsch, C. [CRM2, CNRS, Institut Jean Barriol, Université de Lorraine, Vandoeuvre les Nancy CEDEX (France); Lefebvre, F. [Laboratoire de Chimie Organométallique de Surface (LCOMS), Ecole Supérieure de Chimie Physique Electronique, 69626 Villeurbanne Cedex (France); Nasr, C. Ben, E-mail: cherif_bennasr@yahoo.fr [Université de Carthage, Laboratoire de Chimie des Matériaux, Faculté des Sciences de Bizerte, 7021 Zarzouna (Tunisia)

    2016-05-15

    The chemical preparation, crystal structure, Hirshfeld surface analysis and spectroscopic characterization of the novel cadmium (II) 4-hydroxy-1-methylpiperidine complex, Cd{sub 4}Cl{sub 10}(C{sub 6}H{sub 14}NO){sub 2}·2H{sub 2}O, have been reported. The atomic arrangement can be described as built up by an anionic framework, formed by edge sharing CdCl{sub 6} and CdCl{sub 5}O octahedral linear chains spreading along the a-axis. These chains are interconnected by water molecules via O–H⋯Cl and O–H⋯O hydrogen bonds to form layers parallel to (011) plane. The organic cations are inserted between layers through C–H⋯Cl hydrogen bonds. Investigation of intermolecular interactions and crystal packing via Hirshfeld surface analysis reveals that the H{sub C}⋯Cl and H{sub C}⋯H{sub C} intermolecular interactions are the most abundant contacts of the organic cation in the crystal packing. The statistical analysis of crystal contacts reveals the driving forces in the packing formation. The {sup 13}C and {sup 15}N CP-MAS NMR spectra are in agreement with the X-ray structure. The vibrational absorption bands were identified by infrared spectroscopy. DFT calculations allowed the attribution of the NMR peaks and of the IR bands.

  17. Synthesis and In Vitro Evaluation of C-methylcalix[4]resorcinaryl octacinnamate as the Sunscreen

    Directory of Open Access Journals (Sweden)

    Budiana I Gusti M. Ngurah

    2017-04-01

    Full Text Available Synthesis and in vitro test of C-methylcalix[4]resorcinaryl octacinnamate as the sunscreen has been conducted. The C-methylcalix[4]resorcinaryl octacinnamate was synthesized in 2 steps. They were synthesis of C-methylcalix[4]resorcinarene via acid catalyzed condensation of resorcinol and acetaldehyde, followed by estherification using cinnamoyl chloride and pyridine catalyst. The characterization of the target molecule was performed by infra red spectrophotometer, proton-NMR, carbon-NMR and mass spectromether. The sunscreen activity test was conducted by spectroscopic method and MTT-assay. Spectroscopic analysis (UV showed that the target molecule absorbed the dangerous ultraviolet radiation between 280 and 320 nm (UV B wave length with the maximum absorption at 290 nm (ε = 31.535 M-1 cm-1. The MTT-assay indicated that the IC50 of C-methylcalix[4]resorcinaryl octacinnamate is 12.006 ppm. The sunscreen activity of C-methylcalix[4]resorcinaryl octacinnamate is stronger than commercial sunscreen Intersun (IC50 = 18.235 ppm.

  18. Synthesis, characterization and DFT studies of two new silver(I) complexes with 3,4-lutidine

    Science.gov (United States)

    Soliman, Saied M.; Assem, Rania; Abu-Youssef, Morsy A. M.; Kassem, Taher S.

    2015-04-01

    The synthesis, characterization and molecular structure of two new Ag(I) complexes with 3,4-lutidine (34lut) have been reported. The [Ag(34lut)3(OAC)]; 1 and [Ag(34lut)2(TFA)]; 2 complexes, where OAC and TFA are acetate and trifluoroacetate respectively, have been characterized using elemental analysis, FTIR, NMR and mass spectra. Their molecular structures were calculated using DFT quantum chemical calculations. Both 1 and 2 were found to have distorted tetrahedral geometry around the Ag(I). The spectroscopic properties of the studied complexes have been calculated using the same level of theory. The Infrared vibrational frequencies of the COO stretches confirmed that the OAC is monodentate in 1 while the TFA is bidentate in 2. The calculated polarizability (α0) and HOMO-LUMO energy gap (ΔE) values indicated that 1 has higher NLO activity than 2. The electronic spectra of these complexes are calculated using the TD-DFT calculations. The calculated 1H NMR chemical shift values using GIAO approach showed good correlations with the experimental data. The interaction energies using the second order perturbation theory have been used to study the different intramolecular charge transfer interactions in the studied complexes. The NBO calculations indicated that both the Agsbnd O bonds are almost identical in 2 but not in 1.

  19. Synthesis and characterization of the silver methacrylate and its polymerization with gamma radiation

    International Nuclear Information System (INIS)

    Figueroa de Paz, Y. M.

    2014-01-01

    One of the traditional objectives in research has been the development of new and useful materials that combine the properties of polymers with metals. Synthesis of monomers containing metal, followed by a polymerization process, is a method to introduce metal ions in the structure of a polymer, and the gamma radiation was easily applied to initiate polymerization. The coordination polymers have high insolubility, which is a general problem of these materials, besides the lack of structural information available. Also, due to the difficulty of obtaining single crystals, it has hindered the identification of the structures of some coordination polymers, requiring the use of indirect methods for structural characterization. In this work the synthesis of silver poly-methacrylate (PMAAg), was performed using the gamma radiation as polymerization initiator, having as precursor to silver methacrylate monomer (MAAg). The combination of spectroscopic methods revealed structural changes in the coordination polymers. With scanning electron microscopy, it was observed that the morphology of the monomer and its polymers is fiber, which grows with increasing radiation dose; furthermore, this increase in size is related to Bet analysis result, since the monomer has a bigger superficial area to the irradiated polymers. In monomer and irradiated polymers the crystalline structure CCC was observed by X-ray diffraction. By thermogravimetric analysis the decomposition temperature of the products was determined, finding around 150 degrees C. The infrared spectroscopy confirmed the silver methacrylate polymerization, as with increasing radiation dose, also increases the degree of polymerization; likewise the form of coordination of the monomer was determined and its irradiated polymers which corresponds to a bi-dentate chelate, confirmed by X-ray photoelectron spectroscopy. (Author)

  20. Amino Acid and Peptide Immobilization on Oxidized Nanocellulose: Spectroscopic Characterization

    Science.gov (United States)

    Barazzouk, Saïd; Daneault, Claude

    2012-01-01

    In this work, oxidized nanocellulose (ONC) was synthesized and chemically coupled with amino acids and peptides using a two step coupling method at room temperature. First, ONC was activated by N-ethyl-N’-(3-dimethylaminopropyl) carbodiimide hydrochloride, forming a stable active ester in the presence of N-hydroxysuccinimide. Second, the active ester was reacted with the amino group of the amino acid or peptide, forming an amide bond between ONC and the grafted molecule. Using this method, the intermolecular interaction of amino acids and peptides was avoided and uniform coupling of these molecules on ONC was achieved. The coupling reaction was very fast in mild conditions and without alteration of the polysaccharide. The coupling products (ONC-amino acids and ONC-peptides) were characterized by transmission electron microscopy and by the absorption, emission, Fourier transform infrared spectroscopy (FTIR) and X-ray photoelectron spectroscopy (XPS) spectroscopic techniques. PMID:28348303

  1. Amino Acid and Peptide Immobilization on Oxidized Nanocellulose: Spectroscopic Characterization

    Directory of Open Access Journals (Sweden)

    Claude Daneault

    2012-06-01

    Full Text Available In this work, oxidized nanocellulose (ONC was synthesized and chemically coupled with amino acids and peptides using a two step coupling method at room temperature. First, ONC was activated by N-ethyl-N’-(3-dimethylaminopropyl carbodiimide hydrochloride, forming a stable active ester in the presence of N-hydroxysuccinimide. Second, the active ester was reacted with the amino group of the amino acid or peptide, forming an amide bond between ONC and the grafted molecule. Using this method, the intermolecular interaction of amino acids and peptides was avoided and uniform coupling of these molecules on ONC was achieved. The coupling reaction was very fast in mild conditions and without alteration of the polysaccharide. The coupling products (ONC-amino acids and ONC-peptides were characterized by transmission electron microscopy and by the absorption, emission, Fourier transform infrared spectroscopy (FTIR and X-ray photoelectron spectroscopy (XPS spectroscopic techniques.

  2. Spectroscopic studies, theoretical models and structural characterization. II. Synthesis and X-ray powder diffraction of the elpasolites Cs2NaSmCl6

    International Nuclear Information System (INIS)

    Poblete, V.; Acevedo, R.

    1998-01-01

    In this research work, we report the synthesis and structural characterization of the stoichiometric elpasolite Cs 2 NaSmCl 6 . The synthesis was performed under a solid state reaction in nitrogen atmosphere from the chemicals CsCl, NaCl and SmCl 3 weighted stoichiometrically. The best possible crystallization temperature was obtained using thermal studies of the type DTA/TGA (the thermal treatment was allowed to proceed for 2.5 hours at 755 Centigrade, showing a temperature gradient of 10 Centigrade/minute). The structural characterization by powder X-ray diffraction (XDR) indicates that this elpasolite belongs to the Fm 3m (O h 5 ) space group and the optimized structural parameters are as follows: a 0 = 10.8342 Armstrong, V 1271.72 Armstrong 3 , Z=4, M=651.88, D x =3.406 y D exp=3.41 ± 0.01. The profile refinement, using the Rietveld method, allowed us to fit the experimental and the calculated intensities of a total of 32 lines. The above result indicates that the condition R exp 2+ + 3Cl -1 and the counter ions filling the octahedral holes, in full agreement with anti fluorite type crystal. According to the above description, these elpasolite adopt the form (M 1/3 □ 2/3 ) 4 X 2 , where M labels the central metal, X stand for the chlorine ions and □ represent the vacancies, which may accommodate a significant amount of defects without collapsing. This experimental study provides the necessary input to test theoretical models against experimental data. (Author)

  3. Synthesis and characterization of reactive dye-cassava mesocarp ...

    African Journals Online (AJOL)

    The synthesis of triazine based reactive dyes was carried out. The resultant dyes were characterized by thin layers chromatography, molecular weight, infrared and ultra- violet spectroscopy, and used in dyeing cassava mesocarp to produce dye modified cellulosic substrates. The dyed substrates were tested for dye fixation, ...

  4. Synthesis and characterization of new optically active poly(amide ...

    African Journals Online (AJOL)

    Synthesis and characterization of new optically active poly(amide-imide)s based on N -trimellitimido- ... Bulletin of the Chemical Society of Ethiopia ... (DMAc), dimethyl sulfoxide (DMSO) and N-methyl-2-pyrrolidone (NMP) at room temperature.

  5. Understanding reactivity of two newly synthetized imidazole derivatives by spectroscopic characterization and computational study

    Science.gov (United States)

    Hossain, Mossaraf; Thomas, Renjith; Mary, Y. Sheena; Resmi, K. S.; Armaković, Stevan; Armaković, Sanja J.; Nanda, Ashis Kumar; Vijayakumar, G.; Van Alsenoy, C.

    2018-04-01

    Two newly synthetized imidazole derivatives (1-(4-methoxyphenyl)-4,5-dimethyl-1H-imidazole-2-yl acetate (MPDIA) and 1-(4-bromophenyl)-4,5-dimethyl-1H-imidazole-2-yl acetate (BPDIA)) have been prepared by solvent-free synthesis pathway and their specific spectroscopic and reactive properties have been discussed based on combined experimental and computational approaches. Aside of synthesis, experimental part of this work included measurements of IR, FT-Raman and NMR spectra. All of the aforementioned spectra were also obtained computationally, within the framework of density functional theory (DFT) approach. Additionally, DFT calculations have been used in order to investigate local reactivity properties based on molecular orbital theory, molecular electrostatic potential (MEP), average local ionization energy (ALIE), Fukui functions and bond dissociation energy (BDE). Molecular dynamics (MD) simulations have been used in order to obtain radial distribution functions (RDF), which were used for identification of the atoms with pronounced interactions with water molecules. MEP showed negative regions are mainly localized over N28, O29, O35 atoms, it is represent with red colour in rainbow color scheme for MPDIA and BPDIA (which are most reactive sites for electrophilic attack). The first order hyperpolarizabilities of MPDIA and BPDIA are 20.15 and 6.10 times that of the standard NLO material urea. Potential interaction with antihypertensive protein hydrolase.

  6. LaPO4:Eu fluorescent nanorods, synthesis, characterization and spectroscopic studies on interaction with human serum albumin

    Science.gov (United States)

    Guo, Xingjia; Yao, Jie; Liu, Xuehui; Wang, Hongyan; Zhang, Lizhi; Xu, Liping; Hao, Aijun

    2018-06-01

    Eu3+ doped LaPO4 fluorescent nanorods (LaPO4:Eu) was successfully fabricated by a hydrothermal process. The obtained LaPO4:Eu nanorods under the optimal conditions were characterized by means of transmission electron microscopy (TEM), X-ray diffraction (XRD) technique, Fourier transform infrared (FTIR), UV-vis absorption and fluorescence spectroscopy. The nanorods with a length of 50-100 nm and a diameter of about 10 nm, can emit strong red fluorescence upon excitation at 241 nm. The FTIR result confirmed that there are lots of phosphate groups on the surfaces of nanorods. In order to better understand the physiological behavior of nanorods in human body, multiple spectroscopic methods were used to study the interaction between the LaPO4:Eu nanorods and human serum albumin (HSA) in the simulated physiological conditions. The results indicated that the nanorods can effectively quench the intrinsic fluorescence of HSA through a dynamic quenching mode with the association constants of the order of 103 L mol-1. The values of the thermodynamic parameters suggested that the binding of the nanorods to HSA was a spontaneous process and van der Waals forces and hydrogen bonds played a predominant role. The displacement experiments verified that the binding site of nanorods on HSA was mainly located in the hydrophobic pocket of subdomain IIA (site I) of HSA. The binding distance between nanorods and HSA was calculated to be 4.2 nm according to the theory of Förster non-radiation energy transfer. The analysis of synchronous fluorescence, three-dimensional fluorescence (3D) and circular dichroism (CD) spectra indicated that there the addition of LaPO4:Eu nanorods did not caused significant alterations in conformation of HSA secondary structure and the polarity around the amino acid residues.

  7. Synthesis, structural and electrical characterizations of thermally ...

    African Journals Online (AJOL)

    Synthesis, structural and electrical characterizations of thermally evaporated Cu 2 SnS 3 thin films. ... The surface profilometer shows that the deposited films are rough. The XRD spectra identified the ... The electrical resistivity of the deposited Cu2SnS3 film is 2.55 x 10-3 Ωcm. The conductivity is in the order of 103 Ω-1cm-1.

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

    Indian Academy of Sciences (India)

    Combustion synthesis and structural characterization of Li–Ti mixed nanoferrites ... were prepared by combustion method at lower temperatures compared to the ... first time at low temperatures, using PEG which acts as a new fuel and oxidant.

  9. Spectroscopic characterization of III-V semiconductor nanomaterials

    Science.gov (United States)

    Crankshaw, Shanna Marie

    through a novel spectroscopic technique first formulated for the rather different purpose of dispersion engineering for slow-light schemes. The frequency-resolved technique combined with the unusual (110) quantum wells in a furthermore atypical waveguide experimental geometry has revealed fascinating behavior of electron spin splitting which points to the possibility of optically orienting electron spins with linearly polarized light---an experimental result supporting a theoretical description of the phenomenon itself only a few years old. Lastly, to explore a space of further-restricted dimensionality, the final chapters describe InP semiconductor nanowires with dimensions small enough to be considered truly one-dimensional. Like the bulk GaAs of the first few chapters, the InP nanowires here crystallize in a wurtzite structure. In the InP nanowire case, though, the experimental techniques explored for characterization are temperature-dependent time-integrated photoluminescence at the single-wire level (including samples with InAsP insertions) and time-resolved photoluminescence at the ensemble level. The carrier dynamics revealed through these time-resolved studies are the first of their kind for wurtzite InP nanowires. The chapters are thus ordered as a progression from three (bulk), to two (quantum well), to one (nanowire), to zero dimensions (axially-structured nanowire), with the uniting theme the emphasis on connecting the semiconductor nanomaterials' crystallinity to its exhibited properties by relevant experimental spectroscopic techniques, whether these are standard methods or effectively invented for the case at hand.

  10. Synthesis, characterization and magnetic properties of selected Laves and MAX phases

    International Nuclear Information System (INIS)

    Hamm, Christin Maria

    2017-01-01

    In this work the rare-earth free Laves phases Ti 2 M 3 Si with M = Mn, Fe, Co, Ni were synthesized by microwave heating and were structurally and magnetically characterized. Furthermore, the solid solution Ti 2 (Co 1-x Fe x ) 3 Si was synthesized by arc melting and spark plasma sintering, as well as their magnetic behavior was studied. In addition to the Laves phases, the focus was on the synthesis and characterization of aluminum-based MAX phases. For the first time the ternary carbides were prepared by microwave heating. The phase-pure representation of MAX phases was particularly challenging for synthetic solid-state chemistry. The susceptor-assisted microwave heating allows the synthesis of high-quality samples, which was shown in this work on M 2 AlC (M = Ti, V, Cr) and V 4 AlC 3 . Furthermore, for the first time, the doping of these materials with Mn and Fe was successful. In addition to the structural characterization of the new phases, the microstructure and magnetic properties are discussed in this work. Using these doped compounds as well as the compound V 4 AlC 3 , it has been shown that field-activated synthesis, particularly susceptor-assisted microwave heating, are a very good synthesis method for compounds which are hard or sometimes not synthesized by conventional methods.

  11. Synthesis and characterization of cadmium doped lead–borate ...

    Indian Academy of Sciences (India)

    Unknown

    Mater. Sci., Vol. 29, No. 1, February 2006, pp. 55–58. © Indian Academy of Sciences. 55. Synthesis and characterization of cadmium doped lead–borate glasses. A A ALEMI*, H SEDGHI†, A R MIRMOHSENI and V GOLSANAMLU. Department of Inorganic Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz, Iran.

  12. Synthesis and characterization of europium aluminophosphate

    International Nuclear Information System (INIS)

    Araujo, A.S.; Diniz, J.C.; Silva, A.O.S.

    1998-01-01

    Full text: Aluminophosphate molecular sieves (ALPO) represents a class of materials formed by AlO 2+ and PO 2- tetrahedra linked together through b the oxygen atom. The incorporation of metal cations, specifically rare earths, in the ALPO matrix, gives rise to generation of new materials that can be used as acid catalysts in chemical processes. In this work, it was synthesized hydrothermally a molecular sieve type Eu-ALPO-11, starting from an hydrated alumina (pseudobohemite), phosphoric acid solution, europium chloride, water, and di-isopropylamine (DIPA) as organic template. The gel of synthesis presented the following composition: 1.0 DIPA: 0.05 Eu 2 O 3 :0.95 Al 2 O 3 : 1.0 P 2 O 5 : 80 H 2 O The hydrogel was autoclaved at 170 deg C for a period of 3 days. After that the obtained solid was filtered, washed, dried and calcined at 500 deg C to remove the template. The sample was characterized by several physico-chemical methods, such a atomic absorption, FT-IR spectroscopy, X-ray diffraction, thermal analysis, scanning electron microscopy. Its spectroscopic properties was investigated by europium luminescence. The physico-chemical characterization of the Eu-ALPO-11 showed very good crystallinity, with AEL structure, and orthorhombic symmetry. Also, the material presents excellent thermal stability, with no structural collapse until 950 deg C. Through the luminescence spectra in the visible region, it was observed that the emission of the Eu 3+ is strongly influenced by the increasing of the 5d0 7f0 transition (Electric Dipole), as compared to the 5d0 7f1 transition (Magnetic Dipole) between the levels of 4f configuration perturbed by the crystalline field. The ED/MD ratio to the as synthesized sample was ca. 2.1, against ca. 1.1 relative to the calcined sample. The FT-IR spectra presented well defined absorption bands relative to Al-O and P-O bonds, of the structural internal tetrahedra (IT) and external links (EL): 1250- 950 cm -1 , symmetric stretching due to

  13. Synthesis, characterization, and evaluation of the antimicrobial efficacy of Boswellia ovalifoliolata stem bark-extract-mediated zinc oxide nanoparticles

    Science.gov (United States)

    Supraja, N.; Prasad, T. N. V. K. V.; Krishna, T. Giridhara; David, E.

    2016-04-01

    Synthesis of metal nanoparticles using biological systems is an expanding research area in nanotechnology. Moreover, search for new nanoscale antimicrobials is been always attractive as they find numerous avenues for application in medicine. Biosynthesis of metallic nanoparticles is cost effective and eco-friendly compared to those of conventional methods of nanoparticles synthesis. Herein, we present the synthesis of zinc oxide nanoparticles using the stem bark extract of Boswellia ovalifoliolata, and evaluation of their antimicrobial efficacy. Stable ZnO nanoparticles were formed by treating 90 ml of 1 mM zinc nitrate aqueous solution with 10 ml of 10 % bark extract. The formation of B. ovalifoliolata bark-extract-mediated zinc oxide nanoparticles (BZnNPs) was confirmed by UV-visible spectroscopic analysis and recorded the localized surface plasmon resonance (LSPR) at 230 nm. Fourier transform infrared spectroscopic (FT-IR) analysis revealed that primary and secondary amine groups in combination with the proteins present in the bark extract are responsible for the reduction and stabilization of the BZnNPs. The morphology and crystalline phase of the nanocrystals were determined by Transmission electron microscopy (TEM). The hydrodynamic diameter (20.3 nm) and a positive zeta potential (4.8 mV) were measured using the dynamic light scattering technique. The antimicrobial activity of BZnNPs was evaluated (in vitro) against fungi, Gram-negative, and Gram-positive bacteria using disk diffusion method which were isolated from the scales formed in drinking water PVC pipelines.

  14. Synthesis and characterization β-ketoamine ligands

    Science.gov (United States)

    Zaid, Nurzati Amani Mohamed; Hassan, Nur Hasyareeda; Karim, Nurul Huda Abd

    2018-04-01

    β-ketoamine ligands are important members of heterodonor ligand because of their ease of preparation and modification of both steric and/or electronic effects. Complexes with β-ketoamine has received much less attention and there has been no study about this complex with β-ketoamine in ionic liquid reported. Two type of β-ketoamine ligands which are 4-amino-3-pentene-2-onato (A) and 3-amino-2-butenoic acid methyl ester (B) have been synthesized in this work. The resulting compound formed was characterized using standard spectroscopic and structural techniques which includes 1H and 13C, NMR spectroscopy and FTIR spectroscopy. The 1H and 13C NMR spectrum displayed all the expected signals with correct integration and multiplicity. And it is proved that there are some differences between two ligands as observed in NMR and FTIR spectrum.

  15. Synthesis and characterization of polypyrrole doped with anionic spherical polyelectrolyte brushes

    Directory of Open Access Journals (Sweden)

    N. Su

    2012-09-01

    Full Text Available The procedures for the synthesis of polypyrrole (PPy doped with anionic spherical polyelectrolyte brushes (ASPB (PPy/ASPB nanocomposite by means of in situ chemical oxidative polymerization were presented. Fourier transform infrared spectroscopy (FTIR and Raman spectroscopic analysis suggested the bonding structure of PPy/ASPB nanocomposite. Scanning electron microscopy (SEM was used to confirm the morphologies of samples. The crystallographic structure, chemical nature and thermal stability of conducting polymers were analyzed by X-ray diffraction (XRD, X-ray photoelectron spectroscopy (XPS and Thermo-gravimetric analysis (TGA respectively. Investigation of the electrical conductivity at room temperature showed that the electrical conductivity of PPy/ASPB nanocomposite was 20 S/cm, which was higher than that of PPy (3.6 S/cm.

  16. Synthesis and characterization of new ionic liquids

    International Nuclear Information System (INIS)

    Oliveira, L.M.C. de; Mattedi, S.; Boaventura, J.S.; Iglesias, M.; Universidad de Santiago de Compostela

    2010-01-01

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

  17. Synthesis and spectroscopic properties of transfermium isotopes with Z = 105, 106 and 107

    International Nuclear Information System (INIS)

    Streicher, B.

    2006-01-01

    The quest for production of new elements has been on for several decades. On the way up the ladder of nuclear chart the systematic research of nuclear properties of elements in transfermium region has been severely overlooked. This drawback is being rectified in past few years by systematic synthesis of especially even-even and odd-A isotopes of these elements. This work proceeds forward also with major contribution of velocity filter SHIP, placed at GSI, Darmstadt. This experimental device represents a unique possibility due to high (up to 1 pμA) beam currents provided by UNILAC accelerator and advancing detection systems to study by means of decay spectroscopy the nuclear structure of isotopes for the elements, possibly up to proton number Z = 110. As the low lying single-particle levels are especially determined by the unpaired nucleon, the odd mass nuclei provide a valuable source of information about the nuclear structure. Such results can be directly compared with the predictions of the calculations based on macroscopic-microscopic model of nuclear matter, thus proving an unambiguous test of the correctness of present models and their power to predict nuclear properties towards yet unknown regions. This work concentrates on the spectroscopic analysis of few of such nuclei. Namely it deals with isotopes 261 Sg and 257 Rf with one unpaired neutron, as well as isotopes 257 Db and 253 Lr with one unpaired proton configuration. Moreover, the analysis of odd-odd nuclei of the the decay sequence 262 Bg → 258 Db → 254 Lr → produced in various experiments at SHIP is discussed in detail. Exhaustive spectroscopic analysis of these data is provided, revealing new information on α, β, EC and SF decay modes of these very heavy isotopes, and deepening the knowledge of the low lying single-particle level structure. Outcomes resulting from the comparison with the systematics of experimentally derived nuclear properties as well as with the predictions of the

  18. Yb3+:Sr5(VO4)3F: Crystal growth, spectroscopic characterization and laser development

    International Nuclear Information System (INIS)

    Bustamante, Andrea Nora Pino

    1999-01-01

    Crystal growth, spectroscopic characterization and laser development of Yb 3+ :SVAP [Sr 5 (VO 4 ) 3 F] was performed to demonstrate for the first time, operation of tunable laser emission centered at 1120 nm. Initially, SVAP crystals were grown with high dopant concentrations, up to 6.0 mol % of Yb 2 O 3 in the melt, in order to investigate the material for potential laser operation at a new laser wavelength. Additional research was performed to alleviate highly doped SVAP crystals of defects previously observed. Basic spectroscopic characterization including absorption and luminescent properties were measured to better understand the behavior of Yb 3+ ions in SVAP. Based upon these studies, discussion of the 1120 nm laser transition is presented as it arises from a ground state vibrational level. Investigations of the charge compensation process and the optical parameters as a function of dopant concentration are also presented. The laser development of Yb 3+ :SVAP included continuous and pulsed modes of operation of the 1044 nm and 1120 nm transitions. Initial laser action of the 1044 nm transition was achieved using a Yi: Saphire laser pump source in order to compare with previously results. Further development of a diode-pumped Yb 3+ :SVAP laser system demonstrated continuously tunable laser operation from 1103 nm for the first time. The laser investigations also proved that this high gain media does provide continuous wave laser action at 1044 nm and 1120 simultaneously without significant gain depletion. (author)

  19. Synthesis of imine bond containing insoluble polymeric ligand and its transition metal complexes, structural characterization and catalytic activity on esterification reaction.

    Science.gov (United States)

    Gönül, İlyas; Ay, Burak; Karaca, Serkan; Saribiyik, Oguz Yunus; Yildiz, Emel; Serin, Selahattin

    2017-01-01

    In this study, synthesis of insoluble polymeric ligand (L) and its transition metal complexes [Cu(L)Cl 2 ]·2H 2 O (1) , [Co(L)Cl 2 (H 2 O) 2 ] (2) and [Ni(L)Cl 2 (H 2 O) 2 ] (3) , having the azomethine groups, were synthesized by the condensation reactions of the diamines and dialdehydes. The structural properties were characterized by the analytical and spectroscopic methods using by elemental analysis, Fourier Transform Infrared, Thermo Gravimetric Analysis, Powder X-ray Diffraction, magnetic susceptibility and Inductively Coupled Plasma. The solubilities of the synthesized polymeric materials were also investigated and found as insoluble some organic and inorganic solvents. Additionally, their catalytic performance was carried out for the esterification reaction of acetic acid and butyl acetate. The highest conversion rate is 75.75% by using catalyst 1 . The esterification of butanol gave butyl acetate with 100% selectivity.

  20. 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

  1. Synthesis and characterization of polyglycerols dendrimers for applications in tissue engineering biological

    International Nuclear Information System (INIS)

    Passos, E.D.; Queiroz, A.A.A. de

    2014-01-01

    Full text: Introduction: Over the last twenty years is the growing development in the manufacture of synthetic scaffold in tissue engineering applications. These new materials are based on polyglycerol dendrimers (PGLD's). PGLD's are highly functional polymers with hydroxymethyl side groups, fulfill all structural prerequisites to replace poly(ethylene glycol)s in medical applications. Furthermore, since these materials are based on naturally occurring compounds that degrades over time in the body and can be safely excreted. The objective of this work was the synthesis, physicochemical, biological characterization of HPGL's with potential use as scaffolds in tissue engineering. HPGL's with oligomeric cores, of diglycerol triglycerol and tetraglycerol was used. Theoretical and Experimental Simulation Details: The synthesis of PGLD procedures involves the etherification of glycerol through anionic polymerization of glycidol. The PGLD's were characterized by chromatographic techniques (SEC and HPLC), spectroscopic (FTIR, 1H-NMR and 13C - NMR) electrochemical (zeta potential) and thermal analysis (DSC and TGA) techniques. The structure- activity relationships (SAR's) of compound prototype and its analogs were studied to determine the generation number (G) of the molecule responsible for the biological activity on the adhesion and cell proliferation process. A detailed study of the structure of PGLD's of G=0-4 was performed using the Hyperchem 7. 5 and Gromacs 4 software packages. The biocompatibility studies were studied by scanning electron microscopy (SEM) and fluorescence microscopy (EPF) technique after PGLD (G=0-4) blood contact. The overall electro-negativity/total charge density, dipole moment, frontier orbital's (HOMO - LUMO) and electrostatic potential maps (EPM) were calculated. The most stable form of the resulting compounds was determined by estimating the hydration energy and energy conformation. Results and Discussion: The techniques SEM and EPF

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

    International Nuclear Information System (INIS)

    Correa, P.; Camargo, N.H.A.; Silva, D.F.

    2012-01-01

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

  3. 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.

  4. Synthesis and spectroscopic characterization of magnetic hydroxyapatite nanocomposite using ultrasonic irradiation

    Science.gov (United States)

    Gopi, D.; Ansari, M. Thameem; Shinyjoy, E.; Kavitha, L.

    2012-02-01

    Nowadays magnetic hydroxyapatite (m-HAP) has potential applications in biomedicine more especially for bone cancer treatment. In this paper the functionalization of the hydroxyapatite (HAP) with magnetite nanoparticle (MNP) through ultrasonic irradiation technique is reported and its spectral investigation has been carried out. The ultrasonic irradiation with two different frequencies of 28 kHz and 35 kHz at the power of 150 and 320 W, respectively, was employed for the synthesis of m-HAP. The ultrasound irradiation of 35 kHz at 320 W shows the efficient diffusion of MNP to the HAP host matrix leads to the formation of m-HAP. The ultrasonic irradiation technique does not require stabilizers as in the case of coprecipitation method hence the final product of pure m-HAP is obtained. The X-ray diffraction pattern shows the formation of magnetite nanoparticles which are functionalized with hydroxyapatite host matrix. The vibrating sample magnetometer curve exhibits the super paramagnetic property of the samples and the saturation magnetization ( Ms) value of the functionalized magnetic hydroxyapatite. The Ms value is found to be much less than that of pure magnetite nanoparticle and this decrement in Ms is due to the hindrance of magnetic domain of the particles with HAP. The portrayed Raman spectra discriminate between the m-HAP and MNP with corresponding vibrational modes of frequencies. The transmission electron micrograph shows excellent morphology of functionalized m-HAP in nanometer range. The atomic force microscopic investigation shows the 3-dimensional view of crust and trench shape of m-HAP. All these results confirm the formation of magnetic hydroxyapatite nanocomposite with typical magnetic property for biological applications.

  5. 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.

  6. Synthesis and characterization of transition-metal-doped zinc oxide nanocrystals for spintronics

    Science.gov (United States)

    Wang, Xuefeng

    Spintronics (spin transport electr onics), in which both spin and charge of carriers are utilized for information processing, is believed to challenge the current microelectronics and to become the next-generation electronics. Nanostructured spintronic materials and their synthetic methodologies are of paramount importance for manufacturing future nanoscale spintronic devices. This thesis aims at studying synthesis, characterization, and magnetism of transition-metal-doped zinc oxide (ZnO) nanocrystals---a diluted magnetic semiconductor (DMS)---for potential applications in future nano-spintronics. A simple bottom-up-based synthetic strategy named a solvothermal technique is introduced as the primary synthetic approach and its crystal growth mechanism is scrutinized. N-type cobalt-doped ZnO-based DMS nanocrystals are employed as a model system, and characterized by a broad spectrum of advanced microscopic and spectroscopic techniques. It is found that the self-orientation growth mechanism, imperfect oriented attachment, is intimately correlated with the high-temperature ferromagnetism via defects. The influence of processing on the magnetic properties, such as compositional variations, reaction conditions, and post-growth treatment, is also studied. In this way, an in-depth understanding of processing-structure-property interrelationships and origins of magnetism in DMS nanocrystals are obtained in light of the theoretical framework of a spin-split impurity band model. In addition, a nanoscale spinodal decomposition phase model is also briefly discussed. Following the similar synthetic route, copper- and manganese-doped ZnO nanocrystals have been synthesized and characterized. They both show high-temperature ferromagnetism in line with the aforementioned theoretical model(s). Moreover, they display interesting exchange biasing phenomena at low temperatures, revealing the complexity of magnetic phases therein. The crystal growth strategy demonstrated in this work

  7. SYNTHESIS AND CHARACTERIZATION OF NEW HALOGENATED CURCUMINOIDS

    Directory of Open Access Journals (Sweden)

    Eugenio Torres

    2013-12-01

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

  8. Synthesis and characterization of thermally oxidized ZnO films

    Indian Academy of Sciences (India)

    Administrator

    Synthesis and characterization of thermally oxidized ZnO films. A P RAMBU1,* and N IFTIMIE2 .... R. −. Δ. = = (1) where Ra is the sensor resistance in the air and Rg is the .... ple, Aida and coworkers (2006) reported that the total oxidation is ...

  9. Expedient and click synthesis, spectroscopic characterizations and DFT calculations of novel 1,5-bis(N-substituted 1,2,3‒triazole) benzodiazepinedione scaffolds

    Science.gov (United States)

    Paghandeh, Hossein; Saeidian, Hamid

    2018-04-01

    A practically reliable procedure for synthesis of new 1,5-bis(N-substituted 1,2,3‒triazole) benzodiazepinedione derivatives was reported by sequential amidation, propargylation and a click azide‒alkyne [3 + 2] cycloaddition reaction in a one pot fashion. The desired products were characterized by CHN analysis, 1H and 13C NMR and ESI-MS spectroscopy. Short reaction time, good yields (55-91%), mild reaction conditions and easily available and less expensive starting materials are advantages of this protocol. Natural bond orbital charge distribution and HOMO-LUMO analysis of the characterized structure of 4e have been also calculated by density functional theory (DFT) calculations. The Li+ and Na+ ion affinities of 4e have been also investigated by DFT studies to find the applicability of these products as ligand in coordination chemistry. Sodium ion affinity of 4e was determined as 60 kJ mol-1 is less than its lithium ion affinity, indicating that the lithiation of 4e is more exothermic than the sodiation.

  10. Naphthalene-based fluorophores: Synthesis characterization, and photophysical properties

    International Nuclear Information System (INIS)

    Feng Jinwu; Chen Xiaopeng; Han Qingchuan; Wang Hongbo; Lu Ping; Wang Yanguang

    2011-01-01

    U-type, 1,8-diarylnaphthalenes and 1,8-diarylethynylnaphthalenes were synthesized and their structures were characterized by spectroscopic methods. Emission performance of these compounds with donor and acceptor was largely depended upon the solvent polarity and environmental acidity, which implied that they might be used as solvent polarity sensors or pH sensors as well. Moreover, some 1,8-diarylnaphthalenes exhibited aggregation-induced emission enhancement (AIEE) based on their photophysical investigation and might be used as light emitting materials for optoelectronic applications. - Highlights: → 1,8-Diarylnaphthalenes and 1,8-diarylethynylnaphthalenes were synthesized. → Emission of these compounds depended on solvent polarity and environmental acidity. → Some 1,8-diarylnaphthalenes exhibited aggregation-induced emission enhancement.

  11. Design, Synthesis, and Applications of Carbon Nanohoops

    Science.gov (United States)

    2016-05-23

    rings via one electron reduction reactions was feasible. Therefore, the synthesis and spectroscopic investigations of these ring systems by reducing...Release; Distribution Unlimited UU UU UU UU 23-05-2016 15-Feb-2012 14-Feb-2016 Final Report: Design, Synthesis , and Applications of Carbon Nanohoops The...Office P.O. Box 12211 Research Triangle Park, NC 27709-2211 Caron Nanohoops, paracyclophanes, carbon nanotubes, organic synthesis REPORT

  12. Synthesis and spectroscopic behavior of highly luminescent trinuclear europium complexes with tris-β-diketone ligand

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Dunjia, E-mail: dunjiawang@163.com; Pi, Yan; Liu, Hua; Wei, Xianhong; Hu, Yanjun; Zheng, Jing

    2014-11-15

    Highlights: • Synthesis of the tris-β-diketone ligand and its trinuclear europium complexes. • Photoluminescence behavior of trinuclear europium complexes. • Analysis of the Judd–Ofelt intensity parameters (Ω{sub t}), lifetime (τ) and quantum yield (η). - Abstract: A new tris-β-diketone ligand, 2-[4,6-bis-(1-benzoyl-2-oxo-2-phenyl-ethyl)-[1,3,5]triazin-2-yl] -1,3-diphenyl-propane-1,3-dione (H{sub 3}L), and its trinuclear europium complexes, Eu{sub 3}(DBM){sub 6}L (C1), Eu{sub 3}(DBM){sub 6}(Bipy){sub 3}L (C2) and Eu{sub 3}(DBM){sub 6}(Phen){sub 3}L (C3) were synthesized and their spectroscopic behaviors were studied by FT-IR, {sup 1}H NMR, UV–vis and photoluminescence spectroscopic techniques. These europium complexes exhibited the characteristic emission bands that arise from the {sup 5}D{sub 0} → {sup 7}F{sub J} (J = 0–4) transitions of the europium ion in solid state. The Ω{sub 2} and Ω{sub 4} intensity parameters, lifetime (τ) and luminescence quantum yield (η) were calculated according to the emission spectra and luminescence decay curves in solid state. The results indicated that these trinuclear europium complexes displayed a longer lifetime (τ) and higher luminescence quantum efficiency (η), especially complexes C2 (τ = 0.820 ms, η = 46.5%) and C3 (τ = 0.804 ms, η = 47.4%), which due to the effect of two additional europium ion lumophors and the introduction of the third ligands, Bipy or Phen in trinuclear complexes. Their Ω{sub 2} values demonstrated that the europium ion in these complexes is in a highly polarizable chemical environment.

  13. Synthesis and characterization of amorphous cellulose from triacetate of cellulose

    International Nuclear Information System (INIS)

    Vega-Baudrit, Jose; Sibaja, Maria; Nikolaeva, Svetlana; Rivera A, Andrea

    2014-01-01

    It was carried-out a study for the synthesis and characterization of amorphous cellulose starting from cellulose triacetate. X-rays diffraction was used in order to obtain the cellulose crystallinity degree, also infrared spectroscopy FTIR was used. (author)

  14. Characterization of a spectroscopic detector for application in x-ray computed tomography

    Science.gov (United States)

    Dooraghi, Alex A.; Fix, Brian J.; Smith, Jerel A.; Brown, William D.; Azevedo, Stephen G.; Martz, Harry E.

    2017-09-01

    Recent advances in cadmium telluride (CdTe) energy-discriminating pixelated detectors have enabled the possibility of Multi-Spectral X-ray Computed Tomography (MSXCT) to incorporate spectroscopic information into CT. MultiX ME 100 V2 is a CdTe-based spectroscopic x-ray detector array capable of recording energies from 20 to 160 keV in 1.1 keV energy bin increments. Hardware and software have been designed to perform radiographic and computed tomography tasks with this spectroscopic detector. Energy calibration is examined using the end-point energy of a bremsstrahlung spectrum and radioisotope spectral lines. When measuring the spectrum from Am-241 across 500 detector elements, the standard deviation of the peak-location and FWHM measurements are +/- 0.4 and +/- 0.6 keV, respectively. As these values are within the energy bin size (1.1 keV), detector elements are consistent with each other. The count rate is characterized, using a nonparalyzable model with a dead time of 64 +/- 5 ns. This is consistent with the manufacturer's quoted per detector-element linear-deviation at 2 Mpps (million photons per sec) of 8.9 % (typical) and 12 % (max). When comparing measured and simulated spectra, a low-energy tail is visible in the measured data due to the spectral response of the detector. If no valid photon detections are expected in the low-energy tail, then a background subtraction may be applied to allow for a possible first-order correction. If photons are expected in the low-energy tail, a detailed model must be implemented. A radiograph of an aluminum step wedge with a maximum height of 20 mm shows an underestimation of attenuation by about 10 % at 60 keV. This error is due to partial energy deposition from higher energy (>60 keV) photons into a lower-energy ( 60 keV) bin, reducing the apparent attenuation. A radiograph of a polytetrafluoroethylene (PTFE) cylinder taken using a bremsstrahlung spectrum from an x-ray voltage of 100 kV filtered by 1.3 mm Cu is

  15. Characterization of a spectroscopic detector for application in x-ray computed tomography

    Energy Technology Data Exchange (ETDEWEB)

    Dooraghi, A. A. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Fix, B. J. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Smith, J. A. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Brown, W. D. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Azevedo, S. G. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Martz, H. E. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)

    2017-04-21

    Recent advances in cadmium telluride (CdTe) energy-discriminating pixelated detectors have enabled the possibility of Multi-Spectral X-ray Computed Tomography (MSXCT) to incorporate spectroscopic information into CT. MultiX ME 100 V2 is a CdTe-based spectroscopic x-ray detector array capable of recording energies from 20 to 160 keV in 1.1 keV energy bin increments. Hardware and software have been designed to perform radiographic and computed tomography tasks with this spectroscopic detector. Energy calibration is examined using the end-point energy of a bremsstrahlung spectrum and radioisotope spectral lines. When measuring the spectrum from Am-241 across 500 detector elements, the standard deviation of the peak-location and FWHM measurements are ±0.4 and ±0.6 keV, respectively. As these values are within the energy bin size (1.1 keV), detector elements are consistent with each other. The count rate is characterized, using a nonparalyzable model with a dead time of 64 ± 5 ns. This is consistent with the manufacturer’s quoted per detector-element linear-deviation at 2 Mpps (million photons per sec) of 8.9% (typical) and 12% (max). When comparing measured and simulated spectra, a low-energy tail is visible in the measured data due to the spectral response of the detector. If no valid photon detections are expected in the low-energy tail, then a background subtraction may be applied to allow for a possible first-order correction. If photons are expected in the low-energy tail, a detailed model must be implemented. A radiograph of an aluminum step wedge with a maximum height of about 20 mm shows an underestimation of attenuation by about 10% at 60 keV. This error is due to partial energy deposition from higher-energy (> 60 keV) photons into a lower-energy (~60 keV) bin, reducing the apparent attenuation. A radiograph of a PTFE cylinder taken using a bremsstrahlung spectrum from an x-ray voltage of 100 kV filtered by 1.3 mm Cu is reconstructed using Abel inversion

  16. Characterization structural and morphology ZSM-5 zeolite by hydrothermal synthesis

    International Nuclear Information System (INIS)

    Silva, V.J.; Crispim, A.C.; Queiroz, M.B.; Laborde, H.M.; Rodrigues, M.G.F.; Menezes, R.R.

    2009-01-01

    Solid acids are catalytic materials commonly used in the chemical industry. Among these zeolites are the most important business processes including water treatment, gas separation, and cracking long hydrocarbon chains to produce high octane gasoline. Its synthesis, characterization and applications have been widely studied. The objective this study was to synthesize the ZSM-5 zeolite for future use in separation processes and catalysis. The zeolite ZSM-5 was prepared by hydrothermal synthesis at 170°C, using silica, deionized water and the director of structures (TPABr - tetrapropylammonium bromide). The materials were characterized by X ray diffraction (XRD), scanning electron microscopy (SEM) and semiquantitative chemical analysis by X ray fluorescence (XRF). According to the XRD was possible to observe the formation of ZSM-5 zeolite, with peaks intense and well defined. The SEM showed the formation of individual particles, clean, rounded shapes. (author)

  17. Polymer Brushes: Synthesis, Characterization, Applications

    Science.gov (United States)

    Advincula, Rigoberto C.; Brittain, William J.; Caster, Kenneth C.; Rühe, Jürgen

    2004-09-01

    Materials scientists, polymer chemists, surface physicists and materials engineers will find this book a complete and detailed treatise on the field of polymer brushes, their synthesis, characterization and manifold applications. In a first section, the various synthetic pathways and different surface materials are introduced and explained, followed by a second section covering important aspects of characterization and analysis in both flat surfaces and particles. These specific surface initiated polymerization (SIP) systems such as linear polymers, homopolymers, block copolymers, and hyperbranched polymers are unique compared to previously reported systems by chemisorption or physisorption. They have found their way in both large-scale and miniature applications of polymer brushes, which is covered in the last section. Such 'hairy' surfaces offer fascinating opportunities for addressing numerous problems of both academic and, in particular, industrial interest: high-quality, functional or protective coatings, composite materials, surface engineered particles, metal-organic interfaces, biological applications, micro-patterning, colloids, nanoparticles, functional devices, and many more. It is the desire of the authors that this book will be of benefit to readers who want to "brush-up on polymers".

  18. Magnetic nanoparticle supported phosphotungstic acid: An efficient catalyst for the synthesis of xanthene derivatives

    Science.gov (United States)

    Patel, Nipun; Katheriya, Deepak; Dadhania, Harsh; Dadhania, Abhishek

    2018-05-01

    Magnetic nanoparticle supported phosphotungstic acid (Fe3O4@SiO2-HPW) was applied as a highly efficient catalyst for the synthesis of 14H-dibenzoxanthene derivatives via condensation reaction of 2-naphthol and aryl aldehydes. The catalyst was found highly efficient for the synthesis of xanthene derivatives under solvent free condition. The catalyst showed high activity and stability during the reaction and provided excellent yield of the corresponding products in short reaction time. All the synthesized compounds were characterized through FT-IR, 1H-NMR and 13C-NMR spectroscopic techniques. Furthermore, the catalyst is magnetically recoverable and can be reused several times without significant loss of its catalytic activity.

  19. Preparation and spectroscopic characterization of visible light sensitized N doped TiO2 (rutile)

    International Nuclear Information System (INIS)

    Livraghi, S.; Czoska, A.M.; Paganini, M.C.; Giamello, E.

    2009-01-01

    Nitrogen doped TiO 2 represents one of the most promising material for photocatalitic degradation of environmental pollutants with visible light. However, at present, a great deal of activity is devoted to the anatase polymorph while few data about rutile are available. In the present paper we report an experimental characterization of N doped polycrystalline rutile TiO 2 prepared via sol-gel synthesis. Nitrogen doping does not affect the valence band to conduction band separation but, generates intra band gap localized states which are responsible of the on set of visible light absorption. The intra band gap states correspond to a nitrogen containing defect similar but not coincident with that recently reported for N doped anatase. - Graphical abstract: Nitrogen doped TiO 2 represents one of the most promising material for photocatalitic degradation of environmental pollutants with visible light. However, at present, a great deal of activity is devoted to the anatase polymorph while few data about rutile are available. In the present paper we report an experimental characterization of N doped polycrystalline rutile TiO 2 prepared via sol-gel synthesis

  20. Synthesis of a ruthenium(II) bipyridyl complex coordinated by a functionalized Schiff base ligand: characterization, spectroscopic and isothermal titration calorimetry measurements of M2+ binding and sensing (M2+=Ca2+, Mg2+).

    Science.gov (United States)

    Dixit, Namrata; Mishra, Lallan; Mustafi, Sourajit M; Chary, Kandala V R; Houjou, Hirohiko

    2009-07-01

    Bis-[methylsalicylidine-4'benzoic acid]-ethylene (LH2) complexed with cis-Ru(bpy)2Cl(2).2H2O provides a complex of composition [Ru(bpy)2L].2NH4PF6 (1), which has been characterized spectroscopically. Its binding behaviour towards Mg2+ and Ca2+ ions is monitored using 1H NMR titration, isothermal titration calorimetry (ITC) and luminescence microscopy. The luminescent ruthenium complex binds Ca2+ in a more selective manner as compared to Mg2+.

  1. 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.

  2. [Synthesis and Characterization of a Sugar Based Electrolyte for Thin-film Polymer Batteries

    Science.gov (United States)

    1998-01-01

    The work performed during the current renewal period, March 1,1998 focused primarily on the synthesis and characterization of a sugar based electrolyte for thin-film polymer batteries. The initial phase of the project involved developing a suitable sugar to use as the monomer in the polymeric electrolyte synthesis. The monomer has been synthesized and characterized completely. Overall the yield of this material is high and it can be produced in relatively large quantity easily and in high purity. The scheme used for the preparation of the monomer is outlined along with pertinent yields.

  3. Synthesis and electrical characterization of Graphene Oxide films

    International Nuclear Information System (INIS)

    Yasin, Muhammad; Tauqeer, T.; Zaidi, Syed M.H.; San, Sait E.; Mahmood, Asad; Köse, Muhammet E.; Canimkurbey, Betul; Okutan, Mustafa

    2015-01-01

    In this work, we have synthesized Graphene Oxide (GO) using modified Hummers method and investigated its electrical properties using parallel plate impedance spectroscopic technique. Graphene Oxide films were prepared using drop casting method on Indium Tin Oxide (ITO) coated glass substrate. Atomic force microscopy was used to characterize the films' microstructure and surface topography. Electrical characterization was carried out using LCR meter in frequency regime (100 Hz to 10 MHz) at different temperatures. AC conductivity σ ac of the films was observed to be varied with angular frequency, ω as ω S , with S < 1. The electrical properties of GO were found to be both frequency and temperature dependent. Analysis showed that GO film contains direct current (DC) and Correlated Barrier Hopping (CBH) conductivity mechanisms at low and high frequency ranges, respectively. Photon absorption and transmittance capability in the visible range and excellent electrical parameters of solution processed Graphene Oxide suggest its suitability for the realization of low cost flexible organic solar cells and organic Thin Film Transistors, respectively. - Highlights: • Synthesize and electrical characterization of Graphene Oxide (GO) Film was undertaken. • Temperature dependent impedance spectroscopy was used for electrical analysis. • AFM was used to characterize films' microstructure and surface topography. • Electrical parameters were found to vary with both temperature and frequency. • GO showed DC and CBH conductivity mechanisms at low and high frequency, respectively

  4. X-ray Spectroscopic Characterization of Plasma for a Charged-Particle Energy-Loss Experiment

    Science.gov (United States)

    Hoffman, Nm; Lee, Cl; Wilson, Dc; Barnes, Cris W.; Petrasso, Rd; Li, C.; Hicks, D.

    2000-10-01

    We are pursuing an approach to a charged-particle energy-loss experiment in which charged fusion products from an imploded ICF capsule travel through a well characterized, spatially separate plasma. For this purpose, a fully ionized, uniform, nearly steady-state carbon-hydrogen plasma will be created by laser irradiation of a plastic foil. The temperature and density structure of this plasma must be determined accurately in order to relate observed energy losses to predictions of theory. Various methods for diagnosing the plasma are possible, including Thomson scattering. Alternatively, if a small admixture of higher-Z material such as chlorine is included in the plastic, x-ray spectroscopic techniques will allow the plasma's temperature and density to be determined. Electron temperature is inferred from the ratios of line strengths of various chlorine ion stages, while electron density is determined from the spectra of lithium-like satellite lines near the He beta line of helium-like chlorine. We present results from detailed-configuration accounting (DCA) models of line emission from C+H+Cl plasmas, and estimate the accuracy with which such plasmas can be characterized.

  5. Design and spectroscopic reflectometry characterization of pulsed laser deposition combinatorial libraries

    International Nuclear Information System (INIS)

    Schenck, Peter K.; Bassim, Nabil D.; Otani, Makoto; Oguchi, Hiroyuki; Green, Martin L.

    2007-01-01

    The goal of the design of pulsed laser deposition (PLD) combinatorial library films is to optimize the compositional coverage of the films while maintaining a uniform thickness. The deposition pattern of excimer laser PLD films can be modeled with a bimodal cos n distribution. Deposited films were characterized using a spectroscopic reflectometer (250-1000 nm) to map the thickness of both single composition calibration films and combinatorial library films. These distribution functions were used to simulate the composition and thickness of multiple target combinatorial library films. The simulations were correlated with electron-probe microanalysis wavelength-dispersive spectroscopy (EPMA-WDS) composition maps. The composition and thickness of the library films can be fine-tuned by adjusting the laser spot size, fluence, background gas pressure, target geometry and other processing parameters which affect the deposition pattern. Results from compositionally graded combinatorial library films of the ternary system Al 2 O 3 -HfO 2 -Y 2 O 3 are discussed

  6. Synthesis and structural characterization of inorganic luminescent materials of Cs2NaErBr6 and Cs2NaHoBr6

    International Nuclear Information System (INIS)

    Poblete, V.H; Fack, G

    2003-01-01

    The synthesis and structural characterization is described of two luminescent materials, with technological [1] and spectroscopic [2] interest, whose crystallographic charts have not been published in the literature. The synthesis of both systems: Cs 2 NaErBr 6 and CS 2 NaHoBr 6 , was done using solid state reactions in a controlled environment. The thermal analyses DTA/TGA, applied with a temperature gradient of 10 o C/min., established crystallization ranges of 490,4 o C to 545,4 o C, for the elpasolite CS 2 NaHoBr 6 and 501 o C to 556 o C, for the structure CS 2 NaErBr 6 .. The heat vacuum treatments were carried out at 505 o C and 526 o C respectively, obtaining optimum crystallization. The structural characterization was performed with powdered X-ray diffraction (XRD). The range between 12 o and 80 o (2θ), was analyzed for 3352 points, measured steps of 0.02 o (2θ using the Rietveld profile refining program. The following crystallographic parameters were established: a 0 = 11,279(1), and 11,293(4) Angstroms, for the two structures analyzed, respectively. The relationship R exp wp in both cases is highly accurate for the 32 test lines that were analyzed. The structures present cubic closed packing Cs 1+ 3 Cl 1- , with Ho 3+ and Er 3+ atoms, filling the octahedral holes. The test data obtained will be very useful for completing the mass of experimental data needed to develop the design engineering, with specific applications for luminescent devices (au)

  7. Dispersed metal cluster catalysts by design. Synthesis, characterization, structure, and performance

    Energy Technology Data Exchange (ETDEWEB)

    Arslan, Ilke [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Dixon, David A. [Univ. of Alabama, Tuscaloosa, AL (United States); Gates, Bruce C. [Univ. of California, Davis, CA (United States); Katz, Alexander [Univ. of California, Berkeley, CA (United States)

    2015-09-30

    To understand the class of metal cluster catalysts better and to lay a foundation for the prediction of properties leading to improved catalysts, we have synthesized metal catalysts with well-defined structures and varied the cluster structures and compositions systematically—including the ligands bonded to the metals. These ligands include supports and bulky organics that are being tuned to control both the electron transfer to or from the metal and the accessibility of reactants to influence catalytic properties. We have developed novel syntheses to prepare these well-defined catalysts with atomic-scale control the environment by choice and placement of ligands and applied state-of-the art spectroscopic, microscopic, and computational methods to determine their structures, reactivities, and catalytic properties. The ligands range from nearly flat MgO surfaces to enveloping zeolites to bulky calixarenes to provide controlled coverages of the metal clusters, while also enforcing unprecedented degrees of coordinative unsaturation at the metal site—thereby facilitating bonding and catalysis events at exposed metal atoms. With this wide range of ligand properties and our arsenal of characterization tools, we worked to achieve a deep, fundamental understanding of how to synthesize robust supported and ligand-modified metal clusters with controlled catalytic properties, thereby bridging the gap between active site structure and function in unsupported and supported metal catalysts. We used methods of organometallic and inorganic chemistry combined with surface chemistry for the precise synthesis of metal clusters and nanoparticles, characterizing them at various stages of preparation and under various conditions (including catalytic reaction conditions) and determining their structures and reactivities and how their catalytic properties depend on their compositions and structures. Key characterization methods included IR, NMR, and EXAFS spectroscopies to identify

  8. 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.

  9. Natural precursor based hydrothermal synthesis of sodium carbide for reactor applications

    Science.gov (United States)

    Swapna, M. S.; Saritha Devi, H. V.; Sebastian, Riya; Ambadas, G.; Sankararaman, S.

    2017-12-01

    Carbides are a class of materials with high mechanical strength and refractory nature which finds a wide range of applications in industries and nuclear reactors. The existing synthesis methods of all types of carbides have problems in terms of use of toxic chemical precursors, high-cost, etc. Sodium carbide (Na2C2) which is an alkali metal carbide is the least explored one and also that there is no report of low-cost and low-temperature synthesis of sodium carbide using the eco-friendly, easily available natural precursors. In the present work, we report a simple low-cost, non-toxic hydrothermal synthesis of refractory sodium carbide using the natural precursor—Pandanus. The formation of sodium carbide along with boron carbide is evidenced by the structural and morphological characterizations. The sample thus synthesized is subjected to field emission scanning electron microscopy (FESEM), x-ray powder diffraction (XRD), ultraviolet (UV)—visible spectroscopy, Fourier transform infrared spectroscopy (FTIR), Raman, and photoluminescent (PL) spectroscopic techniques.

  10. Synthesis, spectroscopic and thermochemical studies of some novel carbazole-pyridine co-polymers (abstract)

    International Nuclear Information System (INIS)

    Saeed, A.; Irfan, M.

    2011-01-01

    Two series of a novel class of carbazole-4-phenylpyridine co-polymers has been synthesized by a modified Chichibabin reaction. The synthesis was carried out by a simple and cheaper method compared to the lengthy methods usually adopted for the preparation of carbazole-pyridine copolymers which involve costly catalysts. All the polymers were characterized by IR, /sup 1/H and /sup 13/C NMR, UV-vis spectroscopy, fluorimetry, TGA and DSC. The weight average molecular masses (M/sub w/) of the polymers were estimated by Laser Light Scattering (LLS) technique. (author)

  11. Synthesis and spectroscopic characterization of gold nanoparticles via plasma-liquid interaction technique

    Science.gov (United States)

    Khatoon, N.; Yasin, H. M.; Younus, M.; Ahmed, W.; Rehman, N. U.; Zakaullah, M.; Iqbal, M. Zafar

    2018-01-01

    Fabrication of non-functionalized gold nanoparticles is interesting owing to their potential applications in sensing and biomedicine. We report on the synthesis of surfactant-free gold nanoparticles (AuNPs) by Plasma-Liquid Interaction (PLI) technique, using micro-atmospheric pressure D.C. plasma. The effects of discharge parameters, such as discharge current, precursor concentration and gas flow rates on the structure and morphology of AuNPs have been investigated. Optical Emission Spectroscopy (OES) was employed to estimate the UV radiation intensity and OH radical density. Scanning electron microscopy (SEM) and ultraviolet-visible (UV-Vis) optical spectroscopy were employed to study the morphology and structure of AuNPs. The normalized intensities of UV radiation and OH radical density found to increase with increase in discharge current. We observed that the particle size can be tuned by controlling any of the following parameters: intensity of the UV radiation, OH radical density, and concentration of the Au precursor. Interestingly, we found that addition of 1% Ar in the feedstock gas results in formation of relatively uniform size distribution of nanoparticles. The surfactant-free AuNPs, due to their bare-surface, exhibit excellent surface-enhanced Raman scattering (SERS) properties. The SERS study of Rhodamine 6G using AuNPs as substrates, shows significant Raman enhancement and fluorescence quenching, which makes our technique a potentially powerful route to detection of trace amounts of dangerous explosives and other materials.

  12. Synthesis and spectroscopic properties of transfermium isotopes with Z = 105, 106 and 107

    Energy Technology Data Exchange (ETDEWEB)

    Streicher, B [Comenius University, Faculty of Mathematics, Physics and Informatics, Department of Nuclear Physics and Biopgysics, 84218 Bratislava (Slovakia)

    2006-07-01

    The quest for production of new elements has been on for several decades. On the way up the ladder of nuclear chart the systematic research of nuclear properties of elements in transfermium region has been severely overlooked. This drawback is being rectified in past few years by systematic synthesis of especially even-even and odd-A isotopes of these elements. This work proceeds forward also with major contribution of velocity filter SHIP, placed at GSI, Darmstadt. This experimental device represents a unique possibility due to high (up to 1 p{mu}A) beam currents provided by UNILAC accelerator and advancing detection systems to study by means of decay spectroscopy the nuclear structure of isotopes for the elements, possibly up to proton number Z = 110. As the low lying single-particle levels are especially determined by the unpaired nucleon, the odd mass nuclei provide a valuable source of information about the nuclear structure. Such results can be directly compared with the predictions of the calculations based on macroscopic-microscopic model of nuclear matter, thus proving an unambiguous test of the correctness of present models and their power to predict nuclear properties towards yet unknown regions. This work concentrates on the spectroscopic analysis of few of such nuclei. Namely it deals with isotopes {sup 261}Sg and {sup 257}Rf with one unpaired neutron, as well as isotopes {sup 257}Db and {sup 253}Lr with one unpaired proton configuration. Moreover, the analysis of odd-odd nuclei of the the decay sequence {sup 262}Bg {yields} {sup 258}Db {yields} {sup 254}Lr {yields} produced in various experiments at SHIP is discussed in detail. Exhaustive spectroscopic analysis of these data is provided, revealing new information on {alpha}, {beta}, EC and SF decay modes of these very heavy isotopes, and deepening the knowledge of the low lying single-particle level structure. Outcomes resulting from the comparison with the systematics of experimentally derived

  13. 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.

  14. Biodegradable starch-based films containing saturated fatty acids: thermal, infrared and raman spectroscopic characterization

    Directory of Open Access Journals (Sweden)

    Marcelo M. Nobrega

    Full Text Available Biodegradable films of thermoplastic starch and poly (butylene adipate co-terephthalate (PBAT containing fatty acids were characterized thermally and with infrared and Raman spectroscopies. The symmetrical character of the benzene ring in PBAT provided a means to illustrate the difference between these spectroscopic techniques, because a band appeared in the Raman spectrum but not in the infrared. The thermal analysis showed three degradation stages related to fatty acids, starch and PBAT. The incorporation of saturated fatty acids with different molecular mass (caproic, lauric and stearic did not change the nature of the chemical bonds among the components in the blends of starch, PBAT and glycerol, according to the thermal analysis, infrared and Raman spectroscopies.

  15. Accurate spectroscopic characterization of oxirane: A valuable route to its identification in Titan's atmosphere and the assignment of unidentified infrared bands

    Energy Technology Data Exchange (ETDEWEB)

    Puzzarini, Cristina [Dipartimento di Chimica " Giacomo Ciamician," Università di Bologna, Via Selmi 2, I-40126 Bologna (Italy); Biczysko, Malgorzata; Bloino, Julien; Barone, Vincenzo, E-mail: cristina.puzzarini@unibo.it [Scuola Normale Superiore, Piazza dei Cavalieri 7, I-56126 Pisa (Italy)

    2014-04-20

    In an effort to provide an accurate spectroscopic characterization of oxirane, state-of-the-art computational methods and approaches have been employed to determine highly accurate fundamental vibrational frequencies and rotational parameters. Available experimental data were used to assess the reliability of our computations, and an accuracy on average of 10 cm{sup –1} for fundamental transitions as well as overtones and combination bands has been pointed out. Moving to rotational spectroscopy, relative discrepancies of 0.1%, 2%-3%, and 3%-4% were observed for rotational, quartic, and sextic centrifugal-distortion constants, respectively. We are therefore confident that the highly accurate spectroscopic data provided herein can be useful for identification of oxirane in Titan's atmosphere and the assignment of unidentified infrared bands. Since oxirane was already observed in the interstellar medium and some astronomical objects are characterized by very high D/H ratios, we also considered the accurate determination of the spectroscopic parameters for the mono-deuterated species, oxirane-d1. For the latter, an empirical scaling procedure allowed us to improve our computed data and to provide predictions for rotational transitions with a relative accuracy of about 0.02% (i.e., an uncertainty of about 40 MHz for a transition lying at 200 GHz).

  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 and characterization of polyglycerols dendrimers for applications in tissue engineering biological

    Energy Technology Data Exchange (ETDEWEB)

    Passos, E.D.; Queiroz, A.A.A. de [Universidade Federal de Itajuba (UNIFEI), MG (Brazil)

    2014-07-01

    Full text: Introduction: Over the last twenty years is the growing development in the manufacture of synthetic scaffold in tissue engineering applications. These new materials are based on polyglycerol dendrimers (PGLD's). PGLD's are highly functional polymers with hydroxymethyl side groups, fulfill all structural prerequisites to replace poly(ethylene glycol)s in medical applications. Furthermore, since these materials are based on naturally occurring compounds that degrades over time in the body and can be safely excreted. The objective of this work was the synthesis, physicochemical, biological characterization of HPGL's with potential use as scaffolds in tissue engineering. HPGL's with oligomeric cores, of diglycerol triglycerol and tetraglycerol was used. Theoretical and Experimental Simulation Details: The synthesis of PGLD procedures involves the etherification of glycerol through anionic polymerization of glycidol. The PGLD's were characterized by chromatographic techniques (SEC and HPLC), spectroscopic (FTIR, 1H-NMR and 13C - NMR) electrochemical (zeta potential) and thermal analysis (DSC and TGA) techniques. The structure- activity relationships (SAR's) of compound prototype and its analogs were studied to determine the generation number (G) of the molecule responsible for the biological activity on the adhesion and cell proliferation process. A detailed study of the structure of PGLD's of G=0-4 was performed using the Hyperchem 7. 5 and Gromacs 4 software packages. The biocompatibility studies were studied by scanning electron microscopy (SEM) and fluorescence microscopy (EPF) technique after PGLD (G=0-4) blood contact. The overall electro-negativity/total charge density, dipole moment, frontier orbital's (HOMO - LUMO) and electrostatic potential maps (EPM) were calculated. The most stable form of the resulting compounds was determined by estimating the hydration energy and energy conformation. Results and

  18. 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-

  19. Synthesis and characterization of triangulene

    Science.gov (United States)

    Pavliček, Niko; Mistry, Anish; Majzik, Zsolt; Moll, Nikolaj; Meyer, Gerhard; Fox, David J.; Gross, Leo

    2017-05-01

    Triangulene, the smallest triplet-ground-state polybenzenoid (also known as Clar's hydrocarbon), has been an enigmatic molecule ever since its existence was first hypothesized. Despite containing an even number of carbons (22, in six fused benzene rings), it is not possible to draw Kekulé-style resonant structures for the whole molecule: any attempt results in two unpaired valence electrons. Synthesis and characterization of unsubstituted triangulene has not been achieved because of its extreme reactivity, although the addition of substituents has allowed the stabilization and synthesis of the triangulene core and verification of the triplet ground state via electron paramagnetic resonance measurements. Here we show the on-surface generation of unsubstituted triangulene that consists of six fused benzene rings. The tip of a combined scanning tunnelling and atomic force microscope (STM/AFM) was used to dehydrogenate precursor molecules. STM measurements in combination with density functional theory (DFT) calculations confirmed that triangulene keeps its free-molecule properties on the surface, whereas AFM measurements resolved its planar, threefold symmetric molecular structure. The unique topology of such non-Kekulé hydrocarbons results in open-shell π-conjugated graphene fragments that give rise to high-spin ground states, potentially useful in organic spintronic devices. Our generation method renders manifold experiments possible to investigate triangulene and related open-shell fragments at the single-molecule level.

  20. Synthesis and characterization of some complexes with imidazole and pyrazole from saccharinate transition ions in oxidation state (II)

    International Nuclear Information System (INIS)

    Pineda Cedeno, Leslie William

    2001-01-01

    The synthesis and characterization of metal ions saccharinate of the first serie of transition with the imidazole and pyrazole molecules in water and absolute ethanol were studied. In general, it found that in this series of saccharinate of coordinated water molecules are replaced by imidazole and pyrazole molecules with different substitution patterns, generating neutral complex of molecular formula [M(Sac) 2 (L) n (H 2 O) n-4 ] and cationic complex of molecular formula [M(L) n (H 2 O) 2 ]x2Sac, [M(L) n (H 2 O) 3 ]x2Sac, [M(L) n ]x2Sac, where M = V(II), Cr(II), Mc(II), Fe(II), Co(II), Ni(II) y Zn(II); Sac = saccharinate ion; L = imidazole (imd) and pyrazole (pir) and n = 6,4,3 and 2. These compounds are soluble in DMF and insoluble in all other common solvents. In turn, synthesized compounds in water were characterized by X ray crystallography, where preliminary data of refinement cycles, generate formulas of isostructural type [M(imd) 4 (H 2 O) 2 ]x2Sac and [M(Sac) 2 (pir) 2 (H 2 O) 2 ] where M = Co(II), Ni(II). The imidazole complex crystallize in the triclinic crystal system and space group P-1, while the pyrazole complexes crystallize in the monoclinic crystal system and space group P2 (1)/n. Gradual diminution was observed in the bond distances of M-N (saccharinate ion), M-N (imidazole) and M-N (pyrazole). The complex was characterized by spectroscopic methods, magnetic and electrochemical. (author) [es

  1. Synthesis and spectroscopic studies of stable aqueous dispersion of silver nanoparticles.

    Science.gov (United States)

    El-Shishtawy, Reda M; Asiri, Abdullah M; Al-Otaibi, Maha M

    2011-09-01

    A facile approach for the synthesis of stable aqueous dispersion of silver nanoparticles (AgNPs) using glucose as the reducing agent in water/micelles system, in which cetyltrimethylammonium bromide (CTAB) was used as capping agent (stabilizer) is described. The evolution of plasmon band of AgNPs was monitored under different conditions such as (a) concentration of sodium hydroxide, (b) concentration of glucose, (c) concentration of silver nitrate (d) concentration of CTAB, and (e) reaction time. AgNPs were characterized by UV-visible spectroscopy, transmission electron microscopy (TEM), fluorescence spectroscopy and FT-IR spectroscopy. The results revealed an easy and viable strategy for obtaining stable aqueous dispersion of AgNPs with well controlled shape and size below 30 nm in diameter. Copyright © 2011 Elsevier B.V. All rights reserved.

  2. Microwave hydrothermal synthesis and characterization of PZT 52/48 powders

    International Nuclear Information System (INIS)

    Teixeira, G.F.; Gasparotto, G.; Santos, N.A.; Zaghete, M.A.; Varela, J.A.; Longo, E.

    2009-01-01

    Full text: Lead Zirconate Titanate (PZT) is a ceramic witch has great interest because of their ferroelectric, piezoelectric, and other electrical properties. In this work Pb(ZrxTi1-x)O3 powders were synthesized by microwave hydrothermal synthesis (M-H) at 180°C without excess lead content. This method allows obtaining particles whit nanometer size, good stoichiometric controls, high purity and crystalline degree at low temperatures and short times of synthesis. Powders were synthesized with molar concentration of 0.15 mol.L -1 during different times: 30 min, 2, 4, 6 and 8 h. After that the powders were characterized by X-ray diffraction (XRD), Field Emission Gun (FEG) and photoluminescence (PL). Through analysis it is observed that the crystalline phase of PZT is obtained from 2 hours of synthesis and this same time also presents more intense PL emission. (author)

  3. Spectroscopic and electrochemical characterization of nanostructured optically transparent carbon electrodes.

    Science.gov (United States)

    Benavidez, Tomás E; Garcia, Carlos D

    2013-07-01

    The present paper describes the results related to the optical and electrochemical characterization of thin carbon films fabricated by spin coating and pyrolysis of AZ P4330-RS photoresist. The goal of this paper is to provide comprehensive information allowing for the rational selection of the conditions to fabricate optically transparent carbon electrodes (OTCE) with specific electrooptical properties. According to our results, these electrodes could be appropriate choices as electrochemical transducers to monitor electrophoretic separations. At the core of this manuscript is the development and critical evaluation of a new optical model to calculate the thickness of the OTCE by variable angle spectroscopic ellipsometry. Such data were complemented with topography and roughness (obtained by atomic force microscopy), electrochemical properties (obtained by cyclic voltammetry), electrical properties (obtained by electrochemical impedance spectroscopy), and structural composition (obtained by Raman spectroscopy). Although the described OTCE were used as substrates to investigate the effect of electrode potential on the real-time adsorption of proteins by ellipsometry, these results could enable the development of other biosensors that can be then integrated into various CE platforms. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Electronic, electrical and magnetic ceramics synthesis and characterization

    International Nuclear Information System (INIS)

    Calix, V.S.; Saligan, P.P.; Naval, P.C.

    1989-01-01

    This paper describes the research and development activities of the Philippine Nuclear Research Institute (PNRI) on the synthesis and characterization of soft and hard ferrites and some beta alumina type superionic conductor materials. XRD, XRF and Moessbauer effect spectrometry are used to determine the structure phases, compositions and some magnetic properties of the materials. Effects of composition and preparation methods on the bulk electronic and magnetic properties are also discussed. (Auth.). 6 figs.; 3 tabs

  5. Materials-by-design: computation, synthesis, and characterization from atoms to structures

    Science.gov (United States)

    Yeo, Jingjie; Jung, Gang Seob; Martín-Martínez, Francisco J.; Ling, Shengjie; Gu, Grace X.; Qin, Zhao; Buehler, Markus J.

    2018-05-01

    In the 50 years that succeeded Richard Feynman’s exposition of the idea that there is ‘plenty of room at the bottom’ for manipulating individual atoms for the synthesis and manufacturing processing of materials, the materials-by-design paradigm is being developed gradually through synergistic integration of experimental material synthesis and characterization with predictive computational modeling and optimization. This paper reviews how this paradigm creates the possibility to develop materials according to specific, rational designs from the molecular to the macroscopic scale. We discuss promising techniques in experimental small-scale material synthesis and large-scale fabrication methods to manipulate atomistic or macroscale structures, which can be designed by computational modeling. These include recombinant protein technology to produce peptides and proteins with tailored sequences encoded by recombinant DNA, self-assembly processes induced by conformational transition of proteins, additive manufacturing for designing complex structures, and qualitative and quantitative characterization of materials at different length scales. We describe important material characterization techniques using numerous methods of spectroscopy and microscopy. We detail numerous multi-scale computational modeling techniques that complements these experimental techniques: DFT at the atomistic scale; fully atomistic and coarse-grain molecular dynamics at the molecular to mesoscale; continuum modeling at the macroscale. Additionally, we present case studies that utilize experimental and computational approaches in an integrated manner to broaden our understanding of the properties of two-dimensional materials and materials based on silk and silk-elastin-like proteins.

  6. Synthesis, spectroscopic characterization and structural investigations of a new charge transfer complex of 2,6-diaminopyridine with 3,5-dinitrobenzoic acid: DNA binding and antimicrobial studies

    Science.gov (United States)

    Khan, Ishaat M.; Ahmad, Afaq; Kumar, Sarvendra

    2013-03-01

    A new charge transfer (CT) complex [(DAPH)+(DNB)-] consisting of 2,6-diaminopyridine (DAP) as donor and 3,5-dinitrobenzoic acid (DNB-H) as acceptor, was synthesized and characterized by FTIR, 1H and 13C NMR, ESI mass spectroscopic and X-ray crystallographic techniques. The hydrogen bonding (N+-H⋯O-) plays an important role to consolidate the cation and anion together. CT complex shows a considerable interaction with Calf thymus DNA. The CT complex was also tested for its antibacterial activity against two Gram-positive bacteria Staphylococcus aureus and Bacillus subtilis and two Gram-negative bacteria Escherichia coli and Pseudomonas aeruginosa strains by using Tetracycline as standard, and antifungal property against Aspergillus niger, Candida albicans, and Penicillium sp. by using Nystatin as standard. The results were compared with standard drugs and significant conclusions were obtained. A polymeric net work through H-bonding interactions between neighboring moieties was observed. This has been attributed to the formation of 1:1 type CT complex.

  7. Synthesis and characterization of composites of mixed oxides of iron ...

    Indian Academy of Sciences (India)

    Home; Journals; Bulletin of Materials Science; Volume 34; Issue 4. Synthesis and characterization of composites of mixed oxides of iron and neodymium in polymer matrix of aniline–formaldehyde. Sajdha H N Sheikh B L Kalsotra N Kumar S Kumar. Volume 34 Issue 4 July 2011 pp 843-851 ...

  8. Synthesis and characterization of gold graphene composite with dyes as model substrates for decolorization: A surfactant free laser ablation approach

    Science.gov (United States)

    Sai Siddhardha, R. S.; Lakshman Kumar, V.; Kaniyoor, Adarsh; Sai Muthukumar, V.; Ramaprabhu, S.; Podila, Ramakrishna; Rao, A. M.; Ramamurthy, Sai Sathish

    2014-12-01

    A facile surfactant free laser ablation mediated synthesis (LAMS) of gold-graphene composite is reported here. The material was characterized using transmission electron microscopy, field emission scanning electron microscopy, energy dispersive X-ray spectroscopy, powdered X-ray diffraction, Raman spectroscopy, Zeta potential measurements and UV-Visible spectroscopic techniques. The as-synthesized gold-graphene composite was effectively utilized as catalyst for decolorization of 4 important textile and laser dyes. The integration of gold nanoparticles (AuNPs) with high surface area graphene has enhanced the catalytic activity of AuNPs. This enhanced activity is attributed to the synergistic interplay of pristine gold's electronic relay and π-π stacking of graphene with the dyes. This is evident when the Rhodamine B (RB) reduction rate of the composite is nearly twice faster than that of commercial citrate capped AuNPs of similar size. In case of Methylene blue (MB) the rate of reduction is 17,000 times faster than uncatalyzed reaction. This synthetic method opens door to laser ablation based fabrication of metal catalysts on graphene for improved performance without the aid of linkers and surfactants.

  9. 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.

  10. Adsorption and spectroscopic characterization of lactoferrin on hydroxyapatite nanocrystals.

    Science.gov (United States)

    Iafisco, Michele; Di Foggia, Michele; Bonora, Sergio; Prat, Maria; Roveri, Norberto

    2011-01-28

    Lactoferrin (LF), a well-characterized protein of blood plasma and milk with antioxidant, cariostatic, anticarcinogenic and anti-inflammatory properties, has been adsorbed onto biomimetic hydroxyapatite (HA) nanocrystals at two different pH values (7.4 and 9.0). The interaction was herein investigated by spectroscopic, thermal and microscopic techniques. The positive electrostatic surface potential of LF at pH 7.4 allows a strong surface interaction with the slightly negative HA nanocrystals and avoids the protein-protein interaction, leading to the formation of a coating protein monolayer. In contrast, at pH 9.0 the surface potential of LF is a mix of negative and positive zones favouring the protein-protein interaction and reducing the interaction with HA nanocrystals; as a result a double layer of coating protein was formed. These experimental findings are supported by the good fittings of the adsorption isotherms by different theoretical models according to Langmuir, Freundlich and Langmuir-Freundlich models. The nanosized HA does not appreciably affect the conformation of the adsorbed protein. In fact, using FT-Raman and FT-IR, we found that after adsorption the protein was only slightly unfolded with a small fraction of the α-helix structure being converted into turn, while the β-sheet content remained almost unchanged. The bioactive surface of HA functionalized with LF could be utilized to improve the material performance towards the biological environment for biomedical applications.

  11. Synthesis, crystal structure, spectroscopic characterization, Hirshfeld surface analysis, and DFT calculations of 1,4-dimethyl-2-oxo-pyrimido[1,2-a]benzimidazole hydrate

    Science.gov (United States)

    El Bakri, Youness; Anouar, El Hassane; Ramli, Youssef; Essassi, El Mokhtar; Mague, Joel T.

    2018-01-01

    Imidazopyrimidine derivatives are organic synthesized compounds with a pyrimido[1,2-a]benzimidazole as basic skeleton. They are known for their various biological properties and as an important class of compounds in medicinal chemistry. A new 1,4-dimethyl-2-oxo-pyrimido[1,2-a]benzimidazole hydrate derivative of the tilted group has been synthesized and characterized by spectroscopic techniques NMR and FT-IR; and by a single crystal X-ray diffraction. The X-ray results showed that the tricyclic core of the title compound, C12H11N3O·H2O, is almost planar. The molecules stack along the a-axis direction in head-to- tail fashion through π-stacking interactions involving all three rings. The stacks are tied together by direct Csbnd H⋯O hydrogen bonds and by Osbnd H⋯O, Osbnd N⋯N and Csbnd H⋯O hydrogen bonds with the lattice water. DFT calculations at B3LYP/6-311++G(d,p) in gas phase an polarizable continuum model have been carried out to predict the spectral and geometrical data of the tilted compound. The obtained results showed relatively good correlations between the predicted and experimental data with correlation coefficients higher than 98%.

  12. Synthesis and structural characterization of luminescent inorganic materials of the type CS2NaErBr6 and CS2NaHoBr6

    International Nuclear Information System (INIS)

    Poblete, V.H.; Fack, G.

    2001-01-01

    The synthesis and structural characterization is described of two luminescent materials, with technological [1] and spectroscopic [2] interest, whose crystallographic charts have not been published in the literature. The synthesis of both systems: Cs 2 NaErBr 6 and CS 2 NaHoBr 6 , was done using solid state reactions in a controlled environment. The thermal analyses DTA/TGA, applied with a temperature gradient of 10 o C/min., established crystallization ranges of 490,4 o C to 545,4 o C, for the elpasolite CS 2 NaHoBr 6 and 501 o C to 556 o C, for the structure CS 2 NaErBr 6 .. The heat vacuum treatments were carried out at 505 o C and 526 o C respectively, obtaining optimum crystallization. The structural characterization was performed with powdered X-ray diffraction (XRD). The range between 12 o and 80 o (2θ), was analyzed for 3352 points, measured steps of 0.02 o (2θ using the Rietveld profile refining program. The following crystallographic parameters were established: a 0 = 11,279(1), and 11,293(4) Angstroms, for the two structures analyzed, respectively. The relationship R exp wp in both cases is highly accurate for the 32 test lines that were analyzed. The structures present cubic closed packing Cs 1+ 3 Cl 1- , with Ho 3+ and Er 3+ atoms, filling the octahedral holes. The test data obtained will be very useful for completing the mass of experimental data needed to develop the design engineering, with specific applications for luminescent devices

  13. 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.

  14. 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.

  15. Synthesis and Characterization of Poly(Amidoamine Dendrimers Encapsulatd 198Au Nanoparticles

    Directory of Open Access Journals (Sweden)

    R. Ritawidya1,2

    2012-12-01

    Full Text Available Brachytherapy or internal radiotherapy is one of many methods used for treatment of cancer. This modality requires an agent with radionuclides that emits  or β particle with a proper energy. 198Au (99% β max = 0.96 MeV and t1/2 = 2.69 days is one of radionuclides that has been considered to be effective for the above-mentioned purpose. The purpose of this research was to synthesis and characterize poly(amidoamine (PAMAM G3.0 dendrimers encapsulated 198Au nanoparticles as a new brachytherapy agent. PAMAM G3.0 dendrimers encapsulated 198Au nanoparticles was successfully synthesized by a bottom-up method using sodium borohydride as a reductor. Purification was then performed by a size exclusion chromatography in order to separate large Au nanoparticles that were formed outside the cavity of PAMAM G3.0 dendrimers. Prior to the synthesis of PAMAM G3.0 dendrimers encapsulated 198Au nanoparticles, the synthetic procedure was first established by using a non-radioactive Au. The PAMAM G3.0 dendrimers encapsulated Au nanoparticles produced was then characterized by using an UV-Vis spectroscopy, a transmission electron microscopy (TEM, particle size analyzer (PSA, and an atomic absorption spectroscopy (AAS. Characterization results revealed that PAMAM G3.0 dendrimers encapsulated Au nanoparticles that were prepared from a reaction mixture of PAMAM G3.0 dendrimers and Au HAuCl4 with mol ratio of 2.8, was found to be a proper formula. It produced PAMAM G3.0 dendrimers encapsulated Au nanoparticles with diameter of 1.743 nm, spheris, uniform and drug loading value of 26.34%. This formula was then used in synthesis using radioactive Au, 198Au. Characterization results of PAMAM G3.0 dendrimers encapsulated 198Au nanoparticles gave a radiochemical purity of 99.4% and zero charge.

  16. Synthesis and characterization of dental composites

    Science.gov (United States)

    Djustiana, Nina; Greviana, Nadia; Faza, Yanwar; Sunarso

    2018-02-01

    During the last few decades, the increasing demands in esthetic dentistry have led to the development of dental composites material that provide similar appearance to the natural teeth. Recently, esthetic trend was an issue which increase the demand for teeth restorations that is similar with the origin. The esthetics of dental composite are more superior compared to amalgam, since its color look similar with natural teeth. Various dental composites have been developed using many type of fillers such as amorphous silica, quartz), borosilicate, Li-Sr-Ba-Al glass and oxide: zirconia and alumina. Researchers in Faculty of Dentistry University of Padjadjaran have prepared dental composites using zirconia-alumina-silica (ZAS) system as the filler. The aim is to improve the mechanical properties and the esthetic of the dental composites. The ZAS was obtained from chemical grade purity chemicals and Indonesia's natural sand as precursors its characterization were also presented. This novel method covers the procedure to synthesis and characterize dental composites in Padjadjaran University and some review about dental composites in global research.

  17. Dual emitter IrQ(ppy)2 for OLED applications: Synthesis and spectroscopic analysis

    International Nuclear Information System (INIS)

    Ciobotaru, I.C.; Polosan, S.; Ciobotaru, C.C.

    2014-01-01

    The synthesis of organometallic compound with iridium and two types of ligands, quinoline and phenylpyridine, was done successfully. The absorption spectra of this compound have shown broad peaks in a visible region assigned to metal-to-ligands charge transfer and in UV region assigned to intraligand absorptions. The photoluminescence spectra exhibit dual character in which the red emission is more intense than the green one. In cathodoluminescence measurements, under electron beam, the powder obtained after recrystallization from dichloromethane, shows similar behaviors with photoluminescence spectra. The cathodoluminescence images have shown a luminescent crystalline powder with triclinic structure. This compound exhibits combined vibrational modes, which proves the presence in the same molecule of both ligands. Density Functional Theory calculation was involved in order to identify the main vibrations of this compound. Highlights: • Mixed-ligand of IrQ(ppy) 2 synthesis which gives green and red phosphorescence due to the MCLT processes coming from two types of ligands. • Absorption, photoluminescence, infrared spectroscopy and cathodoluminescence measurements for characterization of IrQ(ppy) 2 organometallic compound. • Experimental results have been compared with the output files obtained from Density Functional Theory by using the Gaussian 03W software

  18. 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, ...

  19. Vibrational and chiroptical spectroscopic characterization of gamma-turn model cyclic tetrapeptides containing two beta-Ala residues.

    Science.gov (United States)

    Vass, Elemér; Majer, Zsuzsa; Kohalmy, Krisztina; Hollósi, Miklós

    2010-08-01

    The optical spectroscopic characterization of gamma-turns in solution is uncertain and their distinction from beta-turns is often difficult. This work reports systematic ECD and vibrational circular dichroism (VCD) spectroscopic studies on gamma-turn model cyclic tetrapeptides cyclo(Ala-beta-Ala-Pro-beta-Ala) (1), cyclo(Pro-beta-Ala-Pro-beta-Ala) (2) and cyclo(Ala-beta-Ala-Ala-beta-Ala) (3). Conformational analysis performed at the 6-31G(d)/B3LYP level of theory using an adequate PCM solvent model predicted one predominant conformer for 1-3, featuring two inverse gamma-turns. The ECD spectra in ACN of 1 and 2 are characterized by a negative n-->pi* band near 230 nm and a positive pi-->pi* band below 200 nm with a long wavelength shoulder. The ECD spectra in TFE of 1-3 show similar spectra with blue-shifted bands. The VCD spectra in ACN-d(3) of 1 and 2 show a +/-/+/- amide I sign pattern resulting from four uncoupled vibrations in the case of 1 and a sequence of two positive couplets in the case of 2. A -/+/+/- amide I VCD pattern was measured for 3 in TFE-d(2). All three peptides give a positive couplet or couplet-like feature (+/-) in the amide II region. VCD spectroscopy, in agreement with theoretical calculations revealed that low frequency amide I vibrations (at approximately 1630 cm(-1) or below) are indicative of a C(7) H-bonded inverse gamma-turns with Pro in position 2, while gamma-turns encompassing Ala absorb at higher frequency (above 1645 cm(-1)). Copyright 2010 Wiley-Liss, Inc.

  20. 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...

  1. Nano-/micro metallic wire synthesis on Si substrate and their characterization

    International Nuclear Information System (INIS)

    Kaur, Jaskiran; Kaur, Harmanmeet; Singh, Surinder; Kanjilal, Dinakar; Chakarvarti, Shiv Kumar

    2014-01-01

    Nano-/micro wires of copper are grown on semiconducting Si substrate using the template method. It involves the irradiation of 8 um thick polymeric layer coated on Si with150 MeV Ni ion beam at a fluence of 2E8. Later, by using the simple technique of electrodeposition, copper nano-/micro wires were grown via template synthesis. Synthesized wires were morphologically characterized using SEM and electrical characterization was carried out by finding I-V plot

  2. Identification and Spectroscopic Characterization of Nonheme Iron(III) Hypochlorite Intermediates

    NARCIS (Netherlands)

    Draksharapu, Apparao; Angelone, Davide; Quesne, Matthew G.; Padamati, Sandeep K.; Gomez, Laura; Hage, Ronald; Costas, Miquel; Browne, Wesley R.; de Visser, Sam P.

    2015-01-01

    Fe-III-hypohalite complexes have been implicated in a wide range of important enzyme-catalyzed halogenation reactions including the biosynthesis of natural products and antibiotics and post-translational modification of proteins. The absence of spectroscopic data on such species precludes their

  3. Electrochemical and spectroscopic studies of tungstencarbonyl complexes containing nitrogen and phosphorous ligands

    Directory of Open Access Journals (Sweden)

    Haddad Paula S.

    2000-01-01

    Full Text Available The present work deals with the synthesis, spectroscopic investigation and electrochemical behaviour of the compounds [W(CO4(bipy] (1, [W(CO3(bipy(dppm] (2 and [W(CO3(bipy(dppf] (3, bipy = 2,2'-bipyridine; dppm = bis(diphenylphosphinomethane; dppf = 1,1'-bis(diphenylphosphinoferrocene. The IR and 31P{¹H} NMR spectroscopic data have shown an octahedral coordination geometry for the tungsten atom with the diphosphines acting as monodentate ligands. The electrochemical behaviour of the complexes was investigated by cyclic voltammetry and controlled potential coulometry. Cyclic voltammograms have indicated that the compounds containing diphosphines ligands are more stable towards oxidation than compound (1.

  4. Spectroscopic characterization of extrasolar planets from ground-, space- and airborne-based observatories

    Science.gov (United States)

    Angerhausen, Daniel

    2010-11-01

    This thesis deals with techniques and results of observations of exoplanets from several platforms. In this work I present and then attempt solutions to particular issues and problems connected to ground- and space-based approaches to spectroscopic characterization of extrasolar planets. Furthermore, I present the future prospects of the airborne observatory, SOFIA, in this field of astronomy. The first part of this thesis covers results of an exploratory study to use near-infrared integral-field-spectroscopy to observe transiting extrasolar planets. I demonstrate how adaptive-optics assisted integral field spectroscopy compares with other spectroscopic techniques currently applied, foremost being slit spectroscopy. An advanced reduction method using elements of a spectral-differential decorrelation and optimized observation strategies is discussed. This concept was tested with K-Band time series observations of secondary eclipses of HD 209458b and HD 189733b obtained with the SINFONI at the Very Large Telescope (VLT), at spectral resolution of R~3000. In ground-based near infrared (NIR) observations, there is considerable likelihood of confusion between telluric absorption features and spectral features in the targeted object. I describe a detailed method that can cope with such confusion by a forward modelling approach employing Earth transmission models. In space-based transit spectroscopy with Hubble's NICMOS instrument, the main source of systematic noise is the perturbation in the instrument's configuration due to the near Earth orbital motion of the spacecraft. I present an extension to a pre-existing data analysis sequence that has allowed me to extract a NIR transmission spectrum of the hot-Neptune class planet GJ 436b from a data set that was highly corrupted by the above mentioned effects. Satisfyingly, I was able to obtain statistical consistency in spectra (acquired over a broad wavelength grid) over two distinct observing visits by HST. Earlier

  5. Synthesis and characterization of poly aniline for electrochemical biosensor construction

    International Nuclear Information System (INIS)

    Magalhaes, Gleice S.L.; Southgate, Erica F.; Alhadeff, Eliana M.; Guimaraes, Maria Jose O.C.

    2011-01-01

    Conductors polymers have many attractive interests to the industry due their highly technological applications. This work treats specially of polyaniline because it's large electrical conductivity, electrochemical properties, associate to the chemical stability in environmental conditions and synthesis facility. The main of this work is the application in a construction of an electrochemical biosensor for ethanol detection and quantification. Different conditions of synthesis of the conductor emeraldine polyaniline form were studied, investigated the influence of the dopant agent and the reactional environment conditions temperature on the reaction yield and conductivities. The polyaniline that showed the best conductivity were characterized by differential and thermal gravimetric analysis, infrared spectroscopy, X ray diffraction, and cycle voltammetry, comparing with the commercial polyaniline. (author)

  6. Synthesis and characterization of Au incorporated Alq3 nanowires

    Science.gov (United States)

    Khan, Mohammad Bilal; Ahmad, Sultan; Parwaz, M.; Rahul, Khan, Zishan H.

    2018-05-01

    We report the synthesis and characterization of pure and Au incorporated Alq3 nanowires. These nanowires are synthesized using thermal vapor transport method. The luminescence intensity of Au incorporated Alq3 nanowires are recorded to be higher than that of pure Alq3 nanowires, which is found to increase with the increase in Au concentration. Fluorescence quenching is also observed when Au concentration is increased beyond the certain limit.

  7. Synthesis and Characterization of Highly Intercalated Graphite Bisulfate

    Science.gov (United States)

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

    2017-03-01

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

  8. Mid-infrared spectroscopic investigation

    International Nuclear Information System (INIS)

    Walter, L.; Vergo, N.; Salisbury, J.W.

    1987-01-01

    Mid-infrared spectroscopic research efforts are discussed. The development of a new instrumentation to permit advanced measurements in the mid-infrared region of the spectrum, the development of a special library of well-characterized mineral and rock specimens for interpretation of remote sensing data, and cooperative measurements of the spectral signatures of analogues of materials that may be present on the surfaces of asteroids, planets or their Moons are discussed

  9. 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.

  10. Green synthesis and characterization of graphene nanosheets

    International Nuclear Information System (INIS)

    Tavakoli, Farnosh; Salavati-Niasari, Masoud; Badiei, Alireza; Mohandes, Fatemeh

    2015-01-01

    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

  11. Synthesis and Characterization of Some Alkaline-Earth-Oxide Nanoparticles

    Science.gov (United States)

    Singh, Jitendra Pal; Lim, Weon Cheol; Won, Sung Ok; Song, Jonghan; Chae, Keun Hwa

    2018-04-01

    The present work reports the synthesis of MgO and CaO nanoparticles by using the sol-gel autocombustion method. The annealing of the precursor at 1200 °C was observed to lead the formation of MgO nanoparticles having average crystallite size of 31 nm. Annealing the precursor at same temperature produced materials having a CaO phase with a minor impure phase of calcium carbonate ( 3%). The crystallite size corresponding to the CaO phase was 38 nm. A change of thermal history in the precursor was observed not to result in an improvement of the CaO phase. The change of thermal history in the precursor gave rise to mixed phases of CaCO3 and Ca(OH)2 rather than the phase of CaO. Further, annealing at 1200 °C for 12 h resulted in the formation of the CaO phase along with almost 1 - 5% of calcium hydroxide as an impurity phase. X-ray absorption spectroscopic measurements carried out on these materials revealed that the local electronic/atomic structure of these oxides was not only affected by the impurity phases but also influenced by the carbaneous impurities attached to the crystallites.

  12. Magnetic Resonance Spectroscopic Imaging of Tumor Metabolic Markers for Cancer Diagnosis, Metabolic Phenotyping, and Characterization of Tumor Microenvironment

    Directory of Open Access Journals (Sweden)

    Qiuhong He

    2004-01-01

    Full Text Available Cancer cells display heterogeneous genetic characteristics, depending on the tumor dynamic microenvironment. Abnormal tumor vasculature and poor tissue oxygenation generate a fraction of hypoxic tumor cells that have selective advantages in metastasis and invasion and often resist chemo- and radiation therapies. The genetic alterations acquired by tumors modify their biochemical pathways, which results in abnormal tumor metabolism. An elevation in glycolysis known as the “Warburg effect” and changes in lipid synthesis and oxidation occur. Magnetic resonance spectroscopy (MRS has been used to study tumor metabolism in preclinical animal models and in clinical research on human breast, brain, and prostate cancers. This technique can identify specific genetic and metabolic changes that occur in malignant tumors. Therefore, the metabolic markers, detectable by MRS, not only provide information on biochemical changes but also define different metabolic tumor phenotypes. When combined with the contrast-enhanced Magnetic Resonance Imaging (MRI, which has a high sensitivity for cancer diagnosis, in vivo magnetic resonance spectroscopic imaging (MRSI improves the diagnostic specificity of malignant human cancers and is becoming an important clinical tool for cancer management and care. This article reviews the MRSI techniques as molecular imaging methods to detect and quantify metabolic changes in various tumor tissue types, especially in extracranial tumor tissues that contain high concentrations of fat. MRI/MRSI methods have been used to characterize tumor microenvironments in terms of blood volume and vessel permeability. Measurements of tissue oxygenation and glycolytic rates by MRS also are described to illustrate the capability of the MR technology in probing molecular information non-invasively in tumor tissues and its important potential for studying molecular mechanisms of human cancers in physiological conditions.

  13. Synthesis, Spectroscopic Characterization, and Biological Activities of Metal Complexes of 4-((4-Chlorophenyldiazenyl-2-((p-tolyliminomethylphenol

    Directory of Open Access Journals (Sweden)

    C. Anitha

    2013-01-01

    Full Text Available Azo Schiff base complexes of VO(II, Mn(II, Co(II, Ni(II, Cu(II, and Zn(II have been synthesized from 4-((4-chlorophenyldiazenyl-2-((p-tolyliminomethylphenol (CDTMP. The nature of bonding and the structural features of the complexes have been deduced from elemental analysis, molar conductance, magnetic susceptibility measurements, IR, UV-Vis, 1H-NMR, EPR, mass, SEM, and fluorescence spectral studies. Spectroscopic and other analytical studies reveal square-planar geometry for copper, square-pyramidal geometry for oxovanadium, and octahedral geometry for other complexes. The EPR spectra of copper(II complex in DMSO at 300 K and 77 K were recorded, and its salient features are reported. Antimicrobial studies against several microorganisms indicate that the complexes are more potent bactericides and fungicides than the ligand. The electrochemical behavior of the copper(II complex was studied by cyclic voltammetry. All the synthesized compounds can serve as potential photoactive materials as indicated from their characteristic fluorescence properties. The second harmonic conversion efficiency of the synthesized azo Schiff base was found to be higher than that of urea and KDP (potassium dihydrogen phosphate. SEM image of copper(II complex implies the crystalline state and surface morphology of the complex.

  14. New aminoporphyrins bearing urea derivative substituents: synthesis, characterization, antibacterial and antifungal activity

    Directory of Open Access Journals (Sweden)

    Gholamreza Karimipour

    2015-06-01

    Full Text Available This work studied the synthesis of 5,10,15-tris(4-aminophenyl-20-(N,N-dialkyl/diaryl-N-phenylurea porphyrins (P1-P4 with alkyl or aryl groups of Ph, iPr, Et and Me, respectively and also the preparation of their manganese (III and cobalt (II complexes (MnP and CoP. The P1-P4 ligands were characterized by different spectroscopic techniques (1H NMR, FTIR, UV-Vis and elemental analysis, and metalated with Mn and Co acetate salts. The antibacterial and antifungal activities of these compounds in vitro were investigated by agar-disc diffusion method against Escherichia coli (-, Pseudomonas aeruginosa (-, Staphylococcus aureus(+, Bacillus subtilis (+ and Aspergillus oryzae and Candida albicans. Results showed that antibacterial and antifungal activity of the test samples increased with increase of their concentrations and the highest activity was obtained when the concentration of porphyrin compounds was 100 µg/mL. The activity for the porphyrin ligands depended on the nature of the urea derivative substituents and increased in the order P1 > P2 > P3 >P4, which was consistent with the order of their liposolubility. MnP and CoP complexes exhibited much higher antibacterial and antifungal activity than P1-P4ligands. Further, the growth inhibitory effects of these compounds was generally in the order CoP complexes > MnP complexes > P1-P4 ligands. Among these porphyrin compounds, CoP1displayed the highest antibacterial and antifungal activity, especially with a concentration of 100 µg/mL, against all the four tested bacteria and two fungi, and therefore it could be potential to be used as drug.

  15. Photocatalytic Properties of Nb/MCM-41 Molecular Sieves: Effect of the Synthesis Conditions

    Directory of Open Access Journals (Sweden)

    Caterine Daza Gomez

    2015-08-01

    Full Text Available The effect of synthesis conditions and niobium incorporation levels on the photocatalytic properties of Nb/MCM-41 molecular sieves was assessed. Niobium pentoxide supported on MCM-41 mesoporous silica was obtained using two methods: sol-gel and incipient impregnation, in each case also varying the percentage of niobium incorporation. The synthesized Nb-MCM-41 ceramic powders were characterized using the spectroscopic techniques of infrared spectroscopy (IR, Raman spectroscopy, X-ray diffraction (XRD, and transmission electron microscopy (TEM. The photodegradation capacity of the powders was studied using the organic molecule, methylene blue. The effect of both the method of synthesis and the percentage of niobium present in the sample on the photodegradation action of the solids was determined. The mesoporous Nb-MCM-41 that produced the greatest photodegradation response was obtained using the sol-gel method and 20% niobium incorporation.

  16. synthesis, antimicrobial and phytotoxic activity of amide derivatives of L-(+)-2,3-diacetoxy-4-methoxy-4-oxo-butanoic acid

    International Nuclear Information System (INIS)

    Malik, M.; Khan, S.W.; Zaidi, J.H.; Khan, K.M.; Hussain, S.

    2014-01-01

    A short, versatile, an efficient asymmetric synthesis of substituted aromatic amides is described. L-Tartaric acid conveniently converted into diacetyl-L-tartaric anhydride. Diacetyl-L-tartaric anhydride was then transformed into half ester which was then reacted with substituted anilines to yield respective chiral amides 3-8. These chiral amides were characterized by spectroscopic techniques i.e. 1H-NMR, 13C-NMR, IR and mass spectrometry. Amides 3-8 were tested for their antimicrobial as well as phytotoxic activities. (author)

  17. Synthesis and spectroscopic characterization of palladium-doped ...

    Indian Academy of Sciences (India)

    Pd-doped TiO2 nanoparticles; gelatin; hydrogen evolution reaction. 1. Introduction ... sol–gel methods16 have been used for production of TiO2 thin films. Besides the ... ports reduced the cost of anode materials in the industrial applications.

  18. Synthesis, crystal structures, spectroscopic characterization and in ...

    Indian Academy of Sciences (India)

    cDepartment of Biotechnology, School of Bio-Sciences and Technology, VIT University, Vellore,. Tamil Nadu .... M. The lower molar conductivity values of 3 and 3.5. −1 cm2mol. −1 ..... the tolerance of pancreatic β-cells against oxida- tive stress ...

  19. Synthesis, spectroscopic characterization and biological activities of ...

    African Journals Online (AJOL)

    The elemental and spectral analysis show that ligand coordinate to the central lanthanide(III)ion by its imine nitrogen, phenolic oxygen and carboxylic oxygen in 1:1 stoichemetry. The complexes were found to be electrolytic in nature on basis of ...

  20. Spectroscopic characterization of the ethyl radical-water complex.

    Science.gov (United States)

    Lin, Chen; Finney, Brian A; Laufer, Allan H; Anglada, Josep M; Francisco, Joseph S

    2016-10-14

    An ab initio investigation has been employed to determine the structural and spectroscopic parameters, such as rotational constants, vibrational frequencies, vertical excitation energies, and the stability of the ethyl-water complex. The ethyl-water complex has a binding energy of 1.15 kcal⋅mol -1 . The interaction takes place between the hydrogen of water and the unpaired electron of the radical. This interaction is found to produce a red shift in the OH stretching bands of water of ca. 84 cm -1 , and a shift of all UV absorption bands to higher energies.

  1. Boron-based nanostructures: Synthesis, functionalization, and characterization

    Science.gov (United States)

    Bedasso, Eyrusalam Kifyalew

    Boron-based nanostructures have not been explored in detail; however, these structures have the potential to revolutionize many fields including electronics and biomedicine. The research discussed in this dissertation focuses on synthesis, functionalization, and characterization of boron-based zero-dimensional nanostructures (core/shell and nanoparticles) and one-dimensional nanostructures (nanorods). The first project investigates the synthesis and functionalization of boron-based core/shell nanoparticles. Two boron-containing core/shell nanoparticles, namely boron/iron oxide and boron/silica, were synthesized. Initially, boron nanoparticles with a diameter between 10-100 nm were prepared by decomposition of nido-decaborane (B10H14) followed by formation of a core/shell structure. The core/shell structures were prepared using the appropriate precursor, iron source and silica source, for the shell in the presence of boron nanoparticles. The formation of core/shell nanostructures was confirmed using high resolution TEM. Then, the core/shell nanoparticles underwent a surface modification. Boron/iron oxide core/shell nanoparticles were functionalized with oleic acid, citric acid, amine-terminated polyethylene glycol, folic acid, and dopamine, and boron/silica core/shell nanoparticles were modified with 3-(amino propyl) triethoxy silane, 3-(2-aminoethyleamino)propyltrimethoxysilane), citric acid, folic acid, amine-terminated polyethylene glycol, and O-(2-Carboxyethyl)polyethylene glycol. A UV-Vis and ATR-FTIR analysis established the success of surface modification. The cytotoxicity of water-soluble core/shell nanoparticles was studied in triple negative breast cancer cell line MDA-MB-231 and the result showed the compounds are not toxic. The second project highlights optimization of reaction conditions for the synthesis of boron nanorods. This synthesis, done via reduction of boron oxide with molten lithium, was studied to produce boron nanorods without any

  2. Synthesis and characterization of KY3F10 and KY3F10:Yb:Nd:Tm crystals for optical applications

    International Nuclear Information System (INIS)

    Linhares, Horacio Marconi da Silva Dantas

    2009-01-01

    In this work, crystals of KY 3 F 10 pure and doped with Yb, Nd and Tm were grown aiming at the attainment of blue emission via Tm 3+ ions up conversion. It was established the best conditions to synthesis and purification of KY 3 F 10 . Crystals doped with 1.3 mol% Nd, 0.5 mol% Tm and some concentrations of Yb (5, 10, 20, 30 and 40 mol%) were obtained by slow cooling of the charge from the melt, using an usual conventional synthesis system and in a reactive HF atmosphere. It was taken into account parameters as cooling rate and different configurations of boats to conditioning the materials. The limit of Yb concentration to obtain a unique cubic phase was determined as 30mol%, for the cooling rates used in this work. The physical and chemical characterizations of the samples were performed by X-ray diffraction, differential thermal analysis, inductively coupled plasma-optical emission spectroscopy (ICP-OES), scanning electron microscopy, optical absorption and emission. An initial spectroscopic study was performed to verify the effect of the Yb 3+ concentration regarding the blue emission efficiency in the KY 3 F 10 :Yb:Nd:Tm. When the Nd 3+ is pumped at 797 nm, it was determined that the suitable Yb concentrations are between 10 and 20 mol% to obtain blue emission at 480 nm, and between 20 and 30 mol% to obtain emission at 450 nm. It was observed that two emissions bands in the UV (350 and 360nm) enhanced proportionally with the Yb 3+ concentration. (author)

  3. Synthesis, purification and characterization of [3,5 - T] p-aminobenzoic acid

    International Nuclear Information System (INIS)

    Corol-Cucu, Delia-Irina; Chiper, Diana; Mihaila, V.; Negoita, N.

    2000-01-01

    This paper refers to the synthesis, purification and characterization of [3,5-T] p-aminobenzoic acid (PAB,H' vitamine). The p-aminobenzoic acid is used in the treatment of rheumatic arthritis and dermatological affections. The advantage of tritium labelling of p-aminobenzoic acid is that some biomedical important aspects of collagen's behaviour are made clear. The PAB stimulate the grow of intestinal bacteria so necessary to synthesis of some vitamins (bio tine, pantothenic acid). Tritium is the only radioactive isotope of hydrogen. Several steps have to be carried out in the synthesis of the final product as well as to study its biological behavior. For the labelling of PAB one prefers the substitution of bromine from PAB-3,5-Br with tritium because of simplicity of reaction and the easy synthesis of halogen compound. The first step in synthesis is the protection of NH 2 group through acetylation of PAB. After that PAB is bromated into the 3 and 5 position with elementary bromine. The raw compound is purified and recrystallized and characterized through thin layer chromatography.The tritium labelling is performed through substitution of bromine from bromate derivative, using Pd/C (10% Pd) as catalyst and low basic conditions for the neutralization of HBr resulting from reaction. After the separation of PAB-3,5-T through filtration, the catalyst remains on the filter paper and the labelled compound goes in aqueous solution. PAB-3,5-T is purified through thin layer chromatography with the solvent system n-BuOH:NH 4 OH(25%):H 2 O:EtOH (8:1:2:2,5, v/v) with silica gel GF 254 as support. The determination of activity is carried out with LSC (Liquid Scintillation Counter). A 98% purity was determined through TLC in the same conditions while determination of activity distribution was performed with a 2π Berthold scanner with gas running and without window. The chemical concentration has been measured through UV spectrophotometry and by comparing extinction with

  4. Sol – Gel synthesis and characterization of magnesium peroxide nanoparticles

    International Nuclear Information System (INIS)

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

    2015-01-01

    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 (MgO 2 ) 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 MgO 2 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. (paper)

  5. Synthesis and Characterization of Block Copolymers with Unique Chemical Functionalities and Entropically-Hindering Moieties

    Science.gov (United States)

    2017-08-14

    methanol as a function of chemistry , morphology and hydration levels. Accomplishments: This section is included in the "upload" section. Training...Copolymer Blend Membranes.” In Press, Polymer Engineering and Science, DOI: 10.1002 /pen.24508, 2017. 5. M. Pérez-Pérez and D. Suleiman. “Synthesis and...Synthesis and Characterization of Sulfonated Amine Block Copolymers for Energy Efficient Applications". Chemical Engineering Symposium, University of

  6. Evolution of containment facilities for spectroscopic analysis at Rockwell Hanford Operations

    International Nuclear Information System (INIS)

    Hiller, J.M.

    1984-01-01

    The analysis of radioactive material requires much thought concerning getting the job done while still maintaining a safe working environment. A Rockwell Hanford Operations, several stages of evolution in instrumentation for spectroscopic elemental analysis have evolved, reflecting different philosophies respect to shielding and contamination control. Atomic absorption and inductively coupled plasma emission spectroscopic systems have been used for analyzing samples in support of a fission product recovery plant, nuclear waste processing and characterization programs, and U and Pu separation plants. Design thoughts, criticisms, and lessons learned in 20 years of containment for spectroscopic analysis are presented

  7. Synthesis and characterization of tantalum organometallic complexes. Catalytic activity for olefins

    International Nuclear Information System (INIS)

    Baley, A.S.

    1990-11-01

    Synthesis of monoaryloxy (alcoxy) neopentyl compounds is investigated. The tantalum-oxygen bond is formed by two parallel ways from TaCl 5 or TaR 2 Cl 3 with R = neopentyl and the tantalum carbon bond from a neopentyl derivative of the main series. Some compounds were isolated and characterized by NMR, elemental analysis and sometimes X-ray structure, some others are characterized in solution only. Catalytic effect is tested by ethylene dimerization and olefin polymerization. Reactivity of tantalum aryloxy neopentyl in respect to complexing and chelating ligands is studied for preparation of neopentylidene complexes

  8. Organic luminescent materials. First results on synthesis and characterization of Alq{sub 3} thin films

    Energy Technology Data Exchange (ETDEWEB)

    Baldacchini, G.; Gagliardi, S.; Montereali, R.M.; Pace, A. [ENEA, Centro Ricerche Frascati, Frascati, RM (Italy). Div. Fisica Applicata; Balaji Pode, R. [Nagpur University, Nagpur (India). Dept. of Physics

    2000-07-01

    Inorganic semiconductor diodes brought a technological revolution in the field of efficient light and laser sources in the last 20 years. New development in this field are expected from organic compounds, thanks to their low cost of synthesis and the relative easiness of growth as thin films. In particular, electrically pumped luminescent devices based on organic thin layers are among the most promising systems for next generation flat panel displays and semiconductor lasers. The tris - (8-hydroxy quinoline)-aluminium complex-Alq{sub 3} - is one of the most studied electro luminescent materials. In this paper, after a short introduction regarding historical development in the field, are reported preliminary results on the growth of Alq{sub 3} films and on their optical and spectroscopic characterization. [Italian] Negli ultimi 20 anni i diodi semiconduttori hanno portato una rivoluzione tecnologica nel campo delle sorgenti luminose e laser. Un nuovo sviluppo possibile in questo campo sono i composti organici, grazie al basso costo di sintesi e la relativa facilita' di crescerli in forma di film sottile. In particolare, dispositivi luminescenti pompati elettricamente basati su film sottili di materiali organici sono promettenti per una nuova generazione di display per schermi piatti e laser a Alq{sub 3} e' uno dei materiali elettroluminescenti piu' studiati. In questo rapporto, dopo una breve introduzione sullo sviluppo storico in questo campo, presentiamo i nostri primi risultati sulla crescita e caratterizzazione ottica di film di Alq{sub 3}.

  9. The Synthesis and Characterization of Gold-Core/LDH-Shell Nanoparticles

    Science.gov (United States)

    Rearick, Colton

    In recent years, the field of nanomedicine has progressed at an astonishing rate, particularly with respect to applications in cancer treatment and molecular imaging. Although organic systems have been the frontrunners, inorganic systems have also begun to show promise, especially those based upon silica and magnetic nanoparticles (NPs). Many of these systems are being designed for simultaneous therapeutic and diagnostic capabilities, thus coining the term, theranostics. A unique class of inorganic systems that shows great promise as theranostics is that of layered double hydroxides (LDH). By synthesis of a core/shell structures, e.g. a gold nanoparticle (NP) core and LDH shell, the multifunctional theranostic may be developed without a drastic increase in the structural complexity. To demonstrate initial proof-of-concept of a potential (inorganic) theranostic platform, a Au-core/LDH-shell nanovector has been synthesized and characterized. The LDH shell was heterogeneously nucleated and grown on the surface of silica coated gold NPs via a coprecipitation method. Polyethylene glycol (PEG) was introduced in the initial synthesis steps to improve crystallinity and colloidal stability. Additionally, during synthesis, fluorescein isothiocyanate (FITC) was intercalated into the interlayer spacing of the LDH. In contrast to the PEG stabilization, a post synthesis citric acid treatment was used as a method to control the size and short-term stability. The heterogeneous core-shell system was characterized with scanning electron microscopy (SEM), energy dispersive x-ray spectroscopy (EDX), dynamic light scattering (DLS), and powder x-ray diffraction (PXRD). A preliminary in vitro study carried out with the assistance of Dr. Kaushal Rege's group at Arizona State University was to demonstrate the endocytosis capability of homogeneously-grown LDH NPs. The DLS measurements of the core-shell NPs indicated an average particle size of 212nm. The PXRD analysis showed that PEG

  10. Synthesis and characterization of mangan oxide coated sand from Capkala kaolin

    Science.gov (United States)

    Destiarti, Lia; Wahyuni, Nelly; Prawatya, Yopa Eka; Sasri, Risya

    2017-03-01

    Synthesis and characterization of mangan oxide coated sand from quartz sand fraction of Capkala kaolin has been conducted. There were two methods on synthesis of Mangan Oxide Coated Sand (MOCS) from Capkala Kaolin compared in this research. Characterization of MOCS was done by using Scanning Electron Microscope/Energy Dispersive X-Ray Spectrometer (SEM/EDX) and X-Ray Diffraction (XRD). The MOCS was tested to reduce phosphate in laundry waste. The result showed that the natural sand had bigger agregates and a relatively uniform structural orientation while both MOCS had heterogen structural orientation and manganese oxide formed in cluster. Manganese in first and second methods were 1,93% and 2,63%, respectively. The XRD spectrum showed clear reflections at 22,80°, 36,04°, 37,60° and a broad band at 26,62° (SiO2). Based on XRD spectrum, it can be concluded that mineral constituents of MOCS was verified corresponding to pyrolusite (MnO2). The former MOCS could reduce almost 60% while the later could reduce 70% phosphate in laundry waste.

  11. Synthesis and characterization of Tin / Titanium mixed oxide nanoparticles doped with lanthanide for biomarking; Sintese e caracterizacao de nanoparticulas de oxido misto de estanho/titanio dopadas com lantanideos para marcacao biologica

    Energy Technology Data Exchange (ETDEWEB)

    Paganini, Paula Pinheiro

    2012-07-01

    This work presents the synthesis, characterization and photo luminescent study of tin and titanium mixed oxide nanoparticles doped with europium, terbium and neodymium to be used with luminescent markers on biological systems. The syntheses were done by co-precipitation, protein sol-gel and Pechini methods and the nanoparticles were characterized by infrared spectroscopy, thermogravimetric analysis, scanning electron microscopy, X-ray diffraction and X-ray absorption spectroscopy. The photo luminescent properties studies were conducted for luminophores doped with europium, terbium and neodymium synthesized by coprecipitation method. For luminophore doped with europium it was possible to calculate the intensity parameters and quantum yield and it showed satisfactory results. In the case of biological system marking it was necessary the functionalization of these particles to allow them to bind to the biological part to be studied. So the nanoparticles were functionalized by microwave and Stoeber methods and characterized by infrared spectroscopy, scanning electron microscopy, energy dispersive X-ray spectroscopy and X-ray diffraction obtaining qualitative response of functionalization efficacy. The ninhydrin spectroscopic method was used for quantification of luminophores functionalization. The photo luminescent studies of functionalized particles demonstrate the potential applying of these luminophores as luminescent markers. (author)

  12. Simple preparation of new N-aryl-N-(3-indolmethyl acetamides and their spectroscopic analysis

    Directory of Open Access Journals (Sweden)

    José A. Henao

    2009-12-01

    Full Text Available To prepare new indolic molecules and characterize them by spectroscopic methods. Materials and methods: All reagentswere purchased from Aldrich, commercial grade. The purity of the products and the composition of the reaction mixtures were monitoredby thin layer chromatography over Silufol UV254 0.25 mm-thick chromatoplates. Product isolation and purification were performed bycolumn chromatography (SiO2, using ethyl acetate-petroleum ether mixtures as eluents. Results. The synthesis of new N-aryl-N-(3-indolmethyl acetamides based on first step iminization reaction of indol-3-carbaldehyde is accomplished. The structures of the C-3substituted indoles were confirmed by 1H-NMR and 13C-NMR studies supported by inverse-detected 2D NMR experiments and alsothrough monocrystal X-ray diffraction. Conclusions. An efficient, economic, and fast synthetic route was designed to the construction ofthe N-aryl-N-(3-indolmethyl acetamides, structural analogues of some alkaloids.

  13. Synthesis, characterization and bioimaging of fluorescent labeled polyoxometalates.

    Science.gov (United States)

    Geisberger, Georg; Gyenge, Emina Besic; Hinger, Doris; Bösiger, Peter; Maake, Caroline; Patzke, Greta R

    2013-07-21

    A fluorescent labeled Wells-Dawson type POM ({P2W17O61Fluo}) was newly synthesized and characterized by a wide range of analytical methods. {P2W17O61Fluo} was functionalized with fluorescein amine through a stable amide bond, and its long time stability was verified by UV/vis spectroscopic techniques at physiologically relevant pH values. No significant impact on the cell viability or morphology of HeLa cells was observed for POM concentrations up to 100 μg mL(-1). Cellular uptake of fluorescent {P2W17O61Fluo} was monitored by confocal laser scanning microscopy. POM uptake occurs mainly after prolonged incubation times of 24 h resulting in different intracellular patterns, i.e. randomly distributed over the entire cytoplasm, or aggregated in larger clusters. This direct monitoring strategy for the interaction of POMs with cells opens up new pathways for elucidating their unknown mode of action on the way to POM-based drug development.

  14. Synthesis and characterization of photoswitchable fluorescent silica nanoparticles.

    Science.gov (United States)

    Fölling, Jonas; Polyakova, Svetlana; Belov, Vladimir; van Blaaderen, Alfons; Bossi, Mariano L; Hell, Stefan W

    2008-01-01

    We have designed and synthesized a new functional (amino reactive) highly efficient fluorescent molecular switch (FMS) with a photochromic diarylethene and a rhodamine fluorescent dye. The reactive group in this FMS -N-hydroxysuccinimide ester- allows selective labeling of amino containing molecules or other materials. In ethanolic solutions, the compound displays a large fluorescent quantum yield of 52 % and a large fluorescence modulation ratio (94 %) between two states that may be interconverted with red and near-UV light. Silica nanoparticles incorporating the new FMS were prepared and characterized, and their spectroscopic and switching properties were also studied. The dye retained its properties after the incorporation into the silica, thereby allowing light-induced reversible high modulation of the fluorescence signal of a single particle for up to 60 cycles, before undergoing irreversible photobleaching. Some applications of these particles in fluorescence microscopy are also demonstrated. In particular, subdiffraction images of nanoparticles were obtained, in the focal plane of a confocal microscope.

  15. One pot electrochemical synthesis of polymer/CNT/metal nanoparticles for fuel cell applications

    Science.gov (United States)

    Ventrapragada, Lakshman; Zhu, Jingyi; Karakaya, Mehmet; Podila, Ramakrishna; Rao, Apparao; Clemson Nanomaterials center Team

    Carbon nanotubes (CNTs) have become a key player in the design of materials for energy applications. They gained their popularity in industrial and scientific research due to their unique properties like excellent conductivity, high surface area, etc. Here we used chemical vapor deposition (CVD) to synthesize two types of CNTs namely, helically coiled CNTs and vertically aligned CNTs. These CNTs were subsequently used to make composites with conducting polymers and metal nanoparticles. One pot electrochemical synthesis was designed to electropolymerize aniline, pyrrole etc. on the surface of the electrode with simultaneous deposition of platinum and gold metal nanoparticles, and CNTs in the polymer matrix. The as synthesized composite materials were characterized with scanning electron microscope for surface morphology and spectroscopic techniques like Raman, UV-Vis for functionality. These were used to study electrocatalytic oxidation of methanol and ethanol for alkaline fuel cell applications. Electrodes fabricated from these composites not only showed good kinetics but also exhibited excellent stability. Uniqueness of this composite lies in its simple two step synthesis and it doesn't involve any surfactants unlike conventional chemical synthesis routes.

  16. Synthesis and characterization of anisotropic magnetic hydrogels

    Energy Technology Data Exchange (ETDEWEB)

    Hinrichs, Stephan, E-mail: stephan.hinrichs@chemie.uni-hamburg.de; Nun, Nils; Fischer, Birgit, E-mail: birgit.fischer@chemie.uni-hamburg.de

    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.

  17. Octalithium plumbate as breeding blanket ceramic: Neutronic performances, synthesis and partial characterization

    International Nuclear Information System (INIS)

    Colominas, S.; Palermo, I.; Abellà, J.; Gómez-Ros, J.M.; Sanz, J.; Sedano, L.

    2012-01-01

    Highlights: ► Definition of a suitable configuration for the Li 8 PbO 6 breeding blanket design. ► Demonstration of the feasibility of Li 8 PbO 6 as a breeding material. ► Synthesis optimization in the Li 8 PbO 6 production. ► Characterization of Li 8 PbO 6 by X-ray phase analysis is discussed. - Abstract: A neutronic assessment of the performances of a helium-cooled Li 8 PbO 6 breeding blanket (BB) for the conceptual design of a DEMO fusion reactor is given. Different BB configurations have been considered in order to minimize the amount of beryllium required for neutron multiplication, including the use of graphite as reflector material. The calculated neutronic responses: tritium breeding ratio (TBR), power deposition in TF coils and power amplification factor, indicate the feasibility of Li 8 PbO 6 as breeding material. Furthermore, the synthesis and characterization of Li 8 PbO 6 by X-ray phase analysis are also discussed.

  18. Spectroscopic identification of rare earth elements in phosphate glass

    Science.gov (United States)

    Devangad, Praveen; Tamboli, Maktum; Muhammed Shameem, K. M.; Nayak, Rajesh; Patil, Ajeetkumar; Unnikrishnan, V. K.; Santhosh, C.; Kumar, G. A.

    2018-01-01

    In this work, rare earth-doped phosphate glasses were synthesized and characterized using three different spectroscopic techniques. The absorption spectra of the prepared praseodymium (Pr) and samarium (Sm) doped glasses, recorded by a UV-VIS-NIR spectrophotometer, show the characteristic absorption bands of these elements. To confirm this inference, laser-induced fluorescence spectra of Pr and Sm were obtained at a laser excitation of 442 nm. Their emission bands are reported here. The elemental analysis of these samples was carried out using a laser-induced breakdown spectroscopy (LIBS) system. Characteristic emission lines of Pr and Sm have been identified and reported by the recorded LIBS spectra of glass samples. Results prove that using these three complimentary spectroscopic techniques (absorption, fluorescence and LIBS), we can meaningfully characterize rare earth-doped glass samples.

  19. Synthesis and characterization of magnetite nanoparticles from mineral magnetite

    Energy Technology Data Exchange (ETDEWEB)

    Morel, Mauricio, E-mail: mmorel@ing.uchile.cl [Laboratorio de Síntesis y Polímeros, Departamento de ciencias de los Materiales, Facultad de Ciencias Físicas y Matemáticas, Universidad de Chile, Santiago (Chile); Laboratorio de Materiales a Nanoescala, Departamento de ciencias de los Materiales, Facultad de Ciencias Físicas y Matemáticas, Universidad de Chile, Avenue Tupper 2069, Santiago (Chile); Martínez, Francisco, E-mail: polimart@ing.uchile.cl [Laboratorio de Síntesis y Polímeros, Departamento de ciencias de los Materiales, Facultad de Ciencias Físicas y Matemáticas, Universidad de Chile, Santiago (Chile); Mosquera, Edgar [Laboratorio de Materiales a Nanoescala, Departamento de ciencias de los Materiales, Facultad de Ciencias Físicas y Matemáticas, Universidad de Chile, Avenue Tupper 2069, Santiago (Chile)

    2013-10-15

    We have synthesized magnetite nanoparticles with sizes that range from 20 to 30 nm from mineral magnetite roughly 45 μm in size. The procedure consists in the dissolution of the mineral in an acidic medium and subsequent precipitation in a basic medium in the presence of oleic acid. Two experiments were conducted in different gaseous environments. The first was carried out in an environment exposed to air (M1) and the second in an N{sub 2} (M2) environment. The x-ray diffraction results showed a slight difference, which corresponds to the surface oxidation of magnetite. The sizes of the modified nanoparticles were determined through the Scherrer equation and transmission electron microscopy. An organic material mass loss corresponding to 18% was observed through a thermogravimetric analysis. The Fourier transform infrared spectroscopic analysis provides information about the type of bond that is formed on the surface of the nanoparticle, which corresponds to a bidentate chelate. The vibrating sample magnetometer results show a superparamagnetic behavior for sample M1. - Highlights: • A new method for synthesis of nanoparticles from mineral microparticles. • Search agreggate value to the mineral by mean nanoscience. • The stoichiometric ratio of the ions Fe{sup 2+} and Fe{sup 3+} from the mineral magnetite is synergistic.

  20. Synthesis and characterization of magnetite nanoparticles from mineral magnetite

    International Nuclear Information System (INIS)

    Morel, Mauricio; Martínez, Francisco; Mosquera, Edgar

    2013-01-01

    We have synthesized magnetite nanoparticles with sizes that range from 20 to 30 nm from mineral magnetite roughly 45 μm in size. The procedure consists in the dissolution of the mineral in an acidic medium and subsequent precipitation in a basic medium in the presence of oleic acid. Two experiments were conducted in different gaseous environments. The first was carried out in an environment exposed to air (M1) and the second in an N 2 (M2) environment. The x-ray diffraction results showed a slight difference, which corresponds to the surface oxidation of magnetite. The sizes of the modified nanoparticles were determined through the Scherrer equation and transmission electron microscopy. An organic material mass loss corresponding to 18% was observed through a thermogravimetric analysis. The Fourier transform infrared spectroscopic analysis provides information about the type of bond that is formed on the surface of the nanoparticle, which corresponds to a bidentate chelate. The vibrating sample magnetometer results show a superparamagnetic behavior for sample M1. - Highlights: • A new method for synthesis of nanoparticles from mineral microparticles. • Search agreggate value to the mineral by mean nanoscience. • The stoichiometric ratio of the ions Fe 2+ and Fe 3+ from the mineral magnetite is synergistic

  1. Principles of asymmetric synthesis

    CERN Document Server

    Gawley, Robert E; Aube, Jeffrey

    2012-01-01

    The world is chiral. Most of the molecules in it are chiral, and asymmetric synthesis is an important means by which enantiopure chiral molecules may be obtained for study and sale. Using examples from the literature of asymmetric synthesis, this book presents a detailed analysis of the factors that govern stereoselectivity in organic reactions. After an explanation of the basic physical-organic principles governing stereoselective reactions, the authors provide a detailed, annotated glossary of stereochemical terms. A chapter on "Practical Aspects of Asymmetric Synthesis" provides a critical overview of the most common methods for the preparation of enantiomerically pure compounds, techniques for analysis of stereoisomers using chromatographic, spectroscopic, and chiroptical methods. The authors then present an overview of the most important methods in contemporary asymmetric synthesis organized by reaction type. Thus, there are four chapters on carbon-carbon bond forming reactions, one chapter on reductions...

  2. New approach in synthesis, characterization and release study of pH-sensitive polymeric micelles, based on PLA-Lys-b-PEGm, conjugated with doxorubicin

    International Nuclear Information System (INIS)

    Efthimiadou, E. K.; Tapeinos, C.; Bilalis, P.; Kordas, G.

    2011-01-01

    Amphiphilic block copolymers are well established as building blocks for the preparation of micellar drug carriers. The functional polymer micelles possess several advantages, such as high drug efficiency, targeted delivery, and minimized cytotoxicity. The synthesis of block copolymers using nano-structured templates has emerged as a useful and versatile approach for preparing drug carriers. Here, we report the synthesis of a smart polymeric compound of a diblock PLA-Lys-b-PEG copolymer containing doxorubicin. We have synthesized functionalized diblock copolymers, with lysinol, poly(lactide) and monomethoxy poly(ethylene glycol) via thermal ring-opening polymerization and a subsequent six-step substitution reaction. A variety of spectroscopic methods were employed here to verify the product of our synthesis. 1 H-Nuclear magnetic resonance and Fourier transform infrared studies validated the expected synthesis of copolymers. Doxorubicin is chemically loaded into micelles, and the ex vitro release can be evaluated either in weak acidic or in SBF solution by UV–vis spectroscopy. Dynamic light scattering, thermo gravimetric analysis, and size exclusion chromatography have also been used.

  3. Colloidal synthesis and characterization of Bi2S3 nanoparticles for photovoltaic applications

    International Nuclear Information System (INIS)

    Piras, R; Aresti, M; Saba, M; Marongiu, D; Mula, G; Quochi, F; Mura, A; Bongiovanni, G; Cannas, C; Mureddu, M; Ardu, A; Ennas, G; Musinu, A; Calzia, V; Mattoni, A

    2014-01-01

    Bismuth sulfide is a promising n-type semiconductor for solar energy conversion. We have explored the colloidal synthesis of Bi 2 S 3 nanocrystals, with the aim of employing them in the fabrication of solution-processable solar cells and to replace toxic heavy metals chalcogenides like PbS or CdS, that are currently employed in such devices. We compare different methods to obtain Bi 2 S 3 colloidal quantum dots, including the use of environmentally benign reactants, through organometallic synthesis. Different sizes and shapes were obtained according to the synthesis parameters and the growth process has been rationalized by comparing the predicted morphology with systematic physical-chemistry characterization of nanocrystals by X-ray diffraction, FT-IR spectroscopy, Transmission Electron Microscopy (TEM)

  4. Novel Organotin(IV) Schiff Base Complexes with Histidine Derivatives: Synthesis, Characterization, and Biological Activity

    Science.gov (United States)

    Garza-Ortiz, Ariadna; Camacho-Camacho, Carlos; Sainz-Espuñes, Teresita; Rojas-Oviedo, Irma; Gutiérrez-Lucas, Luis Raúl; Gutierrez Carrillo, Atilano; Vera Ramirez, Marco A.

    2013-01-01

    Five novel tin Schiff base complexes with histidine analogues (derived from the condensation reaction between L-histidine and 3,5-di-tert-butyl-2-hydroxybenzaldehyde) have been synthesized and characterized. Characterization has been completed by IR and high-resolution mass spectroscopy, 1D and 2D solution NMR (1H, 13C  and 119Sn), as well as solid state 119Sn NMR. The spectroscopic evidence shows two types of structures: a trigonal bipyramidal stereochemistry with the tin atom coordinated to five donating atoms (two oxygen atoms, one nitrogen atom, and two carbon atoms belonging to the alkyl moieties), where one molecule of ligand is coordinated in a three dentate fashion. The second structure is spectroscopically described as a tetrahedral tin complex with four donating atoms (one oxygen atom coordinated to the metal and three carbon atoms belonging to the alkyl or aryl substituents), with one molecule of ligand attached. The antimicrobial activity of the tin compounds has been tested against the growth of bacteria in vitro to assess their bactericidal properties. While pentacoordinated compounds 1, 2, and 3 are described as moderate effective to noneffective drugs against both Gram-positive and Gram-negative bacteria, tetracoordinated tin(IV) compounds 4 and 5 are considered as moderate effective and most effective compounds, respectively, against the methicillin-resistant Staphylococcus aureus strains (Gram-positive). PMID:23864839

  5. 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

  6. Physicochemical and Spectroscopic Characterization of Biofield Treated Triphenyl Phosphate

    OpenAIRE

    Trivedi, Mahendra

    2015-01-01

    Triphenyl phosphate (TPP) is a triester of phosphoric acid and phenol. It is commonly used as a fire-retarding agent and plasticizer for nitrocellulose and cellulose acetate. The present study was an attempt to evaluate the impact of biofield treatment on physicochemical and spectroscopic properties of TPP. The study was carried out in two groups i.e. control and treatment. The treatment group was subjected to Mr. Trivedi's biofield treatment. The control and treated samples of TPP were chara...

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

    International Nuclear Information System (INIS)

    Garcia Junior, E.S.; Gomes Junior, G.G.; Ogasawara, T.

    2010-01-01

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

  8. X-Ray Photoelectron Spectroscopic Characterization of Iron Oxide Nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Radu, T., E-mail: Teodora.Radu@itim-cj.ro [National Institute for Research and Development of Isotopic and Molecular Technologies, 67-103 Donat Street, 400293, Cluj Napoca (Romania); Iacovita, C. [Department of Pharmaceutical Physics-Biophysics, Faculty of Pharmacy, “Iuliu Hatieganu” University of Medicine and Pharmacy, 400349, Cluj-Napoca (Romania); Benea, D. [Faculty of Physics, Babes Bolyai University, 400271, Cluj-Napoca (Romania); Turcu, R. [National Institute for Research and Development of Isotopic and Molecular Technologies, 67-103 Donat Street, 400293, Cluj Napoca (Romania)

    2017-05-31

    Highlights: • Characterization of three types of iron oxides magnetic nanoparticles. • A correlation between valence band XPS and the degree of iron oxidation is proposed. • Theoretical contributions of Fe in tetragonal and octahedral environment are shown. - Abstract: We report X-ray photoelectron spectroscopy (XPS) results on iron oxide magnetic nanoparticle (Fe{sub 3}O{sub 4}) synthesized using solvothermal reduction in the presence of polyethylene glycol. The magnetite obtained was employed as precursor for the synthesis of γ-Fe{sub 2}O{sub 3} (by oxygen dissociation) which in turn was transformed into α-Fe{sub 2}O{sub 3}. We confirmed the magnetite, maghemite and hematite structure by Fourier Transformed Spectroscopy (FTIR) and X-ray diffraction (XRD). The analysis of the XPS core level and valence band (VB) photoemission spectra for all investigated samples is discussed in terms of the degree of iron oxidation. This is of fundamental importance to better understand the electronic structure of the obtained iron oxide nanoparticles in order to control and improve their quality for specific biomedical applications. Moreover, theoretical band structure calculations are performed for magnetite and the separate contributions of Fe in tetragonal and octahedral environment are shown.

  9. 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)

  10. Evolution of containment facilities for spectroscopic analysis at Rockwell Hanford Operations

    International Nuclear Information System (INIS)

    Hiller, J.M.

    1984-01-01

    The analysis of radioactive material requires much thought concerning getting the job done while still maintaining a safe working environment. At Rockwell Hanford Operations, we have gone through several stages of evolution in instrumentation for spectroscopic elemental analysis, reflecting different philosophies with respect to shielding and contamination control. Atomic absorption and inductively coupled plasma emission spectroscopic systems have been used for analyzing samples in support of a fission product recovery plant, nuclear waste processing and characterization programs, and U and Pu separation plants. Design thoughts, criticisms, and lessons learned in 20 years of containment for spectroscopic analysis are presented. 3 refs., 6 figs., 2 tabs

  11. Spectroscopic and nonlinear photophysical characterization of organic octupolar-compounds supported by anodic-alumina nanotube-arrays

    International Nuclear Information System (INIS)

    Morales-Saavedra, O.G.; Ontiveros-Barrera, F.G.; Hennrich, G.; Mata-Zamora, M.E.; Rodriguez-Rosales, A.A.; Banuelos, J.G.

    2011-01-01

    Highlights: → Preparation of organic-inorganic nanostructured hybrid materials. → Insertion of octupolar compounds in alumina nanotube arrays. → Linear and nonlinear photophysical characterization of solid-state hybrid structures. → Fabrication of photonic materials. - Abstract: Amorphous anodic alumina membranes (AAM) comprising highly ordered nanometric porous arrays (porous anodic aluminas: PAA) with 1D-nanotube dimensions of ∼75 nm in diameter and 45 microns in depth were successfully prepared and used as nanostructured host networks for different functionalized octupolar chromophores (named here Oct-(n)). Atomic force microscopy (AFM) studies performed on the developed hybrid systems confirmed a homogeneous insertion of these organic molecules into the PAA nanotube-arrays. Samples with high structural quality were selected for several photophysical characterizations: Comprehensive X-ray diffraction (XRD) and optical spectroscopic characterizations performed according to UV-vis absorption, photoluminescent (PL) and Raman measurements revealed the structural and optical performance of these molecules within the PAA-confinement. Since the implemented optical chromophores were specifically functionalized for nonlinear optical (NLO) applications, the obtained Oct-(n)/PAA-based amorphous hybrids were also characterized according to cubic NLO-techniques such as third harmonic generation (THG) and the Z-Scan method. PAA-confined octupolar chromophores have shown interesting linear and NLO optical properties which have not yet been intensively investigated in bulk hybrid systems; hence, the obtained hybrid nanostructures represent a promising field of investigation in the route to functional octupolar-based materials, where different self-assembled molecular structures may be formed, giving rise to enhanced linear and NLO-properties.

  12. Chemical and spectroscopic characterization of a vegetable oil used as dielectric coolant in distribution transformers

    Energy Technology Data Exchange (ETDEWEB)

    Gomez, Neffer A.; Abonia, Rodrigo, E-mail: rodrigo.abonia@correounivalle.edu.co [Departamento de Quimica, Escuela de Ingenieria Electrica, Universidad del Valle, Cali (Colombia); Cadavid, Hector [Grupo GRALTA, Escuela de Ingenieria Electrica, Universidad del Valle, Cali (Colombia); Vargas, Ines H. [Area de Ingenieria de Distribucion, Empresas Publicas de Medellin (EPM), Medellin (Colombia)

    2011-09-15

    In this work, a complete UV-Vis, IR and (1H, 13C and DEPT) NMR spectroscopic analysis was performed for a FR3 vegetable oil sample used as dielectric coolant in an experimental distribution transformer. The same spectroscopic analysis was performed for three used FR3 oil samples (i.e., 4 months in use, 8 months in use and 7 years in use), removed from several operating distribution transformers. Comparison of the data indicated that no significant spectroscopic changes, and hence, no structural changes occurred to the oils by the use. Chemical transformations like catalytic hydrogenation (hardening) and hydrolysis were performed to the FR3 oil sample and the obtained products were analyzed by spectroscopic methods in order to collect further structural information about the FR3 oil. Accelerated aging tests in laboratory were also performed for three FR3 oil samples affording interesting information about the structure of the degradation products. These findings would be valuable to search for a spectroscopy-based technique for monitoring the lifetime and performance of this insulating vegetable oil. (author)

  13. Sonochemical-assisted magnesium borate synthesis from different boron sources

    Directory of Open Access Journals (Sweden)

    Yildirim Meral

    2017-03-01

    Full Text Available In this study, sonochemical-assisted magnesium borate synthesis is studied from different boron sources. Various reaction parameters are successfully applied by a simple and green method. X-ray diffraction (XRD, Fourier transform infrared (FT-IR and Raman spectroscopies are used to characterize the synthesized magnesium borates on the other hand surface morphologies are investigated by using scanning electron microscope (SEM. The XRD analyses showed that the products were admontite [MgO(B2O33 · 7(H2O] with JCPDS (Joint Committee on Powder Diffraction Standards no. of 01-076-0540 and mcallisterite [Mg2(B6O7(OH62 · 9(H2O] with JCPDS no. of 01-070-1902. The results that found in the spectroscopic studies were in a good agreement with characteristic magnesium borate bands in both regions of infra-red and visible. According to SEM results, obtained borates were in micro and sub-micro scales. By the use of ultrasonication, reaction yields were found between 84.2 and 97.9%. As a result, it is concluded that the sonochemical approach is a practicable synthesis method to get high efficiency and high crystallinity in the synthesis magnesium borate compounds.

  14. Synthesis, spectroscopic characterization and thermogravimetric analysis of two series of substituted (metallotetraphenylporphyrins

    Directory of Open Access Journals (Sweden)

    Rasha K. Al-Shewiki

    2017-06-01

    Full Text Available Subsequent treatment of H2TPP(CO2H4 (tetra(p-carboxylic acid phenylporphyrin, 1 with an excess of oxalyl chloride and HNR2 afforded H2TPP(C(ONR24 (R = Me, 2; iPr, 3 with yields exceeding 80%. The porphyrins 2 and 3 could be converted to the corresponding metalloporphyrins MTPP(C(ONR24 (R = Me/iPr for M = Zn (2a, 3a; Cu (2b, 3b; Ni (2c, 3c; Co (2d, 3d by the addition of 3 equiv of anhydrous MCl2 (M = Zn, Cu, Ni, Co to dimethylformamide solutions of 2 and 3 at elevated temperatures. Metalloporphyrins 2a–d and 3a–d were obtained in yields exceeding 60% and have been, as well as 2 and 3, characterized by elemental analysis, electrospray ionization mass spectrometry (ESIMS and IR and UV–vis spectroscopy. Porphyrins 2, 2a–d and 3, 3a–d are not suitable for organic molecular beam deposition (OMBD, which is attributed to their comparatively low thermal stability as determined by thermogravimetric analysis (TG of selected representatives.

  15. Synthesis, spectroscopic and TD-DFT quantum mechanical study of azo-azomethine dyes. A laser induced trans-cis-trans photoisomerization cycle.

    Science.gov (United States)

    Georgiev, Anton; Kostadinov, Anton; Ivanov, Deyan; Dimov, Deyan; Stoyanov, Simeon; Nedelchev, Lian; Nazarova, Dimana; Yancheva, Denitsa

    2018-03-05

    This paper describes the synthesis, spectroscopic characterization and quantum mechanical calculations of three azo-azomethine dyes. The dyes were synthesized via condensation reaction between 4-(dimethylamino)benzaldehyde and three different 4-aminobenzene azo dyes. Quantum chemical calculations on the optimized molecular geometry and electron densities of the trans (E) and cis (Z) isomers and their vibrational frequencies have been computed by using DFT/B3LYP density-functional theory with 6-311++G(d,p) basis set in vacuo. The thermodynamic parameters such as total electronic energy E (RB3LYP), enthalpy H 298 (sum of electronic and thermal enthalpies), free Gibbs energy G 298 (sum of electronic and thermal free Gibbs energies) and dipole moment μ were computed for trans (E) and cis (Z) isomers in order to estimate the ΔE trans→cis , Δμ trans→cis, ΔH trans→cis , ΔG trans→cis and ΔS trans→cis values. After molecular geometry optimization the electronic spectra have been obtained by TD-DFT calculations at same basis set and correlated with the spectra of vapour deposited nanosized films of the dyes. The NBO analysis was performed in order to understand the intramolecular charge transfer and energy of resonance stabilization. Solvatochromism was investigated by UV-VIS spectroscopy in five different organic solvents with increasing polarity. The dynamic photoisomerization experiments have been performed in DMF by pump lasers λ=355nm (mostly E→Z) and λ=491nm (mostly Z→E) in spectral region 300nm - 800nm at equal concentrations and times of illumination in order to investigate the photodynamical trans-cis-trans properties of the CHN and NN chromophore groups of the dyes. Copyright © 2017 Elsevier B.V. All rights reserved.

  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. Characterizing the structure of lipodisq nanoparticles for membrane protein spectroscopic studies.

    Science.gov (United States)

    Zhang, Rongfu; Sahu, Indra D; Liu, Lishan; Osatuke, Anna; Comer, Raven G; Dabney-Smith, Carole; Lorigan, Gary A

    2015-01-01

    Membrane protein spectroscopic studies are challenging due to the difficulty introduced in preparing homogenous and functional hydrophobic proteins incorporated into a lipid bilayer system. Traditional membrane mimics such as micelles or liposomes have proved to be powerful in solubilizing membrane proteins for biophysical studies, however, several drawbacks have limited their applications. Recently, a nanosized complex termed lipodisq nanoparticles was utilized as an alternative membrane mimic to overcome these caveats by providing a homogeneous lipid bilayer environment. Despite all the benefits that lipodisq nanoparticles could provide to enhance the biophysical studies of membrane proteins, structural characterization in different lipid compositions that closely mimic the native membrane environment is still lacking. In this study, the formation of lipodisq nanoparticles using different weight ratios of POPC/POPG lipids to SMA polymers was characterized via solid-state nuclear magnetic resonance (SSNMR) spectroscopy and dynamic light scattering (DLS). A critical weight ratio of (1/1.25) for the complete solubilization of POPC/POPG vesicles has been observed and POPC/POPG vesicles turned clear instantaneously upon the addition of the SMA polymer. The size of lipodisq nanoparticles formed from POPC/POPG lipids at this weight ratio of (1/1.25) was found to be about 30 nm in radius. We also showed that upon the complete solubilization of POPC/POPG vesicles by SMA polymers, the average size of the lipodisq nanoparticles is weight ratio dependent, when more SMA polymers were introduced, smaller lipodisq nanoparticles were obtained. The results of this study will be helpful for a variety of biophysical experiments when specific size of lipid disc is required. Further, this study will provide a proper path for researchers working on membrane proteins to obtain pertinent structure and dynamic information in a physiologically relevant membrane mimetic environment

  18. Spectroscopic characterization of Au 3+ biosorption by waste biomass of Saccharomyces cerevisiae

    Science.gov (United States)

    Lin, Zhongyu; Wu, Jianming; Xue, Ru; Yang, Yong

    2005-02-01

    Some spectroscopic characteristics of Au 3+ biosorption by waste biomass of Saccharomyces cerevisiae have been reported in this paper. The effect of temperature on the correlation parameters of chemical kinetics and thermodynamics of the binding reaction was investigated by using AAS. XRD diffraction pattern of gold-loaded biomass revealed that the Au 3+ bound on the cell wall of the biomass had been reduced into gold particle. FTIR spectrophotometry on blank and gold-loaded biomass demonstrated that active groups such as the hydroxyl group of saccharides, and the carboxylate anion of amino-acid residues, from the peptidoglycan layer on the cell wall seem to be the sites for the Au 3+ binding, and the free aldehyde group of the hemiacetalic hydroxyl group from reducing sugars, i.e. the hydrolysates of the polysaccharides on the peptidoglycan layer, serving as the electron donor, in situ reduced the Au 3+ to Au 0. XPS and IR characterizations of the interaction between glucose and Au 3+ further supported that the reduction of Au 3+ to Au 0 can directly occur at the aldehyde group of the reducing sugars.

  19. Synthesis and Characterization of Magnesium Substituted Aluminophosphate Molecular Sieves with AEL Structure

    Institute of Scientific and Technical Information of China (English)

    Benjing Xu; Ling Qian; Xinmei Liu; Chunmin Song; Zifeng Yan

    2004-01-01

    MAPO-11 molecular sieves were synthesized by hydrothermal methods. The influence of precursor of magnesium, Mg/Al ratio, synthesis temperature, synthesis time and the type of template on the formation and properties of MAPO-11 molecular sieves was examined. The samples were characterized by the techniques of X-ray diffraction (XRD), scanning electron microscopy (SEM), thermogravimetric/differential thermogravimetric analysis (TG-DGA), etc. The results show that the shape and size of crystal were influenced by the precursor of Mg, the Mg/Al ratio and the type of template, and the TG-DGA analysis shows that MAPO-11 molecular sieves as-synthesized have poor thermal stability.

  20. 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

  1. Syntheses and spectroscopic properties of mercury(II) and nickel(II ...

    African Journals Online (AJOL)

    Syntheses and spectroscopic properties of mercury(II) and nickel(II) ... The complexes were characterized by IR, diffuse reflectance, 1H NMR spectra and elemental ... coordinating through thiolato sulphur and hydrazinic nitrogen atoms.

  2. Synthesis and Characterization of Some Macrocylic Complexes Incorporating Indole and 2,2'-Bipyridine or 1,10-Phenanthroline

    Directory of Open Access Journals (Sweden)

    Muhammad S. Khan

    2015-06-01

    Full Text Available Complexes of anionic pentadentate macrocyclic ligands by the template condensation of bis(hydrazino2,2'-bipyridine or 1,10-phenanthroline with an indoledialdehyde have been synthesized. The new Mn(II, Fe(II, Co(II, Ni(II, Cu(II and Zn(II macrocyclic complexes have been characterized by analytical and spectroscopic techniques and by conductivity and magnetic susceptibility measurements.

  3. Spectroscopic analysis and molecular docking of imidazole derivatives and investigation of its reactive properties by DFT and molecular dynamics simulations

    Science.gov (United States)

    Thomas, Renjith; Hossain, Mossaraf; Mary, Y. Sheena; Resmi, K. S.; Armaković, Stevan; Armaković, Sanja J.; Nanda, Ashis Kumar; Ranjan, Vivek Kumar; Vijayakumar, G.; Van Alsenoy, C.

    2018-04-01

    Solvent-free synthesis pathway for obtaining two imidazole derivatives (2-chloro-1-(4-methoxyphenyl)-4,5-dimethyl-1H-imidazole (CLMPDI) and 1-(4-bromophenyl)-2-chloro-4,5-dimethyl-1H-imidazole (BPCLDI) has been reported in this work, followed by detailed experimental and computational spectroscopic characterization and reactivity study. Spectroscopic methods encompassed IR, FT-Raman and NMR techniques, with the mutual comparison of experimentally and computationally obtained results at DFT/B3LYP level of theory. Reactivity study based on DFT calculations encompassed molecular orbitals analysis, followed by calculations of molecular electrostatic potential (MEP) and average local ionization energy (ALIE) values, Fukui functions and bond dissociation energies (BDE). Additionally, the stability of title molecules in water has been investigated via molecular dynamics (MD) simulations, while interactivity with aspulvinonedimethylallyl transferase protein has been evaluated by molecular docking procedure. CLMPDI compound showed antimicrobial activity against all four bacterial strain in both gram positive and gram negative bacteria while, BPCLDI showed only in gram positive bacteria, Staphylococcus Aureus (MTCC1144). The first order hyperpolarizability of CLMPDI and BPCLDI are 20.15 and 6.10 times that of the standard NLO material urea.

  4. High temperature bismuth cuprate superconductors synthesis and characterization

    International Nuclear Information System (INIS)

    Mansori, M.; Satre, P.; Breandon, C.; Roubin, M.; Sebaoun, A.

    1993-01-01

    High temperature superconductor phases synthesis by coprecipitation in alkaline solution is reported. (Bi 1.6 Pb 0.4 )Sr 2 Ca 1 Cu 2 O 8+x and (Bi 1.6 Pb 0.4 )Sr 2 Ca 2 Cu 3 O 10+y noted (2212) and (2223) have been prepared and studied. From aqueous nitrate solutions of Bi, Pb, Sr, Ca and Cu and oxalic acid aqueous solution as well as ethylene glycol, using an organic base (the triethylamine), the pH was increased up to the path of the precipitation zone (pH = 10.5-11.2). This method assures a good granulometric homogeneity of powders. Thermal analysis and characterization of the different components produced during the synthesis have been studied by DTA (differential thermal analysis)- TGA (thermogravimetric analysis), X-ray diffraction at different temperatures and by Infrared spectroscopy with a Fourier transformation. The measurements of magnetic susceptibility for the 2212 (with and without lead) and 2223 (with lead) phases have permitted us to observe the critical temperatures of 84 K, 87 K and 114 K. (author). 29 refs., 2 figs., 4 tabs

  5. Wet chemical synthesis of soluble gold nanogaps

    DEFF Research Database (Denmark)

    Jain, Titoo; Tang, Qingxin; Bjørnholm, Thomas

    2014-01-01

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

  6. Synthesis and characterization of fluorine compounds

    International Nuclear Information System (INIS)

    Martinez Carrillo, M.

    1991-01-01

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

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

    International Nuclear Information System (INIS)

    Khan, S.M.; Chughtai, A.; Sattar, A.

    2008-01-01

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

  8. Synthesis and Characterization of Biscoumarin and Benzopyrano Dicoumarin Derivatives

    International Nuclear Information System (INIS)

    Nik Khairunissa' Nik Abdullah Zawawi; Muhammad Taha; Norizan Ahmat; Nor Hadiani Ismail; Nik Khairunissa' Nik Abdullah Zawawi; Muhammad Taha; Norizan Ahmat; Nor Hadiani Ismail

    2016-01-01

    The wide-ranging biological activities of 4-hydroxycoumarin have stimulated considerable interest in this class of compounds, and various biscoumarin derivatives have been synthesized. Recently, a number of methods have been reported for the synthesis of biscoumarin by the reaction of 4-hydroxycoumarin and various aldehydes in the presence of catalysts. In the present study, a new series of biscoumarin and benzopyrano dicoumarin were synthesized and physically characterized by nuclear magnetic resonane ( 1 H and 13 C NMR), fourier transform infrared spectroscopy (FTIR), mass spectrometry (MS) and melting point. (author)

  9. Synthesis and characterization of the polyaniline dopant Schiff base

    Directory of Open Access Journals (Sweden)

    Mirian Y. Matsumoto

    2012-06-01

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

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-12-15

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

  12. Design, Synthesis and Spectral Characterization of Novel 2-morpholino-N-(4,6-diarylpyrimidin-2-yl)acetamides

    Energy Technology Data Exchange (ETDEWEB)

    Kanagarajan, Vijayakumar; Thanusu, Jayaraman; Gopalakrishnan, Mannathusamy [Annamalai University, Tamil Nadu (India)

    2010-02-15

    A new series of novel 2-morpholino-N-(4,6-diarylpyrimidin-2-yl)acetamides 34-42 is synthesized by the condensation of 2-chloro-N-(4,6-diarylpyrimidin-2-yl)acetamides 25-33 with morpholine in the presence of anhydrous potassium carbonate. The synthesized compounds have been characterized by melting point, elemental analysis, MS, FT-IR, one-dimensional NMR ({sup 1}H and {sup 13}C) spectroscopic data.

  13. Synthesis of poly(aniline-co-o-toluidine) coatings on copper

    Energy Technology Data Exchange (ETDEWEB)

    Raotole, Pritee, E-mail: priteeraotole@gmail.com; Patil, V. T.; Huse, V. R.; Chaudhari, A. L. [MGSM’s Arts, Science and Commerce, College, Chopda, Dist-Jalgaon 425107, Maharashtra (India); Raotole, Mahesh [Sharacchandrika Suresh Patil, Institute of Technology, Polytechnic, Chopda, Dist-Jalgaon, 425107, Maharashtra (India)

    2016-05-06

    The corrosion protective poly(aniline-co-o-toluidine) (PAOT) coatings were synthesized on copper (Cu) by the electrochemical copolymerization of aniline with o-toluidine under cyclic voltammetry conditions. Aqueous oxalate solutions were used as the supporting electrolytes for the synthesis of PAOT coatings on Cu. The resulting coatings were characterized by different spectroscopic techniques, cyclic voltammetry, ultraviolet-visible absorption spectroscopy, Fourier transform infrared spectroscopy (FTIR), nuclear magnetic resonance spectroscopy (NMR), and scanning electron microscopy. The Fourier Transform InfraRed (FTIR) spectroscopy and Nuclear Magnetic Resonance (NMR) spectroscopy studies reveal that the copolymerization of aniline and o-toluidine takes place on Cu substrates from an aqueous oxalate solutions and resulting in PAOT copolymer, there are more o-toluidine units than aniline units.

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

    OpenAIRE

    Souza, N. S.; Sergeenkov, S.; Speglich, C.; Rivera, V. A. G.; Cardoso, C. A.; Pardo, H.; Mombru, A. W.; Rodrigues, A. D.; de Lima, O. F.; Araujo-Moreira, F. M.

    2009-01-01

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

  15. Spectroscopic characterizations of organic/inorganic nanocomposites

    Science.gov (United States)

    Govani, Jayesh R.

    2009-12-01

    In the present study, pure and 0.3 wt%, 0.4 wt%, as well as 0.5 wt% L-arginine doped potassium dihydrogen phosphate (KDP) crystals were grown using solution growth techniques and further subjected to infrared (IR) absorption and Raman studies for confirmation of chemical group functionalization for investigating the incorporation mechanism of the L-arginine organic material into the KDP crystal structure. Infrared spectroscopic analysis suggests that structural changes are occurring for the L-arginine molecule as a result of its interaction with the KPD crystal. Infrared spectroscopic technique confirms the disturbance of the N-H, C-H and C-N bonds of the amino acid, suggesting successful incorporation of L-arginine into the KDP crystals. Raman analysis also reveals modification of the N-H, C-H and C-N bonds of the amino acid, implying successful inclusion of L-arginine into the KDP crystals. With the help of Gaussian software, a prediction of possible incorporation mechanisms of the organic material was obtained from comparison of the simulated infrared and Raman vibrational spectra with the experimental results. Furthermore, we also studied the effect of L-arginine doping on the thermal stability of the grown KDP crystal by employing Thermo gravimetric analysis (TGA). TGA suggests that increasing the level of L-arginine doping speeds the decomposition process and it weakens the KDP crystal, which indicates successful doping of the KDP crystals with L-arginine amino acid. Urinary stones are one of the oldest and most widely spread diseases in humans, animals and birds. Many remedies have been employed through the ages for the treatment of urinary stones. Recent medicinal measures reflect the modern advances, which are based on surgical removal, percutaneous techniques and extracorporeal shock wave lithotripsy (ESWL). Although these procedures are valuable, they are quite expensive for most people. Furthermore, recurrence of these diseases is awfully frequent with

  16. 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.

  17. Spectroscopic and antimicrobial studies of polystyrene films under ...

    Indian Academy of Sciences (India)

    Spectroscopic and antimicrobial studies of polystyrene films under air plasma and He-Ne laser treatment ... The parameters such as (1) surface area by contact angle measurements, (2) quality of material before and after treatment by SEM and FTIR spectra and (3) material characterization by UV-vis spectra were studied.

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

    Science.gov (United States)

    Ma, Feiyue

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

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

    International Nuclear Information System (INIS)

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

    2015-01-01

    Gold nanobipyramids (NBPs) have attracted much attention because they have potential for applications in smart sensing devices, such as medical diagnostic equippments. This is due to the fact that they show more advantageous plasmonic properties than other gold nanostructures. We describe a chemical reduction method for synthesizing NBPs using conventional heating with ascorbic acid reduction and cetyltrimethylamonium bromide (CTAB) + AgNO_3 as capping agents. The product was characterized by ultraviolet–visible spectroscopy (UV–vis), Fourier transmission infrared spectroscopy (FTIR), transmission electron microscopy (TEM), x-ray powder diffraction (XRD). The results showed that gold nanoparticles were formed with bipyramid shape (tip-to-tip distance of 88.4 ± 9.4 nm and base length of 29.9 ± 3.2 nm) and face-centered-cubic crystalline structure. Optimum parameters for preparation of NBPs are also found. (paper)

  20. Synthesis and spectroscopic characterization of gallic acid and some of its azo complexes

    Science.gov (United States)

    Masoud, Mamdouh S.; Hagagg, Sawsan S.; Ali, Alaa E.; Nasr, Nessma M.

    2012-04-01

    A series of gallic acid and azo gallic acid complexes were prepared and characterized by elemental analysis, IR, electronic spectra and magnetic susceptibility. The complexes were of different geometries: Octahedral, Tetrahedral and Square Planar. ESR was studied for copper complexes. All of the prepared complexes were of isotropic nature. The thermal analyses of the complexes were studied by DTA and DSC techniques. The thermodynamic parameters and the thermal transitions, such as glass transitions, crystallization and melting temperatures for some ligands and their complexes were evaluated and discussed. The entropy change values, ΔS#, showed that the transition states are more ordered than the reacting complexes. The biological activities of some ligands and their complexes are tested against Gram positive and Gram negative bacteria. The results showed that some complexes have a well considerable activity against different organisms.

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

    Science.gov (United States)

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

    2015-12-01

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

  2. Synthesis and Characterization of High Aluminum Zeolite X from Technical Grade Materials

    Directory of Open Access Journals (Sweden)

    Seyed Kamal Masoudian

    2013-06-01

    Full Text Available Zeolites are widely used as ion exchangers, adsorbents, separation materials and catalyst due to their well-tailored and highly-reproducible structures; therefore, the synthesis of zeolite from low grade resources can be interested. In the present work, high aluminum zeolite X was prepared from mixing technical grade sodium aluminate and sodium silicate solutions at temperatures between 70°C and 100°C. The synthesized zeolite X was characterized by SEM and X-ray methods according to ASTM standard procedures. The results showed that aging of the synthesis medium at the room temperature considerably increased the selectivity of zeolite X formation. On the other hand, high temperature of reaction mixture during crystallization formed zeolite A in the product; therefore, it decreased the purity of zeolite X. In addition, it was found that increasing H2O/Na2O and decreasing Na2O/SiO2 molar ratios in the reaction mixture resulted product with higher purity. © 2013 BCREC UNDIP. All rights reservedReceived: 7th January 2013; Revised: 7th April 2013; Accepted: 19th April 2013[How to Cite: Masoudian, S. K., Sadighi, S., Abbasi, A. (2013. Synthesis and Characterization of High Alu-minum Zeolite X from Technical Grade Materials. Bulletin of Chemical Reaction Engineering & Catalysis, 8 (1: 54-60. (doi:10.9767/bcrec.8.1.4321.54-60][Permalink/DOI: http://dx.doi.org/10.9767/bcrec.8.1.4321.54-60] | View in  |

  3. Double-chain phospholipid end-capped polyurethanes: Synthesis, characterization and platelet adhesion study

    International Nuclear Information System (INIS)

    Tan Dongsheng; Zhang Xiaoqing; Li Jiehua; Tan Hong; Fu Qiang

    2012-01-01

    A novel phospholipid containing double chains and phosphotidylcholine polar head groups, 2-(10-(2-aminoethylamino)-10-oxodecanamido)-3-(decyloxy)-3-oxopropyl phosphorylcholine (ADDPC), was synthesized and characterized. Two kinds of double-chain phospholipid end-capped polyurethanes with different soft segments were prepared. The structure of prepared polyurethanes was characterized by X-ray photoelectron spectroscopic (XPS), attenuated total reflection Fourier transform infrared (ATR-FTIR) spectrometry and atomic force microscope (AFM), which indicated that the double-chain phospholipids enriched onto the top surface of the prepared polyurethane films. The preliminary evaluation of blood compatibility showed that these novel phospholipid end-capped polyurethanes could suppress platelet adhesion and activation effectively. This property did not depend on the chemical structure of polyurethanes. In addition, according to tensile test results, the phospholipid polyurethanes kept good mechanical properties in comparison with original polyurethanes. It is suggested that double-chain phospholipid end-caption has good potential for achieving both hemocompatibility and good mechanical properties simultaneously for polyurethanes.

  4. New Dilated LMI Characterization for the Multiobjective Full-Order Dynamic Output Feedback Synthesis Problem

    Directory of Open Access Journals (Sweden)

    Zrida Jalel

    2010-01-01

    Full Text Available This paper introduces new dilated LMI conditions for continuous-time linear systems which not only characterize stability and performance specifications, but also, performance specifications. These new conditions offer, in addition to new analysis tools, synthesis procedures that have the advantages of keeping the controller parameters independent of the Lyapunov matrix and offering supplementary degrees of freedom. The impact of such advantages is great on the multiobjective full-order dynamic output feedback control problem as the obtained dilated LMI conditions always encompass the standard ones. It follows that much less conservatism is possible in comparison to the currently used standard LMI based synthesis procedures. A numerical simulation, based on an empirically abridged search procedure, is presented and shows the advantage of the proposed synthesis methods.

  5. Synthesis, characterization and antibacterial study of tripodal tris-(N-benzoylthioureido)ethylamine

    Energy Technology Data Exchange (ETDEWEB)

    Adan, Dalina; Yamin, Bohari [School of Chemical Sciences and Food Technology, Faculty of Science and Technology, University Kebangsaan Malaysia, 43000, Bangi, Selangor (Malaysia); Leng, Ong Wei; Ibrahim, Nazlina [School of Biosciences and Biotechnology, Faculty of Science and Technology, University Kebangsaan Malaysia, 43000, Bangi, Selangor (Malaysia)

    2014-09-03

    A new tripodal tris-(N-benzoylthiouredoethyl)amine has been successfully synthesized and characterized by spectroscopic technique such as FTIR, ESI MS, {sup 1}H and {sup 13}C NMR. The microanalysis data is in a good agreement with the expected molecular formula. The {sup 1}H NMR chemical shift for both amide and thioamide proton are at lower field than their normal value indicates the presence of the hydrogen bond between the carbonyl oxygen atom and thioamide hydrogen. This is possible when the benzoyl group adopt a trans configuration againts thione group along the C-N bond. The compound has been tested for antibacterial activity against three selected bacteria namely Staphylococcus aureus, Proteus vulgaris and Pseudomanas aeroginosa but there is no significant activities observed.

  6. Synthesis and characterization of boron nitrides nanotubes

    International Nuclear Information System (INIS)

    Ferreira, T.H.; Sousa, E.M.B.

    2010-01-01

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

  7. Characterization of μc-Si:H/a-Si:H tandem solar cell structures by spectroscopic ellipsometry

    International Nuclear Information System (INIS)

    Murata, Daisuke; Yuguchi, Tetsuya; Fujiwara, Hiroyuki

    2014-01-01

    In order to perform the structural characterization of Si thin-film solar cells having submicron-size rough textured surfaces, we have developed an optical model that can be utilized for the spectroscopic ellipsometry (SE) analysis of a multilayer solar cell structure consisting of hydrogenated amorphous silicon (a-Si:H) and microcrystalline silicon (μc-Si:H) layers fabricated on textured SnO 2 :F substrates. To represent the structural non-uniformity in the textured structure, the optical response has been calculated from two regions with different thicknesses of the Si layers. Moreover, in the optical model, the interface layers are modeled by multilayer structures assuming two-phase composites and the volume fractions of the phases in the layers are controlled by the structural curvature factor. The polarized reflection from the μc-Si:H layer that shows extensive surface roughening during the growth has also been modeled. In this study, a state-of-the-art solar cell structure with the textured μc-Si:H (2000 nm)/ZnO (100 nm)/a-Si:H (200 nm)/SnO 2 :F/glass substrate structure has been characterized. The μc-Si:H/a-Si:H textured structure deduced from our SE analysis shows remarkable agreement with that observed by transmission electron microscopy. From the above results, we have demonstrated the high-precision characterization of highly-textured μc-Si:H/a-Si:H solar cell structures. - Highlights: • Characterization of textured μc-Si:H/a-Si:H solar cell structures by ellipsometry • A new optical model using surface area and multilayer models • High precision characterization of submicron-range rough interface structures

  8. Synthesis, characterization, and monoamine transporter activity of the new psychoactive substance 3',4'-methylenedioxy-4-methylaminorex (MDMAR).

    Science.gov (United States)

    McLaughlin, Gavin; Morris, Noreen; Kavanagh, Pierce V; Power, John D; Twamley, Brendan; O'Brien, John; Talbot, Brian; Dowling, Geraldine; Mahony, Olivia; Brandt, Simon D; Patrick, Julian; Archer, Roland P; Partilla, John S; Baumann, Michael H

    2015-07-01

    The recent occurrence of deaths associated with the psychostimulant cis-4,4'-dimethylaminorex (4,4'-DMAR) in Europe indicated the presence of a newly emerged psychoactive substance on the market. Subsequently, the existence of 3,4-methylenedioxy-4-methylaminorex (MDMAR) has come to the authors' attention and this study describes the synthesis of cis- and trans-MDMAR followed by extensive characterization by chromatographic, spectroscopic, mass spectrometric platforms and crystal structure analysis. MDMAR obtained from an online vendor was subsequently identified as predominantly the cis-isomer (90%). Exposure of the cis-isomer to the mobile phase conditions (acetonitrile/water 1:1 with 0.1% formic acid) employed for high performance liquid chromatography analysis showed an artificially induced conversion to the trans-isomer, which was not observed when characterized by gas chromatography. Monoamine release activities of both MDMAR isomers were compared with the non-selective monoamine releasing agent (+)-3,4-methylenedioxymethamphetamine (MDMA) as a standard reference compound. For additional comparison, both cis- and trans-4,4'-DMAR, were assessed under identical conditions. cis-MDMAR, trans-MDMAR, cis-4,4'-DMAR and trans-4,4'-DMAR were more potent than MDMA in their ability to function as efficacious substrate-type releasers at the dopamine (DAT) and norepinephrine (NET) transporters in rat brain tissue. While cis-4,4'-DMAR, cis-MDMAR and trans-MDMAR were fully efficacious releasing agents at the serotonin transporter (SERT), trans-4,4'-DMAR acted as a fully efficacious uptake blocker. Currently, little information is available about the presence of MDMAR on the market but the high potency of ring-substituted methylaminorex analogues at all three monoamine transporters investigated here might be relevant when assessing the potential for serious side-effects after high dose exposure. Copyright © 2014 John Wiley & Sons, Ltd.

  9. Magnetic ionic liquids: synthesis and characterization

    International Nuclear Information System (INIS)

    Medeiros, Anderson M.M.S.; Parize, Alexandre L.; Oliveira, Vanda M.; Neto, Brenno A.D.; Rubim, Joel C.

    2010-01-01

    The synthesis of magnetic ionic liquids (MILs) based on the stable dispersions of magnetic nanoparticles (MNPs) of γ-Fe 2 O 3 , Fe 3 O 4 , and CoFe 2 O 4 in the ionic liquid 1-n-butyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide (BMI.NTf 2 ) is reported. The MNPs were obtained by the coprecipitation method. The surface of the α-Fe 2 O 3 , Fe 3 O 4 , and CoFe 2 O 4 MNPs with mean sizes (XRD) of 9.3, 12.3, and 11.0 nm, respectively were functionalized by 1-n-butyl-3-(3'-trimethoxypropylsilane)- imidazolium chloride. The non functionalized and functionalized MNPs were further characterized by Raman, FTIR-ATR, and FTNIR spectroscopy and by TGA. The stability of the MILs was assigned to the formation of at least one monolayer of the surface modifier agent that mimics the structure of the BMI.NTf 2 IL. (author)

  10. 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.

  11. Synthesis and characterization of iron-cobalt (FeCo) alloy nanoparticles supported on carbon

    DEFF Research Database (Denmark)

    Koutsopoulos, Sotiris; Barfod, Rasmus; Eriksen, Kim Michael

    2017-01-01

    of the alloy nanoparticles differed depending on the preparation method. When the wet impregnation technique of acetate precursor salts of Fe and Co were used for the synthesis, the size of FeCo alloy nanoparticles was approximately 13 nm. FeCo alloy nanoparticles were characterized by crystallography (XRD...

  12. Synthesis, purification and physico-chemical characterization of the deuterized chloroform

    International Nuclear Information System (INIS)

    Mihaila, Vasile; Chiper, Diana

    1999-01-01

    This work refers to deuterized chloroform synthesis and purification methods. Three preparation methods of deuterized chloroform are presented. In the first method the direct chlorination of methane (CH 4 + 3Cl 2 ) in the presence of light and in an oxygen-free atmosphere results in CHCl 3 + 3HCl. The method's drawback is that the resulting product is impure, being obtained also secondary chlorinated compounds, such as CHCl, CH 2 Cl 2 and CCl 4 . The second method consists in chlorination of acetaldehyde or acetone, in basic catalysis and in halogen excess (α substitution with direct synthesis of trihalogen compound), followed by a haloform reaction (hydrolytic splitting) in the presence of chlorinated lime. This method makes use of decarbolyzing of trichlor acetate acid (as a sodium salt), what results in CL 3 CH + NaHCO 3 . This method is the most suitable for the deuterized chloroform synthesis, since the reaction takes place in absence of other hydrogen atoms (protons) and in deuterized water of 99.87% purity, according to the following reaction: Cl 3 C-COONa → (D 2 O) → Cl 2 CD + NaDCO 3 . Another advantage is that this method avoids the synthesis of secondary products, which could entail additional purifications (distillations, rectification, a.s.o.). The deuterized chloroform is separated from the deuterized sodium bicarbonate aqueous solution by washing with deuterized water, in a liquid to liquid separating funnel. After separation, deuterized chloroform is dried in nitrogen atmosphere. The characterization of the final product is carried out by nuclear magnetic resonance spectrometry. (authors)

  13. Chemical synthesis, characterization and evaluation of antimicrobial properties of Cu and its oxide nanoparticles

    CSIR Research Space (South Africa)

    Motlatle, Abesach M

    2016-10-01

    Full Text Available of Nanoparticle Research, vol. 18: DOI: 10.1007/s11051-016-3614-8 Chemical synthesis, characterization and evaluation of antimicrobial properties of Cu and its oxide nanoparticles Motlatle AM Kesevan Pillai S Scriba MR Ray SS ABSTRACT: Cu...

  14. Low-dimensional compounds containing cyano groups. XVII. Crystal structure, spectroscopic, thermal and magnetic properties of [Cu(bmen)2][Pt(CN)4] (bmen=N,N'-dimethylethylenediamine)

    International Nuclear Information System (INIS)

    Potocnak, Ivan; Vavra, Martin; Cizmar, Erik; Kajnakova, Marcela; Radvakova, Alena; Steinborn, Dirk; Zvyagin, Sergei A.; Wosnitza, Jochen; Feher, Alexander

    2009-01-01

    The synthesis, structural analysis, spectroscopic studies, susceptibility and specific-heat measurements of {[Cu(bmen) 2 ][Pt(CN) 4 ]} n (bmen=N,N'-dimethylethylenediamine) are presented. X-ray crystal-structure analysis revealed that the [Pt(CN) 4 ] 2- building blocks are combined with [Cu(bmen) 2 ] 2+ units to form a chain-like structure along the a axis. The Cu(II) atoms are hexacoordinated by four nitrogen atoms in the equatorial plane belonging to two molecules of bidentate bmen ligands with average Cu-N distance of 2.043(18) A. The axial positions are occupied by two nitrogen atoms from bridging [Pt(CN) 4 ] 2- anions at a longer axial Cu-N distance of 2.490(4) A. The compound is characterized by the presence of a weak antiferromagnetic exchange coupling J/k B =0.6 K. Despite the one-dimensional (1D) character of the structure, the analysis of the magnetic properties and specific heat at very low temperatures shows that [Cu(bmen) 2 ][Pt(CN) 4 ] behaves as a two-dimensional (2D) square-lattice Heisenberg magnet with weak interlayer coupling. - Graphical abstract: The synthesis, structural analysis, spectroscopic studies, susceptibility and specific-heat measurements of {[Cu(bmen) 2 ][Pt(CN) 4 ]} n (bmen=N,N'-dimethylethylenediamine) are presented. X-ray crystal-structure analysis revealed that the [Pt(CN) 4 ] 2- building blocks are combined with [Cu(bmen) 2 ] 2+ units to form a chain-like structure. The compound is characterized by the presence of a weak antiferromagnetic exchange coupling J/k B =-0.6 K. Despite the one-dimensional character of the structure, the analysis of the magnetic properties and specific heat at very low temperatures shows that [Cu(bmen) 2 ][Pt(CN) 4 ] behaves as a two-dimensional square-lattice Heisenberg magnet with weak interlayer coupling

  15. Synthesis of palladium nanoparticles with leaf extract of Chrysophyllum cainito (Star apple) and their applications as efficient catalyst for C-C coupling and reduction reactions

    Science.gov (United States)

    Majumdar, Rakhi; Tantayanon, Supawan; Bag, Braja Gopal

    2017-10-01

    A simple green chemical method for the one-step synthesis of palladium nanoparticles (PdNPs) has been described by reducing palladium (II) chloride with the leaf extract of Chrysophyllum cainito in aqueous medium. The synthesis of the palladium nanoparticles completed within 2-3 h at room temperature, whereas on heat treatment (70-80 °C), the synthesis of colloidal PdNPs completed almost instantly. The stabilized PdNPs have been characterized in detail by spectroscopic, electron microscopic and light scattering measurements. The synthesized PdNPs have been utilized as a green catalyst for C-C coupling reactions under aerobic and phosphine-free conditions in aqueous medium. In addition, the synthesized PdNPs have also been utilized as a catalyst for a very efficient sodium borohydride reduction of 3- and 4-nitrophenols. The synthesized PdNPs can retain their catalytic activity for several months.

  16. Phase-dependent Photometric and Spectroscopic Characterization of the MASTER-Net Optical Transient J212444.87+321738.3: An Oxygen-rich Mira

    Science.gov (United States)

    Ghosh, Supriyo; Mondal, Soumen; Das, Ramkrishna; Banerjee, D. P. K.; Ashok, N. M.; Hambsch, Franz-Josef; Dutta, Somnath

    2018-05-01

    We describe the time-dependent properties of a new spectroscopically confirmed Mira variable, which was discovered in 2013 as MASTER-Net Optical Transient J212444.87+321738.3 toward the Cygnus constellation. We have performed long-term optical/near-infrared (NIR) photometric and spectroscopic observations to characterize the object. From the optical/NIR light curves, we estimate a variability period of 465 ± 30 days. The wavelength-dependent amplitudes of the observed light curves range from ΔI ∼ 4 mag to ΔK ∼ 1.5 mag. The (J ‑ K) color index varies from 1.78 to 2.62 mag over phases. Interestingly, a phase lag of ∼60 days between optical and NIR light curves is also seen, as in other Miras. Our optical/NIR spectra show molecular features of TiO, VO, CO, and strong water bands that are a typical signature of oxygen-rich Mira. We rule out S- or C-type as ZrO bands at 1.03 and 1.06 μm and C2 band at 1.77 μm are absent. We estimate the effective temperature of the object from the Spectral Energy Distribution, and distance and luminosity from standard Period–Luminosity relations. The optical/NIR spectra display time-dependent atomic and molecular features (e.g., TiO, Na I, Ca I, H2O, CO), as commonly observed in Miras. Such spectroscopic observations are useful for studying pulsation variability in Miras.

  17. Synthesis and characterization of new polyamino-cyclodextrin materials.

    Science.gov (United States)

    Lo Meo, Paolo; D'Anna, Francesca; Gruttadauria, Michelangelo; Riela, Serena; Noto, Renato

    2012-01-10

    With the aim of the synthesis of chemically modified cyclodextrins bearing polyamine pendant groups, potentially useful as capping agents for the preparation of nanosized metal systems or as auxiliaries for gene transfection, the reaction between the heptakis-(6-iodo)-(6-deoxy)-β-cyclodextrin and various polyamines has been explored. This synthetic approach allows obtaining materials constituted by mixtures of cyclodextrins, having different degrees of substitution, which were satisfactorily characterized by means of various complementary techniques (ESI-MS, NMR, potentiometric titration). The products obtained were successfully subjected to preliminary tests for their binding abilities towards suitable organic guests and as capping agents for the preparation of stable silver nanoparticles. Copyright © 2011 Elsevier Ltd. All rights reserved.

  18. Nano-ilmenite FeTiO3 : synthesis and characterization

    OpenAIRE

    Raghavender, A. T.; Hoa Hong, Nguyen; Lee, Kyu Joon; Jung, Myung-Hwa; Skoko, Z.; Vasilevskiy, Mikhail; Cerqueira, M. F.; Samantilleke, A. P.

    2013-01-01

    In general, ilmenite FeTiO3 is synthesized by solid-state reaction at very high pressure and high temperature. Synthesis of FeTiO3 is not an easy task as the Fe2+ ions are not stable. Therefore, it is really challenging to prepare this material. In this work nano-ilmenite FeTiO3 was synthesized by the sol-gel method. Structural, optical and magnetic characterizations were performed. The bandgap of FeTiO3 was determined to be 2.8 eV showing FeTiO3 as suitable wide bandgap material for technolo...

  19. Synthesis and characterization of N-t-BOC protected pyrrole-sulfur oligomers and polymers

    NARCIS (Netherlands)

    Groenendaal, L.; Pieterse, K.; Vekemans, J.A.J.M.; Meijer, E.W.

    1997-01-01

    The synthesis and characterization of a new class of pyrrole-sulfur compounds is described. These compounds are designed to be precursors for an organic analogue of poly(sulfur nitride). Poly(N-t-BOC-2.5-pyrrolyl sulfide) was prepared from N-t-BOC-2,5-dibromopyrrole by first lithiating this compound

  20. Rare-earth metal compounds with a novel ligand 2-methoxycinnamylidenepyruvate: A thermal and spectroscopic approach

    Energy Technology Data Exchange (ETDEWEB)

    Carvalho, C.T., E-mail: claudiocarvalho@ufgd.edu.br [Federal University of Grande Dourados, UFGD, 79.804-970 Dourados, MS (Brazil); Oliveira, G.F. [Federal University of Grande Dourados, UFGD, 79.804-970 Dourados, MS (Brazil); Fernandes, J. [Federal University of Grande Dourados, UFGD, 79.804-970 Dourados, MS (Brazil); Federal University of Mato Grosso, UFMT, 78.060-900 Cuiabá, MT (Brazil); Federal University of Goiás, UFG, 74.690-900, Goiânia, GO (Brazil); Institute of Chemistry, UNESP, 14.801-970 Araraquara, SP (Brazil); Siqueira, A.B. [Federal University of Mato Grosso, UFMT, 78.060-900 Cuiabá, MT (Brazil); Ionashiro, E.Y. [Federal University of Goiás, UFG, 74.690-900, Goiânia, GO (Brazil); Ionashiro, M. [Institute of Chemistry, UNESP, 14.801-970 Araraquara, SP (Brazil)

    2016-08-10

    Highlights: • 2-Methoxycinnamylidenepyruvate as a novel ligand for the synthesis of complexes. • Complexes with well-defined structural arrangements. • Thermal decomposition dependent on the nature of the metal ion. • Study by TG/FT-IR and TG/MS of the gaseous products released. • Potential technological application. - Abstract: Compounds of 2-methoxycinnamylidenepyruvate with trivalent lanthanide ions (Tb, Ho, Er, Tm, Yb and Lu) were obtained in solid state and studied mainly in terms of their thermal and spectroscopic properties. The analyses of the characterization were performed by thermogravimetric system coupled to a mass and infrared spectrometer (TG–DTA/MS and TG–DTA/FT-IR), X-ray powder diffractometry, differential scanning calorimetry (DSC), infrared (FT-IR), preliminary study of fluorescence as well as classical technique of titration with EDTA. From these results, it was possible to establish the stoichiometry, thermal behavior, hydration water content, and the gaseous products released in the thermal decomposition steps, and suggest the type of metal-ligand coordination.

  1. Spectroscopic and microscopic characterization of silver nanoparticles synthesized using Justicia adhatoda flower

    Science.gov (United States)

    Singh, Tej; Shekhawat, Dharmender Singh; Jyoti, Kumari

    2018-05-01

    The synthesis of silver nanoparticles (SNPs) by chemical and physical methods produce harmful products which may cause various environmental problems, thus, there is an increasing demand to use ecofriendly methods. Therefore, biosynthesis of SNPs using Justicia adhatoda flower extract is demonstrated in the present study. The biosynthesized SNPs were characterized by UV-visible spectroscopy, Fourier transform-infrared spectroscopy (FTIR), transmission electron microscopy (TEM), selected area electron diffraction (SAED) and atomic force microscopy (AFM) analysis. The result of UV-visible spectroscopy peaked at 417 nm corresponding to the plasmon absorbance of SNPs. The TEM and SAED result reveals the crystalline nature of SNPs. FTIR spectroscopy used to identify the possible biomolecules responsible for the conversion of silver ions to SNPs. The study concluded that Justicia adhatoda flower extract act as an excellent reducing agent and the green synthesized SNPs are safer to the environment.

  2. Characterization of plasmonic effects in thin films and metamaterials using spectroscopic ellipsometry

    NARCIS (Netherlands)

    Oates, T.W.H.; Wormeester, Herbert; Arwin, H.

    2011-01-01

    In this article, spectroscopic ellipsometry studies of plasmon resonances at metal–dielectric interfaces of thin films are reviewed. We show how ellipsometry provides valuable non-invasive amplitude and phase information from which one can determine the effective dielectric functions, and how these

  3. Synthesis, spectroscopic, structural and optical studies of Ru2S3 nanoparticles prepared from single-source molecular precursors

    Science.gov (United States)

    Mbese, Johannes Z.; Ajibade, Peter A.

    2017-09-01

    Homonuclear tris-dithiocarbamato ruthenium(III) complexes, [Ru(S2CNR2)3] were prepared and characterized by spectroscopic techniques and thermogravimetric analyses. The thermogravimetric analyses (TGA) of the ruthenium complexes showed that the complexes decompose to ruthenium(III) sulfide nanoparticles. The ruthenium(III) complexes were dispersed in oleic acid and thermolysed in hexadecylamine to prepared oleic acid/hexadecylamine capped Ru2S3 nanoparticles. FTIR revealed that Ru2S3 nanoparticles are capped through the interaction of the -NH2 group of hexadecylamine HDA adsorbed on the surfaces of nanoparticles and it also showed that oleic acid (OA) is acting as both coordinating stabilizing surfactant and capping agent. EDS spectra revealed that the prepared nanoparticles are mainly composed of Ru and S, confirming the formation of Ru2S3 nanoparticles. Powder XRD confirms that the nanoparticles are in cubic phase. The inner morphology of nanoparticles obtained from transmission electron microscopy (TEM) showed nanoparticles with narrow particle size distributions characterized by an average diameter of 8.45 nm with a standard deviation of 1.6 nm. The optical band gap (Eg) determined from Tauc plot are in the range 3.44-4.18 eV.

  4. Synthesis and characterization of copper nanoparticles by using the exploding wire method

    International Nuclear Information System (INIS)

    Das, Rashmita; Das, Basanta Kumar; Shyam, Anurag

    2012-01-01

    During the past few years, the synthesis of copper nanoparticles has attracted much attention because of their huge potential for replacing the expensive nano silver inks utilized in conductive printing. This opens a new possibility in printed electronics. Copper-based inkjet inks can be used to form various devices such as solar cells, RF identification tags and electroluminescence devices. This paper describes controlled synthesis of pure copper nanoparticles, mainly by using the exploding wire method. A wire of 0.26 mm in diameter was exploded in a nitrogen environment. The sample was characterized by using X-ray diffraction (XRD) and atomic force microscopy (AFM). XRD revealed the presence of pure copper and AFM revealed the presence of nanoparticles with an average size of 55 nm.

  5. 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.

  6. Synthesis and characterization of a cerebral radiotracer

    International Nuclear Information System (INIS)

    Ben hamouda, Salem

    2010-01-01

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

  7. Application of spectroscopic techniques for the study of paper documents: A survey

    International Nuclear Information System (INIS)

    Manso, M.; Carvalho, M.L.

    2009-01-01

    For many centuries paper was the main material for recording cultural achievements all over the world. Paper is mostly made from cellulose with small amounts of organic and inorganic additives, which allow its identification and characterization and may also contribute to its degradation. Prior to 1850, paper was made entirely from rags, using hemp, flax and cotton fibres. After this period, due to the enormous increase in demand, wood pulp began to be commonly used as raw material, resulting in rapid degradation of paper. Spectroscopic techniques represent one of the most powerful tools to investigate the constituents of paper documents in order to establish its identification and its state of degradation. This review describes the application of selected spectroscopic techniques used for paper characterization and conservation. The spectroscopic techniques that have been used and will be reviewed include: Fourier-Transform Infrared spectroscopy, Raman spectroscopy, Nuclear Magnetic Resonance spectroscopy, X-Ray spectroscopy, Laser-based Spectroscopy, Inductively Coupled Mass Spectroscopy, Laser ablation, Atomic Absorption Spectroscopy and X-Ray Photoelectron Spectroscopy.

  8. Ruthenium(III) Complexes of Heterocyclic Tridentate (ONN) Schiff Base: Synthesis, Characterization and its Biological Properties as an Antiradical and Antiproliferative Agent

    Science.gov (United States)

    Ejidike, Ikechukwu P.; Ajibade, Peter A.

    2016-01-01

    The current work reports the synthesis, spectroscopic studies, antiradical and antiproliferative properties of four ruthenium(III) complexes of heterocyclic tridentate Schiff base bearing a simple 2′,4′-dihydroxyacetophenone functionality and ethylenediamine as the bridging ligand with RCHO moiety. The reaction of the tridentate ligands with RuCl3·3H2O lead to the formation of neutral complexes of the type [Ru(L)Cl2(H2O)] (where L = tridentate NNO ligands). The compounds were characterized by elemental analysis, UV-vis, conductivity measurements, FTIR spectroscopy and confirmed the proposed octahedral geometry around the Ru ion. The Ru(III) compounds showed antiradical potentials against 2,2-Diphenyl-1-Picrylhydrazyl (DPPH) and 2,2′-azinobis-(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS) radicals, with DPPH scavenging capability in the order: [(PAEBOD)RuCl2] > [(BZEBOD)RuCl2] > [(MOABOD)RuCl2] > [Vit. C] > [rutin] > [(METBOD)RuCl2], and ABTS radical in the order: [(PAEBOD)RuCl2] < [(MOABOD)RuCl2] < [(BZEBOD)RuCl2] < [(METBOD)RuCl2]. Furthermore, in vitro anti-proliferative activity was investigated against three human cancer cell lines: renal cancer cell (TK-10), melanoma cancer cell (UACC-62) and breast cancer cell (MCF-7) by SRB assay. PMID:26742030

  9. Ruthenium(III Complexes of Heterocyclic Tridentate (ONN Schiff Base: Synthesis, Characterization and its Biological Properties as an Antiradical and Antiproliferative Agent

    Directory of Open Access Journals (Sweden)

    Ikechukwu P. Ejidike

    2016-01-01

    Full Text Available The current work reports the synthesis, spectroscopic studies, antiradical and antiproliferative properties of four ruthenium(III complexes of heterocyclic tridentate Schiff base bearing a simple 2′,4′-dihydroxyacetophenone functionality and ethylenediamine as the bridging ligand with RCHO moiety. The reaction of the tridentate ligands with RuCl3·3H2O lead to the formation of neutral complexes of the type [Ru(LCl2(H2O] (where L = tridentate NNO ligands. The compounds were characterized by elemental analysis, UV-vis, conductivity measurements, FTIR spectroscopy and confirmed the proposed octahedral geometry around the Ru ion. The Ru(III compounds showed antiradical potentials against 2,2-Diphenyl-1-Picrylhydrazyl (DPPH and 2,2′-azinobis-(3-ethylbenzothiazoline-6-sulfonic acid (ABTS radicals, with DPPH scavenging capability in the order: [(PAEBODRuCl2] > [(BZEBODRuCl2] > [(MOABODRuCl2] > [Vit. C] > [rutin] > [(METBODRuCl2], and ABTS radical in the order: [(PAEBODRuCl2] < [(MOABODRuCl2] < [(BZEBODRuCl2] < [(METBODRuCl2]. Furthermore, in vitro anti-proliferative activity was investigated against three human cancer cell lines: renal cancer cell (TK-10, melanoma cancer cell (UACC-62 and breast cancer cell (MCF-7 by SRB assay.

  10. Spectroscopic characterization, antimicrobial activity, DFT computation and docking studies of sulfonamide Schiff bases

    Science.gov (United States)

    Mondal, Sudipa; Mandal, Santi M.; Mondal, Tapan Kumar; Sinha, Chittaranjan

    2017-01-01

    Schiff bases synthesised from the condensation of 2-(hydroxy)naphthaldehyde and sulfonamides (sufathiazole (STZ), sulfapyridine (SPY), sulfadiazine (SDZ), sulfamerazine (SMZ) and sulfaguanidine (SGN)) are characterized by different spectroscopic data (FTIR, UV-Vis, Mass, NMR) and two of them, (E)-4-(((2-hydroxynaphthalen-1-yl)methylene)amino)-N-(thiazol-2-yl)benzenesulfonamide (1a) and (E)-N-(diaminomethylene)-4-(((2-hydroxynaphthalen-1-yl)methylene)amino)benzenesulfonamide (1e) have been confirmed by single crystal X-ray structure determination. Antimicrobial activities of the Schiff bases have been evaluated against certified and resistant Gram positive (Staphylococcus aureus, Enterococcus facelis) and Gram negative (Streptococcus pyogenes, Salmonella typhi, Shigella dysenteriae, Shigella flexneri, Klebsiella pneumonia) pathogens. Performance of Schiff base against the resistant pathogens are better than standard stain and MIC data lie 32-128 μg/ml while parent sulfonamides are effectively inactive (MIC >512 μg/ml). The DFT optimized structures of the Schiff bases have been used to accomplish molecular docking studies with DHPS (dihydropteroate synthase) protein structure (downloaded from Protein Data Bank) to establish the most preferred mode of interaction. ADMET filtration, Cytotoxicity (MTT assay) and haemolysis assay have been examined for evaluation of druglike character.

  11. Spectroscopic Characterization of Intermolecular Interaction of Amyloid β Promoted on GM1 Micelles

    Directory of Open Access Journals (Sweden)

    Maho Yagi-Utsumi

    2011-01-01

    Full Text Available Clusters of GM1 gangliosides act as platforms for conformational transition of monomeric, unstructured amyloid β (Aβ to its toxic β-structured aggregates. We have previously shown that Aβ(1–40 accommodated on the hydrophobic/hydrophilic interface of lyso-GM1 or GM1 micelles assumes α-helical structures under ganglioside-excess conditions. For better understanding of the mechanisms underlying the α-to-β conformational transition of Aβ on GM1 clusters, we performed spectroscopic characterization of Aβ(1–40 titrated with GM1. It was revealed that the thioflavin T- (ThT- reactive β-structure is more populated in Aβ(1–40 under conditions where the Aβ(1–40 density on GM1 micelles is high. Under this circumstance, the C-terminal hydrophobic anchor Val39-Val40 shows two distinct conformational states that are reactive with ThT, while such Aβ species were not generated by smaller lyso-GM1 micelles. These findings suggest that GM1 clusters promote specific Aβ-Aβ interactions through their C-termini coupled with formation of the ThT-reactive β-structure depending on sizes and curvatures of the clusters.

  12. Opto-nanomechanical spectroscopic material characterization

    Science.gov (United States)

    Tetard, L.; Passian, A.; Farahi, R. H.; Thundat, T.; Davison, B. H.

    2015-10-01

    The non-destructive, simultaneous chemical and physical characterization of materials at the nanoscale is an essential and highly sought-after capability. However, a combination of limitations imposed by Abbe diffraction, diffuse scattering, unknown subsurface, electromagnetic fluctuations and Brownian noise, for example, have made achieving this goal challenging. Here, we report a hybrid approach for nanoscale material characterization based on generalized nanomechanical force microscopy in conjunction with infrared photoacoustic spectroscopy. As an application, we tackle the outstanding problem of spatially and spectrally resolving plant cell walls. Nanoscale characterization of plant cell walls and the effect of complex phenotype treatments on biomass are challenging but necessary in the search for sustainable and renewable bioenergy. We present results that reveal both the morphological and compositional substructures of the cell walls. The measured biomolecular traits are in agreement with the lower-resolution chemical maps obtained with infrared and confocal Raman micro-spectroscopies of the same samples. These results should prove relevant in other fields such as cancer research, nanotoxicity, and energy storage and production, where morphological, chemical and subsurface studies of nanocomposites, nanoparticle uptake by cells and nanoscale quality control are in demand.

  13. PAMAM dendrimer-coated iron oxide nanoparticles: synthesis and characterization of different generations

    International Nuclear Information System (INIS)

    Khodadust, Rouhollah; Unsoy, Gozde; Yalcın, Serap; Gunduz, Gungor; Gunduz, Ufuk

    2013-01-01

    This study focuses on the synthesis and characterization of different generations (G 0 –G 7 ) of polyamidoamine (PAMAM) dendrimer-coated magnetic nanoparticles (DcMNPs). In this study, superparamagnetic iron oxide nanoparticles were synthesized by co-precipitation method. The synthesized nanoparticles were modified with aminopropyltrimethoxysilane for dendrimer coating. Aminosilane-modified MNPs were coated with PAMAM dendrimer. The characterization of synthesized nanoparticles was performed by X-ray diffraction, X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM), dynamic light scattering, and vibrating sample magnetometry (VSM) analyses. TEM images demonstrated that the DcMNPs have monodisperse size distribution with an average particle diameter of 16 ± 5 nm. DcMNPs were found to be superparamagnetic through VSM analysis. The synthesis, aminosilane modification, and dendrimer coating of iron oxide nanoparticles were validated by FTIR and XPS analyses. Cellular internalization of nanoparticles was studied by inverted light scattering microscopy, and cytotoxicity was determined by XTT analysis. Results demonstrated that the synthesized DcMNPs, with their functional groups, symmetry perfection, size distribution, improved magnetic properties, and nontoxic characteristics could be suitable nanocarriers for targeted cancer therapy upon loading with various anticancer agents.

  14. Bis(pentamethylene)urea complexes of the lanthanide nitrates: synthesis, characterization, properties

    International Nuclear Information System (INIS)

    Souza, H.K.S. de; Pedrosa, A.M.G.; Marinho, E.P.M.; Batista, M.K.S.; Melo, D.M.A.; Zinner, K.; Zinner, L.B.; Zukerman-Schpector, J.; Vicentini, G.

    2003-01-01

    Lanthanide nitrate complexes of bis(pentamethylene)urea (BPMU) with general formula Ln(NO 3 ) 3 3BPMU, where Ln: La, Nd, Sm, Eu, Ho and Er have been prepared and characterized based on CHN elemental analyses, lanthanide titration with EDTA, molar conductivity, spectroscopic data and thermal studies. The infrared spectra show that ligands (BPMU) are bonded through the carbonyl oxygen, nitrate counter-ions are bidentate linked to the central ions. The structure of the neodymium complex was determined. The crystal is monoclinic, P2 1/c ,Z=4, with the following parameters: a=10.148(1) A, b=21.879(2), c=19.154(2) A, β=104.11(1) deg., V=4124.3(7) A 3 . The polyhedron is a distorted tricapped trigonal prism, coordination number nine

  15. Synthesis and Characterization of Nano Scale YBCO

    International Nuclear Information System (INIS)

    Sukirman, E.; Wisnu AA; Yustinus P; Sahidin W, D.; Rina M, Th.

    2009-01-01

    Synthesis and characterization of the nano scale YBCO superconductor have been performed. The nano scale superconductor was synthesized from YBCO system (YBa 2 Cu 3 O 7-X ). Raw materials, namely Y 2 O 3 , BaCO 3 , and Cu°, were balanced and mixed with ethanol using magnetic steering as a churn in a beaker glass. Then, the precursor was calcined at T k = 900°C for 5 hours and repeated it until three times. The resulting precursor was ground by using High Energy Milling (HEM) for t = 0, 30, 50, 70, and 90 hour and hereinafter precursors are successively referred as YKM-00, YKM-30, YKM-50, YKM-70, and YKM-90. The resulting powders phase were characterized by means of x-ray diffraction technique using the Rietveld analysis method. Precursor of YKM-90 was pressed into pellets, and then sintered at various temperatures and periods. The sample phase was then characterized by using the Rietveld analysis method based on the x-ray diffraction data. The crystallites size were calculated using Scherrer formula. Results of analysis indicate that by minimizing crystallites size, period of sinter can be shortened from 10 to 1 hour, resulting crystallite size of D = 925 Å, critical current density of J c = 4 A / cm 2 , and can be grown of about 15 weight % of 211-phase in a matrix of 123-phase. The decrease of crystallite size will generate a change in physical properties dramatically, if the crystallite size of the material, D is smaller or equal to the coherence length of 10 Å. (author)

  16. Synthesis and characterization of ruthenium-decorated nanoporous platinum materials

    International Nuclear Information System (INIS)

    Peng Xinsheng; Koczkur, Kallum; Chen, Aicheng

    2007-01-01

    We report on the synthesis of novel three-dimensional nanoporous Pt-Ru bimetallic networks by decorating nanoporous Pt networks with Ru using a hydrothermally assisted precipitating process. Scanning electron microscopy (SEM) and energy dispersive x-ray spectroscopy (EDS) were used to characterize the morphology and the composition of the nanoporous Pt-Ru networks formed. X-ray diffraction analysis confirmed that, after protected annealing treatment, Pt-Ru bimetallic material was formed. The electrocatalytic activity of the synthesized nanoporous Pt-Ru networks was characterized using electrochemical oxidation of methanol as a probe. The electrocatalytic activity of the nanoporous Pt networks significantly increases with the increments of decorated Ru and reaches the highest value with 41% of Ru. The peak current of methanol oxidation on the nanoporous Pt-Ru(41%) bimetallic networks is over 180% higher than that on the nanoporous Pt networks without Ru decoration. This is very desirable for fuel cell development and electrochemical sensor design

  17. Synthesis and characterization of cobalt sulfide nanoparticles by sonochemical method

    Science.gov (United States)

    Muradov, Mustafa B.; Balayeva, Ofeliya O.; Azizov, Abdulsaid A.; Maharramov, Abel M.; Qahramanli, Lala R.; Eyvazova, Goncha M.; Aghamaliyev, Zohrab A.

    2018-03-01

    Convenient and environmentally friendly synthesis of Co9S8/PVA, CoxSy/EG and CoxSy/3-MPA nanocomposites were carried out in the presence of ultrasonic irradiation by the liquid phase synthesis of the sonochemical method. For the synthesis, cobalt acetate tetrahydrate [Co(CH3COO)2·4H2O] and sodium sulfide (Na2S·9H2O) were used as a cobalt and sulfur precursor, respectively. Polyvinyl alcohol (PVA), ethylene glycol (EG) and 3-mercaptopropionic acid (3-MPA) were used as a capping agent and surfactant. The structural, optical properties and morphology of nanocomposites were characterized using X-ray diffractometer (XRD), Ultraviolet/Visible Spectroscopy (UV-Vis), Fourier-transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM). The optical band gap of Co9S8/PVA is 1.81 eV and for CoxSy/EG is 2.42 eV, where the direct band gap of bulk cobalt sulfide is (0.78-0.9 eV). The wide band gap indicates that synthesised nanocomposites can be used in the fabrication of optical and photonic devices. The growth mechanisms of the Co9S8, CoS2 and Co3S4 nanoparticles were discussed by the reactions. The effects of sonication time and annealing temperature on the properties of the nanoparticles have been studied in detail.

  18. Synthesis and Physicochemical Characterization of Mesoporous SiO2 Nanoparticles

    Directory of Open Access Journals (Sweden)

    Dharani Das

    2014-01-01

    Full Text Available There exists a knowledge gap in understanding potential toxicity of mesoporous silica nanoparticles. A critical step in assessing toxicity of these particles is to have a wide size range with different chemistries and physicochemical properties. There are several challenges when synthesizing mesoporous silica nanoparticles over a wide range of sizes including (1 nonuniform synthesis protocols using the same starting materials, (2 the low material yield in a single batch synthesis (especially for particles below 60–70 nm, and (3 morphological instability during surfactant removal process and surface modifications. In this study, we synthesized a library of mesoporous silica nanoparticles with approximate particle sizes of 25, 70, 100, 170, and 600 nm. Surfaces of the silica nanoparticles were modified with hydrophilic-CH2–(CH22–COOH and relatively hydrophobic-CH2–(CH210–COOH functional groups. All silica nanoparticles were analysed for morphology, surface functionality, surface area/pore volume, surface organic content, and dispersion characteristics in liquid media. Our analysis revealed the synthesis of a spectrum of monodisperse bare and surface modified mesoporous silica nanoparticles with a narrow particle size distribution and devoid of cocontaminants critical for toxicity studies. Complete physicochemical characterization of these synthetic mesoporous silica nanoparticles will permit systematic toxicology studies for investigation of structure-activity relationships.

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

    Science.gov (United States)

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

    2016-06-01

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

  20. Synthesis and Characterization of C-Cinnamal Calix [4] Resorsinarena from Cinnamon Oil Waste West Sumatra

    Science.gov (United States)

    Etika, S. B.; Nasra, E.; Rilaztika, I.

    2018-04-01

    Synthesis and characterization of compound C-Cinnamal Calix [4] Resorsinarena (CCCR) of cinnamon oil waste have been done. This study was aimed to synthesis and characterize C-Cinnamal Calix [4] Resorsinarena from cinnamaldehyde violated cinnamon oil waste. C-Cinnamal Calix [4] Resorsinarena was synthesized by electrophilic substitution reaction of cinnamaldehyde isolated by the acid and resorcinol at 77oC temperature for 2 hour. The data analysis spectrum UV-VIS and FT-IR showed that the compound isolated cinnamaldehyde same as pure cinnamaldehyde compound. The characterization of C-Cinnamal Calix [4] Resorsinarena in the form of reddish-colored solids with melting point 3580C by using UV-VIS showed the presence of double bond, FT-IR showed the absorption at the wave number 3323,94 cm-1 indicating the ‑OH group, the wave number 1610,94 cm-1 showed the vibration C=C, the strong region absorption of 1500,86 cm-1 indicating the presence of an aromatic ring, the at 1442,88 cm-1 wave number indicating the presence of CH3.

  1. Synthesis and characterization of nanocomposites ZnO / polypyrrole for anti corrosive application

    International Nuclear Information System (INIS)

    Valenca, D.P.; Bouchonneau, N.; Vieira, M.R.S.; Alves, K.G.B.; Melo, C.P. de; Urtiga Filho, S.L.

    2014-01-01

    Nanoparticles of metal oxides and conductive polymers have been investigated as alternative additives in corrosion protection of oxidizable metals. In this hybrid nanocomposites work Polypyrrole-ZnO were synthesized and characterized as a potential application as industrial paint anti corrosive additive. The different steps of the synthesis and characterization of nanocomposites are described. The nanocomposites were obtained from the emulsion polymerization of aqueous solutions of pyrrole and sodium dodecyl sulfate containing ZnO nanoparticles dispersed in the mass. The nanoparticles were characterized by scanning electron microscopy and transmission, dynamic light scattering, diffraction of X-rays and techniques of infrared spectroscopy. From the characterization techniques, it was possible to determine the average size of nanoparticles of ZnO and ZnO-Polypyrrole. The peaks in the diffraction pattern of X-rays observed in the nanocomposite were the same as in ZnO, confirming the presence of ZnO in the composite. (author)

  2. Synthesis, Characterization, and Ultrafast Dynamics of Metal, Metal Oxide, and Semiconductor Nanomaterials

    OpenAIRE

    Wheeler, Damon Andreas

    2013-01-01

    SYNTHESIS, CHARACTERIZATION, AND ULTRAFAST DYNAMICS OF METAL, METAL OXIDE, AND SEMICONDUCTOR NANOMATERIALSABSTRACTThe optical properties of each of the three main classes of inorganic nanomaterials, metals, metal oxides, and semiconductors differ greatly due to the intrinsically different nature of the materials. These optical properties are among the most fascinating and useful aspects of nanomaterials with applications spanning cancer treatment, sensors, lasers, and solar cells. One techn...

  3. Infrared spectroscopic characterization of monocytic microvesicles (microparticles) released upon lipopolysaccharide stimulation.

    Science.gov (United States)

    Lee, Joonsup; Wen, Beryl; Carter, Elizabeth A; Combes, Valery; Grau, Georges E R; Lay, Peter A

    2017-07-01

    Microvesicles (MVs) are involved in cell-cell interactions, including disease pathogenesis. Nondestructive Fourier-transform infrared (FTIR) spectra from MVs were assessed as a technique to provide new biochemical insights into a LPS-induced monocyte model of septic shock. FTIR spectroscopy provided a quick method to investigate relative differences in biomolecular content of different MV populations that was complementary to traditional semiquantitative omics approaches, with which it is difficult to provide information on relative changes between classes (proteins, lipids, nucleic acids, carbohydrates) or protein conformations. Time-dependent changes were detected in biomolecular contents of MVs and in the monocytes from which they were released. Differences in phosphatidylcholine and phosphatidylserine contents were observed in MVs released under stimulation, and higher relative concentrations of RNA and α-helical structured proteins were present in stimulated MVs compared with MVs from resting cells. FTIR spectra of stimulated monocytes displayed changes that were consistent with those observed in the corresponding MVs they released. LPS-stimulated monocytes had reduced concentrations of nucleic acids, α-helical structured proteins, and phosphatidylcholine compared with resting monocytes but had an increase in total lipids. FTIR spectra of MV biomolecular content will be important in shedding new light on the mechanisms of MVs and the different roles they play in physiology and disease pathogenesis.-Lee, J., Wen, B., Carter, E. A., Combes, V., Grau, G. E. R., Lay, P. A. Infrared spectroscopic characterization of monocytic microvesicles (microparticles) released upon lipopolysaccharide stimulation. © FASEB.

  4. Self-Assembled Structures of PMAA-PMMA Block Copolymers : Synthesis, Characterization, and Self-Consistent Field Computations

    NARCIS (Netherlands)

    Li, Feng; Schellekens, Mike; de Bont, Jens; Peters, Ron; Overbeek, Ad; Leermakers, Frans A. M.; Tuinier, Remco

    2015-01-01

    Block copolymers composed of methacrylic acid (MAA) and methyl methacrylate (MMA) blocks are interesting candidates for replacing surfactants in emulsion polymerization methods. Here the synthesis and experimental characterization of well-defined PMAA-PMMA block copolymers made via RAFT

  5. Self-assembled structures of PMAA-PMMA block copolymers: Synthesis, characterization, and self-consistent field computations

    NARCIS (Netherlands)

    Li, F.; Schellekens, J.; Bont, de J.A.M.; Peters, R.; Overbeek, A.; Leermakers, F.A.M.; Tuinier, R.

    2015-01-01

    Block copolymers composed of methacrylic acid (MAA) and methyl methacrylate (MMA) blocks are interesting candidates for replacing surfactants in emulsion polymerization methods. Here the synthesis and experimental characterization of well-defined PMAA–PMMA block copolymers made via RAFT

  6. Synthesis, characterization and optimization of poly(p-phenylenediamine)-based organoclay composite for Cr(VI) remediation

    CSIR Research Space (South Africa)

    Mdlalose, L

    2017-04-01

    Full Text Available of these materials for environmental remediation. We report here the synthesis, characterization and application of a poly(para-phenylenediamine) (poly-pPD) organoclay-based composite for removal of Cr(VI) complexes from wastewater. Adsorption capacity...

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

    African Journals Online (AJOL)

    ADOWIE PERE

    The results of the physical and spectroscopic data confirmed that the ligands are chelating agents. .... quiet out of the way location for 21 days for the evaporation of the solvent. ..... El-Ghamry, M.A., Saleh, A.A., Khalil, S.M.E.,. Mohammed, A.A. ...

  8. Synthesis, X-ray diffraction method, spectroscopic characterization (FT-IR, 1H and 13C NMR), antimicrobial activity, Hirshfeld surface analysis and DFT computations of novel sulfonamide derivatives

    Science.gov (United States)

    Demircioğlu, Zeynep; Özdemir, Fethi Ahmet; Dayan, Osman; Şerbetçi, Zafer; Özdemir, Namık

    2018-06-01

    Synthesized compounds of N-(2-aminophenyl)benzenesulfonamide 1 and (Z)-N-(2-((2-nitrobenzylidene)amino)phenyl)benzenesulfonamide 2 were characterized by antimicrobial activity, FT-IR, 1H and 13C NMR. Two new Schiff base ligands containing aromatic sulfonamide fragment of (Z)-N-(2-((3-nitrobenzylidene)amino)phenyl)benzenesulfonamide 3 and (Z)-N-(2-((4-nitrobenzylidene)amino)phenyl)benzenesulfonamide 4 were synthesized and investigated by spectroscopic techniques including 1H and 13C NMR, FT-IR, single crystal X-ray diffraction, Hirshfeld surface, theoretical method analyses and by antimicrobial activity. The molecular geometry obtained from the X-ray structure determination was optimized Density Functional Theory (DFT/B3LYP) method with the 6-311++G(d,p) basis set in ground state. From the optimized geometry of the molecules of 3 and 4, the geometric parameters, vibrational wavenumbers and chemical shifts were computed. The optimized geometry results, which were well represented the X-ray data, were shown that the chosen of DFT/B3LYP 6-311G++(d,p) was a successful choice. After a successful optimization, frontier molecular orbitals, chemical activity, non-linear optical properties (NLO), molecular electrostatic mep (MEP), Mulliken population method, natural population analysis (NPA) and natural bond orbital analysis (NBO), which cannot be obtained experimentally, were calculated and investigated.

  9. 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.

  10. Isolation, characterization, spectroscopic properties and quantum chemical computations of an important phytoalexin resveratrol as antioxidant component from Vitis labrusca L. and their chemical compositions

    Science.gov (United States)

    Güder, Aytaç; Korkmaz, Halil; Gökce, Halil; Alpaslan, Yelda Bingöl; Alpaslan, Gökhan

    2014-12-01

    In this study, isolation and characterization of trans-resveratrol (RES) as an antioxidant compound were carried out from VLE, VLG and VLS. Furthermore, antioxidant activities were evaluated by using six different methods. Finally, total phenolic, flavonoid, ascorbic acid, anthocyanin, lycopene, β-carotene and vitamin E contents were carried out. In addition, the FT-IR, 13C and 1H NMR chemical shifts and UV-vis. spectra of trans-resveratrol were experimentally recorded. Quantum chemical computations such as the molecular geometry, vibrational frequencies, UV-vis. spectroscopic parameters, HOMOs-LUMOs energies, molecular electrostatic potential (MEP), natural bond orbitals (NBO) and nonlinear optics (NLO) properties of title molecule have been calculated by using DFT/B3PW91 method with 6-311++G(d,p) basis set in ground state for the first time. The obtained results show that the calculated spectroscopic data are in a good agreement with experimental data.

  11. Green Synthesis and Characterizations of Flower Shaped CuO Nanoparticles for Biodiesel Application

    Directory of Open Access Journals (Sweden)

    Rintu Varghese

    2017-03-01

    Full Text Available Nanomaterials are primary candidates to play a key role in energy future. In this work, plant-mediated green synthesis of CuO nanoparticles was studied. The CuO nanoparticles were used as the catalysts for the production of biodiesel from coconut oil. An aqueous extract of Centella Asiatica leaves was used as a bio-reducing agent for the synthesis of CuO nanoparticles. This biocatalyst was characterized by using different techniques (FTIR, UV-Vis spectroscopy, XRD, FESEM with EDX which were confirmed the formation of CuO nanoparticles. Further, the presences of FAME (Fatty Acid Methyl Ester groups at the produced biodiesel were confirmed using both the GC-MS and FTIR analysis. From this work, it has been concluded that the plant extract mediated synthesis of CuO nanoparticles is quite simple, cost-effective and environmentally friendly. The produced biodiesel from coconut oil is considered to be a potential source for alternative conventional fuel.

  12. solvent-free synthesis of azomethines, spectral correlations

    African Journals Online (AJOL)

    B. S. Chandravanshi

    attention of organic and medicinal chemists [2, 3]. ... Spectroscopic data is very useful for studying the ground state equilibrium of ... determines the structure of unsaturated systems, such as E- or Z, s-cis and .... The IR and NMR spectra of selective ... The proposed mechanism for the synthesis of E- imines in presence of ...

  13. Application of imaging spectroscopic reflectometry for characterization of gold reduction from organometallic compound by means of plasma jet technology

    Energy Technology Data Exchange (ETDEWEB)

    Vodák, Jiří, E-mail: jiri.vodak@yahoo.com [Institute of Physical Engineering, Faculty of Mechanical Engineering, Brno University of Technology, Technická 2, 616 69 Brno (Czech Republic); Nečas, David [RG Plasma Technologies, CEITEC Masaryk University, Kamenice 5, 625 00 Brno (Czech Republic); Pavliňák, David [Department of Physical Electronics, Masaryk University, Kotlářská 2, 611 37 Brno (Czech Republic); Macak, Jan M [Center of Materials and Nanotechnologies, Faculty of Chemical Technology, University of Pardubice, Nám. Čs. Legií 565, 530 02 Pardubice (Czech Republic); Řičica, Tomáš; Jambor, Roman [Department of General and Inorganic Chemistry, Faculty of Chemical Technology, University of Pardubice, Studentská 573, 532 10 Pardubice (Czech Republic); Ohlídal, Miloslav [Institute of Physical Engineering, Faculty of Mechanical Engineering, Brno University of Technology, Technická 2, 616 69 Brno (Czech Republic); Institute of Physics, Faculty of Mining and Geology, VŠB – Technical University of Ostrava (Czech Republic)

    2017-02-28

    Highlights: • Metallic gold is reduced from an organometallic compound layer using a plasma jet. • Imaging spectroscopic reflectometry is used to locate areas with metallic gold. • The results are completed with XPS and optical microscopy observations. - Abstract: This work presents a new application of imaging spectroscopic reflectometry to determine a distribution of metallic gold in a layer of an organogold precursor which was treated by a plasma jet. Gold layers were prepared by spin coating from a solution of the precursor containing a small amount of polyvinylpyrrolidone on a microscopy glass, then they were vacuum dried. A difference between reflectivity of metallic gold and the precursor was utilized by imaging spectroscopic reflectometry to create a map of metallic gold distribution using a newly developed model of the studied sample. The basic principle of the imaging spectroscopic reflectometry is also shown together with the data acquisition principles. XPS measurements and microscopy observations were made to complete the imaging spectroscopic reflectometry results. It is proved that the imaging spectroscopic reflectometry represents a new method for quantitative evaluation of local reduction of metallic components from metaloorganic compounds.

  14. Synthesis and characterization of "1"3C_3-tristearin

    International Nuclear Information System (INIS)

    Wu Hangyu; Lin Lin; Li Lei; Chen Dazhou

    2011-01-01

    A highly efficient synthesis of "1"3C_3 labeled triglycerides of stearic acids from "1"3C_3-glycerol and stearic acids, by immobilized lipase-catalyzed in solvent-free medium was described. The structure of the product were characterized by fourier transform infrared spectrum (FT-IR), nuclear magnetic resonance (NMR), mass spectra (MS). The results showed that triglycerides of stearic acids contained three "1"3C atoms. The isotope abundance of "1"3C_3-tristearin was more than 99% and the yield was 80% of "1"3C_3-tristearin through calculation. Chemical purity (> 98%) was obtained by differential scanning calorimetry (DSC). (authors)

  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. A facile soft template synthesis and characterization of PbHAsO4 nanocrystals

    International Nuclear Information System (INIS)

    Xiu Zhiliang; Lue Mengkai; Zhou Guangjun; Gu Feng; Zhang Haiping; Xu Dong; Yuan Duorong

    2004-01-01

    Monoclinic lead hydrogen arsenate (LHA) nanocrystals with different crystallization morphologies and crystallite sizes were prepared successfully by a soft template synthesis method in the presence of sodium dodecylbenzenesulfonate (SDBS) or polyvinylpyrrolidone (PVP). The products were characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The possible mechanism of SDBS and PVP in the experiment was briefly illustrated

  17. Electrochemical and Spectroscopic Characterization of Aluminium(III-para-methyl-meso-tetraphenylporphyrin Complexes Containing Substituted Salicylates as Axial Ligands

    Directory of Open Access Journals (Sweden)

    Gauri D. Bajju

    2013-01-01

    Full Text Available A series of aluminium(III-p-methyl-meso-tetraphenylporphyrin (p-CH3TPP-Al(III containing axially coordinated salicylate anion [p-CH3TPP-Al-X], where X = salicylate (SA, 4-chlorosalicylate (4-CSA, 5-chlorosalicylate (5-CSA, 5-flourosalicylate (5-FSA, 4-aminosalicylate (4-ASA, 5-aminosalicylate (5-ASA, 5-nitrosalicylate (5-NSA, and 5-sulfosalicylate (5-SSA, have been synthesized and characterized by various spectroscopic techniques including ultraviolet-visible (UV-vis, infrared (IR spectroscopy, proton nuclear magnetic resonance (1H NMR spectroscopy, 13C NMR, and elemental analysis. A detailed study of electrochemistry of all the synthesized compounds has been done to compare their oxidation and reduction mechanisms and to explain the effect of axial coordination on their redox properties.

  18. Green Synthesis and Antibacterial Effect of Silver Nanoparticles Using Vitex Negundo L.

    Directory of Open Access Journals (Sweden)

    Fatima Abu Bakar

    2011-08-01

    Full Text Available Different biological methods are gaining recognition for the production of silver nanoparticles (Ag-NPs due to their multiple applications. One of the most important applications of Ag-NPs is their use as an anti-bacterial agent. The use of plants in the synthesis of nanoparticles emerges as a cost effective and eco-friendly approach. In this study the biosynthesis of silver nanoparticles using Vitex negundo L. extract and its antimicrobial properties has been reported. The resulting silver particles are characterized using transmission electron microscopy (TEM, X-ray diffraction (XRD and UV–Visible (UV-Vis spectroscopic techniques. The TEM study showed the formation of silver nanoparticles in the 10–30 nm range and average 18.2 nm in size. The XRD study showed that the particles are crystalline in nature, with a face centered cubic (fcc structure. The silver nanoparticles showed the antimicrobial activity against Gram positive and Gram negative bacteria. Vitex negundo L. was found to display strong potential for the synthesis of silver nanoparticles as antimicrobial agents by rapid reduction of silver ions (Ag+ to Ag0.

  19. Investigations on synthesis, coordination behaviour and actinide recovery of unexplored phosphine oxides

    International Nuclear Information System (INIS)

    Veerashekhar Goud, E.; Pavankumar, B.B.; Das, Dhrubajyothi

    2016-01-01

    The search for the development of an optimum extractant for effective separation of a particular metal from a mixture is an active field of research in both chemistry and chemical engineering. These extractants find extensive application in extractive metallurgy and in nuclear fuel cycle (for the separation of actinides from other fission products). In the case of the latter, solvent extraction and ion exchange are two widely employed separation techniques. In this connection, the present paper reports synthesis and structural characterization of various new phosphine oxide derivatives. The coordination behavior of these ligands is studied with some selected lanthanides and actinides shows the proposed structures of La(III) and Th(IV) metal complexes. The purity and structural characterization of the ligands and their corresponding metal complexes are analyzed by various analytical and spectroscopic techniques. Additionally, we have applied Density functional theory (DFT) calculations to understand the electronic structure of some metal complexes formed during the extraction process. (author)

  20. Synthesis and Structural Characterization of 1- and 2-Substituted Indazoles: Ester and Carboxylic Acid Derivatives

    Directory of Open Access Journals (Sweden)

    Isabel Bento

    2006-11-01

    Full Text Available A series of indazoles substituted at the N-1 and N-2 positions with ester-containing side chains -(CH2nCO2R of different lengths (n = 0-6, 9, 10 are described.Nucleophilic substitution reactions on halo esters (X(CH2nCO2R by 1H-indazole inalkaline solution lead to mixtures of N-1 and N-2 isomers, in which the N-1 isomerpredominates. Basic hydrolysis of the ester derivatives allowed the synthesis of thecorresponding indazole carboxylic acids. All compounds were fully characterised bymultinuclear NMR and IR spectroscopies, MS spectrometry and elemental analysis; theNMR spectroscopic data were used for structural assignment of the N-1 and N-2 isomers.The molecular structure of indazol-2-yl-acetic acid (5b was determined by X-raydiffraction, which shows a supramolecular architecture involving O2-H...N1intermolecular hydrogen bonds.

  1. Transition metal complexes of some biologically active ligands; synthesis characterization and bioactivities

    International Nuclear Information System (INIS)

    Rehman, S.; Ali, N.; Nisar, M.

    2009-01-01

    Transition/representative transition metals complexes of biologically active chelating agent 1,2-dipyrolodinoethane were synthesized and characterized through spectral and analytical data. The complexes are of the formula (M(L)X/sub 2/). Where (M = Co (II), Ni (II), Cu (II), Zn (II), Hg (II) and Cd (II) and X = CI, Br, NO/sub 3/). Tetrahedral geometry has been proposed to these-metal complexes with the help of magnetic measurements, elemental analysis, chemical stoichiometry and spectroscopic data Antibacterial activity of the ligand and its metal complexes were screened against Eschereschi coli, Klebsiello pneumonia, Proteus mirabilis, Proteus vulhari, Streptococcus pneumonia, Salmonella Iyphi, Bacilh,s anthrax, Streptococcus fecalis and Staphylococcus aureus. Complexes were found to be active against Eschereschi coli, Klebsiella pneumonia, Proteus mirabilis and Proteus vulharis. (author)

  2. Synthesis, spectroscopic characterization and thermogravimetric analysis of two series of substituted (metallo)tetraphenylporphyrins.

    Science.gov (United States)

    Al-Shewiki, Rasha K; Mende, Carola; Buschbeck, Roy; Siles, Pablo F; Schmidt, Oliver G; Rüffer, Tobias; Lang, Heinrich

    2017-01-01

    Subsequent treatment of H 2 TPP(CO 2 H) 4 (tetra( p -carboxylic acid phenyl)porphyrin, 1 ) with an excess of oxalyl chloride and HNR 2 afforded H 2 TPP(C(O)NR 2 ) 4 (R = Me, 2 ; iPr, 3 ) with yields exceeding 80%. The porphyrins 2 and 3 could be converted to the corresponding metalloporphyrins MTPP(C(O)NR 2 ) 4 (R = Me/iPr for M = Zn ( 2a , 3a ); Cu ( 2b , 3b ); Ni ( 2c , 3c ); Co ( 2d , 3d )) by the addition of 3 equiv of anhydrous MCl 2 (M = Zn, Cu, Ni, Co) to dimethylformamide solutions of 2 and 3 at elevated temperatures. Metalloporphyrins 2a - d and 3a - d were obtained in yields exceeding 60% and have been, as well as 2 and 3 , characterized by elemental analysis, electrospray ionization mass spectrometry (ESIMS) and IR and UV-vis spectroscopy. Porphyrins 2 , 2a - d and 3 , 3a - d are not suitable for organic molecular beam deposition (OMBD), which is attributed to their comparatively low thermal stability as determined by thermogravimetric analysis (TG) of selected representatives.

  3. Synthesis, spectroscopic characterization and pH dependent photometric and electrochemical fate of Schiff bases.

    Science.gov (United States)

    Rauf, Abdur; Shah, Afzal; Abbas, Saghir; Rana, Usman Ali; Khan, Salah Ud-Din; Ali, Saqib; Zia-Ur-Rehman; Qureshi, Rumana; Kraatz, Heinz-Bernhard; Belanger-Gariepy, Francine

    2015-03-05

    A new Schiff base, 1-((4-bromophenylimino) methyl) naphthalen-2-ol (BPIMN) was successfully synthesized and characterized by (1)H NMR, (13)C NMR, FTIR and UV-Vis spectroscopy. The results were compared with a structurally related Schiff base, 1-((4-chlorophenylimino) methyl) naphthalen-2-ol (CPIMN). The photometric and electrochemical fate of BPIMN and CPIMN was investigated in a wide pH range. The experimental findings were supported by quantum mechanical approach. The redox mechanistic pathways were proposed on the basis of results obtained electrochemical techniques. Moreover, pH dependent UV-Vis spectroscopy of BPIMN and CPIMN was carried out and the appearance of isosbestic points indicated the existence of these compounds in different tautomeric forms. Copyright © 2014 Elsevier B.V. All rights reserved.

  4. 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.

  5. Synthesis, Spectral, and In Vitro Antibacterial Studies of Organosilicon(IV) Complexes with Schiff Bases Derived from Amino Acids.

    Science.gov (United States)

    Singh, Har Lal; Singh, Jangbhadur; Mukherjee, A

    2013-01-01

    The present work stems from our interest in the synthesis, characterization, and antibacterial evaluation of organosilicon(IV) complexes of a class of amino-acid-based Schiff base which have been prepared by the interaction of ethoxytrimethylsilane with the Schiff bases (N OH) in 1 : 1 molar ratio. These complexes have been characterized by elemental analysis, molar conductance, and spectroscopic studies including electronic IR and NMR ((1)H, (13)C, and (29)Si) spectroscopy. The analytical and spectral data suggest trigonal bipyramidal geometry around the silicon atom in the resulting complexes. The ligands and their organosilicon complexes have also been evaluated for in vitro antimicrobial activity against bacteria (Bacillus cereus, Nocardia spp., E. aerogenes, Escherichia coli, Klebsiella spp., and Staphylococcus spp.). The complexes were found to be more potent as compared to the ligands.

  6. Chromium(III) Complex Obtained from Dipicolinic Acid: Synthesis, Characterization, X-Ray Crystal Structure and Electrochemical Studies

    Energy Technology Data Exchange (ETDEWEB)

    Ghasemi, Khaled; Rezvani, Ali Reza; Ghasemi, Fatemeh [Univ. of Sistan and Baluchestan, Zahedan (Iran, Islamic Republic of); Razak, Ibrahim Abdul; Rosli, Mohd Mustaqim [Universiti Sains Malaysia, Penang (Malaysia)

    2013-10-15

    The synthesis, X-ray crystallography, spectroscopic (IR, UV-vis), and electrochemical properties of the title compound, [H{sub 3}O][Cr(dipic){sub 2}] [H{sub 3}O{sup +}.Cl{sup -}] (1), (H{sub 2}dipic = 2,6-pyridinedicarboxylic acid), are reported. This complex crystallizes in the monoclinic space group Cc with a = 14.9006(10) A, b = 12.2114(8) A, c = 8.6337(6) A, α = 90.00 .deg., β = 92.7460(10) .deg., γ = 90.00 .deg., and V = 1569.16(18) A3 with Z = 4. The hydrogen bonding and noncovalent interactions play roles in the stabilization of the structure. In order to gain a better understanding of the most important geometrical parameters in the structure of the complex, atoms in molecules (AIM) method at B3LYP/6-31G level of theory has been employed.

  7. Synthesis, Characterization and Applications of One-Dimensional Metal Oxide Nanostructures

    Science.gov (United States)

    Santulli, Alexander

    Nanomaterials have been of keen research interest, owing to their exciting and unique properties (e.g. optical, magnetic, electronic, and mechanical). These properties allow nanomaterials to have many applications in areas of medicine, alternative energy, catalysis, and information storage. In particular, one-dimensional (1D) nanomaterials are highly advantageous, owing to the inherent anisotropic nature, which allows for effective transport and study of properties on the nanoscale. More specifically, 1D metal oxide nanomaterials are of particular interest, owing to their high thermal and chemical stability, as well as their intriguing optical, electronic, and magnetic properties. Herein, we will investigate the synthesis and characterization of vanadium oxide, lithium niobate and chromium oxide. We will explore the methodologies utilized for the synthesis of these materials, as well as the overall properties of these unique nanomaterials. Furthermore, we will explore the application of titanium dioxide nanomaterials as the electron transport layer in dye sensitized solar cells (DSSCs), with an emphasis on the effect of the nanoscale morphology on the overall device efficiency.

  8. β-galactosidase-catalyzed synthesis of galactosyl chlorphenesin and its characterization.

    Science.gov (United States)

    Lee, Sang-Eun; Jo, Tae-Min; Lee, Hyang-Yeol; Lee, Jongsung; Jung, Kyung-Hwan

    2013-11-01

    We synthesized galactosyl chlorphenesin (CPN-G) using β-gal-containing Escherichia coli (E. coli) cells in which the conversion yield of chlorphenesin (CPN) to CPN-G reached about 64 % during 12 h. CPN-G was identified and characterized using high-performance liquid chromatography, liquid chromatography-mass spectrometry, Fourier transform-infrared spectrometry, and nuclear magnetic resonance analysis ((1)H and (13)C). We verified that a galactose was covalently bound to a CPN alcohol group during CPN-G synthesis throughout these analyses. In particular, by the hydrolysis of CPN-G using β-gal, it was confirmed that a galactose was bound to CPN. The minimal inhibitory concentration (MIC) results showed that the CPN-G MICs were fairly similar to those of CPN. HACAT cell viability was significantly higher in CPN-G-treated cells than in CPN-treated cells at concentrations of 0.0-20.0 mM. Finally, we accomplished the synthesis of less toxic CPN-G, compared with CPN, using β-gal-containing E. coli cells as whole cells without changes in the MICs against microorganisms.

  9. New 1-hydroxy-1,1-bisphosphonates derived from 1H-pyrazolo[3,4-b]pyridine: synthesis and characterization

    Energy Technology Data Exchange (ETDEWEB)

    Teixeira, Fatima C.; Lucas, Carla; Curto, M. Joao M., E-mail: fatima.teixeira@lneg.pt [Laboratorio Nacional de Energia e Geologia, Lisboa (Portugal); Neves, M. [Instituto Superior Tecnico, Instituto Tecnologico e Nuclear (IST/ITN), Campus Tecnologico e Nuclear, Universidade Tecnica de Lisboa, Sacavem (Portugal); Duarte, M. Teresa; Andre, Vania; Teixeira, Antonio P.S. [Centro de Quimica Estrutural, Instituto Superior Tecnico, Universidade Tecnica de Lisboa (Portugal)

    2013-07-15

    A number of 1H-pyrazolo[3,4-b]pyridine derivatives, starting from 2-chloro-3-formyl pyridine, was synthesized to obtain new 1-hydroxybisphosphonates, a class of compounds with potential biological interest. Spectroscopic data were used to characterize all compounds and to identify N-1 and N-2 regioisomers, and mono- and bisphosphonates derivatives. X-ray diffractometry studies of compound 7a confirmed the proposed structure. (author)

  10. Synthesis, Characterization, and Antimicrobial Efficacy of Photomicrobicidal Cellulose Paper.

    Science.gov (United States)

    Carpenter, Bradley L; Scholle, Frank; Sadeghifar, Hasan; Francis, Aaron J; Boltersdorf, Jonathan; Weare, Walter W; Argyropoulos, Dimitris S; Maggard, Paul A; Ghiladi, Reza A

    2015-08-10

    Toward our goal of scalable, antimicrobial materials based on photodynamic inactivation, paper sheets comprised of photosensitizer-conjugated cellulose fibers were prepared using porphyrin and BODIPY photosensitizers, and characterized by spectroscopic (infrared, UV-vis diffuse reflectance, inductively coupled plasma optical emission) and physical (gel permeation chromatography, elemental, and thermal gravimetric analyses) methods. Antibacterial efficacy was evaluated against Staphylococcus aureus (ATCC-2913), vancomycin-resistant Enterococcus faecium (ATCC-2320), Acinetobacter baumannii (ATCC-19606), Pseudomonas aeruginosa (ATCC-9027), and Klebsiella pneumoniae (ATCC-2146). Our best results were achieved with a cationic porphyrin-paper conjugate, Por((+))-paper, with inactivation upon illumination (30 min, 65 ± 5 mW/cm(2), 400-700 nm) of all bacterial strains studied by 99.99+% (4 log units), regardless of taxonomic classification. Por((+))-paper also inactivated dengue-1 virus (>99.995%), influenza A (∼ 99.5%), and human adenovirus-5 (∼ 99%). These results demonstrate the potential of cellulose materials to serve as scalable scaffolds for anti-infective or self-sterilizing materials against both bacteria and viruses when employing a photodynamic inactivation mode of action.

  11. Synthesis and characterization of silver nanoparticles in natural rubber

    International Nuclear Information System (INIS)

    Abu Bakar, N.H.H.; Ismail, J.; Abu Bakar, M.

    2007-01-01

    Silver nanoparticles are formed in natural rubber matrix via photo reduction of film cast from natural rubber latex (NRL) containing silver salt. The resulting NR-Ag nanocomposite is characterized using TEM, XRD and UV spectroscopic techniques. The nanoparticles, diameter ranging between 4 and 10 nm, are dispersed within distinct interfaces which correspond to the inter-particle boundaries of the NRL particles that form the matrix. The average width of the interfaces is 8 nm. X-ray diffraction (XRD) analysis confirms the nanoparticles as metallic silver of the face-centered cubic type. UV-vis absorption spectra show peaks characteristic of the surface plasmon resonance of nano-sized silver. A comparison with the results of formation of silver, obtained under similar reduction condition, in a series of matrices namely de-proteinized natural rubber latex (DNRL), NRL containing sodium dodecyl sulfate (SDS), aqueous solutions of bovain serum albumin and SDS, suggests that the protein in natural rubber is responsible for the formation of stable silver nanoparticles in the natural rubber (NR) matrix

  12. SYNTHESIS, CHARACTERIZATION AND ANTIBACTERIAL ...

    African Journals Online (AJOL)

    Preferred Customer

    In the present study, synthesis, and biological evaluation of some novel ... Then slowly cooled and resultant mixture was basified with aqueous sodium hydroxide ... mol), anhydrous potassium carbonate (5.52 g, 0.04 mol) in acetone (25 mL), ...

  13. Synthesis, purification and physico-chemical characterization of the deuterized chloroform

    International Nuclear Information System (INIS)

    Mihaila, V.; Olteanu-Chiper, D.

    1999-01-01

    This work refers to deuterized chloroform synthesis and purification methods. Three methods for obtaining deuterized chloroform are presented. 1. The direct chlorination of methane, in presence of light and in oxygen-free atmosphere: CH 4 + 3 Cl 2 + ℎν→ CHCl 3 + 3 HCl. The method's drawback is that the product obtained is impure, as other chlorinated compounds such as CH 3 Cl, CH 2 Cl 2 , CCl 4 also result. 2. Chlorination of acetaldehyde or acetone, in basic catalysis and in halogen excess (α substitution with direct synthesis of trihalogen compound), followed by a haloform reaction (hydrolytic splitting) in presence of chlorinated lime: CH 3 CHO (Cl 2 /HO - )/(-HCl)Cl 3 C-CHO (CaCl 2 /HOH)/(-(HCOO) 2 Ca) CHCl 3 and CH 3 -CO-CH 3 (Cl 2 /HO)/(-HCl) Cl 3 C-CO-CH 3 (NaOH)/(-CH 3 COONa) CHCl 3 . 3. Decarboxylizing of trichloroacetate acid (as sodium salt): Cl 3 C-COONa (t deg C)/(H 2 O) Cl 3 CH + NaHCO 3 . This method is the most suitable for the deuterized chloroform synthesis since the reaction takes place in absence of other hydrogen atoms (protons) and in deuterized water 99,87% purity, according to the following reaction: Cl 3 C-COONa (t deg C)/(D 2 O) Cl 3 CD + NaDCO 3 . Another advantage is that this method avoids the synthesis of secondary products which could entail additional purifications (distillations, rectifications, a.s.o.). The deuterized chloroform is separated from the deuterized sodium bicarbonate aqueous solution by washing with deuterized water, in a liquid-to-liquid separating funnel. After separation, the deuterized chloroform is dried in nitrogen atmosphere. The characterization of the final product is carried out through Nuclear Magnetic Resonance Spectrometry. (authors)

  14. Synthesis and characterization of homogeneous interstitial solutions of nitrogen and carbon in iron-based lattices

    DEFF Research Database (Denmark)

    Brink, Bastian Klüge

    work in synthesis and characterization of interstitial solutions ofnitrogen and carbon in iron-based lattices. In order to avoid the influences of gradients incomposition and residual stresses, which are typically found in treated surface layers,homogenous samples are needed. These were prepared from...

  15. Synthesis and Characterization of ZnO Nanoparticles Using Sol-gel Process

    Directory of Open Access Journals (Sweden)

    Jayasree ALURI

    2016-05-01

    Full Text Available In the Present work structural, morphological and compositional properties of ZnO nanopowders synthesized using Zinc nitrate and NaOH using sol-gel process were reported. The synthesized nanopowders were further analyzed using X-Ray Diffraction (XRD, Scanning electron microscopy (SEM and Fourier Transform Infrared (FTIR spectroscopic characterizations. Crystalline size and Lattice strain determined from XRD spectra. Morphology of Nanopowders viewed from SEM images observed at different magnifications. The presence of Functional groups analyzed from FTIR spectra. From the results it was very clear that particles synthesized using Zinc nitrate and NaOH plays a vital role on crystalline size, surface morphology of Nanopowders. Synthesized nanopowders can be utilized as building materials in fabrication of various optoelectronic devices including solar cells, LED’s etc. due to its significant structural, morphological and optical properties.

  16. Organic-inorganic hybrid materials. I: Synthesis, characterization ...

    African Journals Online (AJOL)

    Hydrosilylation of 2-chloroethylvinyl ether by octahydridosilsesilsesquioxane catalyzed by hexachloroplatinic acid gives a quantitative yield of 3 as white crystals. Thermogravimetric analysis of Si8O12(CH2CH2OCH2CH2Cl)83 revealed that it is thermally reasonably stable. Spectroscopic data and a crystal structure ...

  17. X-ray micro-beam characterization of a small pixel spectroscopic CdTe detector

    Science.gov (United States)

    Veale, M. C.; Bell, S. J.; Seller, P.; Wilson, M. D.; Kachkanov, V.

    2012-07-01

    A small pixel, spectroscopic, CdTe detector has been developed at the Rutherford Appleton Laboratory (RAL) for X-ray imaging applications. The detector consists of 80 × 80 pixels on a 250 μm pitch with 50 μm inter-pixel spacing. Measurements with an 241Am γ-source demonstrated that 96% of all pixels have a FWHM of better than 1 keV while the majority of the remaining pixels have FWHM of less than 4 keV. Using the Diamond Light Source synchrotron, a 10 μm collimated beam of monochromatic 20 keV X-rays has been used to map the spatial variation in the detector response and the effects of charge sharing corrections on detector efficiency and resolution. The mapping measurements revealed the presence of inclusions in the detector and quantified their effect on the spectroscopic resolution of pixels.

  18. 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.

  19. Spectroscopic characterization of Venus at the single molecule level.

    Science.gov (United States)

    David, Charlotte C; Dedecker, Peter; De Cremer, Gert; Verstraeten, Natalie; Kint, Cyrielle; Michiels, Jan; Hofkens, Johan

    2012-02-01

    Venus is a recently developed, fast maturating, yellow fluorescent protein that has been used as a probe for in vivo applications. In the present work the photophysical characteristics of Venus were analyzed spectroscopically at the bulk and single molecule level. Through time-resolved single molecule measurements we found that single molecules of Venus display pronounced fluctuations in fluorescence emission, with clear fluorescence on- and off-times. These fluorescence intermittencies were found to occupy a broad range of time scales, ranging from milliseconds to several seconds. Such long off-times can complicate the analysis of single molecule counting experiments or single-molecule FRET experiments. This journal is © The Royal Society of Chemistry and Owner Societies 2012

  20. SPECTROSCOPIC CHARACTERIZATION AND DETECTION OF ETHYL MERCAPTAN IN ORION

    International Nuclear Information System (INIS)

    Kolesniková, L.; Alonso, J. L.; Daly, A. M.; Tercero, B.; Cernicharo, J.; Gordon, B. P.; Shipman, S. T.

    2014-01-01

    New laboratory data of ethyl mercaptan, CH 3 CH 2 SH, in the millimeter- and submillimeter-wave domains (up to 880 GHz) provided very precise values of the spectroscopic constants that allowed the detection of gauche-CH 3 CH 2 SH toward Orion KL. This identification is supported by 77 unblended or slightly blended lines plus no missing transitions in the range 80-280 GHz. A detection of methyl mercaptan, CH 3 SH, in the spectral survey of Orion KL is reported as well. Our column density results indicate that methyl mercaptan is ≅ 5 times more abundant than ethyl mercaptan in the hot core of Orion KL

  1. SPECTROSCOPIC CHARACTERIZATION AND DETECTION OF ETHYL MERCAPTAN IN ORION

    Energy Technology Data Exchange (ETDEWEB)

    Kolesniková, L.; Alonso, J. L.; Daly, A. M. [Grupo de Espectroscopía Molecular (GEM), Edificio Quifima, Laboratorios de Espectroscopía y Bioespectroscopía, Parque Científico UVa, Unidad Asociada CSIC, Universidad de Valladolid, E-47011 Valladolid (Spain); Tercero, B.; Cernicharo, J. [Departamento de Astrofísica, Centro de Astrobiología CAB, CSIC-INTA, Ctra. de Torrejón a Ajalvir km 4, E-28850 Madrid (Spain); Gordon, B. P.; Shipman, S. T., E-mail: lucie.kolesnikova@uva.es, E-mail: jlalonso@qf.uva.es, E-mail: adammichael.daly@uva.es, E-mail: terceromb@cab.inta-csic.es, E-mail: jcernicharo@cab.inta-csic.es, E-mail: brittany.gordon@ncf.edu, E-mail: shipman@ncf.edu [Division of Natural Sciences, New College of Florida, Sarasota, FL 34243 (United States)

    2014-03-20

    New laboratory data of ethyl mercaptan, CH{sub 3}CH{sub 2}SH, in the millimeter- and submillimeter-wave domains (up to 880 GHz) provided very precise values of the spectroscopic constants that allowed the detection of gauche-CH{sub 3}CH{sub 2}SH toward Orion KL. This identification is supported by 77 unblended or slightly blended lines plus no missing transitions in the range 80-280 GHz. A detection of methyl mercaptan, CH{sub 3}SH, in the spectral survey of Orion KL is reported as well. Our column density results indicate that methyl mercaptan is ≅ 5 times more abundant than ethyl mercaptan in the hot core of Orion KL.

  2. 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)

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

    Science.gov (United States)

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

    2013-10-01

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

  4. Synthesis and characterization of waterborne polyurethane acrylate copolymers

    International Nuclear Information System (INIS)

    Sultan, Misbah; Bhatti, Haq Nawaz; Zuber, Mohammad; Barikani, Mehdi

    2013-01-01

    Polyurethane acrylate copolymers were synthesized by emulsion polymerization process. To reduce the environmental hazards, organic solvents were replaced by eco-friendly aqueous system. Concentration of polyurethane and acrylate monomer was varied to investigate the effect of chemical composition on performance properties of copolymers. FTIR spectroscopy was used as a key tool to record the chemical synthesis route. The synthesized copolymer emulsions were characterized by evaluating their particle size, viscosity, dry weight content, chemical and water resistance. Thermal decomposition was studied by thermogravimetric analysis. Scanning electron microscope was used to visualize the morphological structure of copolymers. The experimental results indicate better polyurethane acrylate compatibility till the ratio of 30/70. However, these copolymers exhibited synergistic effects between the two polymers and revealed a remarkable improvement in numerous coating properties

  5. Infrared spectroscopic ellipsometry of micrometer-sized SiO2 line gratings

    Science.gov (United States)

    Walder, Cordula; Zellmeier, Matthias; Rappich, Jörg; Ketelsen, Helge; Hinrichs, Karsten

    2017-09-01

    For the design and process control of periodic nano-structured surfaces spectroscopic ellipsometry is already established in the UV-VIS spectral regime. The objective of this work is to show the feasibility of spectroscopic ellipsometry in the infrared, exemplarily, on micrometer-sized SiO2 line gratings grown on silicon wafers. The grating period ranges from 10 to about 34 μm. The IR-ellipsometric spectra of the gratings exhibit complex changes with structure variations. Especially in the spectral range of the oxide stretching modes, the presence of a Rayleigh singularity can lead to pronounced changes of the spectrum with the sample geometry. The IR-ellipsometric spectra of the gratings are well reproducible by calculations with the RCWA method (Rigorous Coupled Wave Analysis). Therefore, infrared spectroscopic ellipsometry allows the quantitative characterization and process control of micrometer-sized structures.

  6. Characterization of the Elusive Conformers of Glycine from State-of-the-Art Structural, Thermodynamic, and Spectroscopic Computations: Theory Complements Experiment.

    Science.gov (United States)

    Barone, Vincenzo; Biczysko, Malgorzata; Bloino, Julien; Puzzarini, Cristina

    2013-03-12

    A state-of-the-art computational strategy for the evaluation of accurate molecular structures as well as thermodynamic and spectroscopic properties along with the direct simulation of infrared (IR) and Raman spectra is established, validated (on the basis of the experimental data available for the Ip glycine conformer) and then used to provide a reliable and accurate characterization of the elusive IVn/gtt and IIIp/tct glycine conformers. The integrated theoretical model proposed is based on accurate post-Hartree-Fock computations (involving composite schemes) of energies, structures, properties, and harmonic force fields coupled to DFT corrections for the proper inclusion of vibrational effects at an anharmonic level (as provided by general second-order perturbative approach). It is shown that the approach presented here allows the evaluation of structural, thermodynamic, and spectroscopic properties with an overall accuracy of about, or better than, 0.001 Å, 20 MHz, 1 kJ·mol(-1), and 10 cm(-1) for bond distances, rotational constants, conformational enthalpies, and vibrational frequencies, respectively. The high accuracy of the computational results allows one to support and complement experimental studies, thus providing (i) an unequivocal identification of several conformers concomitantly present in the experimental mixture and (ii) data not available or difficult to experimentally derive.

  7. Synthesis, characterization and behaviour to gamma radiation of the bis-L-alaninato-copper (II)

    International Nuclear Information System (INIS)

    Passos, B.F.T.

    1985-01-01

    The behaviour of coordinated compound obtained from the copper (II) and the L-(+)- alanine to gamma radiation was determined. A study of synthesis and characterization of this complex was made with elementary analysis, ultraviolet and visible electronic spectroscopy, infrared vibrational spectroscopy, proton magnetic resonance spectroscopy and thermo-gravimetric analysis. (C.G.C.)

  8. Synthesis and characterization of low-valence actinide phosphide tellurides and ternary selenium-halide iridium complexes; Synthese und Charakterisierung niedervalenter Actinoidphosphidtelluride und ternaerer Selen-Halogenid-Komplexe des Iridiums

    Energy Technology Data Exchange (ETDEWEB)

    Stolze, Karoline

    2016-04-07

    The thesis on the synthesis and characterization of low-valence actinide phosphide tellurides and ternary selenium-halide iridium complexes includes two parts: a description of the experimental synthesis of UPTe and U2PTe2O and ThPTe and the synthesis of selenium-chloride iridium complexes and selenium-bromide iridium complexes. The characterization included X-ray diffraction and phase studies.

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

    Science.gov (United States)

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

    2009-07-01

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

  10. Synthesis, characterization, crystal structures and DFT studies of some new 1,2,4-triazole and triazolidin derivatives

    Science.gov (United States)

    Abosadiya, Hamza M.; Anouar, El Hassane; Abusaadiya, Salima M.; Hasbullah, Siti Aishah; Yamin, Bohari M.

    2018-01-01

    A simple efficient method for synthesis of some new 1,2,4-Triazole and Triazolidin derivatives namely, 5-(4-methoxyphenyl)-2-phenyl-2,4-dihydro-3H-1,2,4-triazole-3-thione (1a), (2-chlorophenyl)(3,3-dimethyl-1-phenyl-5-thioxo-1,2,4-triazolidin-4-yl)methanone (1b) and (2-iodophenyl)(3,3-dimethyl-1-phenyl-5-thioxo-1,2,4-triazolidin-4-yl)methanone (1c) have been synthesized in high yields from the reaction of carbonoyl isothiocyanate with phenyl hydrazine. The final products were characterized by FT-IR, 1H and 13C NMR spectroscopic techniques. X-ray crystallographic studies showed that 1a crystallized in triclinic crystal system with space group Pī, while both 1b and 1c crystallized in orthorhombic crystal system with space group Pna21. The asymmetric unit of 1a consists two crystallographically independent molecules, while only one molecule in asymmetric unit for both 1b and 1c compounds. All molecules possess Csbnd H ….S intramolecular hydrogen bonds which formed a pseudo-six-membered ring. Experimental results have been confirmed by the state-of-art density functional theory (DFT) in gas and solvent phase by using five different hybrid functionals B3LYP, B3P86, CAM-B3LYP, M06-2X and PBE0 combined with 6-311++G(d, p) basis set. The experimental data are relatively well produced, and relatively good correlations are obtained between the predicted and experimental data.

  11. Synthesis and characterization of carboxylic acid functionalized silicon nanoparticles

    Science.gov (United States)

    Shaner, Ted V.

    Silicon nanoparticles are of great interest in a great number of fields. Silicon nanoparticles show great promise particularly in the field of bioimaging. Carboxylic acid functionalized silicon nanoparticles have the ability to covalently bond to biomolecules through the conjugation of the carboxylic acid to an amine functionalized biomolecule. This thesis explores the synthesis of silicon nanoparticles functionalized by both carboxylic acids and alkenes and their carboxylic acid functionality. Also discussed is the characterization of the silicon nanoparticles by the use of x-ray spectroscopy. Finally, the nature of the Si-H bond that is observed on the surface of the silicon nanoparticles will be investigated using photoassisted exciton mediated hydrosilation reactions. The silicon nanoparticles are synthesized from both carboxylic acids and alkenes. However, the lack of solubility of diacids is a significant barrier to carboxylic acid functionalization by a mixture of monoacids and diacids. A synthesis route to overcome this obstacle is to synthesize silicon nanoparticles with terminal vinyl group. This terminal vinyl group is distal to the surface of the silicon nanoparticle. The conversion of the vinyl group to a carboxylic acid is accomplished by oxidative cleavage using ozonolysis. The carboxylic acid functionalized silicon nanoparticles were then successfully conjugated to amine functionalized DNA strand through an n-hydroxy succinimide ester activation step, which promotes the formation of the amide bond. Conjugation was characterized by TEM and polyacrylamide gel electrophoresis (PAGE). The PAGE results show that the silicon nanoparticle conjugates move slower through the polyacrylamide gel, resulting in a significant separation from the nonconjugated DNA. The silicon nanoparticles were then characterized by the use of x-ray absorption near edge spectroscopy (Xanes) and x-ray photoelectron spectroscopy (XPS) to investigate the bonding and chemical

  12. Synthesis and Characterization of EDTA Complexes Useful for Trace Elements Supplementation

    Directory of Open Access Journals (Sweden)

    Baran Enrique J.

    2002-01-01

    Full Text Available The synthesis of two heterobimetallic EDTA complexes, MgCu(EDTA.6H2O and ZnCu(EDTA.6H2O, is described. They were characterized by means of vibrational (infrared and Raman and electronic (reflectance spectroscopy. Several dissolution tests in 0.1 N HCl and simulated gastric juice were also performed. The results support the potential usefulness of these complexes for copper supplementation in human and veterinary medicine and to the simultaneous reinforcement of Mg(II and Zn(II levels.

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

    Energy Technology Data Exchange (ETDEWEB)

    Even-Boudjada, S

    1994-12-01

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

  14. On-Surface Synthesis and Characterization of Honeycombene Oligophenylene Macrocycles.

    Science.gov (United States)

    Chen, Min; Shang, Jian; Wang, Yongfeng; Wu, Kai; Kuttner, Julian; Hilt, Gerhard; Hieringer, Wolfgang; Gottfried, J Michael

    2017-01-24

    We report the on-surface formation and characterization of [30]-honeycombene, a cyclotriacontaphenylene, which consists of 30 phenyl rings (C 180 H 120 ) and has a diameter of 4.0 nm. This shape-persistent, conjugated, and unsubstituted hexagonal hydrocarbon macrocycle was obtained by solvent-free synthesis on a silver (111) single-crystal surface, making solubility-enhancing alkyl side groups unnecessary. Side products include strained macrocycles with square, pentagonal, and heptagonal shape. The molecules were characterized by scanning tunneling microscopy and density functional theory (DFT) calculations. On the Ag(111) surface, the macrocycles act as molecular quantum corrals and lead to the confinement of surface-state electrons inside the central cavity. The energy of the confined surface state correlates with the size of the macrocycle and is well described by a particle-in-the-box model. Tunneling spectroscopy suggests conjugation within the planar rings and reveals influences of self-assembly on the electronic structure. While the adsorbed molecules appear to be approximately planar, the free molecules have nonplanar conformation, according to DFT.

  15. Spectroscopic follow up of Kepler planet candidates

    DEFF Research Database (Denmark)

    Latham..[], D. W.; Cochran, W. D.; Marcy, G.W.

    2010-01-01

    Spectroscopic follow-up observations play a crucial role in the confirmation and characterization of transiting planet candidates identified by Kepler. The most challenging part of this work is the determination of radial velocities with a precision approaching 1 m/s in order to derive masses from...... spectroscopic orbits. The most precious resource for this work is HIRES on Keck I, to be joined by HARPS-North on the William Herschel Telescope when that new spectrometer comes on line in two years. Because a large fraction of the planet candidates are in fact stellar systems involving eclipsing stars...... and not planets, our strategy is to start with reconnaissance spectroscopy using smaller telescopes, to sort out and reject as many of the false positives as possible before going to Keck. During the first Kepler observing season in 2009, more than 100 nights of telescope time were allocated for this work, using...

  16. Design, synthesis, and characterization of 0-D, 1-D, and 2-D Zinc–Adeninate coordination assemblies

    Energy Technology Data Exchange (ETDEWEB)

    An, Ji Hyun [Dept. of Chemistry Education, Seoul National University, Seoul (Korea, Republic of); Geib, Steven J. [Dept. of Chemistry, University of Pittsburgh, Pittsburgh (United States); Kim, Myung Gil [Dept. of Chemistry, Chungang University, Seoul (Korea, Republic of)

    2015-08-15

    In this study, we demonstrate the synthesis and characterization of zinc– adeninate coordination polymers with 0-D, 1-D, and 2-D structures. We describe methods for controlling the structure of these materials by applying different synthetic conditions and discuss their structural relationships. 0-D, 1-D, and 2-D zinc–adeninate coordination polymers with the same metal–adeninate coordination mode were synthesized and characterized. By controlling the temperature, a material with 0-D macrocycle or 1-D chain coordination polymer was prepared. A replacement of pyridine with bipyridine formed 2-D sheet structure by connecting 1-D chains with each other. They exhibited an interesting relationship between synthetic methods and structures. Further study of metal–adeninate coordination chemistry will render a precise control of the structure in synthesis and will open a new venue to new materials with fascinating properties.

  17. Graphitic carbon nitride: Synthesis, characterization and photocatalytic decomposition of nitrous oxide

    International Nuclear Information System (INIS)

    Praus, Petr; Svoboda, Ladislav; Ritz, Michal; Troppová, Ivana; Šihor, Marcel; Kočí, Kamila

    2017-01-01

    Graphitic carbon nitride (g-C_3N_4) was synthetized by condensation of melamine at the temperatures of 400–700 °C in air for 2 h and resulting products were characterized and finally tested for the photocatalytic decomposition of nitrous oxide. The characterization methods were elemental analysis, UV–Vis diffuse reflectance spectroscopy (DRS), photoluminescence (PL), Fourier transform infrared (FTIR) and Raman spectroscopy, measurement of specific surface area (SSA), X-ray powder diffraction (XRD), scanning (SEM) and transmission (TEM) electron microscopy. The XRD patterns, FTIR and Raman spectra proved the presence of g-C_3N_4 at above 550 °C but the optimal synthesis temperature of 600–650 °C was found. Under these conditions graphitic carbon nitride of the overall empirical composition of C_6N_9H_2 was formed. At lower temperatures g-C_3N_4 with a higher content of hydrogen was formed but at higher temperatures g-C_3N_4 was decomposed. At the temperatures above 650 °C, its exfoliation was observed. The photocatalytic experiments showed that the activity of all the samples synthetized at 400–700 °C was very similar, that is, within the range of experimental error (5 %). The total conversion of N_2O reached about 43 % after 14 h. - Highlights: • Graphitic carbon nitride (g-C_3N_4) was thermally synthetized from melamine in the range of 400–700 °C. • The optimal temperature was determined at 600–650 °C. • All synthesis products were properly characterized by physico-chemical methods. • Exfoliation of g-C_3N_4 at above 600 °C was observed. • g-C_3N_4 was used for the photocatalytic decomposition of N_2O.

  18. Spectroscopic characterization of galaxy clusters in RCS-1: spectroscopic confirmation, redshift accuracy, and dynamical mass-richness relation

    Science.gov (United States)

    Gilbank, David G.; Barrientos, L. Felipe; Ellingson, Erica; Blindert, Kris; Yee, H. K. C.; Anguita, T.; Gladders, M. D.; Hall, P. B.; Hertling, G.; Infante, L.; Yan, R.; Carrasco, M.; Garcia-Vergara, Cristina; Dawson, K. S.; Lidman, C.; Morokuma, T.

    2018-05-01

    We present follow-up spectroscopic observations of galaxy clusters from the first Red-sequence Cluster Survey (RCS-1). This work focuses on two samples, a lower redshift sample of ˜30 clusters ranging in redshift from z ˜ 0.2-0.6 observed with multiobject spectroscopy (MOS) on 4-6.5-m class telescopes and a z ˜ 1 sample of ˜10 clusters 8-m class telescope observations. We examine the detection efficiency and redshift accuracy of the now widely used red-sequence technique for selecting clusters via overdensities of red-sequence galaxies. Using both these data and extended samples including previously published RCS-1 spectroscopy and spectroscopic redshifts from SDSS, we find that the red-sequence redshift using simple two-filter cluster photometric redshifts is accurate to σz ≈ 0.035(1 + z) in RCS-1. This accuracy can potentially be improved with better survey photometric calibration. For the lower redshift sample, ˜5 per cent of clusters show some (minor) contamination from secondary systems with the same red-sequence intruding into the measurement aperture of the original cluster. At z ˜ 1, the rate rises to ˜20 per cent. Approximately ten per cent of projections are expected to be serious, where the two components contribute significant numbers of their red-sequence galaxies to another cluster. Finally, we present a preliminary study of the mass-richness calibration using velocity dispersions to probe the dynamical masses of the clusters. We find a relation broadly consistent with that seen in the local universe from the WINGS sample at z ˜ 0.05.

  19. Plant-mediated green synthesis of ZnO nanoparticles using Garcinia gummi-gutta seed extract: Photoluminescence, screening of their catalytic activity in antioxidant, formylation and biodiesel production

    Science.gov (United States)

    Raghavendra, M.; Yatish, K. V.; Lalithamba, H. S.

    2017-08-01

    The green synthesis of multifunctional ZnO nanoparticles (NPs) was prepared by treatment of zinc nitrate with an extract of Garcinia gummi-gutta seed by the combustion method. The ZnO NPs were characterized by XRD, scanning electron microscopy, UV-visible, FTIR spectroscopic techniques. The prepared ZnO NPs were evaluated for photoluminescence (PL), antioxidant properties and also utilized as a catalyst for the formylation of aromatic amines and biodiesel production. The study reveals that the reaction is simple, mild and environmental friendly. Furthermore, the reaction results in excellent yield of products.

  20. Synthesis, characterization and electrocatalytic properties of delafossite CuGaO{sub 2}

    Energy Technology Data Exchange (ETDEWEB)

    Ahmed, Jahangeer [Department of Chemistry, University of Texas Rio Grande Valley, 1201 West University Drive, Edinburg, TX 78539 (United States); Department of Chemistry, College of Science, King Saud University, Riyadh 11451 (Saudi Arabia); Mao, Yuanbing, E-mail: yuanbing.mao@utrgv.edu [Department of Chemistry, University of Texas Rio Grande Valley, 1201 West University Drive, Edinburg, TX 78539 (United States)

    2016-10-15

    Delafossite CuGaO{sub 2} has been employed as photocatalysts for solar cells, but their electrocatalytic properties have not been extensively studied, especially no comparison among samples made by different synthesis routes. Herein, we first reported the successful synthesis of delafossite CuGaO{sub 2} particles with three different morphologies, i.e. nanocrystalline hexagons, sub-micron sized plates and micron–sized particles by a modified hydrothermal method at 190 °C for 60 h [1–3], a sono-chemical method followed by firing at 850 °C for 48 h, and a solid state route at 1150 °C, respectively. Morphology, composition and phase purity of the synthesized samples was confirmed by powder X-ray diffraction and Raman spectroscopic studies, and then their electrocatalytic performance as active and cost effective electrode materials to the oxygen and hydrogen evolution reactions in 0.5 M KOH electrolyte versus Ag/AgCl was investigated and compared under the same conditions for the first time. The nanocrystalline CuGaO{sub 2} hexagons show enhanced electrocatalytic activity than the counterpart sub-micron sized plates and micron-sized particles. - Graphical abstract: Representative delafossite CuGaO2 samples with sub-micron sized plate and nanocrystalline hexagon morphologies accompanying with chronoamperometric voltammograms for oxygen evolution reaction and hydrogen evolution reaction in 0.5 M KOH electrolyte after purged with N{sub 2} gas. - Highlights: • Delafossite CuGaO{sub 2} with three morphologies has been synthesized. • Phase purity of the synthesized samples was confirmed. • Comparison on their electrocatalytic properties was made for the first time. • Their use as electrodes for oxygen and hydrogen evolution reactions was evaluated. • Nanocrystalline CuGaO{sub 2} hexagons show highest electrocatalytic activity.

  1. Characterization of PDMS samples with variation of its synthesis parameters for tunable optics applications

    Science.gov (United States)

    Marquez-Garcia, Josimar; Cruz-Félix, Angel S.; Santiago-Alvarado, Agustin; González-García, Jorge

    2017-09-01

    Nowadays the elastomer known as polydimethylsiloxane (PDMS, Sylgard 184), due to its physical properties, low cost and easy handle, have become a frequently used material for the elaboration of optical components such as: variable focal length liquid lenses, optical waveguides, solid elastic lenses, etc. In recent years, we have been working in the characterization of this material for applications in visual sciences; in this work, we describe the elaboration of PDMSmade samples, also, we present physical and optical properties of the samples by varying its synthesis parameters such as base: curing agent ratio, and both, curing time and temperature. In the case of mechanical properties, tensile and compression tests were carried out through a universal testing machine to obtain the respective stress-strain curves, and to obtain information regarding its optical properties, UV-vis spectroscopy is applied to the samples to obtain transmittance and absorbance curves. Index of refraction variation was obtained through an Abbe refractometer. Results from the characterization will determine the proper synthesis parameters for the elaboration of tunable refractive surfaces for potential applications in robotics.

  2. Synthesis and characterization of the Cu2ZnSnS4 system for photovoltaic applications

    Science.gov (United States)

    Sánchez Pinzón, D. L.; Soracá Perez, G. Y.; Gómez Cuaspud, J. A.; López, E. Vera

    2017-01-01

    This paper focuses on the synthesis and characterization of a ceramic material based on the Cu2ZnSnS4 system, through the implementation of a hydrothermal route. For this purpose, we started from nitrate dissolutions in a 1.0mol L-1 concentration, which were mixed and treated in a teflon lined vessel steel at 280°C for 48h. The Physicochemical characterization of the solid was evaluated by means of ultraviolet visible spectroscopy (UV-VIS), X-ray diffraction (XRD), Raman spectroscopy, scanning and transmission electron microscopy (SEM-TEM) and solid state impedance spectroscopy (IS). The initial characterization through UV measurements confirms a Band-gap around 1.46eV obtained by the Kubelka-Munk method, which demonstrates the effectiveness of the synthesis method in the obtaining of a semiconductor material. The XRD results confirm the obtaining of a crystalline material of pure phase with tetragonal geometry and I-42m space group. The preferential crystalline orientation was achieved along (2 2 0) facet, with crystallite sizes of nanometric order (6.0nm). The morphological aspects evaluated by means electron microscopy, confirmed the homogeneity of the material, showing specifically a series of textural and surface properties of relevant importance. Finally, the electrical characterizations allow to validate the semiconductor behaviour of CZTS system for development of photovoltaic technologies.

  3. In-line quantification and characterization of membrane fouling

    KAUST Repository

    Bucs, Szilard

    2016-06-16

    Methods of detecting, quantifying and/or characterizing the fouling of a device from a combination of pressure and spectroscopic data are provided. The device can be any device containing components susceptible to fouling. Components can include membranes, pipes, or reactors. Suitable devices include membrane devices, heat exchangers, and chemical or bio-reactors. Membrane devices can include, for example, microfiltration devices, ultrafiltration devices, nanofiltration devices, reverse osmosis, forward osmosis, osmosis, reverse electrodialysis, electro- deionisation or membrane distillation devices. The methods can be applied to any type of membrane, including tubular, spiral, hollow fiber, flat sheet, and capillary membranes. The spectroscopic characterization can include measuring one or more of the absorption, fluorescence, or raman spectroscopic data of one or more foulants. The methods can allow for the early detection and/or characterization of fouling. The characterization can include determining the specific foulant(s) or type of foulant(s) present. The characterization of fouling can allow for the selection of an appropriate de-fouling method and timing.

  4. Synthesis and characterization of reactions by nanoferrites Co2Fe2O4 combustion

    International Nuclear Information System (INIS)

    Santos, P.T.A.; Dantas, B.B.; Costa, A.C.F.M.; Araujo, P.M.A.G.

    2012-01-01

    In this work CoFe 2 O 4 of magnetic nanoparticles were synthesized by combustion reaction and the structural and morphological characteristics of the synthesized samples as well as the parameters of synthesis temperature and reaction time were investigated in order to assess the reproducibility of the synthesis. The maximum temperature and time of the combustion flame were obtained with pyrometer coupled to a computer with online measurement and a stopwatch. The resulting samples were characterized by X-ray diffraction (XRD), infrared spectroscopy (FTIR) and scanning electron microscopy (SEM). The maximum temperature achieved during synthesis for all reactions ranged from 623 deg C and 755 deg C. The combustion flame time varied between 18 and 23 seconds. The XRD showed the formation of only CoFe 2 O 4 inverse spinel phase, with crystallite size 28 nm and crystallinity 78%, with typical morphology of the formation of agglomerates of uniform size, brittle and comprising nanoparticles together by weak forces. (author)

  5. Synthesis of samarium complexes with the derivative binder of Schiff Quinolinic base. Characterization and photophysical study

    International Nuclear Information System (INIS)

    Lucas H, J.

    2016-01-01

    In this work we determined the metal: binder stoichiometry of the species formed during the UV/Vis spectrophotometric titration of the derivative binder of Schiff quinolinic base, L1 with the samarium nitrate pentahydrate in methanol. Statistical analysis of the data allowed proposing the metal: binder stoichiometry for the synthesis of the complexes which was one mole of samarium salt by 2.5 moles of binder and thus favor the formation of complexes with 1M: 1L and 1M: 2L stoichiometries. They were synthesized in aqueous-organic medium (water-ethanol), isolated and purified two complexes with stoichiometry 1 Sm: 1 L1, complex 1 and 1 Sm: 2 L1, complex 2. The overall yield of the reaction was 76%. The characterization of the formed complexes was performed by visible ultraviolet spectrometry (UV/Vis), nuclear magnetic resonance, X-ray photoelectron spectroscopy (XP S), thermal gravimetric analysis with differential scanning calorimetry (TGA/DSC), and radial distribution function. These complexes were studied by fluorescence and emission phosphorescence at variable temperature. Spectroscopic techniques used in both solution and solid demonstrated the formation and stability of these complexes. In addition XP S indicated that in both complexes the samarium retains its oxidation state 3+. Luminescence studies indicated that there is intra-binding charge transfer which decreases the transfer of light energy from the binder to the samarium. Based on the experimental results, L1 binder molecules and complexes 1 and 2 were modeled that demonstrated the proposed Nc for each complex, as well as allowed to visualize the structural arrangement of the molecules, complexes and binder. (Author)

  6. Synthesis and Characterization of Stimuli Responsive Block Copolymers, Self-Assembly Behavior and Applications

    Energy Technology Data Exchange (ETDEWEB)

    Determan, Michael Duane [Iowa State Univ., Ames, IA (United States)

    2005-12-17

    The central theme of this thesis work is to develop new block copolymer materials for biomedical applications. While there are many reports of stimuli-responsive amphiphilic [19-21] and crosslinked hydrogel materials [22], the development of an in situ gel forming, pH responsive pentablock copolymer is a novel contribution to the field, Figure 1.1 is a sketch of an ABCBA pentablock copolymer. The A blocks are cationic tertiary amine methacrylates blocked to a central Pluronic F127 triblock copolymer. In addition to the prerequisite synthetic and macromolecular characterization of these new materials, the self-assembled supramolecular structures formed by the pentablock were experimentally evaluated. This synthesis and characterization process serves to elucidate the important structure property relationships of these novel materials, The pH and temperature responsive behavior of the pentablock copolymer were explored especially with consideration towards injectable drug delivery applications. Future synthesis work will focus on enhancing and tuning the cell specific targeting of DNA/pentablock copolymer polyplexes. The specific goals of this research are: (1) Develop a synthetic route for gel forming pentablock block copolymers with pH and temperature sensitive properties. Synthesis of these novel copolymers is accomplished with ATRP, yielding low polydispersity and control of the block copolymer architecture. Well defined macromolecular characteristics are required to tailor the phase behavior of these materials. (2) Characterize relationship between the size and shape of pentablock copolymer micelles and gel structure and the pH and temperature of the copolymer solutions with SAXS, SANS and CryoTEM. (3) Evaluate the temperature and pH induced phase separation and macroscopic self-assembly phenomenon of the pentablock copolymer. (4) Utilize the knowledge gained from first three goals to design and formulate drug delivery formulations based on the multi

  7. Synthesis and characterization of nanostructured powders of hydroxyapatite and β-calcium phosphate

    Energy Technology Data Exchange (ETDEWEB)

    Prants, W.T.; Muller, D.T.; Orzechowski, L.G.; Feit, G.; Delima, S.A.; Camargo, N.H.A.; Gemelli, E., E-mail: w_prants@hotmail.com, E-mail: danielt_muller@yahoo.com.br, E-mail: sarahamindelima@hotmail.com, E-mail: dem2nhac@joinville.udesc.br, E-mail: gemelli@joinville.udesc.br [Universidade do Estado de Santa Catarina (UDESC), Joinville, SC (Brazil). Campus Universitario Prof. Avelino Marcante

    2009-07-01

    Biphasic calcium phosphate (BCP) bioceramics are composed in a general manner from a mixture between hydroxyapatite (HA), and β-calcium phosphate. In the recent years, the BCP bioceramics are pointed out in researches from regeneration and reconstitution in osseous tissue, in reason of their similar mineralogical characteristics of the human bone structure, as great biodegradation, absorption and formation of precocious osseous tissue. The biphasic materials (BCP) are detached for use in medical and dental application, as filling bone cavities, maxillofacial treatment, medicaments discharge for treatment cancerous osteomyelitis and antibiotics discharge related with orthopedic injuries reparation. The aim of this work focused in synthesis and characterization of hydroxyapatite and β-calcium phosphate. The presented results are related with the mineralogical characterization with X-ray diffraction, thermal behavior with Differential Scanning Calorimetry and Dilatometer. The Scanning Electronic Microscopy (SEM) was used to help in the morphological characterization of the nanostructured powders. (author)

  8. Synthesis and characterization of nanostructured powders of hydroxyapatite and β-calcium phosphate

    International Nuclear Information System (INIS)

    Prants, W.T.; Muller, D.T.; Orzechowski, L.G.; Feit, G.; Delima, S.A.; Camargo, N.H.A.; Gemelli, E.

    2009-01-01

    Biphasic calcium phosphate (BCP) bioceramics are composed in a general manner from a mixture between hydroxyapatite (HA), and β-calcium phosphate. In the recent years, the BCP bioceramics are pointed out in researches from regeneration and reconstitution in osseous tissue, in reason of their similar mineralogical characteristics of the human bone structure, as great biodegradation, absorption and formation of precocious osseous tissue. The biphasic materials (BCP) are detached for use in medical and dental application, as filling bone cavities, maxillofacial treatment, medicaments discharge for treatment cancerous osteomyelitis and antibiotics discharge related with orthopedic injuries reparation. The aim of this work focused in synthesis and characterization of hydroxyapatite and β-calcium phosphate. The presented results are related with the mineralogical characterization with X-ray diffraction, thermal behavior with Differential Scanning Calorimetry and Dilatometer. The Scanning Electronic Microscopy (SEM) was used to help in the morphological characterization of the nanostructured powders. (author)

  9. 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.

  10. Synthesis and characterization of titanium oxide/bismuth sulfide nanorods for solar cells applications

    International Nuclear Information System (INIS)

    Solis, M.; Rincon, M. E.

    2008-01-01

    In the present work is showed the synthesis and characterization of titanium oxide/bismuth sulfide nanowires hetero-junctions for solar cells applications. Conductive glass substrates (Corning 25 x 75 mm) were coated with a thin layer of sol-gel TiO2 and used as substrates for the subsequent deposition of bismuth sulfide nanorods (BN). TiO2 films (∼400 nm) were deposited with a semiautomatic immersion system with controlled immersion/withdraw velocity, using titanium isopropoxide as the titania precursor [1]. For BN synthesis and deposition, the solvo-thermal method was used, introducing air annealed TiO2-substrates in the autoclave. The typical bilayer TiO2/BN hetero-junction was 600 nm thick. The synthesized materials (powders and films) were characterized by X-Ray Diffraction, Scanning Electron Microscopy, and UV-Visible Spectroscopy. Anatase was the crystalline phase of TiO2, while bismuth sulfide nanotubes show a diffraction pattern characteristic of bismuthinite distorted by the preferential growth of some planes [2-4]. The optoelectronic characterization of TiO2/NB hetero-junctions was compared with hetero-junctions obtained by sensitizing TiO2 with chemically deposited bismuth sulfide films. Bismuth sulfide nanowires are 2µm long and 70nm wide (aspect ratio L/D = 43), while chemically deposited bismuth sulfide have L/D = 1, therefore the effect of particle size evaluation and geometry in the photosensitization phenomena will be discussed in the context of new materials for solar-cells applications. (Full text)

  11. Synthesis and spectroscopic study of high quality alloy Cdx S ...

    Indian Academy of Sciences (India)

    Wintec

    In the present study, we report the synthesis of high quality CdxZn1–xS nanocrystals alloy at. 150°C with .... (XRD) using a Siemens model D 500, powder X-ray ... decays were analysed using IBH DAS6 software. 3. ... This alloying process is.

  12. Synthesis and characterization of rhodium sulfide nanoparticles and thin films

    International Nuclear Information System (INIS)

    Sosibo, Ndabenhle M.; Revaprasadu, Neerish

    2008-01-01

    The synthesis and characterization of a rhodium complex, [Rh(S 2 CNEt 2 ) 2 ] is described. The complex was thermolysed at a high temperature (280 deg. C) in the presence of capping agent, hexadecylamine (HDA) to form Rh 2 S 3 nanoparticles. Rod-shaped Rh 2 S 3 nanoparticles with an average length of 26.7 nm and an average breadth of 7.8 nm were synthesized. The complex was also used as a single molecule precursor for the deposition of Rh 2 S 3 thin films on a glass substrate at 350 deg. C and 450 deg. C using the Aerosol Assisted Chemical Vapour Deposition (AACVD) technique. The resultant thin films showed temperature dependent morphologies and showed (0 2 2), (4 1 1) and (6 1 1) lattice planes characteristic of to the orthorhombic Rh 2 S 3 phase. X-ray diffraction and scanning electron microscopy techniques were used to characterize the films

  13. Synthesis and characterization of rhodium sulfide nanoparticles and thin films

    Energy Technology Data Exchange (ETDEWEB)

    Sosibo, Ndabenhle M. [Department of Chemistry, University of Zululand, Private Bag X1001, KwaDlangezwa 3886 (South Africa); Revaprasadu, Neerish [Department of Chemistry, University of Zululand, Private Bag X1001, KwaDlangezwa 3886 (South Africa)], E-mail: nrevapra@pan.uzulula.za

    2008-05-15

    The synthesis and characterization of a rhodium complex, [Rh(S{sub 2}CNEt{sub 2}){sub 2}] is described. The complex was thermolysed at a high temperature (280 deg. C) in the presence of capping agent, hexadecylamine (HDA) to form Rh{sub 2}S{sub 3} nanoparticles. Rod-shaped Rh{sub 2}S{sub 3} nanoparticles with an average length of 26.7 nm and an average breadth of 7.8 nm were synthesized. The complex was also used as a single molecule precursor for the deposition of Rh{sub 2}S{sub 3} thin films on a glass substrate at 350 deg. C and 450 deg. C using the Aerosol Assisted Chemical Vapour Deposition (AACVD) technique. The resultant thin films showed temperature dependent morphologies and showed (0 2 2), (4 1 1) and (6 1 1) lattice planes characteristic of to the orthorhombic Rh{sub 2}S{sub 3} phase. X-ray diffraction and scanning electron microscopy techniques were used to characterize the films.

  14. Biogenic synthesis and spectroscopic characterization of silver nanoparticles using leaf extract of Indoneesiella echioides: in vitro assessment on antioxidant, antimicrobial and cytotoxicity potential

    Science.gov (United States)

    Kuppurangan, Gunaseelan; Karuppasamy, Balaji; Nagarajan, Kanipandian; Krishnasamy Sekar, Rajkumar; Viswaprakash, Nilmini; Ramasamy, Thirumurugan

    2016-10-01

    Natural synthesis of metal nanoparticles is gaining more attention in recent years. This article demonstrates the phytochemical synthesis of silver nanoparticles (AgNPs) by using Indoneesiella echioides (L) leaf extract as a reducing and stabilizing agent. Biosynthesis of AgNPs was monitored by UV-visible spectroscopy which revealed intense surface plasmon resonance bands at 420 nm. Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction were employed to identify various functional groups and crystalline nature of AgNPs. High-resolution transmission electron microscopy studies demonstrated that synthesized particles were spherical with average size of ~29 nm. In vitro antioxidant effects were analyzed by 2,2'-Azino-bis-(3-ethylbenzothiazoline-6-sulfonic acid) diammonium salt (ABTS) and 2,2-diphenyl-1-picrylhydrazyl (DPPH), which exhibited 69 and 71 % of scavenging activity, respectively. The antimicrobial activity of green AgNPs displayed better zone of inhibition against selected human pathogens. The present study also investigated the toxicity effect of biogenic AgNPs against human lung adenocarcinoma cancer cells (A549) and normal human epithelial cells (HBL-100) in vitro, and the inhibitory concentrations (IC50) were found to be 30 and 60 µg/mL, respectively. Herein, we propose a previously unexplored medicinal plant for the biological synthesis of AgNPs with potent biomedical applications.

  15. 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.

  16. Synthesis, characterization, and reactivity of furan- and thiophene-functionalized bis(n-heterocyclic carbene) complexes of iron(II)

    KAUST Repository

    Rieb, Julia; Raba, Andreas; Haslinger, Stefan; Kaspar, Manuel; Pö thig, Alexander; Cokoja, Mirza; Basset, Jean-Marie; Kü hn, Fritz

    2014-01-01

    The synthesis of iron(II) complexes bearing new heteroatom-functionalized methylene-bridged bis(N-heterocyclic carbene) ligands is reported. All complexes are characterized by single-crystal X-ray diffraction (SC-XRD), nuclear magnetic resonance

  17. Biogenic synthesis of silver nanoparticles by leaf extract of Cassia angustifolia

    Science.gov (United States)

    Amaladhas, T. Peter; Sivagami, S.; Akkini Devi, T.; Ananthi, N.; Priya Velammal, S.

    2012-12-01

    In this study Cassia angustifolia (senna) is used for the environmentally friendly synthesis of silver nanoparticles. Stable silver nanoparticles having symmetric surface plasmon resonance (SPR) band centred at 420 nm were obtained within 10 min at room temperature by treating aqueous solutions of silver nitrate with C. angustifolia leaf extract. The water soluble components from the leaves, probably the sennosides, served as both reducing and capping agents in the synthesis of silver nanoparticles. The nanoparticles were characterized using UV-Vis, Fourier transform infrared (FTIR) spectroscopic techniques and transmission electron microscopy (TEM). The nanoparticles were poly-dispersed, spherical in shape with particle size in the range 9-31 nm, the average size was found to be 21.6 nm at pH 11. The zeta potential was -36.4 mV and the particles were stable for 6 months. The crystalline phase of the nanoparticles was confirmed from the selected area diffraction pattern (SAED). The rate of formation and size of silver nanoparticles were pH dependent. Functional groups responsible for capping of silver nanoparticles were identified from the FTIR spectrum. The synthesized silver nanoparticles exhibited good antibacterial potential against Escherichia coli and Staphylococcus aureus.

  18. Biogenic synthesis of silver nanoparticles by leaf extract of Cassia angustifolia

    International Nuclear Information System (INIS)

    Peter Amaladhas, T; Akkini Devi, T; Ananthi, N; Priya Velammal, S; Sivagami, S

    2012-01-01

    In this study Cassia angustifolia (senna) is used for the environmentally friendly synthesis of silver nanoparticles. Stable silver nanoparticles having symmetric surface plasmon resonance (SPR) band centred at 420 nm were obtained within 10 min at room temperature by treating aqueous solutions of silver nitrate with C. angustifolia leaf extract. The water soluble components from the leaves, probably the sennosides, served as both reducing and capping agents in the synthesis of silver nanoparticles. The nanoparticles were characterized using UV–Vis, Fourier transform infrared (FTIR) spectroscopic techniques and transmission electron microscopy (TEM). The nanoparticles were poly-dispersed, spherical in shape with particle size in the range 9–31 nm, the average size was found to be 21.6 nm at pH 11. The zeta potential was –36.4 mV and the particles were stable for 6 months. The crystalline phase of the nanoparticles was confirmed from the selected area diffraction pattern (SAED). The rate of formation and size of silver nanoparticles were pH dependent. Functional groups responsible for capping of silver nanoparticles were identified from the FTIR spectrum. The synthesized silver nanoparticles exhibited good antibacterial potential against Escherichia coli and Staphylococcus aureus. (paper)

  19. Clays as green catalysts in the cholesterol esterification: spectroscopic characterization and polymorphs identification by thermal analysis methods. An interdisciplinary laboratorial proposal for the undergraduate level

    International Nuclear Information System (INIS)

    Maria, Teresa M R.; Nunes, Rui M. D.; Pereira, Mariette M.; Eusebio, M. Ermelinda S.

    2009-01-01

    A laboratory experiment that enables the professor to introduce the problematic of sustainable development in pharmaceutical chemistry to undergraduate students is proposed, using a simple synthetic procedure. Cholesteryl acetate is prepared by the esterification of cholesterol using Montmorillonite K10 as heterogeneous catalyst. Cholesterol and cholesteryl acetate are characterized by spectroscopic ( 1 H RMN, 13 C RMN, FTIR) and thermal analysis techniques. The thermal methods are used to introduce the concepts of polymorphism and the nature of mesophases. (author)

  20. Synthesis, characterization and properties

    Indian Academy of Sciences (India)

    Unknown

    work, we report herein the synthesis, structural cha- racterization and properties of a chiral Mn(IV) mononuclear ... atmosphere with a platinum disc working electrode, a platinum wire auxiliary electrode and a Ag/AgCl ... SMART APEX CCD area detector system [λ(Mo-. Kα) = 0⋅71073 Å], graphite monochromator, 2400.

  1. Synthesis And Characterization Of Mebrofenin For Hepatobiliary Imaging

    International Nuclear Information System (INIS)

    Purwoko; Tamat, Swasono R.; Yunita, Fitri; Kristanti, Eti

    2003-01-01

    Mebrofenin labeled with Technetium-99m is a new radiopharmaceutical having superior and ideal characteristic as a hepatobiliary-imaging agent. The synthesis and characterization of Mebrofenin (3-Bromo-2,4,6-trimethyl acetanilido iminodiacetic acid) as IDA derivative has been carried out involving three steps of reaction i.e. : acetyllization of 2,4,6-Trimethyl aniline to get 2,4,6-trimethyl chloro acetanilide which upon bromination gives the intermediate bromotrimethyl derivative and [mally by nucleophilic substitution this intermediate product with iminodiacetic acid (IDA) gives mebrofenin. The acetylation and bromination reactions were carried out in acetic acid condition while the substitution was carried out by reflux for 5 hours in ethanol and water adjusted at pH 11. The ethanol was then removed under low pressure, and the unreacted compound was removed by filtration. The filtrate was adjusted to pH 2 - 2.5, and the resulting mebrofenin was isolated by filtration and recrystallized 3 times in ethanol. Characterization of the mebrofenin product was performed by observing its melting point (197-l99 o C), ultra violet and infra red spectra as well as mass spectrometric and high performance liquid chromatographic analysis. The results showed that the product was highly pure and the yield was around 20%

  2. Synthesis and characterization of partially fluorinated poly(acryl) ionomers for polymer electrolyte membrane fuel cells and ESR-spectroscopic investigation of the radically induced degradation of model compounds; Synthese und Charakterisierung teilfluorierter Poly(acryl)-Ionomere als Polymerelektrolytmembranen fuer Brennstoffzellen und ESR-spektroskopische Untersuchung der radikalinduzierten Degradation von Modellverbindungen

    Energy Technology Data Exchange (ETDEWEB)

    Schoenberger, Frank

    2008-07-09

    In the first part of this work different strategies for the design of sulfonated partially fluorinated poly(aryl)s are developed and synthetically realized. The applied concept is that partially fluorinated poly(aryl)s are distinguished from the nonfluorinated ones by an enhanced acidity. Moreover they possess higher bond dissociation energies of both the C-F bonds and any adjacent C-H bonds which should be associated with a gain in radical stability and thus in chemical and thermal stability. In order to investigate the influence of the chemical structure of (partially fluorinated) monomeric building blocks, homo-polymers with different structural units (with aromatic C-F bonds, C(CF3)2-bridged and/or CF3-substituted phenylene rings) are synthesized by polycondensation and structurally characterized (elemental analysis, NMR spectroscopy, gel permeation chromatography). Established organic reactions, such as the Balz-Schiemann reaction, Suzuki reaction and Ullmann's biaryl synthesis, are applied for the synthesis of the specific monomers. After sulfonation of the homo-polymers (ionically crosslinked) membranes are prepared and characterized in terms of suitability as polymer electrolyte membrane in fuel cells (ion-exchange capacity, proton conductivity, thermal and chemical stability, water uptake, dimensional change). Both the chemical nature of the monomers and their constitution in the ionomer are important for the properties of the resulting membranes. Therefore microphase-separated multiblock-co-ionomers based on hydrophilic (sulfonated) and hydrophobic (partially fluorinated) telechelic macromonomers are prepared and characterized. Both the influence of the block length and the chemical nature of the used monomers on the membrane properties are comparatively investigated. On the basis of the findings gained in this part of the work, the advantages and disadvantages of partially fluorinated ionomer membranes are analyzed and discussed. The second part of

  3. Synthesis and characterization of poly aniline/wood and poly aniline/carbon composites

    International Nuclear Information System (INIS)

    Kanwal, F.; Siddiqi, S.A.; Tasleem, S.

    2009-01-01

    Conducting polymers have shown many applications in the field of nano science, nano technology and nuclear science. Poly aniline (PAN I) is the most studied conducting polymer due to its environmental stability, easy availability of its raw materials, and simple synthesis. We have synthesized poly aniline and two of its conducting composites i.e., poly aniline-carbon and poly aniline-wood in acidic medium (HCI) using K/sub 2/Cr/sub 2/O/sub 7/ as oxidizing agent. All samples were characterized by FTIR and four-probe d.c. conductivity methods The synthesis was carried out at two different temperatures (0 degree C and -5 degree C) and it was found that the yield and conductivity were maximum at lower temperature (-5 degree C). The poly aniline-carbon composites showed enhanced conductivity whereas poly aniline-wood composites showed reduced conductivity when compared with the conductivity of pure poly aniline. (author)

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

    Science.gov (United States)

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

    2012-12-01

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

  5. Applications of structural and spectroscopic techniques to the experimental and theoretical study of new luminescent materials

    International Nuclear Information System (INIS)

    Navarro Ahumada, Gustavo Adolfo

    2001-01-01

    This thesis discusses the general problem of the radiation-matter interaction in the case of a family of crystals known as elpasolites, which belong to the spatial group FM3M(O 5 H ). These systems present complications, from a theoretical as well as experimental point of view. The study was carried out in stoichiometric elpasolite type systems, characterized by empirical formulas of the general type Cs2NaLnCl 6 where Ln is a lanthanide of the first series of internal transition with electronic configurations for the trivalent state (Ln +3 ) of the form ∫ 1 → ∫ 13 . An analysis of the atomic spectra for these gaseous phase ions shows a diversity of permitted states, due to relativistic and non relativistic effects. Systems with positive trivalent lanthanide ions of the form Dy 3+ (∫ 9 ), Ho 3+ (∫ 10 ) y Er 3+ (∫ 11 ) have been selected at the level of the stoichiometric elpasolites and are characterized by complex energetic spectra. A careful experimental study of the emission states suggests that the elpasolite of Er 3+ is interesting, and its study is very relevant. The assignments and identifications of the peaks, during absorption as well as during emission, are more precise for the configuration Er 3+ , and careful studies show that fluorescence between terminal states with the rule of selection for the total orbital angular momentum:ΔJ = 6 is observed for this system. A declining cascade that can reasonably explain the unsuspected related spectral intensity, in the order of 10-9, is presented and suggested although a value was predicted for the electric dipolar force of lesser than 4 orders of magnitude what was observed. This problem is discussed and a mechanism is proposed for spectral intensities associated with two emissions characterized by ΔJ = 4 (electric hexadecapole) and ΔJ = 2 (electric cuadrupole). The laboratory tests made, include synthesis by solid state reactions of Dy 3+ and Ho 3+ , type elpasolites, structural characterization

  6. Synthesis, spectroscopic investigations, DFT studies, molecular docking and antimicrobial potential of certain new indole-isatin molecular hybrids: Experimental and theoretical approaches

    Science.gov (United States)

    Almutairi, Maha S.; Zakaria, Azza S.; Ignasius, P. Primsa; Al-Wabli, Reem I.; Joe, Isaac Hubert; Attia, Mohamed I.

    2018-02-01

    Indole-isatin molecular hybrids 5a-i have been synthesized and characterized by different spectroscopic methods to be evaluated as new antimicrobial agents against a panel of Gram positive bacteria, Gram negative bacteria, and moulds. Compound 5h was selected as a representative example of the prepared compounds 5a-i to perform computational investigations. Its vibrational properties have been studied using FT-IR and FT-Raman with the aid of density functional theory approach. The natural bond orbital analysis as well as HOMO and LUMO molecular orbitals investigations of compound 5h were carried out to explore its possible intermolecular delocalization or hyperconjugation and its possible interactions with the target protein. Molecular docking of compound 5h predicted its binding mode with the fungal target protein.

  7. Synthesis and characterization of iron nano particles for the arsenic removal in water

    International Nuclear Information System (INIS)

    Gutierrez M, O. E.

    2011-01-01

    The synthesis of iron nanoparticles for the removal of metallic ions in polluted waters has been during the last years study topic for different world organizations. This work presents a synthesis method of conditioned coal with iron nanoparticles starting from the use of leaves of pineapple crown, with the purpose of using it in arsenic removal processes in aqueous phase. For the synthesis of this material, the leaves of the pineapple crown were used like supports structure of the iron nanoparticles. First, the pyrolysis appropriate temperature was determined. For the preparation of the support material, this had contact with a ferric nitrate and hexamine solution, because the preparation of the material and the coal synthesis were realized during the pyrolysis process, where the hexamine molecules and the ferric nitrate react, causing the reduction of the iron particles and their dispersion on the support material, obtaining as product a conditioned coal with iron nanoparticles. For the characterization of the materials were used techniques as: Scanning electron microscopy, Transmission electron microscopy, X-Rays Diffraction), X-Ray photoelectron spectroscopy and Moessbauer spectroscopy; moreover was determined the isoelectric point and the density of surface sites. The arsenic sorption capacity of the materials was evaluated by means of the methodology type lots where was determined the sorption kinetics and isotherms in terms of arsenic concentration and mass. (Author)

  8. Synthesis and characterization of the natural and burned hydrotalcite

    International Nuclear Information System (INIS)

    Granados C, F.

    2006-01-01

    The synthesis and the structural and surface properties of the natural and burned hydrotalcite using salts of AlCl 3 and MgCl 2 .6H 2 O its were studied. Its were used those analysis of BET, IR, XRD, TGA and SEM to characterize these materials. The obtained product was identified as the natural or carbonated hydrotalcite of chemical formula Mg 6 Al 2 (OH) 16 CO 3 .4H 2 O. The hydrotalcite was roasted at 500 C during 5 h and the was obtained roasted hydrotalcite (HTC) that is a material of high selectivity toward the anions that it can be efficiently used as adsorbent material in studies of adsorption for the treatment of anionic radioactive waste present in watery solution. (Author)

  9. Synthesis and Characterization Pectin-Carboxymethyl Chitosan crosslinked PEGDE as biosorbent of Pb(II) ion

    Science.gov (United States)

    Hastuti, Budi; Siswanta, Dwi; Mudasir; Triyono

    2018-01-01

    Pectin and chitosan are biodegradable polymers, potentially applied as a heavy metal adsorbents. Unfortunately both biosorbents pectin and chitosan have a weakness in acidic media. For this purpose required modified pectin and chitosan. The modified adsorben is intended to obtain a stable adsorbent and resistance under acid. The research was done by experimental method in laboratory. The stages of this research are the synthesis of carboxymethyl chitosan (CMC), synthesis of Pec-CMC-PEGDE film adsorbent, stabily test under acid, the characterization of active group using FTIR, stability characterization of Pec-CMC-PEGDE powder adsorbent using XRD, termo stability using DTA-TGA. The results of the research have shown that: pectin and CMC can be cross-linked using PEGDE crosslinking agent, the film adsorbent was stable under HCl 1 M, the film adsorbent have active group comprise of carboxylate and amine groups. The result of characterization using XRD, shows that the adsorbent is semi-crystalline. Base on termo stability, the film adsorbent Pec-CMC-PEGDE stable up to 600°C. The film can be applied as an adsobent of Pb (II) ion remediation. The optimum pH of pec-CMC-PEGDE in adsorbed of Pb(II) was reached at pH 5 with 99.99% absorbent adsorbed and of and adsorption capacity was 46.11 mg/g.

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

    African Journals Online (AJOL)

    Preferred Customer

    Organophosphorus compounds have wide range of applications in the industrial, agricultural and medicinal chemistry owing to their unique physicochemical and biological properties. Their utility as reagents and potential synthons in organic synthesis is gaining increased attention [1]. Synthesis of a-aminophosphonates, ...

  11. Synthesis, Characterization, and Properties of the Two-Dimensional Chalcogenides: Monolayers, Alloys, and Heterostructures

    Science.gov (United States)

    Cain, Jeffrey D.

    Inspired by the triumphs of graphene, and motivated by its limitations, the science and engineering community is rapidly exploring the landscape of other layered materials in their atomically-thin forms. Dominating this landscape are the layered chalcogenides; diverse in chemistry, crystal structure, and properties, there are well over 100 primary members of this material family. Driven by quantum confinement, single layers (or few, in some cases) of these materials exhibit electronic, optical, and mechanical properties that diverge dramatically from their bulk counterparts. While initially isolated in monolayer form via mechanical exfoliation, the field of two-dimensional (2D) materials is being forced evolve to more scalable and reliable methods. Focusing on the chalcogenides (e.g. MoS2, Bi 2Se3, etc.), this dissertation introduces and mechanistically examines multiple novel synthetic approaches for the direct growth of monolayers, heterostructures, and alloys with the desired quality, reproducibility and generality. The first methods described in this thesis are physical vapor transport (PVT) and evaporative thinning (ET): a facile, top-down synthesis approach for creating ultrathin specimens of layered materials down to the two-dimensional limit. Evaporative thinning, applied in this study to the fabrication of A2X3 (Bi2Se3 and Sb2Te3) monolayers, is based on the controlled evaporation of material from initially thick specimens until the 2D limit is reached. The resultant flakes are characterized with a suite of imaging and spectroscopic techniques and the mechanism of ET is investigated via in-situ heating within a transmission electron microscope. Additionally, the basic transport properties of the resultant flakes are probed. The growth of ultrathin GeSe flakes is explored using PVT and the material's basic structure, properties, and stability are addressed. Second, oxide precursor based chemical vapor deposition (CVD) is presented for the direct growth of

  12. Cobalt(ll) Coordination Compounds of Ethyl 4-Methyl-5-Imidazolecarboxylate: Chemical and Biochemical Characterization on Photosynthesis and Seed Germination

    OpenAIRE

    King-Díaz, Beatriz; Montes-Ayala, Josefina; Escartín-Guzmán, Concepción; Castillo-Blum, Silvia E.; Iglesias-Prieto, Roberto; Lotina-Hennsen, Blas; Barba-Behrens, Norah

    2005-01-01

    In this work we present the synthesis, structural and spectroscopic characterization of Co2+ coordination compounds with ethyl 4-methyl-5-imidazolecarboxylate (emizco). The effects of emizco, the metal salts CoCl2.6H2O, CoBr2, Co(NO3)2.6H2O and their metal coordination compounds [Co(emizco)2Cl2], [Co(emizco)2 Br2].H2O, [Co(emizco)2 (H2O)2(NO2)2.2H2O were evaluated on photosynthesis in spinach chloroplasts. Seed germination and seedling growth of the monocotyledonous species Lolium multiflorum...

  13. Synthesis and structural characterization of piperazino-modified DNA that favours hybridization towards DNA over RNA

    DEFF Research Database (Denmark)

    Skov, Joan; Bryld, Torsten; Lindegaard, Dorthe

    2011-01-01

    We report the synthesis of two C4'-modified DNA analogues and characterize their structural impact on dsDNA duplexes. The 4'-C-piperazinomethyl modification stabilizes dsDNA by up to 5°C per incorporation. Extension of the modification with a butanoyl-linked pyrene increases the dsDNA stabilizati...

  14. Synthesis, molecular structure, spectroscopic properties and stability of (Z)-N-methyl-C-2,4,6-trimethylphenylnitrone

    Science.gov (United States)

    Lasri, Jamal; Ismail, Ali I.; Haukka, Matti; Soliman, Saied M.

    2015-02-01

    New N-methyl-C-2,4,6-trimethylphenylnitrone 1 has been synthesized starting from N-methylhydroxylamine and mesitaldehyde. The product was fully characterized using different spectroscopic techniques; FTIR, NMR, UV-Vis, high resolution mass spectrometry and X-ray diffraction. The relative stability and percent of population of its two possible isomers (E and Z) were calculated using the B3LYP/6-311++G(d,p) method in gas phase and in solution. In agreement with the X-ray results, it was found that Z-isomer is the most stable one in both gas phase and solution. The molecular geometry, vibrational frequencies, gauge-including atomic orbital (GIAO), and chemical shift values were also calculated using the same level of theory. The TD-DFT results of the studied nitrone predicted a π-π∗ transition band at 285.1 nm (fosc = 0.3543) in the gas phase. The rest of the spectral bands undergo either hyperchromic or hypsochromic shifts in the presence of solvent. Polarizability and HOMO-LUMO gap values were used to predict the nonlinear optical properties (NLO) of the studied compound. NBO analysis has been used to determine the most accurate Lewis structure of the studied molecule.

  15. Chemically stabilized reduced graphene oxide/zirconia nanocomposite: synthesis and characterization

    Science.gov (United States)

    Sagadevan, Suresh; Zaman Chowdhury, Zaira; Enamul Hoque, Md; Podder, Jiban

    2017-11-01

    In this research, chemical method was used to fabricate reduced graphene oxide/zirconia (rGO/ZrO2) nanocomposite. X-ray Diffraction analysis (XRD) was carried out to examine the crystalline structure of the nanocomposites. The nanocomposite prepared here has average crystallite size of 14 nm. The surface morphology was observed using scanning electron microscopic analysis (SEM) coupled with electron dispersion spectroscopy (EDS) to detect the chemical element over the surface of the nanocomposites. High-resolution Transmission electron microscopic analysis (HR-TEM) was carried out to determine the particle size and shape of the nanocomposites. The optical property of the prepared samples was determined using UV-visible absorption spectrum. The functional groups were identified using FTIR and Raman spectroscopic analysis. Efficient, cost effective and properly optimized synthesis process of rGO/ZrO2 nanocomposite can ensure the presence of infiltrating graphene network inside the ZrO2 matrix to enhance the electrical properties of the hybrid composites up to a greater scale. Thus the dielectric constant, dielectric loss and AC conductivity of the prepared sample was measured at various frequencies and temperatures. The analytical results obtained here confirmed the homogeneous dispersion of ZrO2 nanostructures over the surface of reduced graphene oxide nanosheets. Overall, the research demonstrated that the rGO/ZrO2 nano-hybrid structure fabricated here can be considered as a promising candidate for applications in nanoelectronics and optoelectronics.

  16. Synthesis of gold nanochains via photoactivation technique and their catalytic applications.

    Science.gov (United States)

    Sinha, Arun Kumar; Basu, Mrinmoyee; Sarkar, Sougata; Pradhan, Mukul; Pal, Tarasankar

    2013-05-15

    The article reports a simple photoactivation technique for the synthesis of chain like assembly of spherical Au nanocrystals using a nontoxic biochemical, β-cyclodextrin under ~365 nm UV-light irradiation. Under UV irradiation, β-cyclodextrin acts as a reducing as well as capping agent and eventually becomes a stabilizing linker for Au nanoparticles. The UV-visible spectroscopy, transmission electron microscopy (TEM), selected area electron diffraction (SAED), X-ray diffraction (XRD), and X-ray photoelectron spectroscopic techniques are employed to systematically characterize the Au nanochains. Additionally, it is shown that the Au nanocrystals act as an effective catalyst for the reduction in nitrobenzene to aniline and methylene blue to leuco methylene blue in presence of suitable reducing agent. The catalytic reduction reactions and kinetic parameters are evaluated from UV-visible spectroscopy. Copyright © 2013 Elsevier Inc. All rights reserved.

  17. The nitro-reduced metabolite of nimesulide: Crystal structure, spectroscopic characterization, ESI-QTOF mass spectrometric analysis and antibacterial evaluation

    Science.gov (United States)

    Nunes, Julia H. B.; Nakahata, Douglas H.; Lustri, Wilton R.; Corbi, Pedro P.; de Paiva, Raphael E. F.

    2018-04-01

    Here we present a synthetic procedure, spectroscopic characterization and single-crystal X-ray structure for the nitro-reduced metabolite of the anti-inflammatory drug nimesulide, hereby referred to as NMS-NH2. The nitro-reduced metabolite was synthesized using the Béchamp reduction (iron powder under acidic media), leading to the conversion of the nitrobenzene group of nimesulide to an aniline. Mass spectrometry, infrared and nuclear magnetic resonance spectroscopies data are also provided for NMS-NH2, and discussed in comparison to nimesulide. NMS-NH2 was also evaluated in terms of its antibacterial activities, considering that the free sbnd NH2 group could allow the compound to act as a dihydropteroate synthase inhibitor. NMS-NH2 had a modest antibacterial activity against P. aeruginosa (5.0 mg mL-1), which was not observed for NMS.

  18. Synthesis of hexavalent molybdenum formo- and aceto-hydroxamates and deferoxamine via liquid-liquid metal partitioning

    Energy Technology Data Exchange (ETDEWEB)

    Breshears, Andrew T.; Brown, M. Alex; Bloom, Ira; Barnes, Charles L.; Gelis, Artem V.

    2018-03-01

    We report a new method of crystal growth and synthesis based on liquid-liquid partitioning that allows for isolation and in-depth characterization of molybdenyl bis(formohydroxamate), Mo-FHA, molybdenyl bis(acetohydroxamate), Mo-AHA, and molybdenyl deferoxamine, Mo-DFO, for the first time. This novel approach affords shorter crystal growth time (hourly timeframe) without sacrificing crystal size or integrity when other methods of crystallization were unsuccessful. All three Mo complexes are characterized in solution via FTIR, NMR, UV-vis, and EXAFS spectroscopy. Mo-AHA and Mo-FHA structures are resolved by single crystal X-ray diffraction. Using the molybdenyl hydroxamate structural information, the speciation of Mo in a siderophore complex (Mo-DFO) is determined via complimentary spectroscopic methods and confirmed by DFT calculations. ESI-MS verifies that a complex of 1:1 molybdenum to deferoxamine is present in solution. Additionally, the Mo solution speciation in the precursor organic phase, MoO2(NO3)2HEH[EHP]2 (where HEH[EHP] is 2-ethylhexylphosphonic acid mono-2-ethylhexyl ester), is characterized by FTIR and EXAFS spectroscopy as well as DFT calculations.

  19. Synthesis and characterization of a new composite based on copper (II) and octa (aminopropil)silsesquioxane; Sintese e caracterizacao de novos compositos a base de cobre (II) e octa(aminopropil)silsesquioxano

    Energy Technology Data Exchange (ETDEWEB)

    Magossi, M.S. de; Carmo, D.R. do, E-mail: marymagossi@gmail.com [Universidade Estadual Paulista Julio de Mesquita Filho (UNESP), Ilha Solteira, SP (Brazil). Faculdade de Engenharia

    2014-07-01

    In this work, a new compound based silsesquioxane and nitroprusside of copper was prepared starting from octa (aminopropyl)silsesquioxane following a new route of synthesis. The composite prepared as described ACCuN was preliminarily characterized by spectroscopic techniques, such as Infrared Spectroscopy in the Region of the Fourier transform (FTIR), Energy Dispersive X-ray (EDX), Scanning Electron Microscopy (SEM) and cyclic voltammetry (VC). The FTIR spectra showed absorption bands at 1106 cm{sup -1} due to stretching Si-O-Si{sub (νSi-O-Si)} characteristic of the structure of octa(aminopropylsilsesquioxane and absorption bands at 2063 cm{sup -1} ascribed to the stretching NO{sub (νN-O}) and 2192 cm{sup -1} attributed to the stretching C≡N{sub (ν≡}N{sub )}. SEM and EDX observed cluster of cubic particles with an average size of approximately 241 nm, containing Si, O, N, Cu and Fe. Cyclic voltammogram of the material (ACCuN) showed a redox couple with average potential Eθ '= 0.73 V. (author)

  20. Characterizing Nanophase Materials on Mars: Spectroscopic Studies of Allophane and Imogolite

    Science.gov (United States)

    Jeute, Thomas; Baker, Leslie; Bishop, Janice; Rampe, Elizabeth; Abidin, Zaenal

    2017-01-01

    Allophane is an amorphous or poorly crystalline hydrous aluminosilicate material. Allophane's chemical structure represents a hollow nanosphere, 5-6 nm in diameter with 4-7 large pores in the structure. Identification of allophane and other amorphous and nanophase minerals on Mars has provided clues about the aqueous geochemical environment there. These materials likely represent partially altered or leached basaltic ash and therefore, could represent a geologic marker for where water was present on the Martian surface; as well as indicate regions of climate change, where surface water was not present long enough or sufficiently warm to form clays. Characterization of these materials is important for increasing spectral recognition capabilities using visible/near-infrared (VNIR) and thermal infrared (TIR) spectra of Mars. A suite of synthetic allophane samples was created using a method that has been modified to produce allophane with Fe isomorphically substituted for Al in octahedral coordination. Compositions of the materials range from high-Si allophane (molar Al:Si = 1:2) to protoimogolite (Al:Si = 2:1), with Fe(3+) and Fe(2+) isomorphically substituted for Al from 0-10 mol% of total Al. These compositions span the range observed in natural terrestrial allophanes. Fe K-edge X-ray absorption spectroscopy provided information on the speciation and electrochemical and structural position of Fe in the framework. Fourier transform infrared spectroscopy confirmed syntheses and demonstrated changes in infrared spectroscopic signature with Fe substitution. VNIR reflectance spectra and TIR Thermal infrared emissivity spectra were also collected for direct comparison to Martian data. By increasing spectral recognition capacities of nanophase materials, more accurate estimates can be made on the aqueous geochemical environment of Mars.

  1. The synthesis, characterization, crystal structure and theoretical calculations of a new meso-BOBIPY substituted phthalonitrile

    International Nuclear Information System (INIS)

    Sen, Pinar; Yildiz, S. Zeki; Atalay, Yusuf; Dege, Necmi; Demirtas, Günes

    2014-01-01

    A novel 4-(2-meso-BOBIPY-phenoxy)phthalonitrile (6) derivative has been synthesized starting from BF 3 –OEt 2 complex and 4-(2-meso-dipyrromethene-phenoxy)phthalonitrile (5) which was prepared by the oxidation of 4-(2-meso-dipyrromethane-phenoxy)phthalonitrile (4). The final product exhibit noticeable spectroscopic properties which were examined by its absorption and fluorescence emission spectra. The original compounds prepared in the reaction pathway were characterized by the combination of FT-IR, 1 H and 13 C NMR, UV–vis, MS and HRMS spectral data. The final product (6) was obtained as single crystal which crystallized in the triclinic space group P-1 with a=7.9411 (6) Å, b=9.0150 (6) Å, c=14.419 (1) Å, α=74.917 (5)°, β=86.824 (6)°, γ=84.109 (5)° and Z=2. The crystal structure has intermolecular C–H···F–B and C–H···N interactions. These interactions construct bifurcated hydrogen bonds in the crystal structure. In this study, It has been calculated; molecular structure, vibrational frequencies, 1 H and 13 C NMR chemical shifts and HOMO and LUMO energies of the title compound by using B3LYP method with 6–311++G(dp) basis set, and the electronic spectral characterization was investigated for the target product, as well. - Highlights: • A novel 4-(2-meso-BOBIPY-phenoxy)phthalonitrile derivative has been synthesized. • The title product exhibit noticeable spectroscopic properties which were examined by its absorption and fluorescence emission spectra. • The final product (6) was obtained as single crystal which crystallized in the triclinic space group. • Molecular structure, vibrational frequencies, 1 H and 13 C NMR chemical shifts and HOMO and LUMO energies of the title compound were calculated theoretically. • The electronic spectral characterization was investigated, as well. • The title compound is also open to prepare further BODIPY substituted oligomeric molecules via on it

  2. Synthesis and Characterization of Pine Needles Reinforced RF Matrix Based Biocomposites

    Directory of Open Access Journals (Sweden)

    A. S. Singha

    2008-01-01

    Full Text Available Synthesis and characterization of pine needles reinforced thermosetting resin (Resorcinol-Formaldehyde which is most suitable as composite matrix has been reported. The polycondensation reaction between resorcinol and formaldehyde (RF in different molar ratios has been applied to the synthesis of RF polymer matrix. A thermosetting resin based composite, containing approximately 10, 20, 30 and 40% of natural fiber by weight, has been obtained by adding pine needles to the Resorcinol-Formaldehyde (RF resin. The mechanical properties of randomly oriented intimately mixed particle reinforced (Pine needles composites were determined. Effect of fiber loading in terms of weight % on mechanical properties such as tensile, compressive, and flexural and wear properties have also been evaluated. The reinforcing of the resin with Pine needles was accomplished in particle size of 200 micron by employing optimized resin. Present work reveals that mechanical properties of the RF resin increases to extensive extent when reinforced with Pine needles. Thermal (TGA/DTA and morphological studies (SEM of the resin, fiber and polymer composites thus synthesized have also been carried out.

  3. Copper nanoparticles mediated by chitosan: synthesis and characterization via chemical methods.

    Science.gov (United States)

    Usman, Muhammad Sani; Ibrahim, Nor Azowa; Shameli, Kamyar; Zainuddin, Norhazlin; Yunus, Wan Md Zin Wan

    2012-12-14

    Herein we report a synthesis of copper nanoparticles (Cu-NPs) in chitosan (Cts) media via a chemical reaction method. The nanoparticles were synthesized in an aqueous solution in the presence of Cts as stabilizer and CuSO(4)·5H(2)O precursor. The synthesis proceeded with addition of NaOH as pH moderator, ascorbic acid as antioxidant and hydrazine( )as the reducing agent. The characterization of the prepared NPs was done using ultraviolet-visible spectroscopy, which showed a 593 nm copper band. The Field Emission Scanning Electron Microscope (FESEM) images were also observed, and found to be in agreement with the UV-Vis result, confirming the formation of metallic Cu-NPs. The mean size of the Cu-NPs was estimated to be in the range of 35-75 nm using X-ray diffraction. XRD was also used in analysis of the crystal structure of the NPs. The interaction between the chitosan and the synthesized NPs was studied using Fourier transform infrared (FT-IR) spectroscopy, which showed the capping of the NPs by Cts.

  4. Synthesis, spectroscopic and catalytic properties of some new boron hybrid molecule derivatives by BF2 and BPh2 chelation

    Science.gov (United States)

    Kilic, Ahmet; Alcay, Ferhat; Aydemir, Murat; Durgun, Mustafa; Keles, Armagan; Baysal, Akın

    2015-05-01

    A new series of Schiff base ligands (L1-L3) and their corresponding fluorine/phenyl boron hybrid complexes [LnBF2] and [LnBPh2] (n = 1, 2 or 3) have been synthesized and well characterized by both analytical and spectroscopic methods. The Schiff base ligands and their corresponding fluorine/phenyl boron hybrid complexes have been characterized by NMR (1H, 13C and 19F), FT-IR, UV-Vis, LC-MS, and fluorescence spectroscopy as well as melting point and elemental analysis. The fluorescence efficiencies of phenyl chelate complexes are greatly red-shifted compared to those of the fluorine chelate analogs based on the same ligands, presumably due to the large steric hindrance and hard π → π∗ transition of the diphenyl boron chelation, which can effectively prevent molecular aggregation. The boron hybrid complexes were applied to the transfer hydrogenation of acetophenone derivatives to 1-phenylethanol derivatives in the presence of 2-propanol as the hydrogen source. The catalytic studies showed that boron hybrid complexes are good catalytic precursors for transfer hydrogenation of aromatic ketones in 0.1 M iso-PrOH solution. Also, we have found that both steric and electronic factors have a significant impact on the catalytic properties of this class of molecules.

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

    African Journals Online (AJOL)

    Purpose: To develop a novel approach to green synthesis of nano-polymer porous gold oxide nanoparticles, and examine the effects of the temperatures on their surface. Methods: Green synthesis of nano-polymer porous gold oxide nanoparticles (GONPs) using cetyle trimethylammonium bromide (CTAB) surfactant with a ...

  6. Synthesis and Characterizations of Poly(3-hexylthiophene and Modified Carbon Nanotube Composites

    Directory of Open Access Journals (Sweden)

    Mohammad Rezaul Karim

    2012-01-01

    Full Text Available Poly(3-hexylthiophene and modified (functionalized and silanized multiwall carbon nanotube (MWNT nanocomposites have been prepared through in situ polymerization process in chloroform medium with FeCl3 oxidant at room temperature. The composites are characterized through Fourier transfer infrared spectroscopy (FT-IR, Raman, and X-ray diffraction (XRD measurements to probe the nature of interaction between the moieties. Optical properties of the composites are measured from ultraviolet-visible (UV-Vis and photoluminescence (PL spectroscopy. Conductivity of the composites is followed by four probe techniques to understand the conduction mechanism. The change (if any in C=C symmetric and antisymmetric stretching frequencies in FT-IR, the shift in G band frequencies in Raman, any alterations in λmax of UV-Vis, and PL spectroscopic measurements are monitored with modified MWNT loading in the polymer matrix.

  7. Synthesis and antimicrobial evaluation of the new Isoxazole and Pyrazole derivatives

    International Nuclear Information System (INIS)

    Goda, F.E.; Maarouf, A.R.; El-Bendary, E.R.

    2003-01-01

    A series of 3-methyl-4-substituted (phenylazo) isoxazolin-5-ones(5a,b),pyrazolin-5-ones (6a-d)and pyrazolidin-3,5-diones(10a-c) have been synthesized and evaluated for their antimicrobial activities.The detailed synthesis , spectroscopic and biogical data are reported. (author)

  8. Synthesis and antibacterial characterization of sustainable nanosilver using naturally-derived macromolecules

    Energy Technology Data Exchange (ETDEWEB)

    Osonga, Francis J.; Kariuki, Victor M.; Yazgan, Idris; Jimenez, Apryl; Luther, David; Schulte, Jürgen; Sadik, Omowunmi A., E-mail: osadik@binghamton.edu

    2016-09-01

    Greener nanosynthesis utilizes fewer amounts of materials, water, and energy; while reducing or replacing the need for organic solvents. A novel approach is presented using naturally-derived flavonoids including Quercetin pentaphosphate (QPP), Quercetin sulfonic acid (QSA) and Apigenin Triphosphate (ATRP). These water soluble, phosphorylated flavonoids were utilized both as reducing agent and stabilizer. The synthesis was achieved at room temperature using water as a solvent and it requires no capping agents. The efficiency of the resulting silver nanoparticle synthesis was compared with naturally-occurring flavonoid such as Quercetin (QCR). Results show that QCR reduced Ag{sup +} faster followed by QPP, QSA and ATRP respectively. This is the first evidence of direct utilization of QCR for synthesis of silver nanoparticles (AgNPs) in water. The percentage conversion of Ag{sup +} to Ag{sup 0} was determined to be 96% after 35 min. The synthesized nanoparticles were characterized using Transmission electron microscopy (TEM), Energy dispersive absorption spectroscopy (EDS), UV–vis spectroscopy, High resolution TEM (HR-TEM) with selected area electron diffraction (SAED). The particle sizes ranged from 2 to 80 nm with an average size of 22 nm and in the case of ATRP, the nanoparticle shapes varied from spherical to hexagonal with dispersed particle size ranging from 2 to 30 nm. Crystallinity was confirmed by XRD and the SAED of (111), (200), and the fringes observed in HRTEM images. Results were in agreement with the UV resonance peaks of 369–440 nm. The particles also exhibit excellent antibacterial activity against Staphylococcus epidermidis, Escherichia coli and Citrobacter freundii in water. - Highlights: • Greener nanosilver prepared using flavonoid derivatives • Synthesized nanosilver exhibits exhibit antibacterial activity. • Approach suitable for industrial synthesis.

  9. SYNTHESIS, CHARACTERIZATION AND DENSITY FUNCTIONAL ...

    African Journals Online (AJOL)

    Preferred Customer

    We synthesized a number of aniline derivatives containing acyl groups to compare their barriers of rotation around ... KEY WORDS: Monoacyl aniline, Synthesis, Density functional theory, Rotation barrier. INTRODUCTION. Developments in ...

  10. Synthesis of 13C and 2H labelled retinals: spectroscopic investigations on isotopically labelled rhodopsin and bacteriorhodopsin

    International Nuclear Information System (INIS)

    Pardoen, J.A.

    1986-01-01

    In order to develop probes of the structure of chromophores, the author introduces isotopic modifications at specific chromophoric positions as structural probes. To obtain bacteriorhodopsin, rhodopsin and their photoproducts labelled in the chromophore at selected positions, bacterioopsin and opsin were reacted with the appropriate labelled a11-trans and 11-cis retinals. The author describes the synthesis of a11-trans retinal selectively 13 C labelled at different positions. The characterization of these labelled a11-trans retinals by mass spectrometry, 300 MHz 1 H NMR and 75 MHz 13 C NMR spectroscopy is given. The photochemical preparation and isolation of the pure 9-, 11- and 13-cis forms is described in the experimental part. (Auth.)

  11. New Homologues Series of Heterocyclic Schiff Base Ester: Synthesis and Characterization

    Directory of Open Access Journals (Sweden)

    Yee-Ting Chong

    2016-01-01

    Full Text Available A homologous series of liquid crystal bearing with heterocyclic thiophene Schiff base ester with alkanoyloxy chain (CH3(CH2nCOO–, where n=4, 6, 8, 10, 12, 14, 16 was successfully synthesized through the modification of some reported methods. The structural information of these compounds was isolated and characterized through some spectroscopic techniques, such as FTIR, 1H, and 13C NMR and elemental analysis. Textural observation was carried out using a polarizing optical microscope (POM over heating and cooling cycles. It was found that all synthesized compounds (3a–g exhibited an enantiotropic nematic phase upon the heating and cooling cycle with high thermal stability. Moreover, a characteristic bar transition texture was observed for compounds 3f and 3g which have shown transition of nematic-to-smectic C phase. This has been further confirmed by obtaining relative phase transition temperature using the differential scanning calorimetry (DSC.

  12. Fluorido complexes of technetium

    International Nuclear Information System (INIS)

    Mariappan Balasekaran, Samundeeswari

    2013-01-01

    Fluorine chemistry has received considerable interest during recent years due to its significant role in the life sciences, especially for drug development. Despite the great nuclear medicinal importance of the radioactive metal technetium in radiopharmaceuticals, its coordination chemistry with the fluorido ligand is by far less explored than that of other ligands. Up to now, only a few technetium fluorides are known. This thesis contains the synthesis, spectroscopic and structural characterization of novel technetium fluorides in the oxidation states ''+1'', ''+2'', ''+4'' and ''+6''. In the oxidation state ''+6'', the fluoridotechnetates were synthesized either from nitridotechnetic(VI) acid or from pertechnetate by using reducing agent and have been isolated as cesium or tetraethylammonium salts. The compounds were characterized spectroscopically and structurally. In the intermediate oxidation state ''+4'', hexafluoridotechnetate(IV) was known for long time and studied spectroscopically. This thesis reports novel and improved syntheses and solved the critical issues of early publications such as the color, some spectroscopic properties and the structure of this key compound. Single crystal analyses of alkali metal, ammonium and tetramethylammonium salts of hexafluoridotechnetate(IV) are presented. In aqueous alkaline solutions, the ammonium salt of hexafluoridotechnetate(IV) undergoes hydrolysis and forms an oxido-bridged dimeric complex. It is the first step hydrolysis product of hexafluoridotechnetate(IV) and was characterized by spectroscopic and crystallographic methods. Low-valent technetium fluorides with the metal in the oxidation states of ''+2'' or ''+1'' are almost unknown. A detailed description of the synthesis and characterization of pentafluoridonitrosyltechnetate(II) is presented. The complex was isolated as alkali metal salts, and spectroscopic as well as structural features of the complexes are presented. Different salts of the trans

  13. Tuned apatitic materials: Synthesis, characterization and potential antimicrobial applications

    Science.gov (United States)

    Fierascu, Irina; Fierascu, Radu Claudiu; Somoghi, Raluca; Ion, Rodica Mariana; Moanta, Adriana; Avramescu, Sorin Marius; Damian, Celina Maria; Ditu, Lia Mara

    2018-04-01

    Inorganic antimicrobial materials can be viable for multiple applications (related to its use for new buildings with special requirements related to microbiological loading, such as hospital buildings and for consolidation of cultural heritage constructions); also the use of substituted hydroxyapatites for protection of stone artefacts against environmental factors (acidic rain) and biodeterioration it's an option to no longer use of toxic substances. This paper presents methods of synthesis and characterization of the material from the point of view of the obtained structures and final applications. The materials were characterized in terms of composition and morphology (using X-ray Diffraction, X-ray Fluorescence, Inductively coupled plasma-atomic emission spectrometry, Fourier Transform Infrared Spectroscopy, X-ray Photoelectron Spectroscopy, Surface area and pore size determination). Antimicrobial activity was tested against filamentous fungi strains and pathogenic bacteria strains, using both spot on lawn qualitative method (on agar medium) and serial microdilution quantitative method (in broth medium). Further, it was evaluated the anti-biofilm activity of the tested samples toward the most important microbial strains implicated in biofilm development, using crystal violet stained biofilms microtiter assay, followed by spectrophotometric quantitative evaluation.

  14. SYNTHESIS AND CHARACTERIZATION OF FUNCTIONALIZED ...

    African Journals Online (AJOL)

    In addition, these compounds have emerged as potential calcium ... As a consequence, the synthesis of dihydropyrimidinone derivatives has ..... Ramazani, A.; Shaghaghi,Z.; Aghahosseini, H.; Asiabi, P.A.; Joo, S.W. Silica nanoparticles.

  15. Synthesis and characterization of functional magnetic nanocomposites

    Science.gov (United States)

    Gass, J.; Sanders, J.; Srinath, S.; Srikanth, H.

    2006-03-01

    Magnetic nanoparticles and carbon nanotubes have been excellent functional materials that could be dispersed in polymer matrices for various applications. However, uniform dispersion of particles in polymers without agglomeration is quite challenging. We have fabricated PMMA/polypyrrole bilayer structures embedded with Fe3O4 magnetite nanoparticles synthesized using wet chemical synthesis. Agglomeration-free dispersion of nanoparticles was achieved by coating the particles with surfactants and by dissolving both the particles and PMMA in chlorobenzene. Structural characterization was done using XRD and TEM. Magnetic properties of the bilayer structures indicated superparamagnetic behavior that is desirable for RF applications as the magnetic losses are reduced. Our polymer nanocomposite bilayer films with conducting polymer coatings are potential candidates for tunable RF applications with integrated EMI suppression. We will also report on our studies of pumped ferrofluids flowing past carbon nanotubes that are arranged in microchannel arrays. Magnetization under various flow conditions is investigated and correlated with the hydrodynamic properties. This scheme provides a novel method of energy conversion and storage using nanocomposite materials.

  16. Improved Synthesis of 2',6'-Dihydroxy-3,4-dimethoxy Chalcone by Grinding Technique to Synthesize 5-Hydroxy-3',4'-dimethoxy Flavone

    Directory of Open Access Journals (Sweden)

    Elfi Susanti VH

    2014-07-01

    Full Text Available 5-hydroxy-3',4'-dimethoxy flavone can be efficiently synthesized in two steps via the formation of 2',6'-dihydroxy-3,4-dimethoxy chalcone with good results. 2',6'-dihydroxy-3,4-dimethoxy chalcone as reactants for synthesis of flavones was prepared through Claisen-Schmidt condensation reaction between 2,6-dihydroxyacetophenones,3,4-dimethoxybenzaldehyde and solid NaOH in mortar for 15 min. The yield of the product (70% is higher than conventional method (65%. This chalcone then oxidatively cyclized with iodine to form 5-hydroxy-3',4'-dimethoxy flavone (yield 62%. Compounds synthesized were characterized by spectroscopic (IR, 1H-NMR, and 13C-NMR.

  17. Synthesis and Doping of Ligand-Protected Atomically-Precise Metal Nanoclusters

    KAUST Repository

    Aljuhani, Maha A.

    2016-05-01

    Rapidly expanding research in nanotechnology has led to exciting progress in a versatile array of applications from medical diagnostics to catalysis. This success resulted from the manipulation of the desired properties of nanomaterials by controlling their size, shape, and composition. Among the most thriving areas of research about nanoparticle is the synthesis and doping of the ligand-protected atomically-precise metal nanoclusters. In this thesis, we developed three different novel metal nanoclusters, such as doped Ag29 with five gold (Au) atoms leading to enhance its quantum yield with remarkable stability. We also developed half-doped (alloyed) cluster of Ni6 nanocluster with molybdenum (Mo). This enabled enhanced stability and better catalytic activity. The third metal nanocluster that we synthesized was Au28 nanocluster by using di-thiolate as the ligand stabilizer instead of mono-thiolate. The new metal clusters obtained have been characterized by spectroscopic, electrochemical and crystallographic methods.

  18. The Synthesis and Luminescence-spectroscopic Properties of Fluorescent Condensation Polymers

    Science.gov (United States)

    Barashkov, Nikolai N.

    1985-07-01

    The results of studies on the synthesis of polycondensation phosphorus-containing aliphatic and aromatic polymers as well as the products of polymer-analogue transformations with phosphorus-groups in the side chain are examined. The light absorption and luminescent properties of the polymers obtained and of model compounds having an analogous structure are discussed. The bibliography includes 108 references.

  19. Spectroscopic and structural study of novel interaction product of pyrrolidine-2-thione with molecular iodine. Presumable mechanisms of oxidation

    Science.gov (United States)

    Chernov'yants, Margarita S.; Burykin, Igor V.; Starikova, Zoya A.; Tereznikov, Alexander Yu.; Kolesnikova, Tatiana S.

    2013-09-01

    Synthesis, spectroscopic and structural characterization of novel interaction product of pyrrolidine-2-thione with molecular iodine is reported. The ability of pyrrolidine-2-thione to form the outer-sphere charge-transfer complex C4H7NS·I2 with iodine molecule in dilute chloroform solution has been studied by UV/vis spectroscopy. Oxidative desulfurization promotes ring fusion of two pyrrolidine-2-thione molecules. The product of iodine induced oxidative desulfurization has been studied by X-ray diffraction method. The crystal structure of the reaction product is formed by 5-(2-thioxopyrrolidine-1-yl)-3,4-dihydro-2H-pyrrolium (C8H13N2S+) cations and pentaiodide anions I5-, which are linked by the intermolecular I⋯Hsbnd C and I⋯C close contacts. The angular pentaiodide anions can be considered as structures formed by coordination of two iodine molecules to the iodide ion (type 1) or by the coordination of iodine molecule to the triiodide ion (type 2).

  20. Spectroscopic, thermogravimetric and structural characterization analyses for comparing Municipal Solid Waste composts and vermicomposts stability and maturity.

    Science.gov (United States)

    Soobhany, Nuhaa; Gunasee, Sanjana; Rago, Yogeshwari Pooja; Joyram, Hashita; Raghoo, Pravesh; Mohee, Romeela; Garg, Vinod Kumar

    2017-07-01

    This is the first-ever study of its kind for an extensive assessment and comparison of maturity indexes between compost and vermicompost that have been derived from Municipal Solid Waste (MSW). The spectroscopic (Fourier transform infrared spectroscopy: FT-IR), thermogravimetric analysis (TG), differential scanning calorimetry (DSC) and structural characterization (scanning electron microscope: SEM) were recorded. FT-IR spectra showed an increase in conversion of polysaccharides species and aliphatic methylene groups in vermicompost compared to compost as depicted from the variation of the intensity of the peaks. TG curves of final vermicompost showed a much lower mass loss when compared to compost, indicating higher stability in feedstock. SEM micrographs of the vermicompost reflected strong fragmentation of material than composts which revealed the extent of intra-structural degradation of MSW. These findings elucidate on a clear comparison between composts and vermicomposts in terms of maturity indexes for soil enhancement and in agriculture as organic fertilizer. Copyright © 2017 Elsevier Ltd. All rights reserved.

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

    International Nuclear Information System (INIS)

    Araujo, Carolina G.L.; Freire, Carolina B.; Tello, Cledola C. de O.

    2013-01-01

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

  2. Characterization and Discrimination of Gram-Positive Bacteria Using Raman Spectroscopy with the Aid of Principal Component Analysis

    Directory of Open Access Journals (Sweden)

    Alia Colniță

    2017-09-01

    Full Text Available Raman scattering and its particular effect, surface-enhanced Raman scattering (SERS, are whole-organism fingerprinting spectroscopic techniques that gain more and more popularity in bacterial detection. In this work, two relevant Gram-positive bacteria species, Lactobacillus casei (L. casei and Listeria monocytogenes (L. monocytogenes were characterized based on their Raman and SERS spectral fingerprints. The SERS spectra were used to identify the biochemical structures of the bacterial cell wall. Two synthesis methods of the SERS-active nanomaterials were used and the recorded spectra were analyzed. L. casei and L. monocytogenes were successfully discriminated by applying Principal Component Analysis (PCA to their specific spectral data.

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

    Directory of Open Access Journals (Sweden)

    N. Shanmugam

    2016-09-01

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

  4. Synthesis, characterization and antioxidant activity of a novel electroactive and biodegradable polyurethane for cardiac tissue engineering application

    International Nuclear Information System (INIS)

    Baheiraei, Nafiseh; Yeganeh, Hamid; Ai, Jafar; Gharibi, Reza; Azami, Mahmoud; Faghihi, Faezeh

    2014-01-01

    There has been a growing trend towards applying conducting polymers for electrically excitable cells to increase electrical signal propagation within the cell-loaded substrates. A novel biodegradable electroactive polyurethane containing aniline pentamer (AP-PU) was synthesized and fully characterized by spectroscopic methods. To tune the physico-chemical properties and biocompatibility, the AP-PU was blended with polycaprolactone (PCL). The presence of electroactive moieties and the electroactivity behavior of the prepared films were confirmed by UV–visible spectroscopy and cyclic voltammetry. A conventional four probe analysis demonstrated the electrical conductivity of the films in the semiconductor range (∼ 10 −5 S/cm). MTT assays using L929 mouse fibroblast and human umbilical vein endothelial cells (HUVECs) showed that the prepared blend (PB) displayed more cytocompatibility compared with AP-PU due to the introduction of a biocompatible PCL moiety. The in vitro cell culture also confirmed that PB was as supportive as tissue culture plate. The antioxidant activity of the AP-PU was proved using 1,1-diphenyl-2-picrylhydrazyl (DPPH) scavenging assay by employing UV–vis spectroscopy. In vitro degradation tests conducted in phosphate-buffered saline, pH 7.4 and pH 5.5, proved that the films were also biodegradable. The results of this study have highlighted the potential application of this bioelectroactive polyurethane as a platform substrate to study the effect of electrical signals on cell activities and to direct desirable cell function for tissue engineering applications. - Highlights: • Straight forward methodology for synthesis of electroactive polyurethane • Biodegradability and non-toxicity through proper selection of starting materials • Supporting cell proliferation and attachment combined with antioxidant property

  5. Synthesis, characterization and antioxidant activity of a novel electroactive and biodegradable polyurethane for cardiac tissue engineering application

    Energy Technology Data Exchange (ETDEWEB)

    Baheiraei, Nafiseh [Department of Tissue Engineering, School of Advanced Medical Technologies, Tehran University of Medical Sciences, 1417755469 Tehran (Iran, Islamic Republic of); Yeganeh, Hamid, E-mail: h.yeganeh@ippi.ac.ir [Department of Polyurethane, Iran Polymer and Petrochemical Institute, P.O. Box: 14965/115, Tehran (Iran, Islamic Republic of); Ai, Jafar [Department of Tissue Engineering, School of Advanced Medical Technologies, Tehran University of Medical Sciences, 1417755469 Tehran (Iran, Islamic Republic of); Brain and Spinal Injury Research Center, Tehran University of Medical Sciences, Tehran (Iran, Islamic Republic of); Gharibi, Reza [Department of Polyurethane, Iran Polymer and Petrochemical Institute, P.O. Box: 14965/115, Tehran (Iran, Islamic Republic of); Azami, Mahmoud; Faghihi, Faezeh [Department of Tissue Engineering, School of Advanced Medical Technologies, Tehran University of Medical Sciences, 1417755469 Tehran (Iran, Islamic Republic of)

    2014-11-01

    There has been a growing trend towards applying conducting polymers for electrically excitable cells to increase electrical signal propagation within the cell-loaded substrates. A novel biodegradable electroactive polyurethane containing aniline pentamer (AP-PU) was synthesized and fully characterized by spectroscopic methods. To tune the physico-chemical properties and biocompatibility, the AP-PU was blended with polycaprolactone (PCL). The presence of electroactive moieties and the electroactivity behavior of the prepared films were confirmed by UV–visible spectroscopy and cyclic voltammetry. A conventional four probe analysis demonstrated the electrical conductivity of the films in the semiconductor range (∼ 10{sup −5} S/cm). MTT assays using L929 mouse fibroblast and human umbilical vein endothelial cells (HUVECs) showed that the prepared blend (PB) displayed more cytocompatibility compared with AP-PU due to the introduction of a biocompatible PCL moiety. The in vitro cell culture also confirmed that PB was as supportive as tissue culture plate. The antioxidant activity of the AP-PU was proved using 1,1-diphenyl-2-picrylhydrazyl (DPPH) scavenging assay by employing UV–vis spectroscopy. In vitro degradation tests conducted in phosphate-buffered saline, pH 7.4 and pH 5.5, proved that the films were also biodegradable. The results of this study have highlighted the potential application of this bioelectroactive polyurethane as a platform substrate to study the effect of electrical signals on cell activities and to direct desirable cell function for tissue engineering applications. - Highlights: • Straight forward methodology for synthesis of electroactive polyurethane • Biodegradability and non-toxicity through proper selection of starting materials • Supporting cell proliferation and attachment combined with antioxidant property.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2002-07-01

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

  7. Low temperature N,N-dimethylformamide-assisted synthesis and characterization of anatase-rutile biphasic nanostructured titania

    Energy Technology Data Exchange (ETDEWEB)

    Estruga, M; Domenech, X; Ayllon, J A [Departament de Quimica, Universitat Autonoma de Barcelona, Campus UAB, E-08193 Bellaterra (Spain); Domingo, C [Institut de Ciencia dels Materials de Barcelona (CSIC), Campus UAB, E-08193 Bellaterra (Spain)], E-mail: joseantonio.ayllon@uab.es, E-mail: mestruga@qf.uab.cat

    2009-03-25

    Anatase and rutile biphasic nanostructured titania (TiO{sub 2}) has been synthesized via hydrolysis of titanium tetraisopropoxide in an aqueous solution of hydrobromic acid (HBr) and N,N-dimethylformamide (DMF) at 80 deg. C for 16 h. The presence of DMF, which was partially hydrolyzed during the process, determined the formation of a biphasic material. Powder x-ray diffraction showed the presence of both anatase and rutile titania phases in a ratio of approx. 1:1. Transmission electron microscope analysis showed that rutile was present as radial flower-like nanorods, which were surrounded by anatase spherical nanoparticles of 5 nm diameter. Low temperature nitrogen adsorption-desorption analysis showed the characteristic hysteresis loop of a mesoporous material. Specific surface area reached a value of 120 m{sup 2} g{sup -1} and the average pore diameter was 50 A. X-ray photoelectron spectroscopic analysis revealed that interstitial nitrogen was incorporated (0.35 at.%) during the annealing process. According to ultraviolet (UV)-visible diffuse reflectance spectroscope characterization, the N-doping caused a bandgap reduction from 3.0 to 2.9 eV. Photocatalytic activity of the material was tested for the degradation of methylene blue, methyl orange and 4-nitrophenol under near-UV and visible light radiation.

  8. Synthesis and characterization of monodispersed orthorhombic manganese oxide nanoparticles produced by Bacillus sp. cells simultaneous to its bioremediation

    Energy Technology Data Exchange (ETDEWEB)

    Sinha, Arvind [Enzyme and Microbial Biochemistry Laboratory, Department of Chemistry, Indian Institute of Technology, Delhi, Hauz Khas, New Delhi 110 016 (India); Singh, Vidya Nand; Mehta, Bodh Raj [Thin Film Laboratory, Department of Physics, Indian Institute of Technology, Delhi Hauz Khas, New Delhi 110016 (India); Khare, Sunil Kumar, E-mail: skhare@rocketmail.com [Enzyme and Microbial Biochemistry Laboratory, Department of Chemistry, Indian Institute of Technology, Delhi, Hauz Khas, New Delhi 110 016 (India)

    2011-08-30

    Highlights: {yields} An efficient process wherein remediated manganese is synthesized into nanoparticles. {yields} A microbial process for manganese nanoparticle synthesis from metal waste streams. {yields} Nanoparticles characterized as monodispersed, spherical and 4.62 {+-} 0.14 nm sized MnO{sub 2}. -- Abstract: A heavy metal resistant strain of Bacillus sp. (MTCC10650) is reported. The strain exhibited the property of bioaccumulating manganese, simultaneous to its remediation. The nanoparticles thus formed were characterized and identified using energy dispersive X-ray analysis (EDAX), high resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), powder X-ray diffraction (PXRD) and atomic force microscopy (AFM). When the cells were challenged with manganese, the cells effectively synthesized nanoparticles of average size 4.62 {+-} 0.14 nm. These were mostly spherical and monodispersed. The ex situ enzymatically synthesized nanoparticles exhibited an absorbance maximum at 329 nm. These were more discrete, small and uniform, than the manganese oxide nanoparticles recovered after cell sonication. The use of Bacillus sp. cells seems promising and advantageous approach. Since, it serves dual purposes of (i) remediation and (ii) nanoparticle synthesis. Considering the increasing demand of developing environmental friendly and cost effective technologies for nanoparticle synthesis, these cells can be exploited for the remediation of manganese from the environment in conjunction with development of a greener process for the controlled synthesis of manganese oxide nanoparticles.

  9. Synthesis and characterization of monodispersed orthorhombic manganese oxide nanoparticles produced by Bacillus sp. cells simultaneous to its bioremediation

    International Nuclear Information System (INIS)

    Sinha, Arvind; Singh, Vidya Nand; Mehta, Bodh Raj; Khare, Sunil Kumar

    2011-01-01

    Highlights: → An efficient process wherein remediated manganese is synthesized into nanoparticles. → A microbial process for manganese nanoparticle synthesis from metal waste streams. → Nanoparticles characterized as monodispersed, spherical and 4.62 ± 0.14 nm sized MnO 2 . -- Abstract: A heavy metal resistant strain of Bacillus sp. (MTCC10650) is reported. The strain exhibited the property of bioaccumulating manganese, simultaneous to its remediation. The nanoparticles thus formed were characterized and identified using energy dispersive X-ray analysis (EDAX), high resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), powder X-ray diffraction (PXRD) and atomic force microscopy (AFM). When the cells were challenged with manganese, the cells effectively synthesized nanoparticles of average size 4.62 ± 0.14 nm. These were mostly spherical and monodispersed. The ex situ enzymatically synthesized nanoparticles exhibited an absorbance maximum at 329 nm. These were more discrete, small and uniform, than the manganese oxide nanoparticles recovered after cell sonication. The use of Bacillus sp. cells seems promising and advantageous approach. Since, it serves dual purposes of (i) remediation and (ii) nanoparticle synthesis. Considering the increasing demand of developing environmental friendly and cost effective technologies for nanoparticle synthesis, these cells can be exploited for the remediation of manganese from the environment in conjunction with development of a greener process for the controlled synthesis of manganese oxide nanoparticles.

  10. Spectroscopic Characterization of GEO Satellites with Gunma LOW Resolution Spectrograph

    Science.gov (United States)

    Endo, T.; Ono, H.; Hosokawa, M.; Ando, T.; Takanezawa, T.; Hashimoto, O.

    The spectroscopic observation is potentially a powerful tool for understanding the Geostationary Earth Orbit (GEO) objects. We present here the results of an investigation of energy spectra of GEO satellites obtained from a groundbased optical telescope. The spectroscopic observations were made from April to June 2016 with the Gunma LOW resolution Spectrograph and imager (GLOWS) at the Gunma Astronomical Observatory (GAO) in JAPAN. The observation targets consist of eleven different satellites: two weather satellites, four communications satellites, and five broadcasting satellites. All the spectra of those GEO satellites are inferred to be solar-like. A number of well-known absorption features such as H-alpha, H-beta, Na-D,water vapor and oxygen molecules are clearly seen in thewavelength range of 4,000 - 8,000 Å. For comparison, we calculated the intensity ratio of the spectra of GEO satellites to that of the Moon which is the natural satellite of the earth. As a result, the following characteristics were obtained. 1) Some variations are seen in the strength of absorption features of water vapor and oxygen originated by the telluric atmosphere, but any other characteristic absorption features were not found. 2) For all observed satellites, the intensity ratio of the spectrum of GEO satellites decrease as a function of wavelength or to be flat. It means that the spectral reflectance of satellite materials is bluer than that of the Moon. 3) A characteristic dip at around 4,800 Å is found in all observed spectra of a weather satellite. Based on these observations, it is indicated that the characteristics of the spectrum are mainly derived from the solar panels because the apparent area of the solar cell is probably larger than that of the satellite body.

  11. Synthesis and characterization of 2-substituted benzimidazoles and their evaluation as anticancer agent

    Science.gov (United States)

    Azam, Mohammad; Khan, Azmat Ali; Al-Resayes, Saud I.; Islam, Mohammad Shahidul; Saxena, Ajit Kumar; Dwivedi, Sourabh; Musarrat, Javed; Trzesowska-Kruszynska, Agata; Kruszynski, Rafal

    2015-05-01

    In this work, we report a series of benzimidazole derivatives synthesized from benzene-1,2-diamine and aryl-aldehydes at room temperature. The synthesized compounds have been characterized on the basis of elemental analysis and various spectroscopic studies viz., IR, 1H- and 13C-NMR, ESI-MS as well by X-ray single X-ray crystallographic study. Interaction of these compounds with CT-DNA has been examined with fluorescence experiments and showed significant binding ability. All the synthesized compounds have been screened for their antitumor activities against various human cancer cell lines viz., Human breast adenocarcinoma cell line (MCF-7), Human leukemia cell line (THP-1), Human prostate cancer cell lines (PC-3) and adenocarcinomic human alveolar basal epithelial cell lines (A-549). Interestingly, all the compounds showed significant anticancer activity.

  12. Crystal growth and spectroscopic characterization of Yb3+:LiTaO3

    International Nuclear Information System (INIS)

    Gruber, John B.; Allik, Toomas H.; Sardar, Dhiraj K.; Yow, Raylon M.; Scripsick, Michael; Wechsler, Barry

    2006-01-01

    Spectroscopic properties are presented for Yb 3+ incorporated into single crystals of LiTaO 3 grown by the top-seeded solution growth method. From an analysis of the absorption and fluorescence spectra, we are able to determine the Stark-level components of the 2 F 7/2 (the ground-state multiplet manifold) and the 2 F 5/2 (the excited-state multiplet manifold of Yb 3+ (4f 13 )). The room-temperature fluorescence lifetime of 2 F 5/2 is 678μs as measured on a thin sample to reduce possibilities for reabsorption. Spectral comparisons of Yb 3+ -doped LiTaO 3 and LiNbO 3 are drawn. The crystal-field splitting of Yb 3+ (4f 13 ) in both crystal hosts is modeled using a set of crystal-field splitting parameters, B nm , determined from a recent spectroscopic analysis of Er 3+ (4f 11 ) in LiNbO 3 . Without adjustment of the B nm parameters, the model predicts the Stark-level energy and the symmetry label for each level in reasonable agreement with the experimental values. Less photorefractive than its niobate cousin, LiTaO 3 has potential for use in numerous integrated electro-optical circuits and devices

  13. Synthesis and transport characterization of electrochemically deposited CdTe nanowires

    Science.gov (United States)

    Kaur, Jaskiran; Kaur, Harmanmeet; Singh, R. C.

    2018-04-01

    This paper reports the synthesis and characterization of CdTe nanowires. A thin polymeric films were irradiated with 80MeV Ag ions at a fluence of 8E7 ions/cm2, followed by UV irradiation and chemically etching in aqueous NaOH. Nanosizes go-through pores so formed were filled using a specially designed cell via electrodeposition. Nanowires so formed were further studied using SEM, I-V, UV and XRD analysis. SEM images show very smooth and uniform CdTe nanowires freely standing on the substrate. The in-situ I-V characteristics of nano-/micro structures was carried out at room temperature by leaving the structures embedded in the insulating template membrane itself.

  14. Ethyl 2,6-Dimethoxybenzoate: Synthesis, Spectroscopic and X-ray Crystallographic Analysis

    Directory of Open Access Journals (Sweden)

    Jonathan M. White

    2012-05-01

    Full Text Available The acid catalyzed esterification of 2,6-dimethoxybenzoic acid (1 in the presence of absolute ethanol afforded ethyl 2, 6-dimethoxybenzoate (2. The structure of the resulting compound was supported by spectroscopic data and unambiguously confirmed by single crystal X-ray diffraction studies. The title compound crystallized in the triclinic space group P ī with unit cell parameters a = 8.5518(3 Å, b = 10.8826(8 Å, c = 11.9939(6 Å, α = 101.273(5°, β = 98.287(3°, γ = 94.092(4°, V = 1077.54(10 Å3, Z = 4, Dc = 1.296 Mg/m3, F(000 = 448 and μ = 0.098 mm−1. Compound (2 crystallizes with two molecules in the asymmetric unit with similar conformations.

  15. Synthesis and characterization of PMMA/clay nanocomposites prepared by in situ polymerization assisted by sonication

    International Nuclear Information System (INIS)

    Prado, Bruna R.; Bartoli, Julio R.; Ito, Edson N.

    2015-01-01

    In this work is presented the synthesis of nanocomposites of poly(methyl methacrylate), PMMA, with organically montmorillonite (OMMT) modified clays by in situ polymerization assisted by sonication. A statistically designed experiment was used, central composing design (CCD), to study the effect of synthesis variables on the dispersion of nanoparticles in PMMA matrix. The processing and formulation factors studied were: energy of sonication and Flory-Huggins interaction parameter between PMMA and organoclay. The structural (XRD) and morphological (TEM) characterizations of the PMMA/OMMT nanocomposites are compared with the literature. It was observed significant exfoliation of OMMT modified with hydroxyl groups in the nanocomposites of PMMA, mainly at the low ultrasonic energy level (90 and 105 kJ) studied. (author)

  16. Synthesis, characterization and thermal decomposition of tetramethylammonium rare earth double selenates

    Science.gov (United States)

    Divekar, Sandesh K.; Achary, S. Nagabhusan; Ajgaonkar, Vishnu R.

    2018-06-01

    A series of double selenates, as (CH3)4NLn(SeO4)2rad 4H2O (Ln = Rare earth ion like La, Pr, Nd, Sm, Gd, Tb, Dy) was crystallized from mixed solution and characterized in detail for their structure, vibrational and optical properties as well as thermal stabilities. The crystal structure of the praseodymium compound was obtained by single crystal X-ray diffraction (XRD) and revealed a monoclinic (C2/c) lattice with chains formed by PrO8 and SeO4 units. The chains with compositions [Pr(SeO4)4(H2O)4]- are stacked in three dimensions and the (CH3)4N+ ions located in between them provide charge neutrality to the structure. The characterization of other compounds were carried out from powder XRD data and revealed that they all are isostructural to Pr-compound. All the functional groups were identified by Raman and IR spectroscopic studies. Solid state 77Se NMR revealed noticeable changes in selenium environment in these compounds. The optical absorption studies on the compounds show strong band edge absorptions in UV region. Thermal stabilities of the compounds, as investigated by simultaneous TG-DTA techniques indicate their sequential decompositions due to loss of H2O, (CH3)4N+ group, SeO2 and finally leaving their corresponding rare earth oxides.

  17. Synthesis, Characterization and Antimicrobial Activities of Transition Metal Complexes of methyl 2-(((E)-(2-hydroxyphenyl)methylidene)amino)benzoate

    International Nuclear Information System (INIS)

    Ikram, M.; Rehman, S.

    2016-01-01

    New metal complexes with Schiff base ligand methyl 2-(((E)-(2-hydroxyphenyl)methylidene)amino)benzoate, were synthesized and characterized. Elemental analyses, EI-MS, 1H and 13C(1H)-NMR were used for ligand characterization whereas elemental analyses, EI-MS, IR and UV-Visible spectroscopic techniques were used for the transition metal compounds. All these analyses reveal the bis arrangement of the ligand around the metal centres. The compounds were studied for their antimicrobial activities against different pathogenic microbial species. It was found that the Schiff base ligand was completely inactive in comparison to the transition metal compounds. It was also observed that nickel based metal complex shown good results against Candida albican (25 mm) and zinc based metal complex against Agrobacterium tumefaciens (16 mm). (author)

  18. Graphitic carbon nitride: Synthesis, characterization and photocatalytic decomposition of nitrous oxide

    Energy Technology Data Exchange (ETDEWEB)

    Praus, Petr, E-mail: petr.praus@vsb.cz [Institute of Environmental Technology, VŠB-Technical University of Ostrava, 17. Listopadu 15/2172, Ostrava 708 33 (Czech Republic); Department of Chemistry, Faculty of Metallurgy and Materials Engineering, VŠB-Technical University of Ostrava, 17. Listopadu 15/2172, Ostrava 708 33 (Czech Republic); Svoboda, Ladislav [Institute of Environmental Technology, VŠB-Technical University of Ostrava, 17. Listopadu 15/2172, Ostrava 708 33 (Czech Republic); Department of Chemistry, Faculty of Metallurgy and Materials Engineering, VŠB-Technical University of Ostrava, 17. Listopadu 15/2172, Ostrava 708 33 (Czech Republic); Ritz, Michal [Department of Chemistry, Faculty of Metallurgy and Materials Engineering, VŠB-Technical University of Ostrava, 17. Listopadu 15/2172, Ostrava 708 33 (Czech Republic); Troppová, Ivana; Šihor, Marcel; Kočí, Kamila [Institute of Environmental Technology, VŠB-Technical University of Ostrava, 17. Listopadu 15/2172, Ostrava 708 33 (Czech Republic)

    2017-06-01

    Graphitic carbon nitride (g-C{sub 3}N{sub 4}) was synthetized by condensation of melamine at the temperatures of 400–700 °C in air for 2 h and resulting products were characterized and finally tested for the photocatalytic decomposition of nitrous oxide. The characterization methods were elemental analysis, UV–Vis diffuse reflectance spectroscopy (DRS), photoluminescence (PL), Fourier transform infrared (FTIR) and Raman spectroscopy, measurement of specific surface area (SSA), X-ray powder diffraction (XRD), scanning (SEM) and transmission (TEM) electron microscopy. The XRD patterns, FTIR and Raman spectra proved the presence of g-C{sub 3}N{sub 4} at above 550 °C but the optimal synthesis temperature of 600–650 °C was found. Under these conditions graphitic carbon nitride of the overall empirical composition of C{sub 6}N{sub 9}H{sub 2} was formed. At lower temperatures g-C{sub 3}N{sub 4} with a higher content of hydrogen was formed but at higher temperatures g-C{sub 3}N{sub 4} was decomposed. At the temperatures above 650 °C, its exfoliation was observed. The photocatalytic experiments showed that the activity of all the samples synthetized at 400–700 °C was very similar, that is, within the range of experimental error (5 %). The total conversion of N{sub 2}O reached about 43 % after 14 h. - Highlights: • Graphitic carbon nitride (g-C{sub 3}N{sub 4}) was thermally synthetized from melamine in the range of 400–700 °C. • The optimal temperature was determined at 600–650 °C. • All synthesis products were properly characterized by physico-chemical methods. • Exfoliation of g-C{sub 3}N{sub 4} at above 600 °C was observed. • g-C{sub 3}N{sub 4} was used for the photocatalytic decomposition of N{sub 2}O.

  19. Synthesis and characterization of MgO nanocrystals for biosensing applications

    Energy Technology Data Exchange (ETDEWEB)

    Li, Hongji [Tianjin Key Laboratory of Organic Solar Cells and Photochemical Conversion, School of Chemistry & Chemical Engineering, Tianjin University of Technology, Tianjin 300384 (China); Li, Mingji, E-mail: limingji@163.com [Tianjin Key Laboratory of Film Electronic and Communication Devices, School of Electronics Information Engineering, Tianjin University of Technology, Tianjin 300384 (China); Qiu, Guojun [Tianjin Key Laboratory of Organic Solar Cells and Photochemical Conversion, School of Chemistry & Chemical Engineering, Tianjin University of Technology, Tianjin 300384 (China); Li, Cuiping; Qu, Changqing; Yang, Baohe [Tianjin Key Laboratory of Film Electronic and Communication Devices, School of Electronics Information Engineering, Tianjin University of Technology, Tianjin 300384 (China)

    2015-05-25

    Highlights: • MgO nanocrystals were prepared using DC arc plasma jet CVD method. • The growth time does not exceed 10 min in process of the synthesis. • The samples were found to consist of cubic MgO nanobelts and nanosheets. • Nanocrystals contain contacts, rough edges, vacancies, and doping defects. • The samples exhibited excellent electrochemical biosensing properties. - Abstract: MgO nanocrystals were prepared using a simple direct current arc plasma jet chemical vapor deposition method. Magnesium nitrate was used as source material and Mo film was used as a substrate and catalyst. The high-temperature plasma produced ensured rapid synthesis of the MgO nanocrystals. The as-prepared nanocrystals were characterized by field-emission scanning electron microscopy, high-resolution transmission electron microscopy, X-ray diffraction, energy-dispersive spectroscopy, Fourier transform infrared spectrometry, ultraviolet–visible spectrophotometry, and photoluminescence measurements. The as-synthesized samples were found to consist of cubic MgO nanobelts and nanosheets with large surface areas and low coordination oxide ions, and contained numerous contacts, rough edges, vacancies, and doping defects. The nanostructures exhibited excellent electrochemical sensing properties with high-sensing sensitivity toward ascorbic acid. Their high electrocatalytic activity was attributed to the effect of defects and the surface electron transfer ability of the one-dimensional MgO nanobelts.

  20. Shell model and spectroscopic factors

    International Nuclear Information System (INIS)

    Poves, P.

    2007-01-01

    In these lectures, I introduce the notion of spectroscopic factor in the shell model context. A brief review is given of the present status of the large scale applications of the Interacting Shell Model. The spectroscopic factors and the spectroscopic strength are discussed for nuclei in the vicinity of magic closures and for deformed nuclei. (author)

  1. Multi-spectroscopic techniques to evaluate the toxicity of alloyed CdSeS quantum dots

    International Nuclear Information System (INIS)

    Zhan Hongju; Zhou Peijiang; Ding Ling; He Zhenyu; Ma Rong

    2012-01-01

    Alloyed CdSeS quantum dots (QDs) were successfully synthesized in aqueous phase using microwave irradiation. UV–vis spectroscopy, fluorescence spectroscopy, transmission electron microscopy (TEM) and X-ray diffraction (XRD) techniques proved that the prepared alloyed QDs are composed of a CdSe-rich core and thick CdS shell with homogeneous size distributions. In order to study its biological toxicity, multi-spectroscopic techniques were adopted to investigate their conjugation with BSA. Fluorescence quenching methods indicated the prepared CdSeS QDs strongly quenched the fluorescence of BSA due to the formation of non-fluorescence ground-state complex. UV–vis absorbance spectra, synchronous fluorescence spectra and CD spectra further confirmed the alloyed CdSeS QDs binded with BSA and destroyed their hydrogen bonding networks, which induced the conformation changes of this macromolecule. - Highlights: ► Synthesis of alloyed CdSeS QDs in aqueous phase via microwave irradiation. ► Characterization of alloyed QDs by PL, UV–vis, XRD and TEM techniques. ► Evidence of static quenching between alloyed QDs and BSA. ► Evidence of the conformation change of BSA molecules induced by alloyed QDs.

  2. Synthesis, spectroscopic characterization and pharmacological evaluation of oxazolone derivatives

    Directory of Open Access Journals (Sweden)

    Fareed Ghulam

    2013-01-01

    Full Text Available A series of 4-aryl methylidene-2-phenyl/methyl-5-(4H-oxazolone derivatives (2-7 have been synthesized using the reported method by condensation of aldehydes with N-benzoyl / N-acetyl glycine in the presence of zinc oxide as a catalyst and acetic anhydride at room temperature in ethanol. The compounds (2-6 are new derivatives. The structures of compounds were evaluated on the basis of 1H-NMR, 13C-NMR, EIMS, FT-IR and elemental analysis. All the compounds were screened for their antibacterial and urease inhibition activity. Antibacterial activity was tested by agar well diffusion method using Mueller Hinton Agar medium. Compound (2 showed excellent activity against S. aureus which has 16 mm (80% inhibition and above 24 mm (70% against S. typhi. The most active compound against E. coli was compound (6 having 20 mm (80% inhibition followed by compound (5 having above 18 mm (70% inhibition. Urease inhibition activity of all the compounds was determined by indophenol method. Compounds (3, 6 and (7 showed significant inhibition against Jacks bean urease.

  3. Hydrothermal synthesis and characterization of zirconia based catalysts

    Science.gov (United States)

    Caillot, T.; Salama, Z.; Chanut, N.; Cadete Santos Aires, F. J.; Bennici, S.; Auroux, A.

    2013-07-01

    In this work, three equimolar mixed oxides ZrO2/CeO2, ZrO2/TiO2, ZrO2/La2O3 and a reference ZrO2 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 NH3 and SO2 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 ZrO2/TiO2 material appears to be the best candidate for further application in acid-base catalysis.

  4. Synthesis and characterization of new ionic liquids; Sintese e caracterizacao de novos liquidos ionicos

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira, L.M.C. de; Mattedi, S.; Boaventura, J.S., E-mail: luanaufrn@hotmail.co [Universidade Federal da Bahia (UFBA), Salvador, BA (Brazil). Escola Politecnica. Programa de Pos-Graduacao em Engenharia Quimica; Iglesias, M. [Universidade Federal da Bahia (UFBA), Salvador, BA (Brazil). Escola Politecnica. Programa de Pos-Graduacao em Engenharia Quimica; Universidad de Santiago de Compostela (Spain). Escuela Tecnica Superior de Ingenieria. Dept. de Ingenieria Quimica

    2010-07-01

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

  5. Synthesis, characterization and electrospinning of corn cob cellulose-graft-polyacrylonitrile and their clay nanocomposites.

    Science.gov (United States)

    Kalaoğlu, Özlem I; Ünlü, Cüneyt H; Galioğlu Atıcı, Oya

    2016-08-20

    This study aims at evaluation of cellulose recovered from agricultural waste (corn cob) in terms of synthesis of graft copolymers, polymer/clay nanocomposites, and nanofibers. The copolymers and nanocomposites were synthesized in aqueous solution using Ce(4+) initiator. Conditions (concentrations of the components, reaction temperature, and period) were determined first for copolymer synthesis to obtain the highest conversion ratio. Then found parameters were used to synthesize nanocomposites adding clay mineral to reaction medium. Although there was a decrease in conversion in nanocomposites syntheses, thermal and rheologic measurements indicated enhancements compared to pristine copolymer. Obtained polymeric materials have been successfully electrospun into nanofibers and characterized. Average diameter of the nanofibers was about 650nm and was strongly influenced by NaMMT amount in the nanocomposite sample. Copyright © 2016 Elsevier Ltd. All rights reserved.

  6. Synthesis, characterization and theoretical study of a new asymmetrical tripodal amine containing morpholine moiety

    Directory of Open Access Journals (Sweden)

    Majid Rezaeivala

    2016-11-01

    Full Text Available A new asymmetrical tripodal amine, [H3L2]Br3 containing morpholine moiety was prepared from reacting of one equivalent of N-(3-aminopropylmorpholine and two equivalents of tosylaziridine, followed by detosylation with HBr/CH3COOH. The products were characterized by various spectroscopic methods such as FAB-MS, elemental analysis, 1H and 13C NMR spectroscopy. The crystal structure of the hydrobromide salt of the latter amine, [H3L2]Br3, was also determined. For triprotonated form of the ligand L2 we can consider several microspecies and/or conformers. A theoretical study at B3LYP/6-31G∗∗ level of theory showed that the characterized microspecies is the most stable microspecies for the triprotonated form of the ligand. It was shown that the experimental NMR data for [H3L2]Br3 in solution have good correlation with the corresponding calculated data for the most stable microspecies of [H3L2]3+ in the gas phase.

  7. Isolation and characterization of a native strain of Aspergillus niger ZRS14 with capability of high resistance to zinc and its supernatant application towards extracellular synthesis of zinc oxide nanoparticles

    Directory of Open Access Journals (Sweden)

    Morahem Ashengroph

    2013-01-01

    Full Text Available Introduction: Zinc oxide nanoparticles have quite a few applications in the fields of biology, optics, mechanics, magnetism, energy, hygiene and medicine. Due to serious problems associated with physiochemical synthesis of ZnO nanoparticles, including environmental pollution, complicated and costly processes, there is a growing need to develop a simple biological procedure for synthesis of nanoparticles to achieve the monodisperse-sized particles with a higher purity, low energy consumption and a cleaner environment. We conducted this investigation to screen and isolate native fungi strains capable of high zinc metal tolerance ability and a potential for extracellular synthesis of ZnO nanoparticles using fungal secretions as biological catalysts.Materials and methods: 15 different strains of fungi were isolated from soil samples collected from lead and zinc mines of Angoran-Zanjan using conventional enrichment process and characterized initially based on macroscopic and microscopic characteristics and colony morphology. The intrinsic tolerance of the isolated strains to zinc toxic metal was measured in the synthetic and complex media using the agar dilution method. The supernatants of isolated fungi were incubated with zinc acetate solution in a shaker incubator for 72h; then, the strain that was able to synthesis ZnO nanoparticle was identified. The ZnO nanoparticles formation was investigated by using spectroscopic techniques and microscopic observations.Results: Among the 15 isolated strains, the strain ZRS14 had highest zinc metal tolerance ability and was selected and identified as Aspergillus niger strain ZRS14 (GenBank accession number KF414527 based on morphological and molecular phylogenetic analysis. For synthesis of ZnO nanoparticles by isolated A. niger ZRS14, fungal cell-free filtrate of the strain was collected and incubated in the presence of zinc acetate solution at a final concentration of 250 mg/l zinc metal ion at 28º C for

  8. Palladium polypyridyl complexes: synthesis, characterization, DNA interaction and biological activity on Leishmania (L.) mexicana

    International Nuclear Information System (INIS)

    Navarro, Maribel; Betancourt, Adelmo; Hernandez, Clara; Marchan, Edgar

    2008-01-01

    This paper describes the search for new potential chemotherapeutic agents based on transition metal complexes with planar ligands. In this study, palladium polypyridyl complexes were synthesized and characterized by elemental analysis, NMR, UV-VIS and IR spectroscopies. The interaction of the complexes with DNA was also investigated by spectroscopic methods. All metal-to-ligand charge transfer (MLCT) bands of the palladium polypyridyl complexes exhibited hypochromism and red shift in the presence of DNA. The binding constant and viscosity data suggested that the complexes [PdCl 2 (phen)] and [PdCl 2 (phendiamine)] interact with DNA by electrostatic forces. Additionally, these complexes induced an important leishmanistatic effect on L. (L.) mexicana promastigotes at the final concentration of 10 μmol L -1 in 48 h. (author)

  9. Synthesis and characterization of platinum supported on alumina doped with cerium catalyst

    International Nuclear Information System (INIS)

    Yusof Abdullah; Abd Fatah Awang Mat; Mohd Ali Sufi; Sarimah Mahat; Razali Kassim; Nurhaslinda Abdullah.

    1996-03-01

    The synthesis and characterization of gamma-alumina doped with cerium as platinum support for the automobile exhaust catalyst are described. Platinum/alumina/ceria catalyst were prepared by impregnation of hexachloroplatinic acid and sintered at 500 degree Celsius to obtain metal dispersions of 1.0 wt%. Catalyst distribution inside the powder and the effects of the addition of cerium to alumina were analyzed by the scanning electron microscopy (SEM) and x-ray fluorescence spectroscopy (XRF). The results showed that the alumina - supported catalysts contained well dispersion of the noble metal

  10. Designing Selectivity in Metal-Semiconductor Nanocrystals: Synthesis, Characterization, and Self-Assembly

    Science.gov (United States)

    Pavlopoulos, Nicholas George

    This dissertation contains six chapters detailing recent advances that have been made in the synthesis and characterization of metal-semiconductor hybrid nanocrystals (HNCs), and the applications of these materials. Primarily focused on the synthesis of well-defined II-VI semiconductor nanorod (NR) and tetrapod (TP) based constructs of interest for photocatalytic and solar energy applications, the research described herein discusses progress towards the realization of key design rules for the synthesis of functional semiconductor nanocrystals (NCs). As such, a blend of novel synthesis, advanced characterization, and direct application of heterostructured nanoparticles are presented. The first chapter is a review summarizing the design, synthesis, properties, and applications of multicomponent nanomaterials composed of disparate semiconductor and metal domains. By coupling two compositionally distinct materials onto a single nanocrystal, synergistic properties can arise that are not present in the isolated components, ranging from self-assembly to photocatalysis. For semiconductor nanomaterials, this was first realized in the ability to tune nanomaterial dimensions from 0-D quantum dot (QD) structures to cylindrical (NR) and branched (TP) structures by exploitation of advanced colloidal synthesis techniques and understandings of NC facet reactivities. The second chapter is focused on the synthesis and characterization of well-defined CdSe-seeded-CdS (CdSe CdS) NR systems synthesized by overcoating of wurtzite (W) CdSe quantum dots with W-CdS shells. 1-dimensional NRs have been interesting constructs for applications such as solar concentrators, optical gains, and photocatalysis. Through synthetic control over CdSe CdS NR systems, materials with small and large CdSe seeds were prepared, and for each seed size, multiple NR lengths were prepared. Through transient absorption studies, it was found that band alignment did not affect the efficiency of charge localization

  11. Synthesis of Cyclic Polymers and Characterization of Their Diffusive Motion in the Melt State at the Single Molecule Level

    KAUST Repository

    Habuchi, Satoshi

    2016-09-26

    We demonstrate a method for the synthesis of cyclic polymers and a protocol for characterizing their diffusive motion in a melt state at the single molecule level. An electrostatic self-assembly and covalent fixation (ESA-CF) process is used for the synthesis of the cyclic poly(tetrahydrofuran) (poly(THF)). The diffusive motion of individual cyclic polymer chains in a melt state is visualized using single molecule fluorescence imaging by incorporating a fluorophore unit in the cyclic chains. The diffusive motion of the chains is quantitatively characterized by means of a combination of mean-squared displacement (MSD) analysis and a cumulative distribution function (CDF) analysis. The cyclic polymer exhibits multiple-mode diffusion which is distinct from its linear counterpart. The results demonstrate that the diffusional heterogeneity of polymers that is often hidden behind ensemble averaging can be revealed by the efficient synthesis of the cyclic polymers using the ESA-CF process and the quantitative analysis of the diffusive motion at the single molecule level using the MSD and CDF analyses.

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

    Directory of Open Access Journals (Sweden)

    Bénédicte Mailhot-Jensen

    2010-01-01

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

  13. Practical routes to (SiH₃)₃P: applications in group IV semiconductor activation and in group III-V molecular synthesis.

    Science.gov (United States)

    Tice, Jesse B; Chizmeshya, A V G; Tolle, J; D' Costa, V R; Menendez, J; Kouvetakis, J

    2010-05-21

    The (SiH₃)₃P hydride is introduced as a practical source for n-doping of group IV semiconductors and as a highly-reactive delivery agent of -(SiH₃)₂P functionalities in exploratory synthesis. In contrast to earlier methods, the compound is produced here in high purity quantitative yields via a new single-step method based on reactions of SiH₃Br and (Me₃Sn)₃P, circumventing the need for toxic and unstable starting materials. As an initial demonstration of its utility we synthesized monosubstituted Me₂M-P(SiH₃)₂ (M = Al, Ga, In) derivatives of Me₃M containing the (SiH₃)₂P ligand for the first time, in analogy to the known Me₂M-P(SiMe₃)₂ counterparts. A dimeric structure of Me₂M-P(SiH₃)₂ is proposed on the basis of spectroscopic characterizations and quantum chemical simulations. Next, in the context of materials synthesis, the (SiH₃)₃P compound was used to dope germanium for the first time by building a prototype p(++)Si(100)/i-Ge/n-Ge photodiode structure. The resultant n-type Ge layers contained active carrier concentrations of 3-4 × 10¹⁹ atoms cm⁻³ as determined by spectroscopic ellipsometry and confirmed by SIMS. Strain analysis using high resolution XRD yielded a Si content of 4 × 10²⁰ atoms cm⁻³ in agreement with SIMS and within the range expected for incorporating Si₃P type units into the diamond cubic Ge matrix. Extensive characterizations for structure, morphology and crystallinity indicate that the Si co-dopant plays essentially a passive role and does not compromise the device quality of the host material nor does it fundamentally alter its optical properties.

  14. Ion beams provided by small accelerators for material synthesis and characterization

    Science.gov (United States)

    Mackova, Anna; Havranek, Vladimir

    2017-06-01

    The compact, multipurpose electrostatic tandem accelerators are extensively used for production of ion beams with energies in the range from 400 keV to 24 MeV of almost all elements of the periodic system for the trace element analysis by means of nuclear analytical methods. The ion beams produced by small accelerators have a broad application, mainly for material characterization (Rutherford Back-Scattering spectrometry, Particle Induced X ray Emission analysis, Nuclear Reaction Analysis and Ion-Microprobe with 1 μm lateral resolution among others) and for high-energy implantation. Material research belongs to traditionally progressive fields of technology. Due to the continuous miniaturization, the underlying structures are far beyond the analytical limits of the most conventional methods. Ion Beam Analysis (IBA) techniques provide this possibility as they use probes of similar or much smaller dimensions (particles, radiation). Ion beams can be used for the synthesis of new progressive functional nanomaterials for optics, electronics and other applications. Ion beams are extensively used in studies of the fundamental energetic ion interaction with matter as well as in the novel nanostructure synthesis using ion beam irradiation in various amorphous and crystalline materials in order to get structures with extraordinary functional properties. IBA methods serve for investigation of materials coming from material research, industry, micro- and nano-technology, electronics, optics and laser technology, chemical, biological and environmental investigation in general. Main research directions in laboratories employing small accelerators are also the preparation and characterization of micro- and nano-structured materials which are of interest for basic and oriented research in material science, and various studies of biological, geological, environmental and cultural heritage artefacts are provided too.

  15. Synthesis, characterization and application of nanozeolite NaX from Vietnamese kaolin

    International Nuclear Information System (INIS)

    Ngoc, Don Ta; Pham, Thanh Huyen; Hong Nguyen, Khanh Dieu

    2013-01-01

    This paper presents the results of synthesis of nanozeolite NaX from Vietnamese kaolin. Influence factors on the control of crystal sizes and application of synthesized materials as adsorbent for organic compound are discussed. The results show that there are several factors that influence the synthesis. When water content in gel increases, crystal size of NaX increases sharply. The increase of alkaline and silica contents increases the crystallinity and decreases the particle size of nano NaX, and the particle size reaches the minimum at Na 2 O/Al 2 O 3 = 5.0 and SiO 2 /Al 2 O 3 = 4.0. Crystal sizes formed at low crystallizing temperature are smaller than those formed at higher temperature. Ageing time and crystallizing time strongly influence the crystallinity and crystal size, which is related to the number of crystal seeds formed during ageing period, the growth of seed and the partial solubility of crystal at maximum formation. Nano NaX was characterized by x-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Brunauer–Emmett–Teller (BET) adsorption, Fourier transform infrared (FTIR) and simultaneous thermogravimetry–differential scanning calorimetry (TG/DSC). At optimized synthesis conditions, nano NaX has surface area of 573 m 2 g −1 with external surface area of 92 m 2 g −1 , pore size distribution at 0.81 and 10.8 nm, average crystal size of 25 nm and thermal stability up to 789 °C. This material can adsorb cumene rapidly with high adsorption capacity and stability. (paper)

  16. Synthesis and dosimetric characterization of LiF-MgF2, doped with Lu

    International Nuclear Information System (INIS)

    Gonzalez, Pedro R.; Nieto, Ana L.; Cruz-Zaragoza, Epifanio; Furetta, Claudio

    2013-01-01

    The results of the synthesis and characterization of dosimetric thermoluminescent material based on the composition LiF-MgF 2 1:1 (Z eff = 9.7) doped Lu 3+ ions, developed at the National Institute of Nuclear Research, Mexico are presented. The TL material synthesis was carried out using the technique of casting solid substances, preparations were made with dopant concentrations of 0.25, 0.83, 1.00 and 2.00 mol%, the 1 mol% resulted in increased sensitivity to radiation. Its brightness curve has the TL peak intensity at 330 deg C when irradiated to 1000 Gy, whereas when irradiated greater than 2500 Gy, occurs at 230 ° C, also has a peak of smaller maximum intensity at 140 ° C. Microstructural characterization of the obtained material was performed using the techniques of scanning electron microscopy and X-ray diffraction Kinetic parameters of the curves of brightness of the material is performed by the deconvolution method using the sequential quadratic programming algorithm, developed in the same institute. This new TL material complies fully with international standards to be used as dosimetry system in medical physics, research and industry, as its TL response (total integrated under the curve) to 60 Co gamma radiation, presents linearity between 1 and 5000 Gy , while the response of commercial TLD dosimeter-100 used as a reference, is only linear up to 10 Gy

  17. Electrospun V2O5 composite fibers: Synthesis, characterization and ammonia sensing properties

    International Nuclear Information System (INIS)

    Modafferi, V.; Trocino, S.; Donato, A.; Panzera, G.; Neri, G.

    2013-01-01

    In the present work, vanadium oxide (V 2 O 5 ) fibers have been investigated for monitoring ammonia (NH 3 ) at ppb levels in air. A simple sol gel-based electrospinning process has been applied for the synthesis of vanadium oxide/polyvinyl acetate (PVAc) and vanadium oxide/polyvinylpyrrolidone (PVP) composite fibers. Composite fibers doped with platinum (Pt) have been also prepared. The pure and Pt-doped metal oxide phase has been subsequently obtained by removing the polymer binder at high temperature in air. The samples have been widely studied to characterize their morphological and microstructural properties by X-Ray Diffraction, Fourier Transform InfraRed spectroscopy, X-ray Photoelectron Spectroscopy, and Scanning Electron Microscopy investigations. The application of the produced fibers in highly sensitive ammonia resistive sensors has been demonstrated. The influence of the nature of polymer binder and platinum addition on the sensing performances of the V 2 O 5 fibers has been investigated and discussed.V 2 O 5 fibers produced by using PVP as a polymer binder have shown higher sensitivity toward ammonia at ppb concentrations than fibers obtained with PVAc. Pt-doped samples have shown a lower response compared to un-doped samples. - Highlights: • Synthesis of vanadium oxide composite fibers by electrospinning • Physical and chemical characterization of prepared samples • Investigation of the sensing properties to ppb concentrations of ammonia in air

  18. Synthesis and thermoluminescent characterization of LiF doped with Ag; Sintesis y caracterizacion termoluminiscente de LiF dopado con Ag

    Energy Technology Data Exchange (ETDEWEB)

    Encarnacion, E. K.; Reyes, J.; Guerrero, Z. [Universidad Autonoma de Santo Domingo, Facultad de Ciencias, Ciudad Universitaria, Santo Domingo (Dominican Republic); Sosa, M. A.; Vallejo, M. A.; Rivera P, E., E-mail: emma.kee@gmail.com [Universidad de Guanajuato, Campus Leon, Division de Ciencias e Ingenierias, Loma del Bosque 103, Col. Lomas del Campestre, 37150 Leon, Guanajuato (Mexico)

    2015-10-15

    Full text: In this paper the synthesis and characterization of lithium fluoride (LiF) crystals pure and activated with silver (Ag) is reported. The synthesis was carried out by the method of co-precipitation; three samples were obtained one of pure LiF and two were activated with 0.02 and 0.04% of Ag. All samples were subjected to X-ray emission and the results were analyzed. The synthesized samples were characterized by X-ray diffraction, thermoluminescence and X-ray fluorescence. The XRD results show complete crystal structures. The radiation dosimetry responses are discussed. These are the first results of a research conducted at the Universidad Autonoma de Santo Domingo in collaboration with the Universidad de Guanajuato. (Author)

  19. Synthesis and characterization of TiO2 nanoparticles by the method Pechini

    International Nuclear Information System (INIS)

    Zoccal, Joao Victor Marques; Arouca, Fabio de Oliveira; Goncalves, Jose Antonio Silveira

    2009-01-01

    In recent years, scientific research showed an increasing interest in the field of nanotechnology, resulting in several techniques for the production of nanoparticles, such as methods of chemical synthesis. Among the various existing methods, the Pechini method has been used to obtain nanoparticles of titanium dioxide (TiO 2 ). Thus, this work aims to synthesize and characterize nanoparticles of TiO 2 obtained by this method. The technique constitutes in the reaction between citric acid with titanium isopropoxide, resulting as the product the titanium citrate. With the addition of the ethylene glycol polymerization occurs, resulting in a polymeric resin. At the end of the process, the resin is calcined to remove organic matter, creating nanoparticles of TiO 2 . The resulting powders were characterized by thermogravimetric analysis (TGA) and thermal differential analysis (DTA), X-ray diffraction, absorption spectrophotometry in the infrared, method of adsorption nitrogen / helium (BET method) and scanning electron microscopy. The results obtained in the characterization techniques showed that the Pechini method is promising in obtaining nanosized TiO 2 . (author)

  20. Synthesis and characterization of ceramic powders of pure and doped with trivalent erbium barium tungstate

    International Nuclear Information System (INIS)

    Sousa, R.B. de; Nascimento, V.A. do; Matos, J. M.E. de; Santos, M.R.M.C.

    2014-01-01

    This research proposes the synthesis and characterization of pure and doped with Er"3"+ (1 and 2 %) barium tungstate powders prepared by the coprecipitation method. In order to characterize the obtained powders were used X-Ray Diffractometry, Raman Spectroscopy and Fourier Transform Infrared Spectroscopy. According to the standard XRD spectra, the crystals exhibited the presence of tetragonal scheelite structure without the presence of secondary phases. Raman spectra showed the presence of eleven vibrational modes and two modes were observed in the infrared spectra. The synthesized oxides showed good crystallinity and structurally ordered at short and long-range. (author)