Quantifying lycopene synthesis and chlorophyll breakdown in tomato fruit using remittance VIS spectroscopy

NARCIS (Netherlands)

Schouten, R.E.; Farneti, B.; Tijskens, L.M.M.; Algarra Alarcon, A.; Woltering, E.J.

2014-01-01

The aim of this study was to increase the understanding of chlorophyll breakdown and lycopene synthesis at a quantitative level in Solanum lycopersicum fruit. To accomplish this, a kinetic model is proposed describing the transition from chloro- to chromoplast. Remittance VIS spectroscopy was used

Synthesis and high (pressure, temperature) stability of ZnTiO3 polymorphs studied by Raman spectroscopy

Science.gov (United States)

Bernert, T.; Ruiz-Fuertes, J.; Bayarjargal, L.; Winkler, B.

2015-05-01

The phase-purity of ilmenite-type ZnTiO3 prepared by the ceramic method was investigated in dependence of the conditions during ball milling. The previously proposed addition of 2 ml ethanol to the starting materials led to a significant contamination of the product phase after a subsequent sintering process at 1073 K. However, by omitting ethanol this synthesis route led to a phase-pure sample of ZnTiO3 as confirmed by X-ray powder diffraction and Raman spectroscopy. High-temperature high-pressure experiments gave an ilmenite-type to perovskite-type phase boundary with a slope of dT/dP∼-135 K GPa-1 crossing ambient temperature conditions at ∼ 24 GPa in good agreement with previous calculations. Room-temperature high-pressure Raman spectroscopy experiments have shown the stability of the ilmenite-type phase up to a pressure of at least 38.5 GPa, the highest pressure applied in this study, indicating the presence of a kinetic barrier in this phase transition. The synthesis of ferroelectric LiNbO3-type ZnTiO3 was confirmed by second harmonic generation.

Improved synthesis with high yield and increased molecular weight of poly(alpha,beta-malic acid) by direct polycondensation.

Science.gov (United States)

Kajiyama, Tetsuto; Kobayashi, Hisatoshi; Taguchi, Tetsushi; Kataoka, Kazunori; Tanaka, Junzo

2004-01-01

The development of synthetic biodegradable polymers, such as poly(alpha-hydroxy acid), is particularly important for constructing medical devices, including scaffolds and sutures, and has attracted growing interest in the biomedical field. Here, we report a novel approach to preparing high molecular weight poly(malic acid) (HMW--PMA) as a biodegradable and bioabsorbable water-soluble polymer. We investigated in detail the reaction conditions for the simple direct polycondensation of l-malic acid, including the reaction times, temperatures, and catalysts. The molecular weight of synthesized alpha,beta-PMA is dependent on both the reaction temperature and time. The optimum reaction condition to obtain alpha,beta-PMA by direct polycondensation using tin(II) chloride as a catalyst was thus determined to be 110 degrees C for 45 h with a molecular weight of 5300. The method for alpha,beta-PMA synthesis established here will facilitate production of alpha,beta-PMA of various molecular weights, which may have a potential utility as biomaterials.

INTERIM RESULTS FROM A STUDY OF THE IMPACTS OF TIN(II) BASED MERCURY TREATMENT IN A SMALL STREAM ECOSYSTEM: TIMS BRANCH, SAVANNAH RIVER SITE

Energy Technology Data Exchange (ETDEWEB)

Looney, B.; Bryan, L.; Mathews, T.

2012-03-30

source control measures have resulted in rapid responses in lake or reservoir fisheries (Joslin 1994, Turner and Southworth 1999; Orihel et al., 2007), but examples of similar responses in Hg-contaminated stream ecosystems are less common. Recent work suggests that stream systems may actually be more susceptible to mercury bioaccumulation than lakes, highlighting the need to better understand the ecological drivers of mercury bioaccumulation in stream-dwelling fish (Chasar et al. 2009, Ward et al. 2010). In the present study we examine the response of fish to remedial actions in Tims Branch, a point-source contaminated stream on the Department of Energy's (DOE) Savannah River Site in Aiken, South Carolina. This second order stream received inorganic mercury inputs at its headwaters from the 1950s-2000s which contaminated the water, sediments, and biota downstream. In 2007, an innovative mercury removal system using tin (II) chloride (stannous chloride, SnCl{sub 2}) was implemented at a pre-existing air stripper. Tin(II) reduces dissolved Hg (II) to Hg (0), which is removed by the air stripper. During this process, tin(II) is oxidized to tin (IV) which is expected to precipitate as colloidal tin(IV) oxides and hydroxides, particulate materials with relatively low toxicity (Hallas and Cooney, 1981, EPA 2002, ATSDR, 2005). The objectives of the present research are to provide an initial assessment of the net impacts of the tin(II) based mercury treatment on key biota and to document the distribution and fate of inorganic tin in this small stream ecosystem after the first several years of operating a full scale system. To support these objectives, we collected fish, sediment, water, invertebrates, and biofilm samples from Tims Branch to quantify the general behavior and accumulation patterns for mercury and tin in the ecosystem and to determine if the treatment process has resulted in: (1) a measurable beneficial impact on (i.e., decrease of) mercury concentration in

Optical properties and extinction spectroscopy to characterize the synthesis of amine capped silver nanoparticles

Energy Technology Data Exchange (ETDEWEB)

Roldan, Maria Virginia [Laboratorio de Materiales Ceramicos, FCEIyA, IFIR, UNR, Rosario (Argentina)], E-mail: vroldan@fceia.unr.edu.ar; Scaffardi, Lucia B. [CIOp - CONICET, CIC, c.c. 124, 1900 La Plata (Argentina) and Area Departamental de Ciencias Basicas, Facultad de Ingenieria, Universidad Nacional de La Plata, La Plata (Argentina); Sanctis, Oscar de [Laboratorio de Materiales Ceramicos, FCEIyA, IFIR, UNR, Rosario (Argentina); Pellegri, Nora [Laboratorio de Materiales Ceramicos, FCEIyA, IFIR, UNR, Rosario (Argentina)], E-mail: pellegri@fceia.unr.edu.ar

2008-12-20

The present work describes a method for preparation of Ag nanoparticles from chemical reduction of AgNO{sub 3} in ethanol with ATS [N-[3-(trimethoxysilyl)propyl] diethylenetriamine] as surface modifier. We study the influence of different parameters such as concentration, time, temperature and reductor agents on the size and shape of the nanoparticles. We present the morphologic and structural characterization of samples by UV-vis extinction spectroscopy, Atomic Force Microscopy (AFM) and X-ray diffraction (XRD). Particularly, using optical extinction spectroscopy, the present work shows the analysis of size evolution in the fabrication process of spherical silver nanoparticles. This evolution is studied as a function of the time elapsed between the beginning of the reaction and the extraction of the sample (temporal delayed synthesis), and as a function of the temperature during the chemical reaction. In both the cases, we propose the study of the plasmon width as a useful, simple and inexpensive method for analysis of the mean radius, specially, for values below 6 nm.

Optical properties and extinction spectroscopy to characterize the synthesis of amine capped silver nanoparticles

International Nuclear Information System (INIS)

Roldan, Maria Virginia; Scaffardi, Lucia B.; Sanctis, Oscar de; Pellegri, Nora

2008-01-01

The present work describes a method for preparation of Ag nanoparticles from chemical reduction of AgNO 3 in ethanol with ATS [N-[3-(trimethoxysilyl)propyl] diethylenetriamine] as surface modifier. We study the influence of different parameters such as concentration, time, temperature and reductor agents on the size and shape of the nanoparticles. We present the morphologic and structural characterization of samples by UV-vis extinction spectroscopy, Atomic Force Microscopy (AFM) and X-ray diffraction (XRD). Particularly, using optical extinction spectroscopy, the present work shows the analysis of size evolution in the fabrication process of spherical silver nanoparticles. This evolution is studied as a function of the time elapsed between the beginning of the reaction and the extraction of the sample (temporal delayed synthesis), and as a function of the temperature during the chemical reaction. In both the cases, we propose the study of the plasmon width as a useful, simple and inexpensive method for analysis of the mean radius, specially, for values below 6 nm

Synthesis of nanocrystalline fluorinated hydroxyapatite

Indian Academy of Sciences (India)

Fluorinated hydroxyapatite; nanocrystalline; microwave synthesis; dissolution. ... HA by the presence of other ions such as carbonate, magnesium, fluoride, etc. ... Fourier transform infrared spectroscopy (FT–IR) and laser Raman spectroscopy.

Chlorococcalean microalgae Ankistrodesmus convolutes biodiesel characterization with Fourier transform-infrared spectroscopy and gas chromatography mass spectroscopy techniques

Directory of Open Access Journals (Sweden)

Swati SONAWANE

2015-12-01

Full Text Available The Chlorococcalean microalgae Ankistrodesmus convolutes was found in fresh water Godawari reservoir, Ahmednagar district of Maharashtra State, India. Microalgae are modern biomass for the production of liquid biofuel due to its high solar cultivation efficiency. The collection, harvesting and drying processes were play vital role in converting algal biomass into energy liquid fuel. The oil extraction was the important step for the biodiesel synthesis. The fatty acid methyl ester (FAME synthesis was carried through base catalyzed transesterification method. The product was analyzed by using the hyphened techniques like Fourier Transform-Infrared spectroscopy (FT-IR and Gas Chromatography Mass Spectroscopy (GCMS. FT-IR Spectroscopy was results the ester as functional group of obtained product while the Gas Chromatography Mass Spectroscopy was results the six type of fatty acid methyl ester with different concentration. Ankistrodesmus convolutes biodiesel consist of 46.5% saturated and 49.14% unsaturated FAME.

FeRu/TiO2 and Fe/TiO2 catalysts after reduction and Fischer-Tropsch synthesis studied by Moessbauer spectroscopy

International Nuclear Information System (INIS)

Kraan, A.M. van der; Nonnekens, R.C.H.; Niemantsverdriet, J.W.

1986-01-01

A series of TiO 2 -supported bimetallic FeRu catalysts with different Fe:Ru ratios (infinity; 10:1; 3:1; 1:1; 1:3) has been studied by means of in situ Moessbauer spectroscopy. The influence of reduction and Fischer-Tropsch synthesis on the state of iron in the FeRu/TiO 2 catalysts is derived. (Auth.)

An unsymmetrical porphyrin and its metal complexes: synthesis, spectroscopy, thermal analysis and liquid crystal properties

Directory of Open Access Journals (Sweden)

CHANGFU ZHUANG

2009-09-01

Full Text Available The synthesis and characterization of a new unsymmetrical porphyrin liquid crystal, 5-(4-stearoyloxyphenylphenyl-10,15,20-triphenylporphyrin (SPTPPH2 and its transition metal complexes (SPTPPM, M(II = Zn, Fe, Co, Ni, Cu or Mn are reported. Their structure and properties were studied by elemental analysis, and UV–Vis, IR, mass and 1H-HMR spectroscopy. Their luminescent properties were studied by excitation and emission spectroscopy. The quantum yields of the S1 ® S0 fluorescence were measured at room temperature. According to thermal studies, the complexes have a higher thermal stability (no decomposition until 200 °C. Differential scanning calorimetry (DSC data and an optical textural photograph, obtained using a polarizing microscope (POM, indicate that the porphyrin ligand had liquid crystalline character and that it exhibited more than one mesophase and a low-lying phase transition temperature, with transition temperatures of 19.3 and 79.4 °C; the temperature range of the liquid crystal (LC phase of the ligand was 70.1 °C.

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.

“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.

BaSnF4 fast ion conductor: Variations versus the method of preparation and anomalous temperature variation of the quadrupole splitting

International Nuclear Information System (INIS)

Hantash, Jamil; Bartlett, Alan; Denes, Georges; Muntasar, Abdualhafeed; Oldfield, Philip

2005-01-01

A new method of preparation of high performance fluoride ion conductor, BaSnF 4 , by water leaching of newly discovered barium tin(II) chloride fluorides, has been designed, and the materials have been studied and compared to the solid prepared by the usual dry method. The unit-cell parameters and crystallite dimensions were found to vary with the method of preparation. In addition, the crystallite dimensions were found to be highly anisotropic for the samples obtained by the wet method. The Moessbauer spectrum is made of a large tin(II) quadrupole doublet, and a broad tin(IV) oxide peak due to surface oxidation. The tin(II) spectrum is in agreement with covalently bonded tin(II) having a strongly stereoactive lone pair. An unusually high dependence of the quadrupole splitting at low temperatures was observed (5.8 times larger than for α-SnF 2 ).

Journal of Chemical Sciences | Indian Academy of Sciences

Indian Academy of Sciences (India)

Transition metal catalysed Grignard-like allylic activation across tetragonal tin(II) oxide · Pradipta Sinha Moloy Banerjee Abhijit Kundu Sujit Roy · More Details Abstract Fulltext PDF. The reaction of allyl halide and a carbonyl compound under the aegis of tetragonal tin(II) oxide and catalytic 8, 10 metal complexes provides ...

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.)

Synthesis of ammonia with microwave plasma

International Nuclear Information System (INIS)

Xu Wenguo; Yu Aimin; Liu Jun; Jin Qinhan

1991-01-01

THe synthesis of ammonia absorbed on 13X zeolite with the aid of microwave plasma is described. The ammonia molecule absorbed on 13X zeolite as ammonium ions were detected by IR spectroscopy. The results obtained show that the ammonia synthesis is facilitated by the surface reactions of NH x (x = 1, 2) radicals adsorbed on zeolite with hydrogen atoms

Photochromism of indolino-benzopyrans studied by NMR and UV-visible spectroscopy

OpenAIRE

S. Delbaere; J. Berthet; M. A. Salvador; G. Vermeersch; M. M. Oliveira

2006-01-01

The synthesis of photochromic 3,3-di(4′-fluorophenyl)-3H-benzopyrans fused to an indole moiety is described. The structures of photomerocyanines elucidated by NMR spectroscopy and spectrokinetic data (λmax⁡ of colored form, colorability, and rate constant of bleaching) obtained by UV-visible spectroscopy are reported.

Synthesis, fabrication, and spectroscopy of nano-scale photonic noble metal materials

Science.gov (United States)

Egusa, Shunji

Nanometer is an interesting scale for physicists, chemists, and materials scientists, in a sense that it lies between the macroscopic and the atomic scales. In this regime, materials exhibit distinct physical and chemical properties that are clearly different from those of atoms or macroscopic bulk. This thesis is concerned about both physics and chemistry of noble metal nano-structures. Novel chemical syntheses and physical fabrications of various noble metal nano-structures, and the development of spectroscopic techniques for nano-structures are presented. Scanning microscopy/spectroscopy techniques inherently perturbs the true optical responses of the nano-structures. However, by using scanning tunneling microscope (STM) tip as the nanometer-confined excitation source of surface plasmons in the samples, and subsequently collecting the signals in the Fourier space, it is shown that the tip-perturbed part of the signals can be deconvoluted. As a result, the collected signal in this approach is the pure response of the sample. Coherent light is employed to study the optical response of nano-structures, in order to avoid complication from tip-perturbation as discussed above. White-light super-continuum excites the nano-structure, the monolayer of Au nanoparticles self-assembled on silicon nitride membrane substrates. The coherent excitation reveals asymmetric surface plasmon resonance in the nano-structures. One of the most important issues in nano-scale science is to gain control over the shape, size, and assembly of nanoparticles. A novel method is developed to chemically synthesize ligand-passivated atomic noble metal clusters in solution phase. The method, named thermal decomposition method, enables facile yet robust synthesis of fluorescent atomic clusters. Thus synthesized atomic clusters are very stable, and show behaviors of quantum dots. A novel and versatile approach for creation of nanoparticle arrays is developed. This method is different from the

Synthesis of Mesoporous Nanocrystalline Zirconia by Surfactant-Assisted Hydrothermal Approach.

Science.gov (United States)

Nath, Soumav; Biswas, Ashik; Kour, Prachi P; Sarma, Loka S; Sur, Ujjal Kumar; Ankamwar, Balaprasad G

2018-08-01

In this paper, we have reported the chemical synthesis of thermally stable mesoporous nanocrystalline zirconia with high surface area using a surfactant-assisted hydrothermal approach. We have employed different type of surfactants such as CTAB, SDS and Triton X-100 in our synthesis. The synthesized nanocrystalline zirconia multistructures exhibit various morphologies such as rod, mortar-pestle with different particle sizes. We have characterized the zirconia multistructures by X-ray diffraction study, Field emission scanning electron microscopy, Attenuated total refection infrared spectroscopy, UV-Vis spectroscopy and photoluminescence spectroscopy. The thermal stability of as synthesized zirconia multistructures was studied by thermo gravimetric analysis, which shows the high thermal stability of nanocrystalline zirconia around 900 °C temperature.

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

International Nuclear Information System (INIS)

Leino, Ewelina; Kumar, Narendra; Mäki-Arvela, Päivi; Aho, Atte; Kordás, Krisztián; Leino, Anne-Riikka; Shchukarev, Andrey; Murzin, Dmitry Yu.; Mikkola, Jyri-Pekka

2013-01-01

Synthesis of cerium (IV) oxide by means of room temperature precipitation method was carried out. The effect of preparation variables such as synthesis time, calcination temperature and pH of the solution on resulting CeO 2 properties was discussed. Moreover, the comparison of CeO 2 samples prepared in a static and rotation mode of synthesis is presented. The solid catalysts were characterized by means of X-ray powder diffraction, scanning electron microscopy, transmission electron microscope, nitrogen physisorption, X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy using pyridine as a probe molecule and temperature programmed desorption of CO 2 . Significant variations in physico-chemical properties of CeO 2 by varying the preparation conditions were observed. Furthermore, the catalytic performances of CeO 2 catalysts were compared in the synthesis of diethyl carbonate starting from ethanol and CO 2 using butylene oxide as a dehydrating agent. The dependence of CeO 2 properties on its catalytic activity is evaluated in detail. - Highlights: • Synthesis of cerium (IV) oxide by precipitation method. • Influence of synthesis time, calcination temperature, mode of stirring and solution pH on properties. • Characterization by XRD, SEM, TEM, nitrogen physisorption, XPS, FTIR. • Catalytic performance diethyl carbonate synthesis from ethanol and CO 2

Phosphoramidates: synthesis, spectroscopy, and X-ray crystallography

Czech Academy of Sciences Publication Activity Database

Shariatinia, Z.; Sohrabi, M.; Yousefi, M.; Kovaľ, Tomáš; Dušek, Michal

2012-01-01

Roč. 23, č. 5 (2012), s. 478-485 ISSN 1042-7163 Grant - others:AV ČR(CZ) AP0701 Program:Akademická prémie - Praemium Academiae Institutional research plan: CEZ:AV0Z10100521 Keywords : phosphoramidates * X-ray diffraction * spectroscopy Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.577, year: 2012

Synthesis and characterization of hydrogen-bond acidic functionalized graphene

Science.gov (United States)

Yang, Liu; Han, Qiang; Pan, Yong; Cao, Shuya; Ding, Mingyu

2014-05-01

Hexafluoroisopropanol phenyl group functionalized materials have great potential in the application of gas-sensitive materials for nerve agent detection, due to the formation of strong hydrogen-bonding interactions between the group and the analytes. In this paper, take full advantage of ultra-large specific surface area and plenty of carbon-carbon double bonds and hexafluoroisopropanol phenyl functionalized graphene was synthesized through in situ diazonium reaction between -C=C- and p-hexafluoroisopropanol aniline. The identity of the as-synthesis material was confirmed by transmission electron microscopy, Raman spectroscopy, ultraviolet visible spectroscopy, X-ray photoelectron spectroscopy and thermo gravimetric analysis. The synthesis method is simply which retained the excellent physical properties of original graphene. In addition, the novel material can be assigned as an potential candidate for gas sensitive materials towards organophosphorus nerve agent detection.

Disproportionation phenema of wistite phase in the model iron catalysts for ammonia synthesis studied by Moessbauer spectroscopy

International Nuclear Information System (INIS)

Pattek-Janczyk, A.; Miczko, B.

1990-01-01

A model iron catalysts for ammonia synthesis containing a large amount of wustite (35 wt%) has been studied during the annealing in an inert atmosphere in the temperature range of 573-773 K. Changes in magnetite and wustite phases were followed by Muessbauer spectroscopy (MS). Before starting the thermal treatment, two kinds of wustite of different structures have been found by MS and X-ray diffraction. The behaviour of both kinds of wustite during the annealing was different. One of them, closer to the stoichiometric compound, disproportionated at once into magnetite and iron; its content decreased systematically without changes in the Muessbauer parameters. In the second wustite, only qualitatieve changes were observed at first (its nonstoichiometry decreases without changes in content and, next, this phase started to disproportionate too. (auhtor). 31 refs.; 6 figs.; 2 tabs

Radiopharmaceutical chelates and method of external imaging

International Nuclear Information System (INIS)

1976-01-01

The preparation of the following chemicals is described: chelates of technetium-99m, cobalt-57, gallium-67, gallium-68, indium-111 or indium-113m and a substituted iminodiacetic acid or an 8-hydroxyquinoline useful as a radiopharmaceutical external imaging agent. The compounds described are suitable for intravenous injection, have an excellent in vivo stability and are good organ seekers. Tin(II) choride or other tin(II) compounds are used as chelating agents

Glycogen synthesis in human gastrocnemius muscle is not representative of whole-body muscle glycogen synthesis.

NARCIS (Netherlands)

Serlie, M.J.; Haan, J.H.A. de; Tack, C.J.J.; Verberne, H.J.; Ackermans, M.T.; Heerschap, A.; Sauerwein, H.P.

2005-01-01

The introduction of 13C magnetic resonance spectroscopy (MRS) has enabled noninvasive measurement of muscle glycogen synthesis in humans. Conclusions based on measurements by the MRS technique assume that glucose metabolism in gastrocnemius muscle is representative for all skeletal muscles and thus

Glycogen synthesis in human gastrocnemius muscle is not representative of whole-body muscle glycogen synthesis

NARCIS (Netherlands)

Serlie, Mireille J. M.; de Haan, Jacco H.; Tack, Cees J.; Verberne, Hein J.; Ackermans, Mariette T.; Heerschap, Arend; Sauerwein, Hans P.

2005-01-01

The introduction of C-13 magnetic resonance spectroscopy (MRS) has enabled noninvasive measurement of muscle glycogen synthesis in humans. Conclusions based on measurements by the MRS technique assume that glucose metabolism in gastrocnemius muscle is representative for all skeletal muscles and thus

Synthesis of fluorescent metal nanoparticles in aqueous solution by photochemical reduction

KAUST Repository

Kshirsagar, Prakash

2014-01-06

A facile green chemistry approach for the synthesis of sub-5 nm silver and gold nanoparticles is reported. The synthesis was achieved by a photochemical method using tyrosine as the photoreducing agent. The size of the gold and silver nanoparticles was about 3 and 4 nm, respectively. The nanoparticles were characterized using x-ray diffraction, transmission electron microscopy, Fourier transform infrared spectroscopy and photoluminescence spectroscopy. Both silver and gold nanoparticles synthesized by this method exhibited fluorescence properties and their use for cell imaging applications has been demonstrated. © 2014 IOP Publishing Ltd.

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.

Tunable synthesis of copper nanotubes

International Nuclear Information System (INIS)

Kaniukov, E; Yakimchuk, D; Kozlovsky, A; Shlimas, D; Zdorovets, M; Kadyrzhanov, K

2016-01-01

Simple method of tunable synthesis of copper nanotubes based on template synthesis was developed. A comprehensive study of the structural, morphological and electrical characteristics of the obtained nanostructures was carried out. Characterization of structural features was made by methods of scanning electron microscopy, energy dispersive spectroscopy and X-ray diffractometry analysis. Evaluation of wall thickness is made by methods of gas permeability. Electrical conductivity of nanotubes was define in the study of their current-voltage characteristics. The possibility to control of copper nanotubes physical properties by variation of the deposition parameters was shown. (paper)

Toxicology of inorganic tin

International Nuclear Information System (INIS)

Burba, J.V.

1982-01-01

Tin(II) or stannous ion as a reducing agent is important in nuclear medicine because it is an essential component and common denominator for many in vivo radiodiagnostic agents, commonly called kits for the preparation of radiopharmaceuticals. This report is intended to alert nuclear medicine community regarding the wide range of biological effects that the stannous ion is capable of producing, and is a review of a large number of selected publications on the toxicological potential of tin(II)

Surface enhanced Raman spectroscopy platform based on graphene with one-year stability

Energy Technology Data Exchange (ETDEWEB)

Tite, Teddy [Univ Lyon, UJM-Saint-Etienne, CNRS, Laboratoire Hubert Curien UMR 5516, 18 rue Professeur Benoit Lauras, F-42000 Saint-Etienne (France); Barnier, Vincent [Ecole Nationale Supérieure des Mines, CNRS, Laboratoire Georges Friedel UMR 5307, 158 cours Fauriel, F-42023 Saint-Etienne (France); Donnet, Christophe, E-mail: Christophe.Donnet@univ-st-etienne.fr [Univ Lyon, UJM-Saint-Etienne, CNRS, Laboratoire Hubert Curien UMR 5516, 18 rue Professeur Benoit Lauras, F-42000 Saint-Etienne (France); Loir, Anne–Sophie; Reynaud, Stéphanie; Michalon, Jean–Yves; Vocanson, Francis; Garrelie, Florence [Univ Lyon, UJM-Saint-Etienne, CNRS, Laboratoire Hubert Curien UMR 5516, 18 rue Professeur Benoit Lauras, F-42000 Saint-Etienne (France)

2016-04-01

We report the synthesis, characterization and use of a robust surface enhanced Raman spectroscopy platform with a stable detection for up to one year of Rhodamine R6G at a concentration of 10{sup −6} M. The detection of aminothiophenol and methyl parathion, as active molecules of commercial insecticides, is further demonstrated at concentrations down to 10{sup −5}–10{sup −6} M. This platform is based on large scale textured few-layer (fl) graphene obtained without any need of graphene transfer. The synthesis route is based on diamond-like carbon films grown by pulsed laser deposition, deposited onto silicon substrates covered by a Ni layer prior to diamond-like carbon deposition. The formation of fl-graphene film, confirmed by Raman spectroscopy and mapping, is obtained by thermal annealing inducing the diffusion of Ni atoms and the concomitant formation of nickel silicide compounds, as identified by Raman and Auger electron spectroscopies. The textured fl-graphene films were decorated with gold nanoparticles to optimize the efficiency of the SERS device to detect organic molecules at low concentrations. - Highlights: • Synthesis of graphene film from amorphous carbon by pulsed laser deposition with nickel catalyst • Large scale textured graphene with nanoscale roughness obtained through nickel silicide formation • Films used for surface enhanced Raman spectroscopy detection of organophosphate compounds • Stability of the SERS platforms over up to one year.

Synthesis, characterization and mechanistic insights of mycogenic iron oxide nanoparticles

Energy Technology Data Exchange (ETDEWEB)

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

2013-11-15

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

Blue green alga mediated synthesis of gold nanoparticles and its antibacterial efficacy against Gram positive organisms

Energy Technology Data Exchange (ETDEWEB)

Uma Suganya, K.S. [Centre for Ocean Research, Sathyabama University, Chennai 600 119 (India); Govindaraju, K., E-mail: govindtu@gmail.com [Centre for Ocean Research, Sathyabama University, Chennai 600 119 (India); Ganesh Kumar, V.; Stalin Dhas, T.; Karthick, V. [Centre for Ocean Research, Sathyabama University, Chennai 600 119 (India); Singaravelu, G. [Nanoscience Division, Department of Zoology, Thiruvalluvar University, Vellore 632115 (India); Elanchezhiyan, M. [Department of Microbiology, Dr ALM Post Graduate Institute of Basic Medical Sciences, University of Madras, Chennai 600113 (India)

2015-02-01

Biofunctionalized gold nanoparticles (AuNPs) play an important role in design and development of nanomedicine. Synthesis of AuNPs from biogenic materials is environmentally benign and possesses high bacterial inhibition and bactericidal properties. In the present study, blue green alga Spirulina platensis protein mediated synthesis of AuNPs and its antibacterial activity against Gram positive bacteria is discussed. AuNPs were characterized using Ultraviolet–visible (UV–vis) spectroscopy, Fluorescence spectroscopy, Fourier Transform-Infrared (FTIR) spectroscopy, Raman spectroscopy, High Resolution-Transmission Electron Microscopy (HR-TEM) and Energy Dispersive X-ray analysis (EDAX). Stable, well defined AuNPs of smaller and uniform shape with an average size of ∼ 5 nm were obtained. The antibacterial efficacy of protein functionalized AuNPs were tested against Gram positive organisms Bacillus subtilis and Staphylococcus aureus. - Highlights: • Size controlled synthesis of gold nanoparticles from blue green alga Spirulina platensis • Stability of gold nanoparticles at different temperatures • Potent antibacterial efficacy against Gram positive organisms.

Waste utilization for the controlled synthesis of nanosized hydroxyapatite

Energy Technology Data Exchange (ETDEWEB)

Nayar, Suprabha, E-mail: Suprabha.nayar@gmail.com [National Metallurgical Laboratory, Jamshedpur (India); Guha, Avijit [National Metallurgical Laboratory, Jamshedpur (India)

2009-05-05

This work uses biomolecules in waste and medicinally important materials for the synthesis of hydroxyapatite nanoparticles. Orange and potato peel, eggshell, papaya leaf and calendula flower extracts have varied biomolecules, which exert a significant, control on the in situ synthesis of nanosized hydroxyapatite particles. The biomimetic synthesis of inorganic particles using known matrices is already well established, however, there are only a few reports using compound extracts. The synthesized nanocomposite has been characterized using X-ray diffraction, Fourier transform infrared spectroscopy and scanning electron microscopy studies. Role of varied biomolecules in controlled inorganic synthesis may have tremendous technological impact.

Combustion synthesis: A new approach for preparation of thermoelectric zinc antimonide compounds

Energy Technology Data Exchange (ETDEWEB)

Rouessac, F., E-mail: Florence.Rouessac@univ-montp2.fr [Institut Charles Gerhardt Montpellier, UMR 5253 CNRS-UM2-ENSCM-UM1, C2M Universite Montpellier 2, CC 1504 Place Eugene Bataillon, 34095 Montpellier Cedex 5 (France); Ayral, R.-M. [Institut Charles Gerhardt Montpellier, UMR 5253 CNRS-UM2-ENSCM-UM1, C2M Universite Montpellier 2, CC 1504 Place Eugene Bataillon, 34095 Montpellier Cedex 5 (France)

2012-07-25

Highlights: Black-Right-Pointing-Pointer Reliable preparation method of thermoelectric materials. Black-Right-Pointing-Pointer Formation of zinc antimonide by the combustion synthesis method is investigated. Black-Right-Pointing-Pointer XRD and Raman spectroscopy as a function of temperature. Black-Right-Pointing-Pointer SHS: a new way for synthesizing thermoelectric materials. - Abstract: Due to the interesting properties of Zn{sub 4}Sb{sub 3} thermoelectric material, a reliable preparation method of this material is required. In this study, the formation of zinc antimonides by the combustion synthesis method is investigated and subjected to characterization using X-ray diffraction and Raman spectroscopy as a function of temperature. The results show that combustion synthesis can be a new way for synthesizing these thermoelectric materials.

Synthesis of fluorescent metal nanoparticles in aqueous solution by photochemical reduction

International Nuclear Information System (INIS)

Kshirsagar, Prakash; Brunetti, Virgilio; Malvindi, Maria Ada; Pompa, Pier Paolo; Sangaru, Shiv Shankar

2014-01-01

A facile green chemistry approach for the synthesis of sub-5 nm silver and gold nanoparticles is reported. The synthesis was achieved by a photochemical method using tyrosine as the photoreducing agent. The size of the gold and silver nanoparticles was about 3 and 4 nm, respectively. The nanoparticles were characterized using x-ray diffraction, transmission electron microscopy, Fourier transform infrared spectroscopy and photoluminescence spectroscopy. Both silver and gold nanoparticles synthesized by this method exhibited fluorescence properties and their use for cell imaging applications has been demonstrated. (paper)

Microwave-Promoted Synthesis of Sulfonated Metallophthalocyanines and Aggregation in Different Solvents

Directory of Open Access Journals (Sweden)

Zhenhua Cheng

2015-01-01

Full Text Available Five metallosulfophthalocyanines (Fe, Ni, Zn, Co, and Cu compounds were synthesized by microwave irradiation. Compared to the conventional method of synthesis in terms of reaction time and yields, the microwave-promoted synthesis is preferred with high product yield and short reaction time. All synthesized products were characterized with MALDI-TOF mass spectrum, Fourier transform infrared spectroscopy (FT-IR, ultraviolet-visible spectroscopy (UV-Vis, and X-ray diffraction (XRD. Aggregation behavior of the five metallosulfophthalocyanines (MSPc in different solvents was studied by UV-Vis spectroscopy separately in N,N-dimethyl formamide (DMF and NaOH aqueous solution (5%wt. A redshift of maximum absorption wavelength and deviations from Lambert-Beer law with increasing the concentration were observed. The dimerization equilibrium constants (K of the five MSPc were determined, respectively.

Room temperature synthesis of ReS2 through aqueous perrhenate sulfidation

Science.gov (United States)

Borowiec, Joanna; Gillin, William P.; Willis, Maureen A. C.; Boi, Filippo S.; He, Y.; Wen, J. Q.; Wang, S. L.; Schulz, Leander

2018-02-01

In this study, a direct sulfidation reaction of ammonium perrhenate (NH4ReO4) leading to a synthesis of rhenium disulfide (ReS2) is demonstrated. These findings reveal the first example of a simplistic bottom-up approach to the chemical synthesis of crystalline ReS2. The reaction presented here takes place at room temperature, in an ambient and solvent-free environment and without the necessity of a catalyst. The atomic composition and structure of the as-synthesized product were characterized using several analysis techniques including energy dispersive x-ray spectroscopy, x-ray photoelectron spectroscopy, x-ray diffraction, transmission electron microscopy, Raman spectroscopy, thermogravimetric analysis and differential scanning calorimetry. The results indicated the formation of a lower symmetry (1Tʹ) ReS2 with a low degree of layer stacking.

Selectivity Enhancement in methylamine synthesis via postsynthesis modification of bronsted acidic mordenite

NARCIS (Netherlands)

Grundling, C.; Gründling, Christian; Mirth, G.C.; Eder-Mirth, Gabriele C.; Lercher, J.A.

1996-01-01

Methylamine synthesis from methanol and ammonia over parent and modified Brønsted acidic mordenites is studied byin situinfrared spectroscopy and kinetic analysis to elucidate the role of elementary steps for activity and selectivity.In situinfrared spectroscopy reveals that all methylammonium ions

Synthesis by plasma of furan particulate polymers

International Nuclear Information System (INIS)

Zuniga L, R.

2014-01-01

This work presents the synthesis of particles derived from furan using low energy plasmas. It is based in the hypothesis that the intense crosslinking of heterocyclic monomers may produce curved surfaces depending on the applied energy in the synthesis. There have been few works related with the synthesis of poly furan as films, but none with morphology of particles within nano or meso dimensions. The syntheses were carried out in a cylindrical reactor at low pressure in gas phase with resistive glow discharges between two electrodes with energy varying from 20 to 120 W. The characterization of the particles was carried out with Energy Dispersive Spectroscopy (EDS), Infrared Spectroscopy (IR), Scanning Electron Microscopy (Sem), Transmission Electron Microscopy (Tem) and X-Ray Photoelectron Spectroscopy (XP S). The morphological studies of the particles were carried out with Sem and Tem showing that the poly furan particles are spherical with a smooth surface and with internal homogeneous composition. They were formed in agglomerates and/or individually with diameters between 214 and 745 nm. The average diameter and the variation of size were reduced by increasing of the applied energy to the synthesis. The structural analysis made by IR and XP S indicates that the poly furan particles have a low content of C-H groups, probably from the monomer, and new multiple bonds such as C=O and C≡C, which suggests dehydrogenation and fragmentation of some furan rings during the synthesis to form crosslinked polymers in combination with other fragments. The energy distribution of C1s orbitals in the particles were adjusted to 5 chemical states at low synthesis energy, 20-60 W, and at higher energy, 80-120 W, another chemical state appeared related to triple bonds, product of a higher oxidation. The hydrogenation in the particles was calculated between 35% and 50%. The energy distribution of O1s orbitals was adjusted to 3 curves, belonging to C-O-H, C-O-C and C=O chemical

Mechanistic aspects of biogenic synthesis of CdS nanoparticles using Bacillus licheniformis

Science.gov (United States)

Tripathi, R. M.; Singh Bhadwal, Akhshay; Singh, Priti; Shrivastav, Archana; Singh, M. P.; Shrivastav, B. R.

2014-06-01

A novel eco-friendly effort has been made for the synthesis of cadmium sulfide (CdS) nanoparticles using bacterial biomass. Although some articles have been reported on CdS nanoparticles synthesis by bacteria, here we have synthesized CdS nanoparticles using non-pathogenic bacteria Bacillus licheniformis MTCC 9555. UV-Vis spectroscopy was carried out to confirm the formation of CdS nanoparticles; the peak occurring at 368 nm gives the indication of synthesis of CdS nanoparticles. The size and morphology of the synthesized CdS nanoparticles were analyzed by transmission electron microscopy (TEM) and the nanoparticles are found to have a narrow size of 5.1 ± 0.5 nm with spherical morphology. Further, the nanoparticles were examined by energy dispersive x-ray (EDX) spectroscopy to identify the presence of elements and confirmed the existence of Cd and S in single nanoparticles. X-ray diffraction (XRD) analysis exhibited 2θ values corresponding to CdS nanocrystals. Fourier transform infrared spectroscopy (FTIR) provides the evidence for the presence of proteins as possible biomolecules responsible for the stabilization of the synthesized CdS nanoparticles.

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.)

A General Chemistry Experiment Incorporating Synthesis and Structural Determination

Science.gov (United States)

van Ryswyk, Hal

1997-07-01

An experiment for the general chemistry laboratory is described wherein gas chromatography-mass spectroscopy (GC-MS) and diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) are used to characterize the products of a series of microscale reactions on vanillin. A single sophisticated instrument can be incorporated into the laboratory given sufficient attention to the use of sampling accessories and software macros. Synthetic experiments coupled with modern instrumental techniques can be used in the general chemistry laboratory to illustrate the concepts of synthesis, structure, bonding, and spectroscopy.

Fast and inexpensive synthesis of pentacene with high yield using 6,13-pentacenequinone as precursor

Science.gov (United States)

Mota, María L.; Rodriguez, Bibiana; Carrillo, Amanda; Ambrosio, Roberto C.; Luque, Priscy A.; Mireles, Marcela; Vivaldo, Israel; Quevedo, Manuel A.

2018-02-01

Pentacene is an important semiconductor in the field of organic electronics. In this work is presented an alternative synthesis procedure to obtain pentacene from 6,13-pentacenequinone as a precursor. Synthesis of pentacene was performed in two reactions, Diels-Adler cycloaddition of 6,13-pentacenequinone followed by 6,13-pentacenequinone reduction to pentacene, employing LiAlH4 as reducing agent. The products were characterized by Fourier Transform Infrared Spectroscopy (FTIR), 1H-Nuclear Magnetic Resonance Spectroscopy (1H-NMR), X-Ray Diffraction (XRD), Thermogravimetric Analysis (TGA) and Ultraviolet-Visible Spectroscopy (UV-VIS). In this work, 6,13-pentacenequinone was synthetized with a high yield (55%) using an alternative method. The optimization process resulted in an overall reduction of reaction time while exhibiting high yield. The method presented here provides an affordable pentacene synthesis route with high purity, which can be further applied for research and development of organic electronic applications.

Sci—Fri AM: Mountain — 04: Label-free Raman spectroscopy of single tumour cells detects early radiation-induced glycogen synthesis associated with increased radiation resistance

International Nuclear Information System (INIS)

Matthews, Q; Lum, JJ; Isabelle, M; Harder, S; Jirasek, A; Brolo, AG

2014-01-01

Purpose: To use label-free Raman spectroscopy (RS) for early treatment monitoring of tumour cell radioresistance. Methods: Three human tumour cell lines, two radioresistant (H460, SF 2 = 0.57 and MCF7, SF 2 = 0.70) and one radiosensitive (LNCaP, SF 2 = 0.36), were irradiated with single fractions of 2, 4, 6, 8 or 10 Gy. In additional experiments, H460 and MCF7 cells were irradiated under co-treatment with the anti-diabetic drug metformin, a known radiosensitizing agent. Treated and control cultures were analyzed with RS daily for 3 days post-treatment. Single-cell Raman spectra were acquired from 20 live cells per sample, and experiments were repeated in triplicate. The combined data sets were analyzed with principal component analysis using standard algorithms. Cells from each culture were also subjected to standard assays for viability, proliferation, cell cycle, and radiation clonogenic survival. Results: The radioresistant cells (H460, MCF7) exhibited a RS molecular radiation response signature, detectable as early as 1 day post-treatment, of which radiation-induced glycogen synthesis is a significant contributor. The radiosensitive cells (LNCaP) exhibited negligible glycogen synthesis. Co-treatment with metformin in MCF7 cells blocked glycogen synthesis, reduced viability and proliferation, and increased radiosensitivity. Conversely, metformin co-treatment in H460 cells did not produce these same effects; importantly, both radiation-induced synthesis of glycogen and radiosensitivity were unaffected. Conclusions: Label-free RS can detect early glycogen synthesis post-irradiation, a previously undocumented metabolic mechanism associated with tumour cell radioresistance that can be targeted to increase radiosensitivity. RS monitoring of intratumoral glycogen may provide new opportunities for personalized combined modality radiotherapy treatments

Sci—Fri AM: Mountain — 04: Label-free Raman spectroscopy of single tumour cells detects early radiation-induced glycogen synthesis associated with increased radiation resistance

Energy Technology Data Exchange (ETDEWEB)

Matthews, Q; Lum, JJ [BC Cancer Agency — Vancouver Island Centre (Canada); Isabelle, M; Harder, S; Jirasek, A [Physics and Astronomy, University of Victoria (Australia); Brolo, AG [Chemistry, University of Victoria (Australia)

2014-08-15

Purpose: To use label-free Raman spectroscopy (RS) for early treatment monitoring of tumour cell radioresistance. Methods: Three human tumour cell lines, two radioresistant (H460, SF{sub 2} = 0.57 and MCF7, SF{sub 2} = 0.70) and one radiosensitive (LNCaP, SF{sub 2} = 0.36), were irradiated with single fractions of 2, 4, 6, 8 or 10 Gy. In additional experiments, H460 and MCF7 cells were irradiated under co-treatment with the anti-diabetic drug metformin, a known radiosensitizing agent. Treated and control cultures were analyzed with RS daily for 3 days post-treatment. Single-cell Raman spectra were acquired from 20 live cells per sample, and experiments were repeated in triplicate. The combined data sets were analyzed with principal component analysis using standard algorithms. Cells from each culture were also subjected to standard assays for viability, proliferation, cell cycle, and radiation clonogenic survival. Results: The radioresistant cells (H460, MCF7) exhibited a RS molecular radiation response signature, detectable as early as 1 day post-treatment, of which radiation-induced glycogen synthesis is a significant contributor. The radiosensitive cells (LNCaP) exhibited negligible glycogen synthesis. Co-treatment with metformin in MCF7 cells blocked glycogen synthesis, reduced viability and proliferation, and increased radiosensitivity. Conversely, metformin co-treatment in H460 cells did not produce these same effects; importantly, both radiation-induced synthesis of glycogen and radiosensitivity were unaffected. Conclusions: Label-free RS can detect early glycogen synthesis post-irradiation, a previously undocumented metabolic mechanism associated with tumour cell radioresistance that can be targeted to increase radiosensitivity. RS monitoring of intratumoral glycogen may provide new opportunities for personalized combined modality radiotherapy treatments.

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

International Nuclear Information System (INIS)

Quispe M, J.; Moreno, M.; Montano, J.; Pillaca, M.; Guzman, A.; Cavero, A.; Arce, M.

2009-01-01

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

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.

Synthesis of nanocrystalline Y2O3 in a specially designed atmospheric pressure radio frequency thermal plasma reactor

International Nuclear Information System (INIS)

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

2015-01-01

Synthesis of yttrium oxide nanoparticles in a specially designed radio frequency thermal plasma reactor is reported. Good crystallinity, narrow size distribution, low defect state concentration, high purity, good production rate, single-step synthesis, and simultaneous formation of nanocrystalline monoclinic and cubic phases are some of the interesting features observed. Synthesized particles are characterized through X-ray diffraction, transmission electron microscopy, scanning electron microscopy, Fourier transform infrared spectroscopy, thermo-luminescence (TL), and Brunauer–Emmett–Teller surface area analysis. Polymorphism of the nanocrystalline yttria is addressed in detail. Synthesis mechanism is explored through in-situ emission spectroscopy. Post-synthesis environmental effects and possible methods to eliminate the undesired phases are probed. Defect states are investigated through the study of TL spectra

Synthesis of [21-13C]-cholesterol

International Nuclear Information System (INIS)

Caballero, G.M.; Gros, E.G.

1994-01-01

The synthesis of [21- 13 C]-cholesterol from 3β-O-(t-butyldimethylsilyl)-17β-cyano-androst-5-ene is described. Labelled carbon-atom was introduced by Grignard reaction of nitrile derivative with [ 13 C]-methylmagnesium iodide. Location of label was confirmed by 13 C-NMR spectroscopy. (author)

Iron Oxide Nanoparticles Employed as Seeds for the Induction of Microcrystalline Diamond Synthesis

Directory of Open Access Journals (Sweden)

Resto Oscar

2008-01-01

Full Text Available AbstractIron nanoparticles were employed to induce the synthesis of diamond on molybdenum, silicon, and quartz substrates. Diamond films were grown using conventional conditions for diamond synthesis by hot filament chemical vapor deposition, except that dispersed iron oxide nanoparticles replaced the seeding. X-ray diffraction, visible, and ultraviolet Raman Spectroscopy, energy-filtered transmission electron microscopy , electron energy-loss spectroscopy, and X-ray photoelectron spectroscopy (XPS were employed to study the carbon bonding nature of the films and to analyze the carbon clustering around the seed nanoparticles leading to diamond synthesis. The results indicate that iron oxide nanoparticles lose the O atoms, becoming thus active C traps that induce the formation of a dense region of trigonally and tetrahedrally bonded carbon around them with the ensuing precipitation of diamond-type bonds that develop into microcrystalline diamond films under chemical vapor deposition conditions. This approach to diamond induction can be combined with dip pen nanolithography for the selective deposition of diamond and diamond patterning while avoiding surface damage associated to diamond-seeding methods.

Mechanistic aspects of biogenic synthesis of CdS nanoparticles using Bacillus licheniformis

International Nuclear Information System (INIS)

Tripathi, R M; Shrivastav, Archana; Bhadwal, Akhshay Singh; Singh, Priti; Singh, M P; Shrivastav, B R

2014-01-01

A novel eco-friendly effort has been made for the synthesis of cadmium sulfide (CdS) nanoparticles using bacterial biomass. Although some articles have been reported on CdS nanoparticles synthesis by bacteria, here we have synthesized CdS nanoparticles using non-pathogenic bacteria Bacillus licheniformis MTCC 9555. UV-Vis spectroscopy was carried out to confirm the formation of CdS nanoparticles; the peak occurring at 368 nm gives the indication of synthesis of CdS nanoparticles. The size and morphology of the synthesized CdS nanoparticles were analyzed by transmission electron microscopy (TEM) and the nanoparticles are found to have a narrow size of 5.1 ± 0.5 nm with spherical morphology. Further, the nanoparticles were examined by energy dispersive x-ray (EDX) spectroscopy to identify the presence of elements and confirmed the existence of Cd and S in single nanoparticles. X-ray diffraction (XRD) analysis exhibited 2θ values corresponding to CdS nanocrystals. Fourier transform infrared spectroscopy (FTIR) provides the evidence for the presence of proteins as possible biomolecules responsible for the stabilization of the synthesized CdS nanoparticles. (papers)

Facile and green synthesis of highly stable L-cysteine functionalized copper nanoparticles

International Nuclear Information System (INIS)

Kumar, Nikhil; Upadhyay, Lata Sheo Bachan

2016-01-01

Highlights: • A facile and eco-friendly method for the synthesis of L-cysteine functionalized copper nanoparticles is reported. • Synthesis of Highly stable L-cysteine functionalized copper nanoparticles (∼40 nm) was done in an aqueous medium. • FTIR analysis shows that L-cysteine bound to the nanoparticle surface via thiol group. - Abstract: A simple eco-friendly method for L-cysteine capped copper nanoparticles (CCNPs) synthesis in aqueous solution has been developed. Glucose and L-cysteine were used as reducing agent and capping/functionalizing agent, respectively. Different parameters such as capping agent concentration, pH, reaction temperature, and reducing agent concentration were optimized during the synthesis. The L-cysteine capped copper nanoparticle were characterized by ultraviolet-visible spectroscopy, Fourier-transform infrared spectroscopy, X-ray diffraction, Particle size and zeta potential analyser, and high resolution transmission electron microscopy. Spherical shaped cysteine functionalized/capped copper nanoparticles with an average size of 40 nm were found to be highly stable at room temperature (RT) for a period of 1 month

Facile and green synthesis of highly stable L-cysteine functionalized copper nanoparticles

Energy Technology Data Exchange (ETDEWEB)

Kumar, Nikhil, E-mail: nkumar.phd2011.bt@nitrr.ac.in; Upadhyay, Lata Sheo Bachan, E-mail: contactlataupadhyay@gmail.com

2016-11-01

Highlights: • A facile and eco-friendly method for the synthesis of L-cysteine functionalized copper nanoparticles is reported. • Synthesis of Highly stable L-cysteine functionalized copper nanoparticles (∼40 nm) was done in an aqueous medium. • FTIR analysis shows that L-cysteine bound to the nanoparticle surface via thiol group. - Abstract: A simple eco-friendly method for L-cysteine capped copper nanoparticles (CCNPs) synthesis in aqueous solution has been developed. Glucose and L-cysteine were used as reducing agent and capping/functionalizing agent, respectively. Different parameters such as capping agent concentration, pH, reaction temperature, and reducing agent concentration were optimized during the synthesis. The L-cysteine capped copper nanoparticle were characterized by ultraviolet-visible spectroscopy, Fourier-transform infrared spectroscopy, X-ray diffraction, Particle size and zeta potential analyser, and high resolution transmission electron microscopy. Spherical shaped cysteine functionalized/capped copper nanoparticles with an average size of 40 nm were found to be highly stable at room temperature (RT) for a period of 1 month.

Scanning Angle Raman spectroscopy in polymer thin film characterization

Energy Technology Data Exchange (ETDEWEB)

Nguyen, Vy H.T. [Iowa State Univ., Ames, IA (United States)

2015-12-19

The focus of this thesis is the application of Raman spectroscopy for the characterization of thin polymer films. Chapter 1 provides background information and motivation, including the fundamentals of Raman spectroscopy for chemical analysis, scanning angle Raman scattering and scanning angle Raman scattering for applications in thin polymer film characterization. Chapter 2 represents a published manuscript that focuses on the application of scanning angle Raman spectroscopy for the analysis of submicron thin films with a description of methodology for measuring the film thickness and location of an interface between two polymer layers. Chapter 3 provides an outlook and future directions for the work outlined in this thesis. Appendix A, contains a published manuscript that outlines the use of Raman spectroscopy to aid in the synthesis of heterogeneous catalytic systems. Appendix B and C contain published manuscripts that set a foundation for the work presented in Chapter 2.

Precision Spectroscopy, Diode Lasers, and Optical Frequency Measurement Technology

Science.gov (United States)

Hollberg, Leo (Editor); Fox, Richard (Editor); Waltman, Steve (Editor); Robinson, Hugh

1998-01-01

This compilation is a selected set of reprints from the Optical Frequency Measurement Group of the Time and Frequency Division of the National Institute of Standards and Technology, and consists of work published between 1987 and 1997. The two main programs represented here are (1) development of tunable diode-laser technology for scientific applications and precision measurements, and (2) research toward the goal of realizing optical-frequency measurements and synthesis. The papers are organized chronologically in five, somewhat arbitrarily chosen categories: Diode Laser Technology, Tunable Laser Systems, Laser Spectroscopy, Optical Synthesis and Extended Wavelength Coverage, and Multi-Photon Interactions and Optical Coherences.

Two-Nozzle Flame Spray Pyrolysis (FSP) Synthesis of CoMo/Al2O3 Hydrotreating Catalysts

DEFF Research Database (Denmark)

Høj, Martin; Pham, David K.; Brorson, Michael

2013-01-01

and the hydrodenitrogenation activity improved from 70 to 90 % relative activity. This suggests that better promotion of the active molybdenum sulfide phase was achieved when using two-nozzle FSP synthesis, probably due to less formation of the undesired phase CoAl2O4, which makes Co unavailable for promotion.......Two-nozzle frame spray analysis (FSP) synthesis of CoMo/Al2O3 where Co and Al are sprayed in separate flames was applied to minimize the formation of CoAl2O4 observed in one-nozzle flame spray pyrolysis (FSP) synthesis and the materials were characterized by N2-adsorption (BET), X-ray diffraction...... (XRD), UV–vis diffuse reflectance spectroscopy, Raman spectroscopy, transmission electron microscopy, and catalytic performances in hydrotreating. By varying the flame mixing distances (81–175 mm) the amount of CoAl2O4 could be minimized. As evidenced by UV–vis spectroscopy, CoAl2O4 was detected only...

Isobutylene Dimerization: A Discovery-Based Exploration of Mechanism and Regioselectivity by NMR Spectroscopy and Molecular Modeling

Science.gov (United States)

Schuster, Mariah L.; Peterson, Karl P.; Stoffregen, Stacey A.

2018-01-01

This two-period undergraduate laboratory experiment involves the synthesis of a mixture of isomeric unknowns, isolation of the mixture by means of distillation, and characterization of the two products primarily by NMR spectroscopy (1D and 2D) supported with IR spectroscopy and GC-MS techniques. Subsequent calculation and examination of the…

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.

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.

Synthesis, characterization and impedance spectroscopy study of magnetite/epoxidized natural rubber nanocomposites

Energy Technology Data Exchange (ETDEWEB)

Tan, W.L. [Nanoscience Research Laboratory, School of Chemical Sciences, Universiti Sains Malaysia, 11800 Penang (Malaysia); Abu Bakar, M., E-mail: bmohamad@usm.my [Nanoscience Research Laboratory, School of Chemical Sciences, Universiti Sains Malaysia, 11800 Penang (Malaysia)

2013-06-05

Highlights: ► The Fe{sub 3}O{sub 4}/ENR nanocomposites have not been synthesized and reported. ► Nanocomposites were obtained via in situ synthesis of Fe{sub 3}O{sub 4} in the presence of ENR. ► The use of ENR enabled control of the size of Fe{sub 3}O{sub 4} particles to <20 nm. ► Conductivity of the nanocomposites increases with the increase in Fe{sub 3}O{sub 4} loading. ► The equivalent circuit for the nanocomposites is proposed and discussed. -- Abstract: The magnetite (Fe{sub 3}O{sub 4}) particles were synthesized in situ in the presence of epoxidized natural rubber (ENR) to produce the various Fe{sub 3}O{sub 4}/ENR nanocomposites. The X-ray diffraction (XRD) analysis confirmed the existence of Fe{sub 3}O{sub 4} particles in the composites. The FTIR and DSC studies suggested that no chemical interactions between the particles and the matrix. The SEM and X-mapping micrographs revealed that the Fe{sub 3}O{sub 4} particles were distributed within the ENR matrix. The ENR matrix exerts control on the Fe{sub 3}O{sub 4} particles with a size of <20 nm in the composites. The Fe{sub 3}O{sub 4} particles also affect the electrical properties of the composites. Impedance spectroscopy studies show that the electrical conductivity of the nanocomposites increases with the increase in Fe{sub 3}O{sub 4} loading in the composite. The equivalent circuit for the Fe{sub 3}O{sub 4}/ENR nanocomposites is proposed and discussed.

Anchoring of Cu(II) onto surface of porous metal-organic framework through post-synthesis modification for the synthesis of benzimidazoles and benzothiazoles

Science.gov (United States)

Kardanpour, Reihaneh; Tangestaninejad, Shahram; Mirkhani, Valiollah; Moghadam, Majid; Mohammadpoor-Baltork, Iraj; Zadehahmadi, Farnaz

2016-03-01

Efficient synthesis of various benzimidazoles and benzothiazoles under mild conditions catalyzed by Cu(II) anchored onto UiO-66-NH2 metal organic framework is reported. In this manner, first, the aminated UiO-66 was modified with thiophene-2-carbaldehyde and then the prepared Schiff base was reacted with CuCl2. The prepared catalyst was characterized by FT-IR, UV-vis, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), N2 adsorption, inductively coupled plasma atomic emission spectroscopy (ICP-AES) and field emission scanning electron microscopy (FE-SEM). The UiO-66-NH2-TC-Cu was applied as a highly efficient catalyst for synthesis of benzimidazole and benzothiazole derivatives by the reaction of aldehydes with 1,2-diaminobenzene or 2-aminothiophenol. The Cu(II)-containing MOF was reused several times without any appreciable loss of its efficiency.

Room temperature synthesis of ReS2 through aqueous perrhenate sulfidation.

Science.gov (United States)

Borowiec, Joanna; Gillin, William P; Willis, Maureen; Boi, Filippo; He, Yi; Wen, Jiqiu; Wang, Shanling; Schulz, Leander

2017-12-29

In this study, a direct sulfidation reaction of ammonium perrhenate (NH₄ReO₄) leading to a synthesis of rhenium disulfide (ReS₂) is demonstrated. These finding reveal the first example of a simplistic bottom-up approach to the chemical synthesis of crystalline ReS₂. The reaction presented here takes place at room temperature, in an ambient and solvent-free environment and without the necessity of a catalyst. The atomic composition and structure of the as-synthesized product were characterized using several analysis techniques including energy dispersive X-ray (EDX) spectroscopy, X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), transmission electron microscopy (TEM), Raman spectroscopy, thermogravimetric analysis (TGA) and differential scannig calorimetry (DSC). The results indicated the formation of a lower symmetry (1T_d) ReS₂ with a low degree of layer stacking. © 2017 IOP Publishing Ltd.

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.

Combustion Synthesis Of Ultralow-density Nanoporous Gold Foams

Energy Technology Data Exchange (ETDEWEB)

Tappan, Bruce C [Los Alamos National Laboratory; Mueller, Alex H [Los Alamos National Laboratory; Steiner, Stephen A [Los Alamos National Laboratory; Luther, Erik P [Los Alamos National Laboratory

2008-01-01

A new synthetic pathway for producing nanoporous gold monoliths through combustion synthesis from Au bistetrazoJeamine complexes has been demonstrated. Applications of interest for Au nanofoams include new substrates for nanoparticle-mediated catalysis, embedded antennas, and spectroscopy. Integrated support-and-catalystin-one nanocomposites prepared through combustion synthesis of mixed AuBTA/metal oxide pellets would also be an interesting technology approach for low-cost in-line catalytic conversion media. Furthermore, we envision preparation of ultrahigh surface area gold electrodes for application in electrochemical devices through this method.

Facile and green synthesis of highly stable L-cysteine functionalized copper nanoparticles

Science.gov (United States)

Kumar, Nikhil; Upadhyay, Lata Sheo Bachan

2016-11-01

A simple eco-friendly method for L-cysteine capped copper nanoparticles (CCNPs) synthesis in aqueous solution has been developed. Glucose and L-cysteine were used as reducing agent and capping/functionalizing agent, respectively. Different parameters such as capping agent concentration, pH, reaction temperature, and reducing agent concentration were optimized during the synthesis. The L-cysteine capped copper nanoparticle were characterized by ultraviolet-visible spectroscopy, Fourier-transform infrared spectroscopy, X-ray diffraction, Particle size and zeta potential analyser, and high resolution transmission electron microscopy. Spherical shaped cysteine functionalized/capped copper nanoparticles with an average size of 40 nm were found to be highly stable at room temperature (RT) for a period of 1 month

Extracellular synthesis gold nanotriangles using biomass of Streptomyces microflavus.

Science.gov (United States)

Soltani Nejad, Meysam; Khatami, Mehrdad; Shahidi Bonjar, Gholam Hosein

2016-02-01

Applications of nanotechnology and nano-science have ever-expanding breakthroughs in medicine, agriculture and industries in recent years; therefore, synthesis of metals nanoparticle (NP) has special significance. Synthesis of NPs by chemical methods are long, costly and hazardous for environment so biosynthesis has been developing interest for researchers. In this regard, the extracellular biosynthesis of gold nanotriangles (AuNTs) performed by use of the soil Streptomycetes. Streptomycetes isolated from rice fields of Guilan Province, Iran, showed biosynthetic activity for producing AuNTs via in vitro experiments. Among all 15 Streptomyces spp. isolates, isolate No. 5 showed high biosynthesis activity. To determine the bacterium taxonomical identity at genus level, its colonies characterised morphologically by use of scanning electron microscope. The polymerase chain reaction (PCR) molecular analysis of active isolate represented its identity partially. In this regard, 16S rRNA gene of the isolate was amplified using universal bacterial primers FD1 and RP2. The PCR products were purified and sequenced. Sequence analysis of 16S rDNA was then conducted using National Center for Biotechnology Information Basic Local Alignment Search Tool method. The AuNTs obtained were characterised by ultraviolet-visible spectroscopy, atomic force microscopy, transmission electron microscopy and energy dispersive X-ray spectroscopy, Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction spectroscopy analyses. The authors results indicated that Streptomyces microflavus isolate 5 bio-synthesises extracellular AuNTs in the range of 10-100 nm. Synthesised SNPs size ranged from 10 to 100 nm. In comparison with chemical methods for synthesis of metal NPs, the biosynthesis of AuNTs by Streptomyces source is a fast, simple and eco-friendly method. The isolate is a good candidate for further investigations to optimise its production efficacy for further industrial goals in

Study of the influence in crystallization period in MCM-22 zeolite synthesis

International Nuclear Information System (INIS)

Barbosa, A.S.; Santos, E.R.F.; Rodrigues, M.G.F.

2011-01-01

The synthesis of MCM-22 is accomplished by hydrothermal treatment and long periods needed for crystallization, with the gradual growth of crystals of 10-14 days. MCM-22 catalyst is studied intensively as promising, with high thermal stability. As part of a line of research focused on the development of zeolite with lowest cost, this study aimed to examine the effect in decreasing the period of crystallization in the synthesis of zeolite MCM-22. The materials were characterized by X-ray diffraction (XRD) spectroscopy, X-ray Energy Dispersive (EDX) and Fourier transform infrared spectroscopy and Fourier transform (FT-IR). By XRD it was observed that the hydrothermal treatment used in the synthesis was effective during periods of crystallization and EDX was observed that the samples have a high percentage of silica and low alumina content, which gives them a high ratio SiO 2 /Al 2 O 3 characteristic of the MWW structure. (author)

Synthesis of indium nanoparticles at ambient temperature; simultaneous phase transfer and ripening

Energy Technology Data Exchange (ETDEWEB)

Aghazadeh Meshgi, Mohammad; Kriechbaum, Manfred [Graz University of Technology, Institute of Inorganic Chemistry (Austria); Biswas, Subhajit; Holmes, Justin D., E-mail: j.holmes@ucc.ie [University College Cork, Materials Chemistry and Analysis Group, Department of Chemistry and the Tyndall National Institute (Ireland); Marschner, Christoph, E-mail: christoph.marschner@tugraz.at [Graz University of Technology, Institute of Inorganic Chemistry (Austria)

2016-12-15

The synthesis of size-monodispersed indium nanoparticles via an innovative simultaneous phase transfer and ripening method is reported. The formation of nanoparticles occurs in a one-step process instead of well-known two-step phase transfer approaches. The synthesis involves the reduction of InCl{sub 3} with LiBH{sub 4} at ambient temperature and although the reduction occurs at room temperature, fine indium nanoparticles, with a mean diameter of 6.4 ± 0.4 nm, were obtained directly in non-polar n-dodecane. The direct synthesis of indium nanoparticles in n-dodecane facilitates their fast formation and enhances their size-monodispersity. In addition, the nanoparticles were highly stable for more than 2 months. The nanoparticles were characterised by dynamic light scattering (DLS), small angle X-ray scattering (SAXS), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDS) and Fourier transform infrared (FT-IR) spectroscopy to determine their morphology, structure and phase purity.

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, ...

Synthesis and characterization of graphene quantum dots/cobalt ferrite nanocomposite

Science.gov (United States)

Ramachandran, Shilpa; Sathishkumar, M.; Kothurkar, Nikhil K.; Senthilkumar, R.

2018-02-01

A facile method has been developed for the synthesis of a graphene quantum dots/cobalt ferrite nanocomposite. Graphene quantum dots (GQDs) were synthesized by a simple bottom-up method using citric acid, followed by the co-precipitation of cobalt ferrite nanoparticles on the graphene quantum dots. The morphology, structural analysis, optical properties, magnetic properties were investigated using transmission electron microscopy (TEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), UV-vis absorption spectroscopy, fluorescence spectroscopy, vibrating sample magnetometry (VSM) measurements. The synthesized nanocomposite showed good fluorescence and superparamagnetic properties, which are important for biomedical applications.

Solution-Phase Synthesis of SnSe Nanocrystals for Use in Solar Cells

KAUST Repository

Franzman, Matthew A.

2010-03-31

Nanocrystals of phase-pure tin(II) selenide (SnSe) were synthesized via a solution-phase route employing stoichiometric amounts of di-tert-butyl dlselenlde as a novel and facile selenium source. The direct band gap of the resulting nanocrystals (E8 = 1.71 eV) is significantly blue-shifted relative to the bulk value (E8 = 1.30 eV), a likely consequence of quantum confinement resulting from the relatively small average diameter of the nanocrystals (μD < 20 nm). Preliminary solar cell devices incorporating SnSe nanocrystals into a poly[2-methoxy5-(3\\',7\\'-d1methyloctyloxy)-1,4- phenylenev1nylene] matrix demonstrate a significant enhancement In quantum efficiency and short-circuit current density, suggesting that this earth-abundant material could be a valuable component In future photovoltaic devices. Copyright © 2010 American Chemical Society.

Synthesis of Diblock Codendrimer by Double Click Chemistry

Energy Technology Data Exchange (ETDEWEB)

Lee, Jae Wook; Han, Seung Choul; Ji, Won Ho [Dong-A Univ., Busan (Korea, Republic of); Jin, Sungho [Pusan National Univ., Busan (Korea, Republic of); Kim, Ji Hyeon [Gachon Univ., Seongnam (Korea, Republic of)

2012-12-15

Efficient double click methods for the synthesis of diblock codendrimers were developed. The synthetic strategy involved the sequential click reactions between an alkyne and an azide. The short core building block, 1,4-diazidobutane, was chosen to serve as the azide functionalities for dendrimer growth via click reactions with the alkyne-functionalized PAMAM dendrons as hydrophilic dendron and alkyne-functionalized Frechet-type dendrons as hydrophobic dendron. The structure of diblock codendrimers was confirmed by {sup 1}H and {sup 13}C NMR spectroscopy, IR spectroscopy, mass spectrometry, and GPC analysis.

Synthesis of Diblock Codendrimer by Double Click Chemistry

International Nuclear Information System (INIS)

Lee, Jae Wook; Han, Seung Choul; Ji, Won Ho; Jin, Sungho; Kim, Ji Hyeon

2012-01-01

Efficient double click methods for the synthesis of diblock codendrimers were developed. The synthetic strategy involved the sequential click reactions between an alkyne and an azide. The short core building block, 1,4-diazidobutane, was chosen to serve as the azide functionalities for dendrimer growth via click reactions with the alkyne-functionalized PAMAM dendrons as hydrophilic dendron and alkyne-functionalized Frechet-type dendrons as hydrophobic dendron. The structure of diblock codendrimers was confirmed by 1 H and 13 C NMR spectroscopy, IR spectroscopy, mass spectrometry, and GPC analysis

Fundamental aspects of nucleation and growth in the solution-phase synthesis of germanium nanocrystals

KAUST Repository

Codoluto, Stephen C.

2010-01-01

Colloidal Ge nanocrystals (NCs) were synthesized via the solution phase reduction of germanium(ii) iodide. We report a systematic investigation of the nanocrystal nucleation and growth as a function of synthesis conditions including the nature of coordinating solvents, surface bound ligands, synthesis duration and temperature. NC synthesis in reaction environments with weakly bound phosphine surface ligand led to the coalescence of nascent particles leading to ensembles with broad lognormal particle diameter distributions. Synthesis in the presence of amine or alkene ligands mitigated particle coalescence. High-resolution transmission electron micrographs revealed that NCs grown in the presence of weak ligands had a high crystal defect density whereas NCs grown in amine solutions were predominantly defect-free. We applied infrared spectroscopy to study the NC surface chemistry and showed that alkene ligands project the NCs from surface oxidation. Photoluminescence spectroscopy measurements showed that alkene ligands passivate surface traps, as indicated by infrared fluorescence, conversely oxidized phosphine and amine passivated NCs did not fluoresce. © 2010 The Royal Society of Chemistry.

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)

Green synthesis, characterization and antibacterial efficacy of palladium nanoparticles synthesized using Filicium decipiens leaf extract

Science.gov (United States)

Sharmila, G.; Farzana Fathima, M.; Haries, S.; Geetha, S.; Manoj Kumar, N.; Muthukumaran, C.

2017-06-01

Synthesis of metal nanoparticles through green chemistry route is an emerging eco-friendly approach in the present days. An eco-friendly, biogenic synthesis of palladium nanoparticles (PdNPs) using Filicium decipiens leaf extract was reported in the present study. The synthesized PdNPs were characterized by UV-visible spectroscopy, Transmission electron microscopy (TEM), X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR). The PdNPs formation was confirmed by UV-visible spectrophotometer and spherical shaped PdNPs with size range of 2-22 nm was observed in TEM analysis. Energy dispersive X-ray spectroscopy (EDS) analysis confirmed the presence of palladium in the synthesized nanoparticles. The crystalline nature of PdNPs was confirmed by XRD pattern and compared with the standard. The phytochemicals and proteins were identified by their functional groups in FT-IR spectrum and revealed the amide, amine groups present in F. decipiens may have involved in the bio-reduction reaction for PdNPs synthesis. Prepared PdNPs showed potential antibacterial activity against both Gram-positive and Gram-negative bacteria. F. decipiens leaf extract based PdNPs showed high bactericidal activity against Escherichia coli, Pseudomonas aeruginosa as compared to Staphylococcus aureus and Bacillus subtilis Results showed that phytochemicals rich F. decipiens leaf extract may be utilized as an effective non-toxic reducing agent for PdNPs synthesis and prepared PdNPs may useful in biomedical applications.

Synthesis and structure of the unligated carbene of chromium

Energy Technology Data Exchange (ETDEWEB)

Billups, W.E.; Souchan Chang; Hauge, R.H.; Margrave, J.L. (Rice Univ., Houston, TX (United States))

1993-04-14

Complexes with metal-carbon double bonds have found applications as intermediates in many important catalytic reactions including cyclopropanation of alkenes by diazoalkanes, Fischer-Tropsch synthesis, olefin metathesis, Ziegler-Natta polymerization, alkane activation, and in the decomposition of transition metal alkyl complexes. However, complexes with the simplest carbene, CH[sub 2], coordinated to the metal center are relatively rare. In this paper the authors report the synthesis and characterization of the simple unligated carbene of chromium by FTIR matrix isolation spectroscopy. 7 refs., 3 figs., 4 tabs.

The Synthesis of "N"-Benzyl-2-Azanorbornene via Aqueous Hetero Diels-Alder Reaction: An Undergraduate Project in Organic Synthesis and Structural Analysis

Science.gov (United States)

Sauvage, Xavier; Delaude, Lionel

2008-01-01

The synthesis of "N"-benzyl-2-azanorbornene via aqueous hetero Diels-Alder reaction of cyclopentadiene and benzyliminium chloride formed in situ from benzylamine hydrochloride and formaldehyde is described. Characterization of the product was achieved by IR and NMR spectroscopies. The spectral data acquired are thoroughly discussed. Numerous…

Microwave Assisted Rapid and Green Synthesis of Silver Nanoparticles Using a Pigment Produced by Streptomyces coelicolor klmp33

OpenAIRE

Manikprabhu, Deene; Lingappa, K.

2013-01-01

Traditional synthesis of silver nanoparticles using chemical methods produces toxic substances. In contrast biological synthesis is regarded as a safe and nontoxic process but the major drawback of biological synthesis is, this process is slow. In the present investigation, we developed a rapid and green synthesis of silver nanoparticles employing a pigment produced by Streptomyces coelicolor klmp33 in just 90?s. The silver nanoparticles were characterized by UV-visible spectroscopy, transmis...

Synthesis and characterization of CuGeO3 photocatalyst using Green Chemistry and its application for the degradation of direct black dye

Directory of Open Access Journals (Sweden)

Ashok. V. Borhade

2013-03-01

Full Text Available In this paper, we report synthesis of CuGeO3 photocatalyst by mechanochemical, solid state synthesis, method with green chemistry approach. The product obtained was characterized by various investigative techniques like UV-Diffuse Reflectance Spectroscopy, Fourier Transform Infrared Spectroscopy, X-ray Diffraction, Scanning Electron Microscopy, with Energy Dispersive X-ray Spectroscopy, and BET Surface area. The study confirm orthorhombic pervoskite crystal structure of photocatalyst with band gap 3.7 eV. The photocatalytic activity of the catalysts CuGeO3 was evaluated by photochemical bleaching of Direct black dye, under sun light.

Synthesis of mesomeric betaine compounds with imidazolium-enolate structure

Directory of Open Access Journals (Sweden)

Nina Gonsior

2012-03-01

Full Text Available The synthesis of a heterocyclic mesomeric betaine by quaternization reaction of 1-butylimidazole and tetrabromo-1,4-benzoquinone is presented. The structure was verified by means of X-ray single-crystal analysis, NMR and IR spectroscopy. Inclusion complexes of the heterocyclic mesomeric betaine with randomly methylated (1.8 β-cyclodextrin were investigated by UV–vis spectroscopy. Furthermore, the reaction conditions were applied to poly(vinylimidazole and 1,4-bis(1H-imidazol-1-ylbutane to obtain functionalized polymer networks and condensate polymers, respectively.

From single-site tantalum complexes to nanoparticles of TaxNy and TaOxNy supported on silica: elucidation of synthesis chemistry by dynamic nuclear polarization surface enhanced NMR spectroscopy and X-ray absorption spectroscopy

KAUST Repository

Mohandas, Janet Chakkamadathil

2017-06-08

Air-stable catalysts consisting of tantalum nitride nanoparticles represented as a mixture of TaxNy and TaOxNy with diameters in the range of 0.5 to 3 nm supported on highly dehydroxylated silica were synthesized from TaMe5 (Me = methyl) and dimeric Ta-2(OMe)(10) with guidance by the principles of surface organometallic chemistry (SOMC). Characterization of the supported precursors and the supported nanoparticles formed from them was carried out by IR, NMR, UV-Vis, extended X-ray absorption fine structure, and X-ray photoelectron spectroscopies complemented with XRD and high-resolution TEM, with dynamic nuclear polarization surface enhanced NMR spectroscopy being especially helpful by providing enhanced intensities of the signals of H-1, C-13, Si-29, and N-15 at their natural abundances. The characterization data provide details of the synthesis chemistry, including evidence of (a) O-2 insertion into Ta-CH3 species on the support and (b) a binuclear to mononuclear transformation of species formed from Ta-2(OMe)(10) on the support. A catalytic test reaction, cyclooctene epoxidation, was used to probe the supported nanoparticles, with 30% H2O2 serving as the oxidant. The catalysts gave selectivities up to 98% for the epoxide at conversions as high as 99% with a 3.4 wt% loading of Ta present as TaxNy/TaOxNy.

Synthesis of nanostructured SiC using the pulsed laser deposition technique

International Nuclear Information System (INIS)

Zhang, H.X.; Feng, P.X.; Makarov, V.; Weiner, B.R.; Morell, G.

2009-01-01

We report the new results on the direct synthesis of nanostructured silicon carbide (SiC) materials using the pulsed laser deposition technique. Scanning electron microscopy images revealed that SiC nanoholes, nanosprouts, nanowires, and nanoneedles were obtained. The crystallographic structure, chemical composition, and bond structure of the nanoscale SiC materials were investigated using X-ray diffraction, energy dispersive X-ray spectroscopy, X-ray photoelectron spectroscopy, and Raman scattering spectroscopy. The transverse optical mode and longitudinal optical mode in Raman spectra were found to become sharper as the substrate temperature was increased, while the material structure evolved from amorphous to crystalline

Green Chemistry Techniques for Gold Nanoparticles Synthesis

Science.gov (United States)

Cannavino, Sarah A.; King, Christy A.; Ferrara, Davon W.

Gold nanoparticles (AuNPs) are often utilized in many technological and research applications ranging from the detection of tumors, molecular and biological sensors, and as nanoantennas to probe physical processes. As these applications move from the research laboratory to industrial settings, there is a need to develop efficient and sustainable synthesis techniques. Recent research has shown that several food products and beverages containing polyphenols, a common antioxidant, can be used as reducing agents in the synthesis of AuNPs in solution. In this study, we explore a variety of products to determine which allow for the most reproducible solution of nanoparticles based on the size and shapes of particles present. We analyzed the AuNPs solutions using extinction spectroscopy and atomic force microscopy. We also develop a laboratory activity to introduce introductory chemistry and physics students to AuNP synthesis techniques and analysis.

Synthesis and in vacuo deposition of iron oxide nanoparticles by microplasma-assisted decomposition of ferrocene

International Nuclear Information System (INIS)

Schaefer, Michael; Kumar, Ajay; Mohan Sankaran, R.; Schlaf, Rudy

2014-01-01

Microplasma-assisted gas-phase nucleation has emerged as an important new approach to produce high-purity, nanometer-sized, and narrowly dispersed particles. This study aims to integrate this technique with vacuum conditions to enable synthesis and deposition in an ultrahigh vacuum compatible environment. The ultimate goal is to combine nanoparticle synthesis with photoemission spectroscopy-based electronic structure analysis. Such measurements require in vacuo deposition to prevent surface contamination from sample transfer, which can be deleterious for nanoscale materials. A homebuilt microplasma reactor was integrated into an existing atomic layer deposition system attached to a surface science multi-chamber system equipped with photoemission spectroscopy. As proof-of-concept, we studied the decomposition of ferrocene vapor in the microplasma to synthesize iron oxide nanoparticles. The injection parameters were optimized to achieve complete precursor decomposition under vacuum conditions, and nanoparticles were successfully deposited. The stoichiometry of the deposited samples was characterized in situ using X-ray photoelectron spectroscopy indicating that iron oxide was formed. Additional transmission electron spectroscopy characterization allowed the determination of the size, shape, and crystal lattice of the particles, confirming their structural properties.

Cellulase assisted synthesis of nano-silver and gold: Application as immobilization matrix for biocatalysis.

Science.gov (United States)

Mishra, Abhijeet; Sardar, Meryam

2015-01-01

In the present study, we report in vitro synthesis of silver and gold nanoparticles (NPs) using cellulase enzyme in a single step reaction. Synthesized nanoparticles were characterized by UV-VIS spectroscopy, Dynamic Light Spectroscopy (DLS), Transmission Electron Microscopy (TEM), Energy-dispersive X-ray Spectroscopy (EDX), X-ray Diffraction (XRD), Circular Dichroism (CD) and Fourier Transform Infrared Spectroscopy (FTIR). UV-visible studies shows absorption band at 415nm and 520nm for silver and gold NPs respectively due to surface plasmon resonance. Sizes of NPs as shown by TEM are 5-25nm for silver and 5-20nm for gold. XRD peaks confirmed about phase purity and crystallinity of silver and gold NPs. FTIR data shows presence of amide I peak on both the NPs. The cellulase assisted synthesized NPs were further exploited as immobilization matrix for cellulase enzyme. Thermal stability analysis reveals that the immobilized cellulase on synthesized NPs retained 77-80% activity as compared to free enzyme. While reusability data suggests immobilized cellulase can be efficiently used up to sixth cycles with minimum loss of enzyme activity. The secondary structural analysis of cellulase enzyme during the synthesis of NPs and also after immobilization of cellulase on these NPs was carried out by CD spectroscopy. Copyright © 2015 Elsevier B.V. All rights reserved.

Synthesis of gold nanoparticles with graphene oxide.

Science.gov (United States)

Wang, Wenshuo; He, Dawei; Zhang, Xiqing; Duan, Jiahua; Wu, Hongpeng; Xu, Haiteng; Wang, Yongsheng

2014-05-01

Single sheets of functionalized graphene oxide are derived through chemical exfoliation of natural flake graphite. We present an effective synthetic method of graphene-gold nanoparticles hybrid nanocomposites. AFM (Atomic Force Microscope) was used to measure the thickness of the individual GO nanosheet. FTIR (Fourier transform infrared) spectroscopy was used to verify the attachment of oxygen functionalities on the surface of graphene oxide. TEM (Transmission Electron Microscope) data revealed the average diameters of the gold colloids and characterized the composite particles situation. Absorption spectroscopy showed that before and after synthesis the gold particle size did not change. Our studies indicate that the hybrid is potential substrates for catalysts and biosensors.

Green Synthesis of Silver Nanoparticles and the Study of Optical Properties

OpenAIRE

Vasireddy, Ramakrishna; Paul, Rima; Mitra, Apurba Krishna

2012-01-01

The synthesis of silver nanoparticles of varying size has been achieved using different molar concentrations of NaOH while the effect of changing the temperature has been studied. AgNO3, gelatine, glucose and NaOH are used as a silver precursor, stabilizer, reducing agent and accelerator respectively. The synthesized nanoparticles have been characterized by a FESEM study, X‐ray diffractometry, Raman spectroscopy and UV‐vis spectroscopy. The colloidal sols of the silver nanoparticles in a biop...

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.

Green Synthesis of Robust, Biocompatible Silver Nanoparticles Using Garlic Extract

International Nuclear Information System (INIS)

White, G.V.; Kerscher, P.; Brown, R.M.; Morella, J.D.; Kitchens, C.L.; McAllister, W.; Dean, D.

2012-01-01

This paper details a facile approach for the synthesis of stable and monodisperse silver nanoparticles performed at ambient/low temperature, where Allium sativum (garlic) extract functions as the silver salt reducing agent during nanoparticle synthesis as well as the post synthesis stabilizing ligands. Varying the synthesis conditions provides control of particle size, size-distribution, and kinetics of particle formation. Infrared spectroscopy, energy dispersive X-ray chemical analysis, and high-performance liquid chromatography indicated that allicin and other carbohydrates in the garlic extract are the primary nanoparticle stabilizing moieties. The synthesized silver nanoparticles also demonstrate potential for biomedical applications, owing to (1) enhanced stability in biological media, (2) resistance to oxidation by the addition of H 2 O 2 , (3) ease and scalability of synthesis, and (4) lack of harsh chemicals required for synthesis. Cytotoxicity assays indicated no decrease in cellular proliferation for vascular smooth muscle cells and 3T3 fibroblasts at a concentration of 25 μg/mL, confirming that silver nanoparticles synthesized with garlic extract are potential candidates for future experimentation and implementation in the biomedical field.

Allenylidene Complexes of Ruthenium: Synthesis, Spectroscopy and Electron Transfer Properties

Czech Academy of Sciences Publication Activity Database

Winter, R. F.; Záliš, Stanislav

2004-01-01

Roč. 248, 15/16 (2004), s. 1565-1583 ISSN 0010-8545 R&D Projects: GA ČR GA203/03/0821; GA MŠk OC D14.20 Institutional research plan: CEZ:AV0Z4040901 Keywords : spectroscopy * allenylidine complexes of ruthenium * electron transfer Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 6.446, year: 2004

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...

Synthesis, spectroscopy and photosensitizing properties of hydroxynitrophenyl porphyrins

Energy Technology Data Exchange (ETDEWEB)

Maestrin, Ana Paula J.; Tedesco, Antonio Claudio; Neri, Claudio R.; Gandini, Maria Elisa F.; Serra, Osvaldo A.; Iamamoto, Yassuko [Sao Paulo Univ., Ribeirao Preto, SP (Brazil). Faculdade de Filosofia, Ciencias e Letras. Inst. de Quimica]. E-mail: osaserra@usp.br

2004-10-01

The hydroxynitrophenyl porphyrins, 5,10,15,20-tetrakis(2-hydroxy-5-nitrophenyl)porphyrin and 5-mono(carboxyphenyl)-10,15,20-tris(2-hydroxy-5-nitrophenyl)porphyrin described in this work were prepared through Adler's method. These compounds were characterized by {sup 1}H NMR and light absorption and emission spectroscopy in the visible region. In order to demonstrate the involvement of {sup 1}O{sub 2} production, the uric (UA) acid test was carried out, which considers the decrease in the absorbance of UA at 293 nm following laser light irradiation of a solution containing UA and a photosensitizer. The results obtained demonstrate that these hydroxynitrophenyl porphyrins can be considered as promising photosensitizers in PDT. (author)

Green synthesis of silver nanoparticles using tannins

Science.gov (United States)

Raja, Pandian Bothi; Rahim, Afidah Abdul; Qureshi, Ahmad Kaleem; Awang, Khalijah

2014-09-01

Colloidal silver nanoparticles were prepared by rapid green synthesis using different tannin sources as reducing agent viz. chestnut (CN), mangrove (MG) and quebracho (QB). The aqueous silver ions when exposed to CN, MG and QB tannins were reduced which resulted in formation of silver nanoparticles. The resultant silver nanoparticles were characterized using UV-Visible, X-ray diffraction (XRD), scanning electron microscopy (SEM/EDX), and transmission electron microscopy (TEM) techniques. Furthermore, the possible mechanism of nanoparticles synthesis was also derived using FT-IR analysis. Spectroscopy analysis revealed that the synthesized nanoparticles were within 30 to 75 nm in size, while XRD results showed that nanoparticles formed were crystalline with face centered cubic geometry.

Synthesis of monodispersed silver nanoparticles using Hibiscus cannabinus leaf extract and its antimicrobial activity

Science.gov (United States)

Bindhu, M. R.; Umadevi, M.

2013-01-01

Synthesis of silver nanoparticles using leaf extract of Hibiscus cannabinus has been investigated. The influences of different concentration of H. cannabinus leaf extract, different metal ion concentration and different reaction time on the above cases on the synthesis of nanoparticles were evaluated. The synthesized nanoparticles were characterized using UV-vis spectroscopy, Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD) and Transmission Electron Microscopy (TEM). The prepared silver nanoparticles were monodispersed, spherical in shape with the average particle size of 9 nm and shows surface plasmon peak at 446 nm. The study also reveals that the ascorbic acid present in H. cannabinus leaf extract has been used as reducing agent. The prepared silver nanoparticle shows good antimicrobial activity against Escherichia coli, Proteus mirabilis and Shigella flexneri.

Chemienzymatic synthesis of Uridine. Nucleotides labeled with [15N] and [13C

DEFF Research Database (Denmark)

Gilles, Anne-Marie; Cristea, Ioan; Palibroda, Nicolae

1995-01-01

+necessary for the oxidation of glucose 6-phosphate and 6-phosphogluconate was recycled by glutamate dehydrogenase and excess of ammonia and a-oxoglutarate. Despite the number and complexity of the enzymatic steps, the synthesis of [15N,13C]UTP is straightforward with an overall yield exceeding 60%. This method, extended...... and diversified to the synthesis of all natural ribonucleotides, is a more economical alternative for obtaining nucleic acids for structural analysis by heteronuclear NMR spectroscopy....

Influence of the phase composition on the catalytic properties of ammonia synthesis catalysts

International Nuclear Information System (INIS)

Peev, T.M.; Bojinova, A.I.; Krylova, A.V.

1981-01-01

The phase composition of CA-1-type catalysts for ammonia synthesis was investigated by means of Moessbauer spectroscopy. A correlation was found between the catalytic activity of the samples and their wuestite content. (author)

Synthesis of nano-sized amorphous boron powders through active dilution self-propagating high-temperature synthesis method

Energy Technology Data Exchange (ETDEWEB)

Wang, Jilin [The State Key Laboratory of Advanced Technology for Materials Synthesis and Processing, Wuhan University of Technology, Wuhan 430070 (China); Gu, Yunle [School of Material Science and Engineering, Wuhan Institute of Technology, Wuhan 430073 (China); Li, Zili [The State Key Laboratory of Advanced Technology for Materials Synthesis and Processing, Wuhan University of Technology, Wuhan 430070 (China); Wang, Weimin, E-mail: wangwm@hotmail.com [The State Key Laboratory of Advanced Technology for Materials Synthesis and Processing, Wuhan University of Technology, Wuhan 430070 (China); Fu, Zhengyi [The State Key Laboratory of Advanced Technology for Materials Synthesis and Processing, Wuhan University of Technology, Wuhan 430070 (China)

2013-06-01

Graphical abstract: Nano-sized amorphous boron powders were synthesized by active dilution self-propagating high-temperature synthesis (SHS) method. The effects of endothermic reaction rate, the possible chemical reaction mechanism and active dilution model for synthesis of the product were also discussed. Highlights: ► Nano-sized amorphous boron powders were synthesized by active dilution self-propagating high-temperature synthesis method. ► The morphology, particle size and purity of the samples could be effectively controlled via changing the endothermic rate. ► The diluter KBH{sub 4} played an important role in active dilution synthesis of amorphous nano-sized boron powders. ► The active dilution method could be further popularized and become a common approach to prepare various inorganic materials. - Abstract: Nano-sized amorphous boron powders were synthesized by active dilution self-propagating high-temperature synthesis (SHS) method at temperatures ranging from 700 °C to 850 °C in a SHS furnace using Mg, B{sub 2}O{sub 3} and KBH{sub 4} as raw materials. Samples were characterized by X-ray powder diffraction (XRD), Laser particle size analyzer, Fourier transform infrared spectra (FTIR), X-ray energy dispersive spectroscopy (EDX), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and high-resolution transmission TEM (HRTEM). The boron powders demonstrated an average particle size of 50 nm with a purity of 95.64 wt.%. The diluter KBH{sub 4} played an important role in the active dilution synthesis of amorphous nano-sized boron powders. The effects of endothermic reaction rate, the possible chemical reaction mechanism and active dilution model for synthesis of the product were also discussed.

Synthesis of nano-sized amorphous boron powders through active dilution self-propagating high-temperature synthesis method

International Nuclear Information System (INIS)

Wang, Jilin; Gu, Yunle; Li, Zili; Wang, Weimin; Fu, Zhengyi

2013-01-01

Graphical abstract: Nano-sized amorphous boron powders were synthesized by active dilution self-propagating high-temperature synthesis (SHS) method. The effects of endothermic reaction rate, the possible chemical reaction mechanism and active dilution model for synthesis of the product were also discussed. Highlights: ► Nano-sized amorphous boron powders were synthesized by active dilution self-propagating high-temperature synthesis method. ► The morphology, particle size and purity of the samples could be effectively controlled via changing the endothermic rate. ► The diluter KBH 4 played an important role in active dilution synthesis of amorphous nano-sized boron powders. ► The active dilution method could be further popularized and become a common approach to prepare various inorganic materials. - Abstract: Nano-sized amorphous boron powders were synthesized by active dilution self-propagating high-temperature synthesis (SHS) method at temperatures ranging from 700 °C to 850 °C in a SHS furnace using Mg, B 2 O 3 and KBH 4 as raw materials. Samples were characterized by X-ray powder diffraction (XRD), Laser particle size analyzer, Fourier transform infrared spectra (FTIR), X-ray energy dispersive spectroscopy (EDX), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and high-resolution transmission TEM (HRTEM). The boron powders demonstrated an average particle size of 50 nm with a purity of 95.64 wt.%. The diluter KBH 4 played an important role in the active dilution synthesis of amorphous nano-sized boron powders. The effects of endothermic reaction rate, the possible chemical reaction mechanism and active dilution model for synthesis of the product were also discussed

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.

Sustainable synthesis of magnetically separable SiO2/Co@Fe2O4 nanocomposite and its catalytic applications for the benzimidazole synthesis

Science.gov (United States)

Jithendra Kumara, K. S.; Krishnamurthy, G.; Sunil Kumar, N.; Naik, Nagaraja; Praveen, T. M.

2018-04-01

The Co(II) and Fe(III) centres magnetically separable two new mesoporous nanocatalyst were synthesised via chemical synthesis method. The transmission electron microscopic studies (TEM) show that, the particles are spherical shape with mean size of 20 nm. The Raman spectroscopy and X-ray photoelectron spectroscopy (XPS) reveals that SiO2 is coating on the surface of the cobalt ferrate nanoparticle (CoFe2O4). The SiO2 coating is efficiently preventing the aggregated collision of nanoparticles. Magnetic measurements show that diamagnetic character of the SiO2 is unaffected to the coercivity of SiO2 coated CoFe2O4 particles. In addition, these nanoparticles are used as nanocatalyst for high yielding, facile and expeditious synthesis of various functionalized 2-arylbenzimidazoles via one-pot condensation. The cascade including imine formation, cyclization, condensation, and aromatization occurs, without addition of any reducing or oxidizing agents. In all situations, the desired product was synthesised with excellent yield. The shorter reaction time, mild reaction condition, simplicity, non-toxicity, safe reaction and easy workup are the impotent merits of this protocol.

Facile synthesis of ZrO2 powders: Control of morphology

International Nuclear Information System (INIS)

Grover, V.; Shukla, R.; Tyagi, A.K.

2007-01-01

Tetragonal (t-)ZrO 2 rods and spheres were prepared by simple and time-saving low-temperature synthesis and characterized by X-ray diffraction, Raman spectroscopy and scanning electron microscopy. The morphology of the product can be changed from rods to spheres by changing the reaction conditions slightly. The t-ZrO 2 rods (0.5-0.1 mm approximately) were obtained by topotactic reaction. The work illustrates the utility of Raman spectroscopy as a powerful characterization tool when XRD is not able to conclusively identify the phases

Sol-gel synthesis of hydroxyapatite

International Nuclear Information System (INIS)

Zupanski, M.D.; Lucena, M.P.P.; Bergmann, C.P.

2010-01-01

Hydroxyapatite (HAp) has been established as the calcium phosphate based compound with most applications in the biological field. Among the numerous techniques for synthesis of HAp, the sol-gel processing route affords great control over purity and formed phases using low processing temperatures. In addition, the sol-gel approach offers an option for homogeneous HAp coating on metal substrates, as well as the ability to generate nanocrystalline powders. In this work, the sol-gel synthesis of HAp was investigated employing triethyl phosphate and calcium nitrate tetrahydrate as phosphorous and calcium precursors, respectively. The aging effect on phase composition and powder morphology of the final product was studied in terms of temperature and aging time. The powders were studied by using X-ray diffraction, Fourier transform infrared spectroscopy, particle size distribution by laser diffraction and scanning electron microscopy. (author)

Development of Hydrotalcite Based Cobalt Catalyst by Hydrothermal and Co-precipitation Method for Fischer-Tropsch Synthesis

Directory of Open Access Journals (Sweden)

Muhammad Faizan Shareef

2017-10-01

Full Text Available This paper presents the effect of a synthesis method for cobalt catalyst supported on hydrotalcite material for Fischer-Tropsch synthesis. The hydrotalcite supported cobalt (HT-Co catalysts were synthesized by co-precipitation and hydrothermal method. The prepared catalysts were characterized by using various techniques like BET (Brunauer–Emmett–Teller, SEM (Scanning Electron Microscopy, TGA (Thermal Gravimetric Analysis, XRD (X-ray diffraction spectroscopy, and FTIR (Fourier Transform Infrared Spectroscopy. Fixed bed micro reactor was used to test the catalytic activity of prepared catalysts. The catalytic testing results demonstrated the performance of hydrotalcite based cobalt catalyst in Fischer-Tropsch synthesis with high selectivity for liquid products. The effect of synthesis method on the activity and selectivity of catalyst was also discussed. Copyright © 2017 BCREC Group. All rights reserved Received: 3rd November 2016; Revised: 26th February 2017; Accepted: 9th March 2017; Available online: 27th October 2017; Published regularly: December 2017 How to Cite: Sharif, M.S., Arslan, M., Iqbal, N., Ahmad, N., Noor, T. (2017. Development of Hydrotalcite Based Cobalt Catalyst by Hydrothermal and Co-precipitation Method for Fischer-Tropsch Synthesis. Bulletin of Chemical Reaction Engineering & Catalysis, 12(3: 357-363 (doi:10.9767/bcrec.12.3.762.357-363

Green synthesis and structural control of metal and mineral nanostructures

DEFF Research Database (Denmark)

Engelbrekt, Christian

of nanoparticle formation which, however, entails the development of new methods. Two approaches to the advancement of solution synthesis of gold nanomaterials for energy technology were exploited, namely the development of techniques to study nanoparticle formation and the synthesis of active, composite...... nanomaterials. In the first approach, time-resolved chronopotentiometry, pH, conductivity and turbidity, and ultraviolet-visible light spectroscopy were employed to follow the green synthesis of gold nanoparticles. Several distinct phases were observed with all techniques providing a broad picture...... of the complex processes. Strong indications of sequential reduction were found and details about ligands and surface immobilized molecules disclosed. This platform is a widely available alternative to traditionally used synchrotron techniques. In the second approach, systematic efforts toward size and shape...

Total Synthesis of Ionic Liquid Systems for Dissolution of Lunar Simulant

Science.gov (United States)

Sharpe, Robert J.; Karr, Laurel J.; Paley, Mark S.

2010-01-01

For purposes of Space Resource Utilization, work in the total synthesis of a new ionic liquid system for the extraction of oxygen and metals from lunar soil is studied and described. Reactions were carried out according to procedures found in the chemical literature, analyzed via Thin-Layer Chromatography and 1H Nuclear Magnetic Resonance Spectroscopy and purified via vacuum distillation and rotary evaporation. Upon final analysis via 1H NMR, it was found that while the intermediates of the synthesis had been achieved, unexpected side products were also present. The mechanisms and constraints of the synthesis are described as well as the final results of the project and recommendations for continued study

Effect of the raw material type and the reaction time on the synthesis of halloysite based Zeolite Na-P1

Directory of Open Access Journals (Sweden)

Mahdi Meftah

Full Text Available Zeolites are currently one of the most important classes of inorganic materials because of their multiple applications not only as ions exchangers and molecular sieves, but also as catalysts. This works focus the synthesis and the characterization of Zeolite Na-P1 using halloysite (collected near Ain Khemouda, western Tunisia as the starting material. Two parameters, such as the host materials type (natural or treated and the reaction time, involved in the synthesis process are investigated. The intermediate phases and final products were characterized by X-ray diffraction, Infrared IR spectroscopy, scanning electron microscopy and high-resolution 29Si and 27Al MAS NMR. Obtained results show that the hydrothermal synthesis from natural and heated-halloysite leads to formation of homogenous Zeolite Na-P1. The difference in the crystallization/transformation time process is explained by the effect of the dissolution rate of the starting materials in sodium hydroxide solution. In the case of heated halloysite, the synthesis reaction with alkali solution occurs very readily and achieved without prior thermal activation at high temperature. The optimal conditions of Zeolite Na-P1 crystallization, from heated-halloysite, are reached at 120 °C. Keywords: Zeolite Na-P1, Halloysite, X-ray, FTIR spectroscopy, SEM, 29Si and 27Al MAS NMR spectroscopy

Yttrium orthoferrite powder obtained by the mechanochemical synthesis

Directory of Open Access Journals (Sweden)

Lazarević Zorica Ž.

2017-01-01

Full Text Available Yttrium orthoferrite (YFeO3 powder was prepared by a mechanochemical synthesis from a mixture of Y2O3 and α-Fe2O3 powders in a planetary ball mill for 2.5 h. The obtained YFeO3 powder sample was characterized by X-ray diffraction (XRD, Raman and infrared spectroscopy. The average crystallite size calculated by the Scherrer equation was 12 nm. The Mössbauer spectroscopy at room temperature confirms the superparamagnetic character of YFeO3 orthoferrite sample. [Project of the Serbian Ministry of Education, Science and Technological Development, Grant no. III 45003, Grant no. III 45015, Grant no. III 45018

Synthesis of triangular Au core-Ag shell nanoparticles

International Nuclear Information System (INIS)

Rai, Akhilesh; Chaudhary, Minakshi; Ahmad, Absar; Bhargava, Suresh; Sastry, Murali

2007-01-01

In this paper, we demonstrate a simple and reproducible method for the synthesis of triangular Au core-Ag shell nanoparticles. The triangular gold core is obtained by the reduction of gold ions by lemongrass extract. Utilizing the negative charge on the gold nanotriangles, silver ions are bound to their surface and thereafter reduced by ascorbic acid under alkaline conditions. The thickness of the silver shell may be modulated by varying the pH of the reaction medium. The formation of the Au core-Ag shell triangular nanostructures has been followed by UV-vis-NIR Spectroscopy, X-ray photoelectron spectroscopy, transmission electron microscopy (TEM) and atomic force microscopy (AFM) measurements. The sharp vertices of the triangles coupled with the core-shell structure is expected to have potential for application in surface enhanced Raman spectroscopy and in the sensitive detection of biomolecules

Diameter grouping in bulk samples of single-walled carbon nanotubes from optical absorption spectroscopy

NARCIS (Netherlands)

Golden, M.S.; Fink, J.; Dunsch, L.; Bauer, H.-D.; Reibold, M.; Knupfer, M.; Friedlein, R.; Pichler, T.; Jost, O.

1999-01-01

The influence of the synthesis parameters on the mean characteristics of single-wall carbon nanotubes in soot produced by the laser vaporization of graphite has been analyzed using optical absorption spectroscopy. The abundance and mean diameter of the nanotubes were found to be most influenced by

Metabolic regulation in Streptomyces parvulus during actinomycin D synthesis, studied with 13C- and 15N-labeled precursors by 13C and 15N nuclear magnetic resonance spectroscopy and by gas chromatography-mass spectrometry

International Nuclear Information System (INIS)

Inbar, L.; Lapidot, A.

1988-01-01

Recent studies have suggested that the onset of synthesis of actinomycin D in Streptomyces is due to a release from L-glutamate catabolic repression. In the present investigation we showed that S. parvulus has the capacity to maintain high levels of intracellular glutamate during the synthesis of actinomycin D. The results seem contradictory, since actinomycin D synthesis cannot start before a release from L-glutamate catabolic repression, but a relatively high intracellular pool of glutamate is needed for the synthesis of actinomycin D. Utilizing different labeled precursors, D-[U- 13 C]fructose and 13 C- and 15 N-labeled L-glutamate, and nuclear magnetic resonance techniques, we showed that carbon atoms of an intracellular glutamate pool of S. parvulus were not derived biosynthetically from the culture medium glutamte source but rather from D-fructose catabolism. A new intracellular pyrimidine derivative whose nitrogen and carbon skeletons were derived from exogenous L-glutamate was obtained as the main glutamate metabolite. Another new pyrimidine derivative that had a significantly reduced intracellular mobility and that was derived from D-fructose catabolism was identified in the cell extracts of S. parvulus during actinomycin D synthesis. These pyrimidine derivatives may serve as a nitrogen store for actinomycin D synthesis. In the present study, the N-trimethyl group of a choline derivative was observed by 13 C nuclear magnetic resonance spectroscopy in growing S. parvulus cells. The choline group, as well as the N-methyl groups of sarcosine, N-methyl-valine, and the methyl groups of an actinomycin D chromophore, arose from D-fructose catabolism. The 13 C enrichments found in the peptide moieties of actinomycin D were in accordance with a mechanism of actinomycin D synthesis from L-glutamate and D-fructose

Facile Synthesis of Calcium Carbonate Nanoparticles from Cockle Shells

Directory of Open Access Journals (Sweden)

Kh. Nurul Islam

2012-01-01

Full Text Available A simple and low-cost method for the synthesis of calcium carbonate nanoparticles from cockle shells was described. Polymorphically, the synthesized nanoparticles were aragonites which are biocompatible and thus frequently used in the repair of fractured bone and development of advanced drug delivery systems, tissue scaffolds and anticarcinogenic drugs. The rod-shaped and pure aragonite particles of 30±5 nm in diameter were reproducibly synthesized when micron-sized cockle shells powders were mechanically stirred for 90 min at room temperature in presence of a nontoxic and nonhazardous biomineralization catalyst, dodecyl dimethyl betaine (BS-12. The findings were verified using a combination of analytical techniques such as variable pressure scanning electron microscopy (VPSEM, transmission electron microscopy (TEM, Fourier transmission infrared spectroscopy (FT-IR, X-ray diffraction spectroscopy (XRD, and energy dispersive X-ray analyser (EDX. The reproducibility and low cost of the method suggested that it could be used in industry for the large scale synthesis of aragonite nanoparticles from cockle shells, a low cost and easily available natural resource.

Features of nanomodifiers synthesis based on trifunctional oxyphenyls for mineral suspensions

Directory of Open Access Journals (Sweden)

Shapovalov Nikolay Afanasyevich

2016-10-01

Full Text Available The focused influence on the rheological characteristics of highly-concentrated mineral suspensions used in the building industry is possible due to the directed synthesis of nano-sized macromolecules that have the certain structure and high adsorbing capacity on the surface of mineral particles and that are able to modify the boundary layer composition. The adsorbing capacity of organic compounds depends mostly on the hydrocarbon chain length and the molecular weight of the compound. The result of the condensate interaction of phenol and its derivatives with aldehydes is oligomers and polymers whose structure depends on the phenol functionality, the kind of aldehyde, molecular ration of reagents, the Ph medium of the reaction. So, changing the type or the functionality of initial monomers or the synthesis conditions one can produce linear thermoplastic oligomers (novolacs or highly branched thermosetting oligomers (resols. It has been found that the resole production takes place under softer conditions, and there is no necessity to neutralize reaction products as with novolac production that usually requires acid environment. A number of thermosetting oligomers based on trifunctional polyatomic phenols have been synthesized. The theoretical and practical characteristics of resole oligomer synthesis have been studied, synthesis optimal conditions have been determined, the composition and structure of macromolecules were revealed by the methods of infrared spectroscopy, proton magnetic resonance spectroscopy, liquid chromatography and conductivity measurement, the length of the enlarged oligomer molecule was calculated. Obtained compounds can be qualified as nanoscaled modifiers of mineral dispersions.

Facile synthesis of soluble functional graphene by reduction of graphene oxide via acetylacetone and its adsorption of heavy metal ions

International Nuclear Information System (INIS)

Xu, Minghan; Chai, Jing; Hu, Nantao; Huang, Da; Wang, Yuxi; Huang, Xiaolu; Wei, Hao; Yang, Zhi; Zhang, Yafei

2014-01-01

The synthesis of graphene (GR) from graphene oxide (GO) typically involves harmful chemical reducing agents that are undesirable for most practical applications. Here we report a green and facile synthesis method for the synthesis of GR that is soluble in water and organic solvents and that includes the additional benefit of adsorption of heavy metal ions. Acetylacetone, as both a reducing agent and a stabilizer, was used to prepare soluble GR from GO. Transmission electron microscopy and atomic force microscopy provide clear evidence for the formation of few-layer GR. The results from Fourier transform infrared spectroscopy and ultraviolet-visible spectroscopy show that reduction of GO to GR has occurred. Raman spectroscopy and X-ray photoelectron spectroscopy also indicate the removal of oxygen-containing functional groups from GO, resulting in the formation of GR. The results of dispersion experiments show that GR can be highly dispersed in water and N,N-Dimethylformamide. The reaction mechanism for acetylacetone reduction of exfoliated GO was also proposed. This method is a facile and environmentally friendly approach to the synthesis of GR and opens up new possibilities for preparing GR and GR-based nanomaterials for large-scale applications. Of even greater interest is that inductively coupled plasma atomic emission spectroscopy suggests that synthesized GR may be applied in the absorption of Cd 2+ and Co 2+ due to the strong coordination capacity of acetylacetone on the surfaces and edges of GR and the large surface area of GR in aqueous solutions. The maximum adsorptions are 49.28 mg g −1 for Cd 2+ , which is 4.5 times higher than that of carbon nanotubes, and 27.78 mg g −1 for Co 2+ , which is 3.6 times higher than that of titania beans. (paper)

Indium nanoparticles for ultraviolet surface-enhanced Raman spectroscopy

Science.gov (United States)

Das, Rupali; Soni, R. K.

2018-05-01

Ultraviolet Surface-enhanced Raman spectroscopy (UVSERS) has emerged as an efficient molecular spectroscopy technique for ultra-sensitive and ultra-low detection of analyte concentration. The generic SERS substrates based on gold and silver nanostructures have been extensively explored for high local electric field enhancement only in visible-NIR region of the electromagnetic spectrum. The template synthesis of controlled nanoscale size metallic nanostructures supporting localized surface plasmon resonance (LSPR) in the UV region have been recently explored due to their ease of synthesis and potential applications in optoelectronic, catalysis and magnetism. Indium (In0) nanoparticles exhibit active surface plasmon resonance (SPR) in ultraviolet (UV) and deep-ultaviolet (DUV) region with optimal absorption losses. This extended accessibility makes indium a promising material for UV plasmonic, chemical sensing and more recently in UV-SERS. In this work, spherical indium nanoparticles (In NPs) were synthesized by modified polyol reduction method using NaBH4 having local surface plasmon resonance near 280 nm. The as-synthesized spherical In0 nanoparticles were then coated with thin silica shells of thickness ˜ 5nm by a modified Stober method protecting the nanoparticles from agglomeration, direct contact with the probed molecules as well as prevent oxidation of the nanoparticles. Morphological evolution of In0 nanoparticles and SiO2 coating were characterized by transmission electron microscope (TEM). An enhanced near resonant shell-isolated SERS activity from thin film of tryptophan (Tryp) molecules deposited on indium coated substrates under 325nm UV excitation was observed. Finite difference time domain (FDTD) method is employed to comprehend the experimental results and simulate the electric field contours which showed amplified electromagnetic field localized around the nanostructures. The comprehensive analysis indicates that indium is a promising alternate

Biogenic silver nanoparticles using Rhinacanthus nasutus leaf extract: synthesis, spectral analysis, and antimicrobial studies.

Science.gov (United States)

Pasupuleti, Visweswara Rao; Prasad, T N V; Shiekh, Rayees Ahmad; Balam, Satheesh Krishna; Narasimhulu, Ganapathi; Reddy, Cirandur Suresh; Ab Rahman, Ismail; Gan, Siew Hua

2013-01-01

Nanotechnology is gaining momentum due to its ability to transform metals into nanoparticles. The synthesis, characterization, and applications of biologically synthesized nanomaterials have become an important branch of nanotechnology. Plant extracts are a cost-effective, ecologically friendly, and efficient alternative for the large-scale synthesis of nanoparticles. In this study, silver nanoparticles (AgNps) were synthesized using Rhinacanthus nasutus leaf extract. After exposing the silver ions to the leaf extract, the rapid reduction of silver ions led to the formation of AgNps in solution. The synthesis was confirmed by ultraviolet-visible spectroscopy, Fourier transform infrared spectroscopy, and transmission electron microscopy. The in vitro antimicrobial activity of the AgNps synthesized using R. nasutus leaf extract was investigated against Bacillus subtilis, Staphylococcus aureus, Pseudomonas aeruginosa, Klebsiella pneumonia, Escherichia coli, Aspergillus niger, and Aspergillus flavus using a disc diffusion method. The AgNps showed potential activity against all of the bacterial strains and fungal colonies, indicating that R. nasutus has the potential to be used in the development of value-added products in the biomedical and nanotechnology-based industries.

Synthesis of monodispersed silver nanoparticles using Hibiscus cannabinus leaf extract and its antimicrobial activity.

Science.gov (United States)

Bindhu, M R; Umadevi, M

2013-01-15

Synthesis of silver nanoparticles using leaf extract of Hibiscus cannabinus has been investigated. The influences of different concentration of H. cannabinus leaf extract, different metal ion concentration and different reaction time on the above cases on the synthesis of nanoparticles were evaluated. The synthesized nanoparticles were characterized using UV-vis spectroscopy, Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD) and Transmission Electron Microscopy (TEM). The prepared silver nanoparticles were monodispersed, spherical in shape with the average particle size of 9 nm and shows surface plasmon peak at 446 nm. The study also reveals that the ascorbic acid present in H. cannabinus leaf extract has been used as reducing agent. The prepared silver nanoparticle shows good antimicrobial activity against Escherichia coli, Proteus mirabilis and Shigella flexneri. Copyright © 2012 Elsevier B.V. All rights reserved.

The effect of reactor geometry on the synthesis of graphene materials in plasma jets

Science.gov (United States)

Shavelkina, M. B.; Amirov, R. H.; Shatalova, T. B.

2017-05-01

The possibility of synthesis of graphene and graphane (hydrogenated graphene) using the decomposition of hydrocarbons by thermal plasma has been investigated. Investigations of the influence of the plasma-forming gas on the efficiency of synthesis and the morphology of graphene materials were carried out. The synthesis products have been characterized by the methods of scanning microscopy, Raman spectroscopy and thermal analysis. It is found that the morphology of graphene materials is affected by the geometry of the reactor. It was demonstrated that the obtained graphene materials are uniformly distributed in the volume of plastic based on cyanate ester resins under mixing.

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.

SYNTHESIS AND FABRICATION OF MO-W COMPONENTS FOR NEUTRON RESONANCE SPECTROSCOPY TEMPERATURE MEASUREMENT

International Nuclear Information System (INIS)

BINGERT, S.; DESCH, P.; TRUJILLO, E.

1999-01-01

A Molybdenum-- 182 Tungsten (Mo- 182 W) alloy was specified for an application that would ultimately result in the measurement of temperature and particle velocity during the steady state time following the shock loading of various materials. The 182 W isotope provides a tag for the analysis of neutron resonance line shape from which the temperature may be calculated. The material was specified to have 1.8 atom percent W, with W-rich regions no larger than 1 microm in size. Both the composition and W distribution were critical to the experiment. Another challenge to the processing was the very small quantity of 182 W material available for the synthesis of the alloy. Therefore, limited fabrication routes were available for evaluation. Several synthesis and processing routes were explored to fabricate the required alloy components. First, precipitation of W onto Mo powder using ammonium metatungstate was investigated for powder synthesis followed by uniaxial hot pressing. Second, mechanical alloying (MA) followed by hot isostatic pressing (HIP) and warm forging was attempted. Finally, arc-melting techniques followed by either hot rolling or crushing the alloyed button into powder and consolidation were pursued. The results of the processing routes and characterization of the materials produced will be discussed

Synthesis and Antimicrobial Studies Of Mn(II), Co(II), Ni(Ii), Zn(II) and ...

African Journals Online (AJOL)

2017-08-20

Aug 20, 2017 ... was isolated by filtration, washed with water-ethanol mixture and characterized by FTIR, UV-visible spectroscopy, melting ..... (2012) Catalytic oxidation of alcohols by a ... Revinder Kumar Ravikant (2014) Review on synthesis ...

Synthesis, characterization and electrochemical properties of 4.8 V LiNi{sub 0.5}Mn{sub 1.5}O{sub 4} cathode material in lithium-ion batteries

Energy Technology Data Exchange (ETDEWEB)

Chi, Le Ha [Faculty of Engineering Physics and NanoTechnology, College of Technology, 144 Xuan Thuy Road, Hanoi (Viet Nam)] [Vietnamese Academy of Science and Technology, 18 Hoang Quoc Viet Street, Cau Giay District, Hanoi (Viet Nam); Dinh, Nguyen Nang [Faculty of Engineering Physics and NanoTechnology, College of Technology, 144 Xuan Thuy Road, Hanoi (Viet Nam); Brutti, Sergio, E-mail: sergio.brutti@uniroma1.i [Department of Chemistry, University of Rome ' La Sapienza' , P.le Aldo Moro 5, 00185 Rome (Italy); Scrosati, Bruno [Department of Chemistry, University of Rome ' La Sapienza' , P.le Aldo Moro 5, 00185 Rome (Italy)

2010-07-15

In this work the synthesis of a nickel doped cubic manganese spinel has been studied for application as cathode material in secondary lithium batteries. Six different experimental approaches have been tested in order to carry out a screening of the various possible synthetic routes. The used synthetic strategies were wet chemistry (WC), solid state (SS), combustion synthesis (CS), cellulose-based sol-gel synthesis (SG-C), ascorbic acid-based sol-gel synthesis (SG-AA) and resorcinol/formaldehyde-based sol-gel synthesis (SG-RF). The goal of our study is to obtain insights about how the synthesis conditions can be modified in order to achieve a material with improved electrochemical performances in such devices, especially in high current operating regimes. The synthesized materials have been characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) with energy dispersive spectroscopy (EDS), atomic absorption, inductively coupled plasma (ICP-MS) atomic emission spectroscopy, surface area measurements and tested as high voltage cathodes in Li-ion electrochemical devices.

Controlled synthesis of single-crystalline graphene

Directory of Open Access Journals (Sweden)

Wang Xueshen

2014-02-01

Full Text Available This paper reports the controlled synthesis of single-crystalline graphene on the back side of copper foil using CH4 as the precursor. The influence of growth time and the pressure ratio of CH4/H2 on the structure of graphene are examined. An optimized polymer-assisted method is used to transfer the synthesized graphene onto a SiO2/Si substrate. Scanning electron microscopy and Raman spectroscopy are used to characterize the graphene.

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)

Microwave-assisted synthesis of iron oxide nanoparticles in biocompatible organic environment

Science.gov (United States)

Aivazoglou, E.; Metaxa, E.; Hristoforou, E.

2018-04-01

The development of magnetite and maghemite particles in uniform nanometer size has triggered the interest of the research community due to their many interesting properties leading to a wide range of applications, such as catalysis, nanomedicine-nanobiology and other engineering applications. In this study, a simple, time-saving and low energy-consuming, microwave-assisted synthesis of iron oxide nanoparticles, is presented. The nanoparticles were prepared by microwave-assisted synthesis using polyethylene glycol (PEG) or PEG and β-cyclodextrin (β-CD)/water solutions of chloride salts of iron in the presence of ammonia solution. The prepared nano-powders were characterized using X-Ray Diffraction (XRD), Transition Electron Microscopy (TEM), Fourier-transform Infrared Spectroscopy (FTIR), Raman Spectroscopy, Vibrating Sample Magnetometer (VSM), X-Ray Photoelectron Spectroscopy (XPS) and Thermal analysis (TG/DSC). The produced nanoparticles are crystallized mostly in the magnetite and maghemite lattice exhibiting very similar shape and size, with indications of partial PEG coating. Heating time, microwave power and presence of PEG, are the key factors shaping the size properties of nanoparticles. The average size of particles ranges from 10.3 to 19.2 nm. The nanoparticles exhibit a faceted morphology, with zero contamination levels. The magnetic measurements indicate that the powders are soft magnetic materials with negligible coercivity and remanence, illustrating super-paramagnetic behavior.

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.

Vibrational properties of gold nanoparticles obtained by green synthesis

Science.gov (United States)

Alvarez, Ramón A. B.; Cortez-Valadez, M.; Bueno, L. Oscar Neira; Britto Hurtado, R.; Rocha-Rocha, O.; Delgado-Beleño, Y.; Martinez-Nuñez, C. E.; Serrano-Corrales, Luis Ivan; Arizpe-Chávez, H.; Flores-Acosta, M.

2016-10-01

This study reports the synthesis and characterization of gold nanoparticles through an ecological method to obtain nanostructures from the extract of the plant Opuntia ficus-indica. Colloidal nanoparticles show sizes that vary between 10-20 nm, and present various geometric morphologies. The samples were characterized through optical absorption, Raman Spectroscopy and Transmission Electron Microscopy (TEM). Additionally, low energy metallic clusters of Aun (n=2-20 atoms) were modeled by computational quantum chemistry. The theoretical results were obtained with Density Functional Theory (DFT). The predicted results of Au clusters show a tendency and are correlated with the experimental results concerning the optical absorption bands and Raman spectroscopy in gold nanoparticles.

Solvent-assisted in situ synthesis of cysteamine-capped silver nanoparticles

Science.gov (United States)

Oliva, José M.; Ríos de la Rosa, Julio M.; Sayagués, María J.; Sánchez-Alcázar, José A.; Merkling, Patrick J.; Zaderenko, Ana P.

2018-03-01

Silver nanoparticles offer a huge potential for biomedical applications owing to their exceptional properties and small size. Specifically, cysteamine-capped silver nanoparticles could form the basis for new anticancer therapies combining the cytotoxic effect of the silver core with the inherent antitumor activity of cysteamine, which inhibit cancer cell proliferation and suppress invasion and metastasis. In addition, the capability of the cysteamine coating monolayer to couple a variety of active principles and targeting (bio)molecules of interest proves key to the tailoring of this platform in order to exploit the pathophysiology of specific tumor types. Nevertheless, the chain length and conformational flexibility of cysteamine, together with its ability to attach to the surface of silver nanoparticles via both the thiol and the amine group, have made the in situ synthesis of these particles an especially challenging task. Herein we report a solvent-assisted in situ synthesis method that solves this problem. The obtained nanoparticles have been fully characterized by UV-visible absorption spectroscopy, Fourier transform infrared spectroscopy, transmission electron microscopy, electron diffraction measurement, high resolution transmission electron microscopy, scanning transmission electron microscopy, energy dispersive x-ray spectroscopy nanoanalysis, and dynamic light scattering measurement. Our synthesis method achieves extremely high yield and surface coating ratio, and colloidal stability over a wide range of pH values including physiological pH. Additionally, we have demonstrated that cysteamine-capped nanoparticles obtained by this method can be conjugated to an antibody for active targeting of the epidermal growth factor receptor, which plays an important role in the pathogenesis and progression of a wide variety of tumors, and induce cell death in human squamous carcinoma cells. We believe this method can be readily extended to combinations of noble

Semiconductor-to-metallic flipping in a ZnFe2O4–graphene based smart nano-system: Temperature/microwave magneto-dielectric spectroscopy

International Nuclear Information System (INIS)

Ameer, Shahid; Gul, Iftikhar Hussain; Mahmood, Nasir; Mujahid, Muhammad

2015-01-01

Zn-(FeO 2 ) 2 –graphene smart nano-composites were synthesized using a novel modified solvothermal synthesis with different percentages of graphene. The structure of the nanocomposite was confirmed through X-ray diffraction, micro-Raman scattering spectroscopy, Ultraviolet–Visible spectroscopy, and Fourier transform infrared spectroscopy. The structural growth and morphological aspects were analyzed using scanning/transmission electron microscopy, revealing marvelous micro-structural features of the assembled nano-system resembling a maple leaf. To determine the composition, energy dispersive spectroscopy and X-ray photoelectron spectroscopy were used. Microwave magneto-dielectric spectroscopy revealed the improved dielectric properties of the nano-composite compared to those of the parent functional nanocrystals. Temperature gradient dielectric spectroscopy was used over the spectral range from 100 Hz to 5 MHz to reveal the phenomenological effect that the nanosystem flips from its usual semiconductor nature to a metallic nature with sensing temperature. Electrical conductivity and dielectric analysis indicated that the dielectric loss and the dielectric permittivity increased at room temperature. This extraordinary switching capability of the functionalized graphene nanosystem opens up a new dimension for engineering advanced and efficient smart composite materials. - Graphical abstract: Display Omitted - Highlights: • Zn-(FeO 2 ) 2 –graphene smart nano-composites were synthesized using a novel modified solvothermal synthesis. • The synthesized nano-system exhibits marvelous leaf like microstructure. • These nano-composites show improved magneto dielectric response. • This engineered smart nano-system shows phenomenological flipping from semiconductor like nature to metallic behavior

Synthesis of gold nanoparticles using renewable Punica granatum juice and study of its catalytic activity

Science.gov (United States)

Dash, Shib Shankar; Bag, Braja Gopal

2014-01-01

Punica granatum juice, a delicious multivitamin drink of great medicinal significance, is rich in different types of phytochemicals, such as terpenoids, alkaloids, sterols, polyphenols, sugars, fatty acids, aromatic compounds, amino acids, tocopherols, etc. We have demonstrated the use of the juice for the synthesis of gold nanoparticles (AuNPs) at room temperature under very mild conditions. The synthesis of the AuNPs was complete in few minutes and no extra stabilizing or capping agents were necessary. The size of the nanoparticles could be controlled by varying the concentration of the fruit extract. The AuNPs were characterized by surface plasmon resonance spectroscopy, high resolution transmission electron microscopy, fourier transform infrared spectroscopy and X-ray diffraction studies. Catalytic activity of the synthesized colloidal AuNPs has also been demonstrated.

Synthesis and characterization of acrylate copolymer containing fluorescein functional group

International Nuclear Information System (INIS)

Hui, Guodong; Huang, Weiyun; Song, Yunzhao; Chen, Deben; Zhong, Anyong

2013-01-01

We report a novel method to fabricate fluorescent polymer (F-CPA) based on the esterification between acrylate copolymer (CPA) and fluorescein using N, N-dicyclohexylcarbodiimide (DCC)/4-dimethylaminopyridine (DMAP) as catalyst. The resulting copolymer was characterized by Fourier transform-infrared spectroscopy (FT-IR), gel permeation chromatography (GPC), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), ultraviolet-visible spectroscopy (UV-Vis) and fluorescence spectroscopy. In addition, the influences of concentration, solvents, pH and metal cations (Cu"2"+, Fe"3"+ and Zn"2"+) on the fluorescent behaviors of F-CPA are discussed in detail. All those observations suggest that the synthesized F-CPA is an excellent luminescent macromolecular material with simple synthesis method and excellent solubility. Moreover, its sensitive fluorescence response behaviors to solvents, pH and metal cations make it to become a polymer-based probe

Simple Synthesis Method for Alumina Nanoparticle

Directory of Open Access Journals (Sweden)

Daniel Damian

2017-11-01

Full Text Available Globally, the human population steady increase, expansion of urban areas, excessive industrialization including in agriculture, caused not only decrease to depletion of non-renewable resources, a rapid deterioration of the environment with negative impact on water quality, soil productivity and of course quality of life in general. This paper aims to prepare size controlled nanoparticles of aluminum oxide using a simple synthesis method. The morphology and dimensions of nanomaterial was investigated using modern analytical techniques: SEM/EDAX and XRD spectroscopy.

Synthesis of Carbon nano structures by plasma discharge

International Nuclear Information System (INIS)

Jimenez L, M.L.

2007-01-01

Due to the great quantity of applications of the carbon nano structures (NEC) in diverse areas like: synthesis of super-resistant materials, hydrogen storage, nano sensors generation and nano catalysts, it has seen the necessity to generate new processes of synthesis of this materials as well as to already improve those existent. The present work has as objective to optimize the NEC synthesis process by means of the electric arc method which uses alternating current to high frequencies (HF), obtaining relatively clean products; that is to say, it hardly presents amorphous material neither sludges. They stand out the obtaining of carbon nano fibers (NFC) by means of a luminescent-arch discharge, in a gas mixture of He-CH 4 with 34% at. Ni/10.32% at.Y like catalyst; at a frequency of 42 kHz and low power (300 W). This method benefits the amass of the particles in both electrodes due to the high frequencies. The time of duration of the process oscillates between 5 and 20 minutes. The obtained product was characterized by scanning electron microscopy (MEB), transmission electron microscopy (MET) to determine the NEC type obtained and by X-ray diffraction analysis and Raman spectroscopy for determining the purity of the samples. The NFC is relatively free of amorphous coal. The surface and structural analysis indicates that the fibers have a half diameter of 80 nm. It is also made, a study by optical emission spectroscopy of plasma using the Swan band for determining the temperature. (Author)

Synthesis of carbon nano structures by plasma discharge

International Nuclear Information System (INIS)

Jimenez L, M.L.

2007-01-01

Due to the great quantity of applications of carbon neocarcinostatin (NEC) in diverse areas like: synthesis of super-resistant materials, hydrogen storage, nano sensors generation and nano catalysts, one has seen the necessity to generate new synthesis processes of these materials as well as to already improve those existent. The present work has as objective to optimize the NEC synthesis process by means of the electric arc method which uses alternating current to high frequencies (HF), obtaining relatively clean products; that is to say, it hardly presents amorphous material neither impurities. They stand out the obtaining of carbon nano fibers (NFC) by means of a luminescent-arc discharge, in a gas mixture He-CH 4 with 34% at.Ni/10.32%at.Y like catalyst; to a frequency of 42 k Hz and low power (300 W). This method benefits the agglomeration of the particles in both electrodes due to the high frequencies. The time of duration of the process oscillates between 5 and 20 minutes. The obtained product was characterized by scanning electron microscopy (MEB), transmission electron microscopy (MET) to determine the type of obtained NEC and by X-ray diffraction analysis and Raman spectroscopy to determine the purity of the samples. The NFC are relatively free of amorphous coal. The surface and structural analysis indicates that the fibers have a half diameter of 80 nm. It is also made, a study by optical emission spectroscopy of the plasma using the Swan band to determine the temperature. (Author)

Synthesis of Silver Nanoparticles Using Buchu Plant Extracts and Their Analgesic Properties

Directory of Open Access Journals (Sweden)

Herbert Chiguvare

2016-06-01

Full Text Available We herein report for the first time the synthesis and analgesic properties of silver nanoparticles (Ag-NPs using buchu plant extract. The as-synthesised Ag-NPs at different temperatures were characterised by UV-Vis spectroscopy, Fourier transform infra-red spectroscopy (FTIR and transmission transform microscopy (TEM to confirm the formation of silver nanoparticles. Phytochemical screening of the ethanolic extract revealed the presence of glycosides, proteins, tannins, alkaloids, flavonoids and saponins. The absorption spectra showed that the synthesis is temperature and time dependent. The TEM analysis showed that the as-synthesised Ag-NPs are polydispersed and spherical in shape with average particle diameter of 19.95 ± 7.76 nm while the FTIR results confirmed the reduction and capping of the as-synthesised Ag-NPs by the phytochemicals present in the ethanolic extract. The analgesic study indicated that the combined effect of the plant extract and Ag-NPs is more effective in pain management than both the aspirin drug and the extract alone.

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

Directory of Open Access Journals (Sweden)

Mohammed Rafi Shaik

2017-01-01

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

Amine-catalyzed direct aldol reactions of hydroxy- and dihydroxyacetone: biomimetic synthesis of carbohydrates.

Science.gov (United States)

Popik, Oskar; Pasternak-Suder, Monika; Leśniak, Katarzyna; Jawiczuk, Magdalena; Górecki, Marcin; Frelek, Jadwiga; Mlynarski, Jacek

2014-06-20

This article presents comprehensive studies on the application of primary, secondary, and tertiary amines as efficient organocatalysts for the de novo synthesis of ketoses and deoxyketoses. Mimicking the actions of aldolase enzymes, the synthesis of selected carbohydrates was accomplished in aqueous media by using proline- and serine-based organocatalysts. The presented methodology also provides direct access to unnatural L-carbohydrates from the (S)-glyceraldehyde precursor. Determination of the absolute configuration of all obtained sugars was feasible using a methodology consisting of concerted ECD and VCD spectroscopy.

Advances in the synthesis of nitroxide radicals for use in biomolecule spin labelling.

Science.gov (United States)

Haugland, Marius M; Lovett, Janet E; Anderson, Edward A

2018-02-05

EPR spectroscopy is an increasingly useful analytical tool to probe biomolecule structure, dynamic behaviour, and interactions. Nitroxide radicals are the most commonly used radical probe in EPR experiments, and many methods have been developed for their synthesis, as well as incorporation into biomolecules using site-directed spin labelling. In this Tutorial Review, we discuss the most practical methods for the synthesis of nitroxides, focusing on the tunability of their structures, the manipulation of their sidechains into spin labelling handles, and their installation into biomolecules.

Synthesis and Single Crystal Structures of Substituted-1,3-Selenazol-2-amines

Directory of Open Access Journals (Sweden)

Guoxiong Hua

2016-12-01

Full Text Available The synthesis and X-ray single crystal structures of a series of new 4-substituted-1,3-selenazol-2-amines is reported. The efficient preparation of these compounds was carried out by two-component cyclization of the selenoureas with equimolar amounts of α-haloketones. The selenoureas were obtained from the reaction of Woollins’ reagent with cyanamides, followed by hydrolysis with water. All new compounds have been characterized by IR spectroscopy, multi-NMR (1H, 13C, 77Se spectroscopy, accurate mass measurement and single crystal X-ray structure analysis.

Synthesis of Natural Cyclopentapeptides Isolated from Dianthus chinensis.

Science.gov (United States)

Zhang, Shengping; Amso, Zaid; De Leon Rodriguez, Luis M; Kaur, Harveen; Brimble, Margaret A

2016-07-22

The first syntheses of the naturally occurring cyclic peptides dianthin I (1), pseudostellarin A (2), and heterophyllin J (3) are described. The linear protected peptide precursors were prepared efficiently via Fmoc-solid-phase synthesis and subsequently cyclized in solution under dilute conditions. The structures of the synthetic cyclopentapeptides were confirmed by NMR spectroscopy and mass spectrometry and were in agreement with the literature data reported for the natural products.

Microwave-assisted rapid extracellular synthesis of stable bio-functionalized silver nanoparticles from guava ( Psidium guajava) leaf extract

Science.gov (United States)

Raghunandan, Deshpande; Mahesh, Bedre D.; Basavaraja, S.; Balaji, S. D.; Manjunath, S. Y.; Venkataraman, A.

2011-05-01

Our research interest centers on microwave-assisted rapid extracellular synthesis of bio-functionalized silver nanoparticles of 26 ± 5 nm from guava ( Psidium guajava) leaf extract with control over dimension and composition. The reaction occurs very rapidly as the formation of spherical nanoparticles almost completed within 90 s. The probable pathway of the biosynthesis is suggested. Appearance, crystalline nature, size and shape of nanoparticles are understood by UV-vis (UV-vis spectroscopy), FTIR (fourier transform infrared spectroscopy), XRD (X-ray diffraction), FESEM (field emission scanning electron microscopy) and TEM (transmission electron microscopy) techniques. Microwave-assisted route is selected for the synthesis of silver nanoparticles to carry out the reaction fast, suppress the enzymatic action and to keep the process environmentally clean and green.

Microwave-assisted rapid extracellular synthesis of stable bio-functionalized silver nanoparticles from guava (Psidium guajava) leaf extract

Energy Technology Data Exchange (ETDEWEB)

Raghunandan, Deshpande [H.K.E.S' s College of Pharmacy (India); Mahesh, Bedre D. [Gulbarga University, Materials Chemistry Laboratory, Department of Material Science (India); Basavaraja, S. [Jawaharlal Nehru Centre for Advanced Scientific Research, Veeco-India Nanotechnology Laboratory (India); Balaji, S. D. [Gulbarga University, Materials Chemistry Laboratory, Department of Material Science (India); Manjunath, S. Y. [Sri Krupa, Institute of Pharmaceutical Science (India); Venkataraman, A., E-mail: raman_chem@rediffmail.com [Gulbarga University, Materials Chemistry Laboratory, Department of Material Science (India)

2011-05-15

Our research interest centers on microwave-assisted rapid extracellular synthesis of bio-functionalized silver nanoparticles of 26 {+-} 5 nm from guava (Psidium guajava) leaf extract with control over dimension and composition. The reaction occurs very rapidly as the formation of spherical nanoparticles almost completed within 90 s. The probable pathway of the biosynthesis is suggested. Appearance, crystalline nature, size and shape of nanoparticles are understood by UV-vis (UV-vis spectroscopy), FTIR (fourier transform infrared spectroscopy), XRD (X-ray diffraction), FESEM (field emission scanning electron microscopy) and TEM (transmission electron microscopy) techniques. Microwave-assisted route is selected for the synthesis of silver nanoparticles to carry out the reaction fast, suppress the enzymatic action and to keep the process environmentally clean and green.

Microwave-assisted rapid extracellular synthesis of stable bio-functionalized silver nanoparticles from guava (Psidium guajava) leaf extract

International Nuclear Information System (INIS)

Raghunandan, Deshpande; Mahesh, Bedre D.; Basavaraja, S.; Balaji, S. D.; Manjunath, S. Y.; Venkataraman, A.

2011-01-01

Our research interest centers on microwave-assisted rapid extracellular synthesis of bio-functionalized silver nanoparticles of 26 ± 5 nm from guava (Psidium guajava) leaf extract with control over dimension and composition. The reaction occurs very rapidly as the formation of spherical nanoparticles almost completed within 90 s. The probable pathway of the biosynthesis is suggested. Appearance, crystalline nature, size and shape of nanoparticles are understood by UV–vis (UV–vis spectroscopy), FTIR (fourier transform infrared spectroscopy), XRD (X-ray diffraction), FESEM (field emission scanning electron microscopy) and TEM (transmission electron microscopy) techniques. Microwave-assisted route is selected for the synthesis of silver nanoparticles to carry out the reaction fast, suppress the enzymatic action and to keep the process environmentally clean and green.

Microfibrous Matrices: Optimization of Synthesis Conditions

Directory of Open Access Journals (Sweden)

Amogh N. Karwa

2012-01-01

Full Text Available This study focuses on the process of optimization for carbon nanofiber synthesis at the exterior and the interior of 3-dimensional sintered nickel microfibrous networks. Synthesis of carbon nanofibers (CNF by catalytic decomposition of acetylene (ethyne was conducted at atmospheric pressure and short reaction times (10 min. Two factors evaluated during the study were (a CNF quality (observed by SEM and Raman spectroscopy and (b rate of reaction (gravimetrically measured carbon yield. Independent optimization variables included redox faceting pretreatment of nickel, synthesis temperature, and gas composition. Faceting resulted in an 8-fold increase in the carbon yield compared to an untreated substrate. Synthesis with varying levels of hydrogen maximized the carbon yield (9.31 mg C/cm2 catalyst. The quality of CNF was enhanced via a reduction in amorphous carbon that resulted from the addition of 20% ammonia. Optimized growth conditions that led to high rates of CNF deposition preferentially deposited this carbon at the exterior layer of the nickel microfibrous networks (570°C, 78% H2, 20% NH3, 2% C2H2, faceted Ni.. CNF growth within the 3-dimensional nickel networks was accomplished at the conditions selected to lower the gravimetric reaction rate (470°C, 10% H2, 88% N2, 2% C2H2, nonfaceted Ni.

Green chemistry approach for the synthesis of biocompatible graphene

Directory of Open Access Journals (Sweden)

Gurunathan S

2013-07-01

Full Text Available Sangiliyandi Gurunathan, Jae Woong Han, Jin-Hoi Kim Department of Animal Biotechnology, Konkuk University, Seoul, South Korea Background: Graphene is a single-atom thick, two-dimensional sheet of hexagonally arranged carbon atoms isolated from its three-dimensional parent material, graphite. One of the most common methods for preparation of graphene is chemical exfoliation of graphite using powerful oxidizing agents. Generally, graphene is synthesized through deoxygenation of graphene oxide (GO by using hydrazine, which is one of the most widespread and strongest reducing agents. Due to the high toxicity of hydrazine, it is not a promising reducing agent in large-scale production of graphene; therefore, this study focused on a green or sustainable synthesis of graphene and the biocompatibility of graphene in primary mouse embryonic fibroblast cells (PMEFs. Methods: Here, we demonstrated a simple, rapid, and green chemistry approach for the synthesis of reduced GO (rGO from GO using triethylamine (TEA as a reducing agent and stabilizing agent. The obtained TEA reduced GO (TEA-rGO was characterized by ultraviolet (UV–visible absorption spectroscopy, X-ray diffraction (XRD, particle size dynamic light scattering (DLS, scanning electron microscopy (SEM, Raman spectroscopy, and atomic force microscopy (AFM. Results: The transition of graphene oxide to graphene was confirmed by UV–visible spectroscopy. XRD and SEM were used to investigate the crystallinity of graphene and the surface morphologies of prepared graphene respectively. The formation of defects further supports the functionalization of graphene as indicated in the Raman spectrum of TEA-rGO. Surface morphology and the thickness of the GO and TEA-rGO were analyzed using AFM. The presented results suggest that TEA-rGO shows significantly more biocompatibility with PMEFs cells than GO. Conclusion: This is the first report about using TEA as a reducing as well as a stabilizing agent for the

Synthesis of silver doped hydroxyapatite nanospheres using Ouzo effect

Directory of Open Access Journals (Sweden)

Marija Prekajski

2016-09-01

Full Text Available Nanoemulsion technique, based on Ouzo effect, was applied for synthesis of the pure and silver doped (2.5 and 5 mol% calcium hydroxyapatite (HAp. After calcination at 500 °C fully crystallized powders were obtained. X-ray powder diffraction analysis accompanied with Rietveld refinement revealed that the synthesized powders were single-phase hydroxyapatite. Raman spectroscopy also confirmed that the synthesized powders were single-phase. The obtained HAp particles were spherical in shape and their sizes were in the nanometer range which was revealed by field emission scanning electron microscopy analysis (FESEM. The successful synthesis of the single-phase Ag doped HAp showed that nanoemulsion method is a simple technique for obtaining pure and doped hydroxyapatite nanospheres.

Síntese e caracterização térmica e química do copolímero poli(D,L-lactídeo-co-glicolídeo Synthesis and thermal and chemical characterization of the poly(D,L-lactide-co-glycolide copolymer

Directory of Open Access Journals (Sweden)

Cynthia D. C. Erbetta

2011-01-01

Full Text Available O copolímero poli(D,L-lactídeo-co-glicolídeo apresenta-se como um dos polímeros de maior interesse para aplicação na área médica. O fato de ser biorreabsorvível, biocompatível, atóxico e ter uma cinética de degradação que pode ser modificada pela razão entre os monômeros na copolimerização justifica tal interesse. Neste trabalho, os copolímeros foram sintetizados a 175 ºC, por meio da abertura dos anéis dos dímeros cíclicos dos monômeros D,L-lactídeo e glicolídeo, na presença do iniciador octanoato de estanho e do co-iniciador álcool laurílico. O controle eficiente do vácuo no meio reacional, aliado à adequada agitação, foram fundamentais para o sucesso da síntese. Para caracterização dos copolímeros sintetizados foram empregadas as técnicas de calorimetria exploratória diferencial (DSC, termogravimetria (TG e espectroscopia na região do infravermelho (FTIR. Foram analisados não somente os produtos de reação, mas também os monômeros de partida. A nova rota de síntese utilizada mostrou-se adequada, sendo os copolímeros poli(D,L-lactídeo-co-glicolídeo obtidos com sucesso.Poly (D, L-lactide-co-glycolide copolymer (PLGA has attracted a great deal of interest due to their special characteristics as biomaterials since it is bioreabsorbable, biocompatible, nontoxic and the kinetics of degradation can be modified by the ratio of monomers in copolymerization. In this work, the copolymers were synthesized at 175 ºC, by opening the ring of cyclic dimers of D,L-lactide and glycolide monomers in the presence of tin(II octanoate initiator and lauryl alcohol co-initiator. The efficient control of the vacuum in the medium combined with adequate stirring were essential to the success of the synthesis. Characterization of the copolymers samples was carried out by using differential scanning calorimetry (DSC, thermogravimetry (TG and Fourier transform infrared spectroscopy (FTIR. We analyzed not only the products

Raman spectroscopy of pharmaceutical cocrystals in nanosized pores of mesoporous silica

International Nuclear Information System (INIS)

Ohta, Ryuichi; Ajito, Katsuhiro; Ueno, Yuko

2017-01-01

The Raman spectroscopy of pharmaceutical cocrystals based on caffeine and oxalic acid in nanosized pores of mesoporous silica has been demonstrated at various molar amounts. The Raman peak shifts of caffeine molecules express the existence of pharmaceutical cocrystals in mesoporous silica. The molar amount dependence of the peak shifts describes that caffeine and oxalic acid cocrystallized on the surface of the nanosized pores and piled up layer by layer. This is the first report that shows the Raman spectroscopy is a powerful tool to observe the synthesis of pharmaceutical cocrystals incorporated in the nanosized pores of mesoporous silica. The results indicate a way to control the size of cocrystals on a nanometer scale, which will provide higher bioavailability of pharmaceuticals. (author)

Electrochemical synthesis of highly crystalline copper nanowires

International Nuclear Information System (INIS)

Kaur, Amandeep; Gupta, Tanish; Kumar, Akshay; Kumar, Sanjeev; Singh, Karamjeet; Thakur, Anup

2015-01-01

Copper nanowires were fabricated within the pores of anodic alumina template (AAT) by template synthesis method at pH = 2.9. X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) were used to investigate the structure, morphology and composition of fabricated nanowires. These characterizations revealed that the deposited copper nanowires were highly crystalline in nature, dense and uniform. The crystalline copper nanowires are promising in application of future nanoelectronic devices and circuits

Novel green synthesis of gold nanoparticles using Citrullus lanatus rind and investigation of proteasome inhibitory activity, antibacterial, and antioxidant potential

Directory of Open Access Journals (Sweden)

Patra JK

2015-12-01

Full Text Available Jayanta Kumar Patra, Kwang-Hyun Baek School of Biotechnology, Yeungnam University, Gyeongsan, Gyeongbuk, Republic of Korea Abstract: Biological synthesis of nanoparticles using nontoxic, eco-friendly approaches is gaining importance owing to their fascinating biocompatibility and environmentally benign nature. This study describes the green synthesis approach for synthesis of gold nanoparticles (ANPs using aqueous extract of the rind of watermelon as a fruit waste and evaluate its biopotential in terms of proteasome inhibitory activity, antibacterial, and antioxidant potential. The synthesized ANPs were characterized using UV–vis spectroscopy, scanning electron microscopy, X-ray diffraction, Fourier-transform infrared spectroscopy, and thermogravimetric analysis. The surface plasmon resonance spectra of ANPs were obtained at 560 nm. Scanning electron microscopy image revealed that particles had a spherical shape and have a size distribution of 20–140 nm, followed by the elemental analysis by energy-dispersive X-ray spectroscopy. X-ray diffraction analysis confirmed the crystallite nature of the ANPs and Fourier-transform infrared spectroscopy revealed the involvement of bioactive compounds from watermelon rind in the synthesis, capping, and stabilization of ANPs. ANPs exhibited potential antibacterial activity against five different foodborne pathogenic bacteria with diameter of inhibition zones ranged between 9.23 and 11.58 mm. They also displayed strong synergistic antibacterial activity together with kanamycin (11.93–21.08 mm inhibition zones and rifampicin (10.32–24.84 mm inhibition zones. ANPs displayed strong antioxidant activity in terms of DPPH radical scavenging (24.69%, nitric oxide scavenging (25.62%, ABTS scavenging (29.42%, and reducing power. Significantly high proteasome inhibitory potential of the ANPs (28.16% could be highly useful for cancer treatment and targeted cancer drug delivery. Overall, results highlight a

Green synthesis of monodisperse silver nanoparticles using hydroxy propyl methyl cellulose

Energy Technology Data Exchange (ETDEWEB)

Dong, Chunfa; Zhang, Xianglin, E-mail: hust_zxl@mail.hust.edu.cn; Cai, Hao

2014-01-15

Graphical abstract: -- Highlights: • Synthesis of silver nanoparticles using hydroxy propyl methyl cellulose is reported. • HPMC and glucose are used as capping agent and reducing agent respectively. • It is the first time to use HPMC for synthesis of silver nanoparticles. • The small, spherical and well-dispersed particle is observed in the range of 3–17 nm. • The green method can be extended to other noble metals. -- Abstract: A simple and environmentally friendly method for the synthesis of highly stable and small sized silver nanoparticles with narrow distribution from 3 nm to 17 nm is reported. Silver nitrate, hydroxy propyl methyl cellulose (HPMC) and glucose, were used as silver precursor, capping agents and reducing agents respectively. The formation of silver nanoparticles was observed by change of color from colorless to wine red. The silver nanoparticles were characterized by transmission electron microscopy (TEM), UV–visible spectroscopy (UV–vis), X-ray diffraction (XRD) and Fourier-transform infrared spectroscopy (FT-IR). The results demonstrated that the obtained metallic nanoparticles were single crystalline silver nanoparticles capped with HPMC. The effects of the reaction time, reaction temperature and the concentration of silver ion and reducing agents on the particle size were investigated. A possible formation mechanism was proposed. The method may be extended to other noble metal for other technological applications such as additional medicinal, industrial applications.

Green synthesis of monodisperse silver nanoparticles using hydroxy propyl methyl cellulose

International Nuclear Information System (INIS)

Dong, Chunfa; Zhang, Xianglin; Cai, Hao

2014-01-01

Graphical abstract: -- Highlights: • Synthesis of silver nanoparticles using hydroxy propyl methyl cellulose is reported. • HPMC and glucose are used as capping agent and reducing agent respectively. • It is the first time to use HPMC for synthesis of silver nanoparticles. • The small, spherical and well-dispersed particle is observed in the range of 3–17 nm. • The green method can be extended to other noble metals. -- Abstract: A simple and environmentally friendly method for the synthesis of highly stable and small sized silver nanoparticles with narrow distribution from 3 nm to 17 nm is reported. Silver nitrate, hydroxy propyl methyl cellulose (HPMC) and glucose, were used as silver precursor, capping agents and reducing agents respectively. The formation of silver nanoparticles was observed by change of color from colorless to wine red. The silver nanoparticles were characterized by transmission electron microscopy (TEM), UV–visible spectroscopy (UV–vis), X-ray diffraction (XRD) and Fourier-transform infrared spectroscopy (FT-IR). The results demonstrated that the obtained metallic nanoparticles were single crystalline silver nanoparticles capped with HPMC. The effects of the reaction time, reaction temperature and the concentration of silver ion and reducing agents on the particle size were investigated. A possible formation mechanism was proposed. The method may be extended to other noble metal for other technological applications such as additional medicinal, industrial applications

Synthesis of porous gold nanoshells by controlled transmetallation reaction

Energy Technology Data Exchange (ETDEWEB)

Pattabi, Manjunatha, E-mail: manjupattabi@yahoo.com; M, Krishnaprabha [Department of Materials Science, Mangalore University, Mangalagangothri-574199 (India)

2015-06-24

Aqueous synthesis of porous gold nanoshells in one step is carried out through controlled transmetallation (TM) reaction using a naturally available egg shell membrane (ESM) as a barrier between the sacrificial silver particles (AgNPs) and the gold precursor solution (HAuCl{sub 4}). The formation of porous gold nanoshells via TM reaction is inferred from UV-Vis spectroscopy and the scanning electron microscopic (SEM) studies.

Bismuth molybdate catalysts prepared by mild hydrothermal synthesis: Influence of pH on the selective oxidation of propylene

DEFF Research Database (Denmark)

Schuh, Kirsten; Kleist, Wolfgang; Høj, Martin

2015-01-01

A series of bismuth molybdate catalysts with relatively high surface area was prepared via mild hydrothermal synthesis. Variation of the pH value and Bi/Mo ratio during the synthesis allowed tuning of the crystalline Bi-Mo oxide phases, as determined by X-ray diffraction (XRD) and Raman...... spectroscopy. The pH value during synthesis had a strong influence on the catalytic performance. Synthesis using a Bi/Mo ratio of 1/1 at pH ≥ 6 resulted in γ-Bi2MoO6, which exhibited a better catalytic performance than phase mixtures obtained at lower pH values. However, a significantly lower catalytic...

Studies on potassium chlorate as a primary oxidimetric reagent.

Science.gov (United States)

Murty, C R; Rao, G G

1972-01-01

Conditions have been established for the use of potassium chlorate as a primary oxidizing agent in the direct titration of vanadium(III), tin(II) and titanium(III) with visual or potentiometric end-points.

Microwave-assisted synthesis of iron oxide nanoparticles in biocompatible organic environment

Directory of Open Access Journals (Sweden)

E. Aivazoglou

2018-04-01

Full Text Available The development of magnetite and maghemite particles in uniform nanometer size has triggered the interest of the research community due to their many interesting properties leading to a wide range of applications, such as catalysis, nanomedicine-nanobiology and other engineering applications. In this study, a simple, time-saving and low energy-consuming, microwave-assisted synthesis of iron oxide nanoparticles, is presented. The nanoparticles were prepared by microwave-assisted synthesis using polyethylene glycol (PEG or PEG and β-cyclodextrin (β-CD/water solutions of chloride salts of iron in the presence of ammonia solution. The prepared nano-powders were characterized using X-Ray Diffraction (XRD, Transition Electron Microscopy (TEM, Fourier-transform Infrared Spectroscopy (FTIR, Raman Spectroscopy, Vibrating Sample Magnetometer (VSM, X-Ray Photoelectron Spectroscopy (XPS and Thermal analysis (TG/DSC. The produced nanoparticles are crystallized mostly in the magnetite and maghemite lattice exhibiting very similar shape and size, with indications of partial PEG coating. Heating time, microwave power and presence of PEG, are the key factors shaping the size properties of nanoparticles. The average size of particles ranges from 10.3 to 19.2 nm. The nanoparticles exhibit a faceted morphology, with zero contamination levels. The magnetic measurements indicate that the powders are soft magnetic materials with negligible coercivity and remanence, illustrating super-paramagnetic behavior.

Synthesis and characterization of acrylate copolymer containing fluorescein functional group

Energy Technology Data Exchange (ETDEWEB)

Hui, Guodong; Huang, Weiyun; Song, Yunzhao; Chen, Deben; Zhong, Anyong [Sichuan University, Chengdu (China)

2013-08-15

We report a novel method to fabricate fluorescent polymer (F-CPA) based on the esterification between acrylate copolymer (CPA) and fluorescein using N, N-dicyclohexylcarbodiimide (DCC)/4-dimethylaminopyridine (DMAP) as catalyst. The resulting copolymer was characterized by Fourier transform-infrared spectroscopy (FT-IR), gel permeation chromatography (GPC), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), ultraviolet-visible spectroscopy (UV-Vis) and fluorescence spectroscopy. In addition, the influences of concentration, solvents, pH and metal cations (Cu{sup 2+}, Fe{sup 3+} and Zn{sup 2+}) on the fluorescent behaviors of F-CPA are discussed in detail. All those observations suggest that the synthesized F-CPA is an excellent luminescent macromolecular material with simple synthesis method and excellent solubility. Moreover, its sensitive fluorescence response behaviors to solvents, pH and metal cations make it to become a polymer-based probe.

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.

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.

Synthesis, physicochemical and optical properties of bis-thiosemicarbazone functionalized graphene oxide

Science.gov (United States)

Kumar, Santosh; Wani, Mohmmad Y.; Arranja, Claudia T.; Castro, Ricardo A. E.; Paixão, José A.; Sobral, Abilio J. F. N.

2018-01-01

Fluorescent materials are important for low-cost opto-electronic and biomedical sensor devices. In this study we present the synthesis and characterization of graphene modified with bis-thiosemicarbazone (BTS). This new material was characterized using Fourier transform infrared spectroscopy (FT-IR), Ultraviolet-visible (UV-Vis) and Raman spectroscopy techniques. Further evaluation by X-ray diffraction (XRD), thermo-gravimetric analysis (TGA), differential scanning calorimetry (DSC), scanning electron microscopy (SEM) and atomic-force microscopy (AFM) allowed us to fully characterize the morphology of the fabricated material. The average height of the BTSGO sheet is around 10 nm. Optical properties of BTSGO evaluated by photoluminescence (PL) spectroscopy showed red shift at different excitation wavelength compared to graphene oxide or bisthiosemicarbazide alone. These results strongly suggest that BTSGO material could find potential applications in graphene based optoelectronic devices.

A shortcut hydrothermal strategy for the synthesis of zinc nanowires

International Nuclear Information System (INIS)

Hu Jianqiang; Chen Zhiwu; Xie Jingsi; Yu Ying

2008-01-01

Synthesis of metal nanowires has opened many new possibilities for designing ideal building blocks for future nanodevices. In this work, zinc nanowires with lengths of micrometre magnitude were synthesized in high yield by a shortcut hydrothermal strategy. The synthesis involves a template-free, non-seed and catalyst-free solution-phase process to high-quality zinc nanowires, which is low-cost and proceeds at relatively short time. In this process, zinc nanowires were prepared through the reduction of zinc acetate with absolute ethanol in the presence of silver nitrate under hydrothermal atmosphere. The strategy suggests that silver ion plays a vital role in the synthesis of zinc nanowires, without which the substituted product is zinc oxide nanowires. X-ray diffraction and energy-dispersive x-ray spectroscopy measurements confirm the final formation of zinc nanowires and component transformation from zinc oxide nanowires in the introduction of silver ion. We believe that with the efficient synthesis, longer zinc nanowires can be fabricated and may find potential applications for superconductors and nanodevices. (fast track communication)

Synthesis and Characterization of CdS/TiO2-Montmorillonite Nanocomposite with Enhanced Visible-Light Absorption

OpenAIRE

Feng-shan Zhou; Dai-mei Chen; Bao-lin Cui; Wei-heng Wang

2014-01-01

Sodium montmorillonite (MMT) was chosen as the carrier; a serial of CdS/TiO2-MMT nanocomposites with enhanced visible-light absorption ability was prepared by hydrothermal synthesis method combination with semiconductor compound modification method. The samples are characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and ultraviolet visible (UV-Vis) spectroscopy; the results showed that TiO2 and CdS nanoparticles were loaded on the surface of montmorillonite unifo...

From single-site tantalum complexes to nanoparticles of Ta x N y and TaO x N y supported on silica: elucidation of synthesis chemistry by dynamic nuclear polarization surface enhanced NMR spectroscopy and X-ray absorption spectroscopy.

Science.gov (United States)

Mohandas, Janet C; Abou-Hamad, Edy; Callens, Emmanuel; Samantaray, Manoja K; Gajan, David; Gurinov, Andrei; Ma, Tao; Ould-Chikh, Samy; Hoffman, Adam S; Gates, Bruce C; Basset, Jean-Marie

2017-08-01

Air-stable catalysts consisting of tantalum nitride nanoparticles represented as a mixture of Ta x N y and TaO x N y with diameters in the range of 0.5 to 3 nm supported on highly dehydroxylated silica were synthesized from TaMe 5 (Me = methyl) and dimeric Ta 2 (OMe) 10 with guidance by the principles of surface organometallic chemistry (SOMC). Characterization of the supported precursors and the supported nanoparticles formed from them was carried out by IR, NMR, UV-Vis, extended X-ray absorption fine structure, and X-ray photoelectron spectroscopies complemented with XRD and high-resolution TEM, with dynamic nuclear polarization surface enhanced NMR spectroscopy being especially helpful by providing enhanced intensities of the signals of 1 H, 13 C, 29 Si, and 15 N at their natural abundances. The characterization data provide details of the synthesis chemistry, including evidence of (a) O 2 insertion into Ta-CH 3 species on the support and (b) a binuclear to mononuclear transformation of species formed from Ta 2 (OMe) 10 on the support. A catalytic test reaction, cyclooctene epoxidation, was used to probe the supported nanoparticles, with 30% H 2 O 2 serving as the oxidant. The catalysts gave selectivities up to 98% for the epoxide at conversions as high as 99% with a 3.4 wt% loading of Ta present as Ta x N y /TaO x N y .

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

International Nuclear Information System (INIS)

Luiz, J.M.

1989-01-01

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

Novel green synthesis of gold nanoparticles using Citrullus lanatus rind and investigation of proteasome inhibitory activity, antibacterial, and antioxidant potential

Science.gov (United States)

Patra, Jayanta Kumar; Baek, Kwang-Hyun

2015-01-01

Biological synthesis of nanoparticles using nontoxic, eco-friendly approaches is gaining importance owing to their fascinating biocompatibility and environmentally benign nature. This study describes the green synthesis approach for synthesis of gold nanoparticles (ANPs) using aqueous extract of the rind of watermelon as a fruit waste and evaluate its biopotential in terms of proteasome inhibitory activity, antibacterial, and antioxidant potential. The synthesized ANPs were characterized using UV–vis spectroscopy, scanning electron microscopy, X-ray diffraction, Fourier-transform infrared spectroscopy, and thermogravimetric analysis. The surface plasmon resonance spectra of ANPs were obtained at 560 nm. Scanning electron microscopy image revealed that particles had a spherical shape and have a size distribution of 20–140 nm, followed by the elemental analysis by energy-dispersive X-ray spectroscopy. X-ray diffraction analysis confirmed the crystallite nature of the ANPs and Fourier-transform infrared spectroscopy revealed the involvement of bioactive compounds from watermelon rind in the synthesis, capping, and stabilization of ANPs. ANPs exhibited potential antibacterial activity against five different foodborne pathogenic bacteria with diameter of inhibition zones ranged between 9.23 and 11.58 mm. They also displayed strong synergistic antibacterial activity together with kanamycin (11.93–21.08 mm inhibition zones) and rifampicin (10.32–24.84 mm inhibition zones). ANPs displayed strong antioxidant activity in terms of DPPH radical scavenging (24.69%), nitric oxide scavenging (25.62%), ABTS scavenging (29.42%), and reducing power. Significantly high proteasome inhibitory potential of the ANPs (28.16%) could be highly useful for cancer treatment and targeted cancer drug delivery. Overall, results highlight a potential low-cost green method of synthesizing ANPs from food waste materials. Significant biopotentials of synthesized ANPs could make it a potential

Green synthesis and antibacterial activity screening of silver nanoparticles reduced by papaya (Carica papaya L.) leaves extract

International Nuclear Information System (INIS)

Esplana, Camille S.; Cabling, Mercedes Q.

2013-01-01

The field of nano technology is the most active area of research in modern material sciences. Though there are many chemical, as well as physical methods, green synthesis is the most emerging method of synthesis. This study aimed to describe a cost effective and environment friendly technique for green synthesis of silver nanoparticles. The synthesis of silver nanoparticles was prepared by adding Carica papaya L. leaves extract to 1mM silver nitrate solution. The color change in reaction mixture (pale yellow to dark brown color was observed during the incubation period , due to excitation of surface plasmon vibrations in silver nanoparticles. Nanoparticles were characterized using UV-Visible absorption spectroscopy, X-Ray Diffraction (XRD) pattern, Scanning Electron Microscopy (SEM) and Energy-Dispersive Spectroscopy (EDX) analysis. Absorption spectra of silver nanoparticles formed in the reaction media has absorbance peak at 280 nm, broadening of peak indicates that the particles are poly dispersed. SEM analysis described the morphology and the size of the particles. XRD confirmed the crystalline structure of the nanoparticles. The presence of the elemental silver was observed in the graph obtained from EDX analysis, which also supports the XRD results. The biomass of plants produces their nano materials by a process called bio mineralization. The tests cultures included in the study were Staphylococcus aureus, Escherichia coli and Salmonella. Results showed that the maximum inhibitory effect using 1mM silver nitrates against the microbes were obtained. The approach of plant-mediated synthesis appears to be cost efficient, eco-friendly and easy alternative to conventional methods of silver nanoparticles synthesis (author)

Novel method for synthesis of silver nanoparticles and their application on wool

Energy Technology Data Exchange (ETDEWEB)

Boroumand, Majid Nasiri [Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of); Montazer, Majid [Amirkabir University of Technology, Tehran (Iran, Islamic Republic of); Simon, Frank [Leibniz-Institut für Polymerforschung Dresden e.V., Dresden (Germany); Liesiene, Jolanta [Faculty of Chemical Technology, Kaunas University of Technology, Kaunas (Lithuania); Šaponjic, Zoran [Vinča Institute of Nuclear Sciences, University of Belgrade, Belgrade (Serbia); Dutschk, Victoria, E-mail: v.dutschk@utwente.nl [Faculty of Engineering Technology, University of Twente, Enschede (Netherlands)

2015-08-15

Graphical abstract: Tentative mechanism for reduction of Ag{sup +} by polyphenols having two hydroxy groups in ortho-position – the use of silver nanoparticles and an aqueous solution of extracted dye from Pomegranate peel as a reducing agent for synthesis silver nanoparticles from silver nitrate. - Highlights: • A new method for the synthesis of silver nanoparticles suitable to impart antibacterial properties of wool fabric proposed. • Silver nanopartilces were synthesized by a biochemical reduction method. • An aqueous solution of extracted dye from Pomegranate peel was used as a reducing agent for synthesis of silver nanoparticles from silver nitrate. - Abstract: In this study, a new method for the synthesis of silver nanoparticles (AgNPs) suitable to impart antibacterial properties of wool fabric is proposed. AgNPs were synthesized by a biochemical reduction method. An aqueous solution of extracted dye from Pomegranate peel was used as a reducing agent for the synthesis of AgNPs from silver nitrate. The ratio of dye to silver nitrate concentration (R{sub Dye}/{sub Ag} = [Dye]/[AgNO{sub 3}]) is the influencing factor in the synthesis of silver nanoparticles. The nanoparticles formation was followed by UV/Vis absorption spectroscopy. The size and shape of AgNPs were studied by transmission electron microscopy (TEM). The size distribution and Zetapotential of nanoparticles were evaluated using diffraction light scattering (DLS) measurements. The antibacterial potential of biosynthesized silver nanoparticles against Escherichia coli (E. coli) was examined qualitatively and quantitatively. Kinetic analysis of the bacteria reduction using AgNPs synthesized in different way was performed. AgNPs were applied on wool fabrics by exhaustion. The changes in surface morphology of wool fibers after AgNPs loading were studied using scanning electron microscopy (SEM). The amounts of silver deposited on wool fabrics at different pH and temperature were compared applying

Novel method for synthesis of silver nanoparticles and their application on wool

International Nuclear Information System (INIS)

Boroumand, Majid Nasiri; Montazer, Majid; Simon, Frank; Liesiene, Jolanta; Šaponjic, Zoran; Dutschk, Victoria

2015-01-01

Graphical abstract: Tentative mechanism for reduction of Ag + by polyphenols having two hydroxy groups in ortho-position – the use of silver nanoparticles and an aqueous solution of extracted dye from Pomegranate peel as a reducing agent for synthesis silver nanoparticles from silver nitrate. - Highlights: • A new method for the synthesis of silver nanoparticles suitable to impart antibacterial properties of wool fabric proposed. • Silver nanopartilces were synthesized by a biochemical reduction method. • An aqueous solution of extracted dye from Pomegranate peel was used as a reducing agent for synthesis of silver nanoparticles from silver nitrate. - Abstract: In this study, a new method for the synthesis of silver nanoparticles (AgNPs) suitable to impart antibacterial properties of wool fabric is proposed. AgNPs were synthesized by a biochemical reduction method. An aqueous solution of extracted dye from Pomegranate peel was used as a reducing agent for the synthesis of AgNPs from silver nitrate. The ratio of dye to silver nitrate concentration (R Dye / Ag = [Dye]/[AgNO 3 ]) is the influencing factor in the synthesis of silver nanoparticles. The nanoparticles formation was followed by UV/Vis absorption spectroscopy. The size and shape of AgNPs were studied by transmission electron microscopy (TEM). The size distribution and Zetapotential of nanoparticles were evaluated using diffraction light scattering (DLS) measurements. The antibacterial potential of biosynthesized silver nanoparticles against Escherichia coli (E. coli) was examined qualitatively and quantitatively. Kinetic analysis of the bacteria reduction using AgNPs synthesized in different way was performed. AgNPs were applied on wool fabrics by exhaustion. The changes in surface morphology of wool fibers after AgNPs loading were studied using scanning electron microscopy (SEM). The amounts of silver deposited on wool fabrics at different pH and temperature were compared applying energy

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.

Biological synthesis of silver nanoparticles

International Nuclear Information System (INIS)

Maliszewska, I; Szewczyk, K; Waszak, K

2009-01-01

Fungus-mediated synthesis of silver nanoparticles is reported. The nanosilver was formed in contact with the cell-free filtrate of Penicillium strain studied. The nanoparticles were characterized by means of the UV-Vis spectroscopy, scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The synthesized nanosilver showed a absorbed maximum at 425 nm in the visible region. The SEM characterization of the fungus cells treated with silver nitrite indicated that the protein might be responsible for the reduction of silver ions. Transmission electron microscopy (TEM) micrograph showed formation of silver nanoparticles in the range of 10-100 nm.

Green synthesis of highly fluorescent carbon quantum dots from sugarcane bagasse pulp

Energy Technology Data Exchange (ETDEWEB)

Thambiraj, S. [Nano-Bio Materials and Sensors Laboratory, PSG Institute of Advanced Studies, Coimbatore, 641 004, Tamil Nadu (India); Ravi Shankaran, D., E-mail: dravishankaran@hotmail.com [Nano-Bio Materials and Sensors Laboratory, PSG Institute of Advanced Studies, Coimbatore, 641 004, Tamil Nadu (India); National Centre for Nanoscience and Nanotechnology, University of Madras, Guindy Campus, Chennai, 600 025, Tamil Nadu (India)

2016-12-30

Graphical abstract: Schematic representation of CQDs from sugarcane bagasse carbon. - Highlights: • CQDs were synthesised from sugarcane bagasse waste with top down approaches. • Synthesis method is green, simple and efficient process. • CQDs possess high quantum yield, good stability and highly fluorescent in nature. • The morphological and topographical study of CQDs was done by HR-TEM and AFM and was observed that the average size is 4.1 ± 0.17 nm and surface thickness is 5 nm. - Abstract: Carbon quantum dots (CQDs) have great potential due to its advantageous characteristics of highly fluorescent nature and good stability. In this study, we aimed to develop a simple and efficient method for the green synthesis of fluorescent CQDs from sugarcane bagasse, a renewable and sustainable resource. The process involves the top down approach of chemical oxidation followed by exfoliation of sugarcane carbon. The synthesized CQDs was characterized by UV–vis absorption spectroscopy, Spectrofluorophotometry, Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), Raman spectroscopy, X-ray photon spectroscopy (XPS), Atomic force microscopy (AFM) and High-resolution transmission electron microscopy (HR-TEM). The synthesized CQDs possess stable fluorescent properties, good bio-compatibility and high quantum yield. The CQDs are highly crystalline with longitudinal dimensions of 4.1 ± 0.17 nm with an average roughness of around 5 nm. The XRD and TEM analysis indicates that the synthesized CQDs possess face centred cubic crystal structure. The results suggest that the proposed CQDs could be utilized for bio-sensor, bio-imaging and drug delivery applications.

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)

GC of catalytic reactions products involved in the promising fuel synthesis

Energy Technology Data Exchange (ETDEWEB)

Zheivot, V.; Sazonova, N. [Russian Academy of Sciences, Novosibirsk (Russian Federation). Boreskov Inst. of Catalysis

2012-09-15

Catalytic reactions involved in the synthesis of the promising kinds of novel fuel and products formed in these reactions were systematized according to the resulting fuel type. Generalization of the retention of the substances comprising these products is presented. Chromatograms exhibiting their separation on chromatographic materials with the surface of different chemical properties are summarized. We propose procedures for gas-chromatographic analysis of the catalytic reactions products formed in the synthesis of hydrogen, methanol, dimethyl ether and hydrocarbons as a new generation of fuel alternative to petroleum and coal. For partial oxidation of methane into synthesis gas, on-line determination of the components obtained in the reaction was carried out by gas chromatography and gas analyzer based on different physicochemical methods (IR spectroscopy and electrochemical methods). Similarity of the results obtained using these methods is demonstrated. (orig.)

Structure and spectroscopy of uranyl salicylaldiminate complexes

Energy Technology Data Exchange (ETDEWEB)

Tamasi, A.L.; Barnes, C.L.; Walensky, J.R. [Missouri Univ., Columbia, MO (United States). Dept. of Chemistry

2013-07-01

The synthesis of uranyl complexes coordinated to tridentate, monoanionic salicylaldiminate (Schiff base) ligands was achieved by the reaction of UO{sub 2}Cl{sub 2}(THF){sub 3}, 1, with one equivalent of the corresponding sodium salicylaldiminate salts affording [(C{sub 9}H{sub 6}N)N=C(H)C{sub 6}H{sub 2}'Bu{sub 2}O]UO{sub 2}Cl(THF), 2, [(NC{sub 5}H{sub 4})N=C(H)C{sub 6}H{sub 2}'Bu{sub 2}O]UO{sub 2}Cl(THF), 3, and [(C{sub 6}H{sub 4}SCH{sub 3})N=C(H)C{sub 6}H{sub 2}'Bu{sub 2}O]UO{sub 2}Cl(THF), 4. These are uncommon examples of uranyl complexes with a monoanionic ancillary ligand to stabilize the coordination sphere and one chloride ligand. Compounds 2-4 have been characterized by {sup 1}H and {sup 13}C NMR spectroscopy as well as IR and UVVis spectroscopy and their structures determined by X-ray crystallography. (orig.)

Synthesis, Characterization, and Spectroscopy of Model Molybdopterin Complexes‡

Science.gov (United States)

Burgmayer, Sharon J. Nieter; Kim, Mary; Petit, Rebecca; Rothkopf, Amy; Kim, Alison; BelHamdounia, Shadia; Hou, Ying; Somogyi, Arpad; Habel-Rodriguez, Diana; Williams, Antonio; Kirk, Martin L.

2012-01-01

The preparation and characterization of new model complexes for the molybdenum cofactor are reported. The new models are distinctive for the inclusion of pterin-substituted dithiolene chelates and have the formulation Tp*MoX(pterin-R-dithiolene) (Tp* = tris(3,5,-dimethylpyrazolyl)borate), X= O, S, R= aryl or −C(OH)(CH3)2). Syntheses of Mo(4+) and (5+) complexes of two pterin-dithiolene derivatives as both oxo and sulfido compounds, and improved syntheses for pterinyl alkynes and [Et4N][Tp*MoIV(S)S4] reagents are described. Characterization methods include electrospray ionization mass spectrometry, electrochemistry, infrared spectroscopy, electron paramagnetic resonance and magnetic circular dichroism. Cyclic voltammetry reveals that the Mo(5+/4+) reduction potential is intermediate between that for dithiolene with electron-withdrawing substituents and simple dithiolate chelates. Electron paramagnetic resonance and magnetic circular dichroism of Mo(5+) complexes where X = O, R = aryl indicates that the molybdenum environment in the new models is electronically similar to that in Tp*MoO(benzenedithiolate). PMID:17765313

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.

Synthesis and behavior at heating of amorphous calcium diphosphate

International Nuclear Information System (INIS)

Levchenko, L.V.; Nurkina, Z.S.; Griggs, D.; Sinyayev, V.A.

2005-01-01

There is description of synthesis of amorphous calcium diphosphate in the article. The compound was received via exchange reaction between sodium diphosphate and calcium chloride in water solution. The results of investigation of behavior when heated of produced substance are presented here as well. Composition and structure of precipitated substances and products of its thermal convention were determined by methods of IR-, NMR 31 P and X-ray spectroscopy

Synthesis of allyl amine on glass by continuous plasma

International Nuclear Information System (INIS)

Morales, J.; Olayo, R.; Vasquez, M.; OLayo, M.G.; Cruz, G.

2003-01-01

In this work the synthesis by plasma of thin films of polyallyl amine under continuous plasma conditions for possible use in biomaterials is presented. It is shown that the thickness of the film depends so much of the time of synthesis like of the used power. The polymers were analyzed by X-ray photoelectron spectroscopy (XPS) and angle of contact before and after of being immersed in distilled water by 10 days. The allylamine shows lost of nitrogen and an increase in the content of oxygen with the immersion time due to the interaction among the water and the polymer. The angle of contact shows an increase of approximately 10 degrees, what indicates a change in the surface energy of the polymer. (Author)

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)

Green synthesis of silver nanoparticles by Bacillus methylotrophicus, and their antimicrobial activity.

Science.gov (United States)

Wang, Chao; Kim, Yeon Ju; Singh, Priyanka; Mathiyalagan, Ramya; Jin, Yan; Yang, Deok Chun

2016-06-01

The synthesis of silver nanoparticles (AgNPs) by microorganisms is an area attracting growing interest in nanobiotechnology, due to the applications of these nanoparticles in various products including cosmetics and biosensors, and in the biomedical, clinical, and bioimaging fields as well. Various microorganisms have been found to be able to synthesize AgNPs when silver salts are supplied in the reaction system. The main objectives of this study were to evaluate the efficiency of synthesis of AgNPs by the strain Bacillus methylotrophicus DC3, isolated from the soil of Korean ginseng, a traditionally known oriental medicinal plant in Korea. The AgNPs showed maximum absorbance at 416 nm, when assayed by ultraviolet-visible spectroscopy (UV-vis). The field emission transmission electron micrograph (FE-TEM) results showed that the particles were spherical and 10-30 nm in size. In addition, the product was also characterized by energy dispersive X-ray spectroscopy (EDX), which displayed a 3 keV peak corresponding to the silver nanocrystal. Elemental mapping results also confirmed the presence of silver elements in the electron micrograph region. Furthermore, the AgNPs demonstrated antimicrobial activity against various pathogenic microorganisms such as Candida albicans, Salmonella enterica, Escherichia coli, and Vibrio parahaemolyticus, with enhanced antimicrobial activity being exhibited against C. albicans. Therefore, the current study describes the simple, efficient, and green method of synthesis of AgNPs by B. methylotrophicus DC3.

Green synthesis of gold nanoparticles for trace level detection of a hazardous pollutant (nitrobenzene) causing Methemoglobinaemia

International Nuclear Information System (INIS)

Emmanuel, R.; Karuppiah, Chelladurai; Chen, Shen-Ming; Palanisamy, Selvakumar; Padmavathy, S.; Prakash, P.

2014-01-01

Graphical abstract: Schematic representation for green synthesis of Au-NPs and its electroreduction of nitrobenzene. - Highlights: • A green synthesis of size controlled Au-NPs from plant extract. • Trace level detection of nitro benzene, a pollutant causing Methemoglobinaemia, at Au-NPs modified electrode. • Achievement of lower LOD and wider linear response. • The proposed sensor exhibits excellent practicality in various water samples. - Abstract: The present study involves a green synthesis of gold nanoparticles (Au-NPs) using Acacia nilotica twig bark extract at room temperature and trace level detection of one of the hazardous materials, viz. nitrobenzene (NB) that causes Methemoglobinaemia. The synthesis protocol demonstrates that the bioreduction of chloroauric acid leads to the formation of Au-NPs within 10 min, suggesting a higher reaction rate than any other chemical methods involved. The obtained Au-NPs have been characterized by UV–vis spectroscopy, X-ray diffraction, transmission electron microscopy, Energy-Dispersive X-ray Spectroscopy and Fourier Transform Infrared Spectroscopy. The electrochemical detection of NB has been investigated at the green synthesized Au-NPs modified glassy carbon electrode by using differential pulse voltammetry (DPV). The Au-NPs modified electrode exhibits excellent reduction ability toward NB compared to unmodified electrode. The developed NB sensor at Au-NPs modified electrode displays a wide linear response from 0.1 to 600 μM with high sensitivity of 1.01 μA μM −1 cm −2 and low limit of detection of 0.016 μM. The modified electrode shows exceptional selectivity in the presence of ions, phenolic and biologically coactive compounds. In addition, the Au-NPs modified electrode exhibits an outstanding recovery results toward NB in various real water samples

Green synthesis of gold nanoparticles for trace level detection of a hazardous pollutant (nitrobenzene) causing Methemoglobinaemia

Energy Technology Data Exchange (ETDEWEB)

Emmanuel, R. [Post Graduate and Research Department of Chemistry, Thiagarajar College, Madurai 625009, Tamil Nadu (India); Karuppiah, Chelladurai [Department of Chemical Engineering and Biotechnology, National Taipei University of Technology, Taipei 106, Taiwan, ROC (China); Chen, Shen-Ming, E-mail: smchen78@ms15.hinet.net [Department of Chemical Engineering and Biotechnology, National Taipei University of Technology, Taipei 106, Taiwan, ROC (China); Palanisamy, Selvakumar [Department of Chemical Engineering and Biotechnology, National Taipei University of Technology, Taipei 106, Taiwan, ROC (China); Padmavathy, S. [Department of Zoology and Microbiology, Thiagarajar College, Madurai 625009, Tamil Nadu (India); Prakash, P., E-mail: kmpprakash@gmail.com [Post Graduate and Research Department of Chemistry, Thiagarajar College, Madurai 625009, Tamil Nadu (India)

2014-08-30

Graphical abstract: Schematic representation for green synthesis of Au-NPs and its electroreduction of nitrobenzene. - Highlights: • A green synthesis of size controlled Au-NPs from plant extract. • Trace level detection of nitro benzene, a pollutant causing Methemoglobinaemia, at Au-NPs modified electrode. • Achievement of lower LOD and wider linear response. • The proposed sensor exhibits excellent practicality in various water samples. - Abstract: The present study involves a green synthesis of gold nanoparticles (Au-NPs) using Acacia nilotica twig bark extract at room temperature and trace level detection of one of the hazardous materials, viz. nitrobenzene (NB) that causes Methemoglobinaemia. The synthesis protocol demonstrates that the bioreduction of chloroauric acid leads to the formation of Au-NPs within 10 min, suggesting a higher reaction rate than any other chemical methods involved. The obtained Au-NPs have been characterized by UV–vis spectroscopy, X-ray diffraction, transmission electron microscopy, Energy-Dispersive X-ray Spectroscopy and Fourier Transform Infrared Spectroscopy. The electrochemical detection of NB has been investigated at the green synthesized Au-NPs modified glassy carbon electrode by using differential pulse voltammetry (DPV). The Au-NPs modified electrode exhibits excellent reduction ability toward NB compared to unmodified electrode. The developed NB sensor at Au-NPs modified electrode displays a wide linear response from 0.1 to 600 μM with high sensitivity of 1.01 μA μM{sup −1} cm{sup −2} and low limit of detection of 0.016 μM. The modified electrode shows exceptional selectivity in the presence of ions, phenolic and biologically coactive compounds. In addition, the Au-NPs modified electrode exhibits an outstanding recovery results toward NB in various real water samples.

Synthesis of Y-Tip Graphitic Nanoribbons from Alcohol Catalytic Chemical Vapor Deposition on Piezoelectric Substrate

Directory of Open Access Journals (Sweden)

Zainab Yunusa

2015-01-01

Full Text Available We report the synthesis of Graphitic Nanoribbons (GNRs using Alcohol Catalytic Chemical Vapor Deposition (ACCVD. Bulk GNR was synthesized directly on a piezoelectric substrate using one-step ACCVD. The synthesized GNRs were characterized by X-Ray Diffraction (XRD, Scanning Electron Microscope (SEM, Transmission Electron Microscope (TEM, Energy Dispersive X-Ray (EDX, Atomic Force Microscopy (AFM, and Raman spectroscopy. The characterization results showed Y-tip morphology of bulk and filamentous as-grown GNR having varying width that lies between tens and hundreds of nm and length of several microns. Based on the thickness obtained from the AFM and the analysis from the Raman spectroscopy, it was concluded that the synthesized GNRs are multiple-layered and graphitic in nature. With the direct synthesis of GNR on a piezoelectric substrate, it could have applications in the sensor industries, while the Y-tip GNR could have potentialities in semiconductor applications.

Green mediated synthesis and characterization of ZnO nanoparticles using Euphorbia Jatropa latex as reducing agent

Directory of Open Access Journals (Sweden)

M.S. Geetha

2016-09-01

Full Text Available Presently the progress of green chemistry in the synthesis of nanoparticles with the use of plants has engrossed a great attention. This study reports the synthesis of ZnO using latex of Euphorbia Jatropa as reducing agent. As prepared product was characterized by powder X-ray diffractometer (PXRD, Fourier transform infra-red spectroscopy (FTIR, scanning electron microscopy–energy dispersive spectroscopy (SEM–EDS, transmission electron microscopy (TEM, X-ray photo electron spectroscopy (XPS, Rietveld refinement, UV–Visible spectroscopy and photoluminescence (PL. The concentration of plant latex plays an important role in controlling the size of the particle and its morphology. PXRD graphs showed the well crystallisation of the particles. The average particle size was calculated using Scherrer equation and advanced Williamson Hall (WH plots. The average particle size was around 15 nm. This result was also supported by SEM and TEM analyses. FTIR shows the characteristic peak of ZnO at 435 cm−1. SEM and TEM micrographs show that the particles were almost hexagonal in nature. EDS of SEM analysis confirmed that the elements are only Zn and O. EDS confirmed purity of ZnO. Atomic states were confirmed by XPS results. Crystal parameters were determined using Rietveld refinement. From UV–Visible spectra average energy gap was calculated which is ∼3.63 eV. PL studies showed UV emission peak at 392 nm and broad band visible emission centred in the range 500–600 nm. The Commission International de I'Eclairage and colour correlated temperature coordinates were estimated for ZnO prepared using 2 ml, 4 ml and 6 ml Jatropa latex. The results indicate that the phosphor may be suitable for white light emitting diode (WLED. The study fruitfully reveals simple, fast, economical and eco friendly method of synthesis of multifunctional ZnO nanoparticles (Nps.

Efficient synthesis of highly fluorescent nitrogen-doped carbon dots for cell imaging using unripe fruit extract of Prunus mume

International Nuclear Information System (INIS)

Atchudan, Raji; Edison, Thomas Nesakumar Jebakumar Immanuel; Sethuraman, Mathur Gopalakrishnan; Lee, Yong Rok

2016-01-01

Graphical abstract: The green synthesis of highly fluorescent N-CDs was achieved using the extract of unripe P. mume fruit as a carbon precursor by a one-pot simple hydrothermal-carbonization method. The resulting N-CDs were used as a staining agent for the fluorescence imaging of MDA-MB-231 cells. Display Omitted - Highlights: • The green synthesis of highly fluorescent N-CDs using the extract of unripe P. mume. • The N-CDs were synthesized by one-pot hydrothermal-carbonization method. • This method of synthesis is a simple, cost effective and eco-friendly route. • N-CDs will be a good alternative for fluorescent dyes and SQDs for bio-applications. - Abstract: Highly fluorescent nitrogen-doped carbon dots (N-CDs) were synthesized using the extract of unripe Prunus mume (P. mume) fruit by a simple one step hydrothermal-carbonization method. The N-CDs were synthesized at different pH ranges, 2.3, 5, 7, and 9. The pH of the P. mume extract was adjusted using an aqueous ammonia solution (25%). The optical properties of N-CDs were examined by UV–vis and fluorescence spectroscopy. The N-CDs synthesized at pH 9 emitted high fluorescence intensity compared to other obtained N-CDs. The N-CDs synthesized at pH 9 was further characterized by high resolution transmission electron microscopy (HR-TEM), X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), and Fourier transform-infra red (FT-IR) spectroscopy. HR-TEM showed that the average size of the synthesized N-CDs was approximately 9 nm and the interlayer distance was 0.21 nm, which was validated by XRD. The graphitic nature of the synthesized N-CDs were confirmed by Raman spectroscopy. XPS and FT-IR spectroscopy confirmed the doping of the nitrogen moiety over the synthesized CDs. The synthesized nitrogen doped CDs (N-CDs) were low toxicity and were used as a staining probe for fluorescence cell imaging.

Efficient synthesis of highly fluorescent nitrogen-doped carbon dots for cell imaging using unripe fruit extract of Prunus mume

Energy Technology Data Exchange (ETDEWEB)

Atchudan, Raji; Edison, Thomas Nesakumar Jebakumar Immanuel [School of Chemical Engineering, Yeungnam University, Gyeongsan 38541 (Korea, Republic of); Sethuraman, Mathur Gopalakrishnan, E-mail: mgsethu@gmail.com [Department of Chemistry, Gandhigram Rural Institute-Deemed University, Gandhigram 624 302, Tamilnadu (India); Lee, Yong Rok, E-mail: yrlee@yu.ac.kr [School of Chemical Engineering, Yeungnam University, Gyeongsan 38541 (Korea, Republic of)

2016-10-30

Graphical abstract: The green synthesis of highly fluorescent N-CDs was achieved using the extract of unripe P. mume fruit as a carbon precursor by a one-pot simple hydrothermal-carbonization method. The resulting N-CDs were used as a staining agent for the fluorescence imaging of MDA-MB-231 cells. Display Omitted - Highlights: • The green synthesis of highly fluorescent N-CDs using the extract of unripe P. mume. • The N-CDs were synthesized by one-pot hydrothermal-carbonization method. • This method of synthesis is a simple, cost effective and eco-friendly route. • N-CDs will be a good alternative for fluorescent dyes and SQDs for bio-applications. - Abstract: Highly fluorescent nitrogen-doped carbon dots (N-CDs) were synthesized using the extract of unripe Prunus mume (P. mume) fruit by a simple one step hydrothermal-carbonization method. The N-CDs were synthesized at different pH ranges, 2.3, 5, 7, and 9. The pH of the P. mume extract was adjusted using an aqueous ammonia solution (25%). The optical properties of N-CDs were examined by UV–vis and fluorescence spectroscopy. The N-CDs synthesized at pH 9 emitted high fluorescence intensity compared to other obtained N-CDs. The N-CDs synthesized at pH 9 was further characterized by high resolution transmission electron microscopy (HR-TEM), X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), and Fourier transform-infra red (FT-IR) spectroscopy. HR-TEM showed that the average size of the synthesized N-CDs was approximately 9 nm and the interlayer distance was 0.21 nm, which was validated by XRD. The graphitic nature of the synthesized N-CDs were confirmed by Raman spectroscopy. XPS and FT-IR spectroscopy confirmed the doping of the nitrogen moiety over the synthesized CDs. The synthesized nitrogen doped CDs (N-CDs) were low toxicity and were used as a staining probe for fluorescence cell imaging.

Chemical changes in non-reduced catalysts used for ammonia synthesis

International Nuclear Information System (INIS)

Peev, T.M.; Kyrova, Z.; Bojinova, A.I.

1980-01-01

Samples of non-reduced industrial catalysts CA-1 for ammonia synthesis were studied by using Moessbauer spectroscopy. The conditions of the normal storing of this catalyst were changed. After 6 months it was found that under the influence of moisture and air oxygen a considerable part of the magnetite was converted to α-Fe 2 O 3 , α-FeOOH and γ-FeOOH. (author)

High-throughput flow injection analysis mass spectroscopy with networked delivery of color-rendered results. 2. Three-dimensional spectral mapping of 96-well combinatorial chemistry racks.

Science.gov (United States)

Görlach, E; Richmond, R; Lewis, I

1998-08-01

For the last two years, the mass spectroscopy section of the Novartis Pharma Research Core Technology group has analyzed tens of thousands of multiple parallel synthesis samples from the Novartis Pharma Combinatorial Chemistry program, using an in-house developed automated high-throughput flow injection analysis electrospray ionization mass spectroscopy system. The electrospray spectra of these samples reflect the many structures present after the cleavage step from the solid support. The overall success of the sequential synthesis is mirrored in the purity of the expected end product, but the partial success of individual synthesis steps is evident in the impurities in the mass spectrum. However this latter reaction information, which is of considerable utility to the combinatorial chemist, is effectively hidden from view by the very large number of analyzed samples. This information is now revealed at the workbench of the combinatorial chemist by a novel three-dimensional display of each rack's complete mass spectral ion current using the in-house RackViewer Visual Basic application. Colorization of "forbidden loss" and "forbidden gas-adduct" zones, normalization to expected monoisotopic molecular weight, colorization of ionization intensity, and sorting by row or column were used in combination to highlight systematic patterns in the mass spectroscopy data.

Green synthesis of gold nanoparticles using plant extract: Mini-review

Directory of Open Access Journals (Sweden)

Reza Teimuri-mofrad

2017-01-01

Full Text Available In this review, we examine the greenest nanoparticles of zero-valent metals, metal oxides and metal salts, with emphasis on recent developments routes. Products from nature or those derived from natural products, such as extracts of several plants or parts of plants, tea, coffee, banana, simple amino acids, as well as wine, table sugar and glucose, have been used as reductants and as capping agents during the present synthesis method. Polyphenols found in plant material often play a key role in the processes mentioned here. The techniques involved are generally one-pot processes, environmentally friendly and simple. Green synthesis of gold nanoparticles using several extracts and spices extracts was conducted, in which aqueous extracts HAuCl4.3H2O reduce to Au° has establishing themselves in specific crystal phase. Synthesized nanoparticles were confirmed by the color change of auric chloride which is yellow. The growth of nanoparticles was monitored by the behavior of surface Plasmon using UV-Vis spectroscopy; also the pH was determined meanwhile. Moreover, this approach is not only of a green rapid synthesis kind and considered as a better alternative to chemical synthesis, but also found to be effective for large scale synthesis of gold nanoparticles.

Synthesis and characterization of novel silver nanoparticles using Chamaemelum nobile extract for antibacterial application

Science.gov (United States)

Erjaee, Hoda; Rajaian, Hamid; Nazifi, Saeed

2017-06-01

The present study reports green synthesis of silver nanoparticles (AgNPs) at room temperature using aqueous Chamaemelum nobile extract for the first time. The effect of silver nitrate concentration, quantity of the plant extract and the reaction time on particle size was optimized and studied by UV-Vis spectroscopy and dynamic light scattering. The appearance of brownish color with λ max of 422 nm confirmed the formation of AgNPs. Synthesized nanoparticles were further characterized by Fourier transform infrared spectroscopy, x-ray diffraction and transmission electron microscopy. In addition, antimicrobial activity of the AgNPs against Escherichia coli, Salmonella typhimurium, Staphylococcus aureus and Bacillus subtilis was evaluated based on the inhibition zone using the disc-diffusion assay and measurement of minimal inhibition concentration and minimal bactericidal concentration by standard microdilution method. In conclusion, synthesis of nanoparticle with aqueous Chamaemelum nobile extract is simple, rapid, environmentally benign and inexpensive. Moreover, these synthesized nanoparticles exhibit significant antibacterial activity.

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.

Piper betle-mediated green synthesis of biocompatible gold nanoparticles

Science.gov (United States)

Punuri, Jayasekhar Babu; Sharma, Pragya; Sibyala, Saranya; Tamuli, Ranjan; Bora, Utpal

2012-08-01

Here, we report the novel use of the ethonolic leaf extract of Piper betle for gold nanoparticle (AuNP) synthesis. The successful formation of AuNPs was confirmed by UV-visible spectroscopy, and different parameters such as leaf extract concentration (2%), gold salt concentration (0.5 mM), and time (18 s) were optimized. The synthesized AuNPs were characterized with different biophysical techniques such as transmission electron microscopy (TEM), Fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD), and energy-dispersive X-ray spectroscopy (EDX). TEM experiments showed that nanoparticles were of various shapes and sizes ranging from 10 to 35 nm. FT-IR spectroscopy revealed that AuNPs were functionalized with biomolecules that have primary amine group -NH2, carbonyl group, -OH groups, and other stabilizing functional groups. EDX showed the presence of the elements on the surface of the AuNPs. FT-IR and EDX together confirmed the presence of biomolecules bounded on the AuNPs. Cytotoxicity of the AuNPs was tested on HeLa and MCF-7 cancer cell lines, and they were found to be nontoxic, indicating their biocompatibility. Thus, synthesized AuNPs have potential for use in various biomedical applications.

Synthesis of LaNiO3 perovskite type by chelating precursor method using EDTA: optimization of chelating content

International Nuclear Information System (INIS)

Santos, Jose Carlos dos; Pedrosa, Anne Michelle Garrido; Mesquita, Maria Eliane; Souza, Marcelo Jose Barros de

2011-01-01

The perovskites are strategic materials due their catalytic, electronic and magnetic properties. These properties are influenced by the calcination and synthesis conditions. In this work was carried out the synthesis of LaNiO 3 perovskite type by chelating precursor method using EDTA and also was studied the optimization of the EDTA content in the synthesis. The synthesized materials were characterized by X-ray diffraction (XRD), thermal gravimetric analysis (TG) and Infrared Spectroscopy (FTIR). In the optimization of the EDTA content the lowest ratio of metal / EDTA used was 1.0 / 0.1, where it was possible to obtain monophasic perovskite. (author)

Viscoelastic wormlike micelles formed by ionic liquid-type surfactant [C16imC8]Br towards template-assisted synthesis of CdS quantum dots.

Science.gov (United States)

Hu, Yimin; Han, Jie; Ge, Lingling; Guo, Rong

2018-01-31

In this paper, viscoelastic wormlike micelles consisting of cationic liquid-type surfactant, 1-hexadecyl-3-octyl imidazolium bromide ([C 16 imC 8 ]Br), water and different additives were utilized for the synthesis of CdS quantum dots. First, the influence of different additives, such as [Cd(NH 3 ) 6 ]Cl 2 and ethanethioamid (precursors for the synthesis of CdS quantum dots), and temperature on the viscoelasticity of the [C 16 imC 8 ]Br aqueous solution was studied by dynamic and steady rheology. Furthermore, the synthesized CdS quantum dots and their photoluminescence properties were characterized by transmission electron microscopy (TEM), UV-Vis absorption spectroscopy, X-ray diffraction (XRD) and energy-dispersive X-ray spectroscopy (EDX). In the end, the mechanism for the synthesis of CdS quantum dots in [C 16 imC 8 ]Br wormlike micelles is proposed.

Aerosol assisted synthesis of hierarchical tin–carbon composites and their application as lithium battery anode materials

KAUST Repository

Guo, Juchen

2013-01-01

We report a method for synthesizing hierarchically structured tin-carbon (Sn-C) composites via aerosol spray pyrolysis. In this method, an aqueous precursor solution containing tin(ii) chloride and sucrose is atomized, and the resultant aerosol droplets carried by an inert gas are pyrolyzed in a high-temperature tubular furnace. Owing to the unique combination of high reaction temperature and short reaction time, this method is able to achieve a hetero-structure in which small Sn particles (15 nm) are uniformly embedded in a secondary carbon particle. This procedure allows the size and size distribution of the primary Sn particles to be tuned, as well as control over the size of the secondary carbon particles by addition of polymeric surfactant in the precursor solution. When evaluated as anode materials for lithium-ion batteries, the resultant Sn-C composites demonstrate attractive electrochemical performance in terms of overall capacity, electrochemical stability, and coulombic efficiency. © 2013 The Royal Society of Chemistry.

Semiconductor-to-metallic flipping in a ZnFe{sub 2}O{sub 4}–graphene based smart nano-system: Temperature/microwave magneto-dielectric spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Ameer, Shahid, E-mail: shahidameer@scme.nust.edu.pk [School of Chemical and Materials Engineering (SCME), National University of Sciences and Technology (NUST), H-12, Islamabad (Pakistan); Gul, Iftikhar Hussain [School of Chemical and Materials Engineering (SCME), National University of Sciences and Technology (NUST), H-12, Islamabad (Pakistan); Mahmood, Nasir [Department of Materials Science and Engineering, College of Engineering, Peking University, Beijing 100871 (China); Mujahid, Muhammad [School of Chemical and Materials Engineering (SCME), National University of Sciences and Technology (NUST), H-12, Islamabad (Pakistan)

2015-01-15

Zn-(FeO{sub 2}){sub 2}–graphene smart nano-composites were synthesized using a novel modified solvothermal synthesis with different percentages of graphene. The structure of the nanocomposite was confirmed through X-ray diffraction, micro-Raman scattering spectroscopy, Ultraviolet–Visible spectroscopy, and Fourier transform infrared spectroscopy. The structural growth and morphological aspects were analyzed using scanning/transmission electron microscopy, revealing marvelous micro-structural features of the assembled nano-system resembling a maple leaf. To determine the composition, energy dispersive spectroscopy and X-ray photoelectron spectroscopy were used. Microwave magneto-dielectric spectroscopy revealed the improved dielectric properties of the nano-composite compared to those of the parent functional nanocrystals. Temperature gradient dielectric spectroscopy was used over the spectral range from 100 Hz to 5 MHz to reveal the phenomenological effect that the nanosystem flips from its usual semiconductor nature to a metallic nature with sensing temperature. Electrical conductivity and dielectric analysis indicated that the dielectric loss and the dielectric permittivity increased at room temperature. This extraordinary switching capability of the functionalized graphene nanosystem opens up a new dimension for engineering advanced and efficient smart composite materials. - Graphical abstract: Display Omitted - Highlights: • Zn-(FeO{sub 2}){sub 2}–graphene smart nano-composites were synthesized using a novel modified solvothermal synthesis. • The synthesized nano-system exhibits marvelous leaf like microstructure. • These nano-composites show improved magneto dielectric response. • This engineered smart nano-system shows phenomenological flipping from semiconductor like nature to metallic behavior.

Synthesis of interlocked molecules by olefin metathesis

Science.gov (United States)

Clark, Paul Gregory

polyammonium scaffold. Diolefin polyether fragments were coordinated and "clipped" around the ammonium sites within the polymer backbone using ring-closing olefin metathesis, giving the molecular "charm bracelet". Confirmation of the interlocked nature of the product was achieved via 1H NMR spectroscopy and two-dimensional diffusion ordered NMR spectroscopy. A simple strategy for a one-pot, multi-component synthesis of polyrotaxanes using acyclic diene metathesis polymerization was developed. The polyrotaxanes were characterized by traditional 1H NMR spectroscopy as well as size exclusion chromatography, and the interlocked topology was confirmed using two-dimension diffusion-ordered NMR spectroscopy. The dynamic, self-correcting nature of the ADMET polymerization was also explored through the equilibration of a capped polyammonium polymer in the presence of dibenzo-24-crown-8 ether and olefin metathesis catalysts. The efficiency and ease with which these mechanically interlocked macromolecules can be assembled should facilitate rapid modulation to achieve versatile polyrotaxane architectures. Flexible, switchable [c2]daisy-chain dimers (DCDs) were synthesized, where the macromer ammonium binding site was adjacent to the crown-type recognition structure and separated from the cap by an alkyl chain. A DCD of this topology is expected to have an extended structure in the bound conformation (when the ammonium was coordinated to the crown). Several different macromer candidates were designed to allow access to DCDs with flexible alkyl chains between the ammonium binding site and the cap, and a number of synthetic routes were explored in an effort to access these challenging materials. While the first generation DCD structure proved to be unstable due to a labile ester linkage, work is continuing toward the development of several cap structures in an effort to replace the ester linkage with an ether linkage, which, in the second generation model systems, has proven much more stable

Synthesis and Ligand-Exchange Reactions of a Tri-Tungsten Cluster with Applications in Biomedical Imaging

Science.gov (United States)

Noey, Elizabeth; Curtis, Jeff C.; Tam, Sylvia; Pham, David M.; Jones, Ella F.

2011-01-01

In this experiment students are exposed to concepts in inorganic synthesis and various spectroscopies as applied to a tri-tungsten cluster with applications in biomedical imaging. The tungsten-acetate cluster, Na[W[superscript 3](mu-O)[subscript 2](CH[superscript 3]COO)[superscript 9

Green synthesis of gold nanoparticles using Stevia rebaudiana leaf extracts: Characterization and their stability.

Science.gov (United States)

Sadeghi, Babak; Mohammadzadeh, M; Babakhani, B

2015-07-01

Various methods invented and developed for the synthesis of gold nanoparticles that increases daily consumed. According to this method, including potential environmental pollution problems and the complexity of the synthesis, in this study, the feasibility of using the leaves extract of Stevia rebaudiana (SR) for the reduction of gold ions to nanoparticles form have been studied. Stevia leaves were used to prepare the aqueous extract for this study. Gold nanoparticles were characterized with different techniques such as UV-vis spectroscopy, FT-IR spectroscopy, X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). Transmission electron microscopy experiments showed that these nanoparticles are spherical and uniformly distributed and its size is from 5 to 20 nm. FT-IR spectroscopy revealed that gold nanoparticles were functionalized with biomolecules that have primary amine group (NH2), carbonyl group, OH groups and other stabilizing functional groups. X-ray diffraction pattern showed high purity and face centered cubic structure of gold nanoparticles with size of 17 nm. The scanning electron microscopy (SEM) implies the right of forming gold nanoparticles. The results, confirm that gold nanoparticles have synthesized by the leaves extract of S. rebaudiana (SR). Copyright © 2015 Elsevier B.V. All rights reserved.

Single step vacuum-free and hydrogen-free synthesis of graphene

Directory of Open Access Journals (Sweden)

Christian Orellana

2017-08-01

Full Text Available We report a modified method to grow graphene in a single-step process. It is based on chemical vapor deposition and considers the use of methane under extremely adverse synthesis conditions, namely in an open chamber without requiring the addition of gaseous hydrogen in any of the synthesis stages. The synthesis occurs between two parallel Cu plates, heated up via electromagnetic induction. The inductive heating yields a strong thermal gradient between the catalytic substrates and the surrounding environment, promoting the enrichment of hydrogen generated as fragments of the methane molecules within the volume confined by the Cu foils. This induced density gradient is due to thermo-diffusion, also known as the Soret effect. Hydrogen and other low mass molecular fractions produced during the process inhibit oxidative effects and simultaneously reduce the native oxide on the Cu surface. As a result, high quality graphene is obtained on the inner surfaces of the Cu sheets as confirmed by Raman spectroscopy.

Synthesis of nanosized powders of stabilized zirconia

International Nuclear Information System (INIS)

Takodoro, Sandra Kiyoko

2000-01-01

Zirconia solid solutions containing 3 mol % Yttria or 12 mol % ceria have been prepared by the coprecipitation technique followed by azeotropic distillation. The aim of this work is the synthesis of tetragonal zirconia polycrystals nanosized powders that sinter at comparatively lower temperatures attaining high densification, and without using any milling procedure. The main results show that: 1- the dopant cation has a strong influence on the crystallization behavior of the precipitates; 2- the used techniques allowed for obtaining high values of specific surface area (∼130 m 2 .g -1 ); 3- the optimization of the synthesis and processing parameters are responsible for obtaining high densification (≥97% of the theoretical value), at lower temperatures (∼1200 deg C) with average grain sizes lower than 500 nm; 4- impedance spectroscopy results show a strong correlation between the electrical resistivity and the microstructure of sintered ceramics.(author)

A self-propagation high-temperature synthesis and annealing route to synthesis of wave-like boron nitride nanotubes

Energy Technology Data Exchange (ETDEWEB)

Wang, Jilin; Zhang, Laiping [School of Materials Science and Engineering, Wuhan Institute of Technology, Wuhan, Hubei, 430073 (China); Gu, Yunle, E-mail: ncm@mail.wit.edu.cn [School of Materials Science and Engineering, Wuhan Institute of Technology, Wuhan, Hubei, 430073 (China); Pan, Xinye; Zhao, Guowei; Zhang, Zhanhui [School of Materials Science and Engineering, Wuhan Institute of Technology, Wuhan, Hubei, 430073 (China)

2013-03-15

Highlights: ► Large quantities of wave-like BN nanotubes were synthesized by SHS-annealing method. ► The catalytic boron-containing porous precursor was produced by self-propagation high-temperature synthesis method. ► Three growth models were proposed to explain the growth mechanism of the wave-like BN nanotubes. - Abstract: Large quantities of boron nitride (BN) nanotubes were synthesized by annealing a catalytic boron-containing porous precursor in flowing NH{sub 3} gas at 1180 °C. The porous precursor was prepared by self-propagation high-temperature synthesis (SHS) method at 800 °C using Mg, B{sub 2}O{sub 3} and amorphous boron powder (α-B) as the starting materials. The porous precursor played an important role in large quantities synthesis of BN nanotubes. The as-synthesized product was characterized by X-ray diffractometer (XRD), Fourier transform infrared spectrometer (FTIR), Raman, Scanning electron microscopy (SEM), X-ray energy dispersive spectroscopy (EDS), Transmission electron microscopy (TEM) and High-resolution transmission electron microscopy (HRTEM). Characterization results indicated that the BN nanotubes displayed wave-like inner structures with diameters in the range of 50–300 nm and average lengths of more than 10 μm. The possible growth mechanism of the BN nanotubes was also discussed.

Synthesis of pure monetite by heterogeneous acid-base reaction

OpenAIRE

Luis Carlos Moreno Aldana; Davier Olarte Cárdenas; Edgar Delgado Mejía

2017-01-01

Five variations of the monetite (M) synthesis were evaluated modifying the stirring, the phosphoric acid addition rate, the homogeneity and the drying temperature. Products were assessed by means of XRD, FTIR, SEM-EDS analysis and chemical assay of Ca/P (calcium by titration with potassium permanganate and phosphorus by colorimetric assessment of the molybdenum blue complex). X-ray diffraction, infrared spectroscopy and Ca/P ratio indicate that the synthesized phosphate corresponds to pure mo...

Green synthesis of silver nanoparticles using Alternanthera dentata leaf extract at room temperature and their antimicrobial activity.

Science.gov (United States)

Kumar, Deenadayalan Ashok; Palanichamy, V; Roopan, Selvaraj Mohana

2014-06-05

A green rapid biogenic synthesis of silver nanoparticles AgNPs using Alternanthera dentata (A. dentata) aqueous extract was demonstrated in this present study. The formation of silver nanoparticles was confirmed by Surface Plasmon Resonance (SPR) at 430nm using UV-visible spectrophotometer. The reduction of silver ions to silver nanoparticles by A. dentata extract was completed within 10min. Synthesized nanoparticles were characterized using UV-visible spectroscopy; Fourier transformed infrared spectroscopy (FT-IR), X-ray diffraction (XRD), scanning electron microscopy and transmission electron microscopy (TEM). The extracellular silver nanoparticles synthesis by aqueous leaf extract demonstrates rapid, simple and inexpensive method comparable to chemical and microbial methods. The colloidal solution of silver nanoparticles were found to exhibit antibacterial activity against Escherichia coli, Pseudomonas aeruginosa, Klebsiella pneumonia and, Enterococcus faecalis. Copyright © 2014 Elsevier B.V. All rights reserved.

Pseudo template synthesis of poly (1-naphthylamine): effect of environment on nanostructured morphology

International Nuclear Information System (INIS)

Riaz, Ufana; Ahmad, Sharif; Ashraf, S. M.

2008-01-01

A template free approach was adopted to explore the effect of polymerization environment on the synthesis of nanostructured poly (1-naphthylamine) (PNA) using cupric chloride as oxidant and methyl alcohol as medium. The polymerization environment was varied by carrying out the synthesis in the presence of nitrogen and oxygen. The morphology of the synthesized nanostructured PNA was investigated using scanning electron microscopy (SEM), transmission electron microscopy (TEM), UV-vis and FT-IR spectroscopies. PNA nanorods of sizes varying between 50-100 nm were obtained in presence of nitrogen while in presence of oxygen, it formed aggregated globular particles of sizes varying between 80-100 nm. The results provide valuable information on controlling the synthesis of one-dimensional nanostructured conducting polymers that exhibit superior processibility as compared to the conventional conducting polymers.

Soft x-ray spectroscopy for probing electronic and chemical states of battery materials

International Nuclear Information System (INIS)

Yang Wanli; Qiao Ruimin

2016-01-01

The formidable challenge of developing high-performance battery system stems from the complication of battery operations, both mechanically and electronically. In the electrodes and at the electrode–electrolyte interfaces, chemical reactions take place with evolving electron states. In addition to the extensive studies of material synthesis, electrochemical, structural, and mechanical properties, soft x-ray spectroscopy provides unique opportunities for revealing the critical electron states in batteries. This review discusses some of the recent soft x-ray spectroscopic results on battery binder, transition-metal based positive electrodes, and the solid-electrolyte-interphase. By virtue of soft x-ray’s sensitivity to electron states, the electronic property, the redox during electrochemical operations, and the chemical species of the interphases could be fingerprinted by soft x-ray spectroscopy. Understanding and innovating battery technologies need a multimodal approach, and soft x-ray spectroscopy is one of the incisive tools to probe the chemical and physical evolutions in batteries. (topical review)

The Application of Moessbauer Emission Spectroscopy to Industrial Cobalt Based Fischer-Tropsch Catalysts

International Nuclear Information System (INIS)

Loosdrecht, J. van de; Berge, P. J. van; Craje, M. W. J.; Kraan, A. M. van der

2002-01-01

The application of Moessbauer emission spectroscopy to study cobalt based Fischer-Tropsch catalysts for the gas-to-liquids process was investigated. It was shown that Moessbauer emission spectroscopy could be used to study the oxidation of cobalt as a deactivation mechanism of high loading cobalt based Fischer-Tropsch catalysts. Oxidation was observed under conditions that are in contradiction with the bulk cobalt phase thermodynamics. This can be explained by oxidation of small cobalt crystallites or by surface oxidation. The formation of re-reducible Co 3+ species was observed as well as the formation of irreducible Co 3+ and Co 2+ species that interact strongly with the alumina support. The formation of the different cobalt species depends on the oxidation conditions. Iron was used as a probe nuclide to investigate the cobalt catalyst preparation procedure. A high-pressure Moessbauer emission spectroscopy cell was designed and constructed, which creates the opportunity to study cobalt based Fischer-Tropsch catalysts under realistic synthesis conditions.

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.

Auger electron spectroscopy, ionization loss spectroscopy, appearance potential spectroscopy

International Nuclear Information System (INIS)

Riwan, R.

1973-01-01

The spectroscopy of surfaces using an incident electron beam is studied. The fundamental mechanisms are discussed together with the parameters involved in Auger emission: excitation of the atom, de-excitation by electron emission, and the migration of electrons towards the surface and their ejection. Some examples of applications are given (surface structures, metallurgy, chemical information). Two new techniques for analyzing surfaces are studied: ionization spectroscopy, and appearance potential spectroscopy [fr

Phosphine-free synthesis and characterization of type-II ZnSe/CdS core-shell quantum dots

Science.gov (United States)

Ghasemzadeh, Roghayyeh; Armanmehr, Mohammad Hasan; Abedi, Mohammad; Fateh, Davood Sadeghi; Bahreini, Zaker

2018-01-01

A phosphine-free route for synthesis of type-II ZnSe/CdS core-shell quantum dots, using green, low cost and environmentally friendly reagents and phosphine-free solvents such as 1-octadecene (ODE) and liquid paraffin has been reported. Hot-injection technique has been used for the synthesis of ZnSe core quantum dots. The CdS shell quantum dots prepared by reaction of CdO precursor and S powder in 1-octadecene (ODE). The ZnSe/CdS core-shell quantum dots were synthesized via successive ion layer adsorption and reaction (SILAR) technique. The characterization of produced quantum dots were performed by absorption and fluorescence spectroscopy, X-ray diffraction (XRD) and energy dispersive X-ray spectroscopy (EDX) and transmission electron microscopy (TEM). The results showed the formation of type-II ZnSe/CdS core-shell quantum dots with FWHM 32 nm and uniform size distribution.

Synthesis of water soluble glycine capped silver nanoparticles and their surface selective interaction

International Nuclear Information System (INIS)

Agasti, Nityananda; Singh, Vinay K.; Kaushik, N.K.

2015-01-01

Highlights: • Synthesis of water soluble silver nanoparticles at ambient reaction conditions. • Glycine as stabilizing agent for silver nanoparticles. • Surface selective interaction of glycine with silver nanoparticles. • Glycine concentration influences crystalinity and optical property of silver nanoparticles. - Abstract: Synthesis of biocompatible metal nanoparticles has been an area of significant interest because of their wide range of applications. In the present study, we have successfully synthesized water soluble silver nanoparticles assisted by small amino acid glycine. The method is primarily based on reduction of AgNO 3 with NaBH 4 in aqueous solution under atmospheric air in the presence of glycine. UV–vis spectroscopy, transmission electron microscopy (TEM), X–ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, thermogravimetry (TG) and differential thermal analysis (DTA) techniques used for characterization of resulting silver nanoparticles demonstrated that, glycine is an effective capping agent to stabilize silver nanoparticles. Surface selective interaction of glycine on (1 1 1) face of silver nanoparticles has been investigated. The optical property and crystalline behavior of silver nanoparticles were found to be sensitive to concentration of glycine. X–ray diffraction studies ascertained the phase specific interaction of glycine on silver nanoparticles. Silver nanoparticles synthesized were of diameter 60 nm. We thus demonstrated an efficient synthetic method for synthesis of water soluble silver nanoparticles capped by amino acid under mild reaction conditions with excellent reproducibility

Collaborative Student Laboratory Exercise Using FT-IR Spectroscopy for the Kinetics Study of a Biotin Analogue

Science.gov (United States)

Leong, Jhaque; Ackroyd, Nathan C.; Ho, Karen

2014-01-01

The synthesis of N-methoxycarbonyl-2-imidazolidone, an analogue of biotin, was conducted by organic chemistry students and confirmed using FT-IR and H NMR. Spectroscopy students used FT-IR to measure the rate of hydrolysis of the product and determined the rate constant for the reaction using the integrated rate law. From the magnitude of the rate…

Synthesis and Characterization of Fluoro- and Chlorobimetallic Alkoxides as Precursors for Luminescent Metal Oxide Materials via Sol-Gel Technique

Institute of Scientific and Technical Information of China (English)

ATHAR, Taimur; SEOK, Sang II; KWON, Jeong Oh

2007-01-01

Heterobimetallic alkoxides are broadly recognized as versatile precursors for luminescence materials, and efforts are being made to develop novel routes by applying the concept of geometrical molecular design, for their synthesis and to design a single source precursor suited to photoluminescent materials. Novel and new series of bimetallic alkoxides has been prepared by metathesis route. They exhibit a lower sensitivity towards hydrolysis and so they are easier to handle as compared to other alkoxides. All the compounds were characterized by elemental analysis, FT-IR and multinuclear NMR spectroscopies. FT-IR revealed that the molecular structure of these metal spectroscopy provided useful information about chemical shifts for better understanding the likely structure based on interactions with their coordinate metals. The mass spectra show similar types of fragmentation pattern.SEM-EDS analyses showed consistency with the formulation. XRD patterns show an enhanced homogeneity at high temperature. TGA measurements show that thermal decomposition occured in steps that depended entirely on the chemical compositions and the synthesis routes. SEM observation reveals that the morphology and particle size strongly depend on synthesis routes for their precursors.

Synthesis of β-tricalcium phosphate.

Science.gov (United States)

Chaair, H; Labjar, H; Britel, O

2017-09-01

Ceramics play a key role in several biomedical applications. One of them is bone grafting, which is used for treating bone defects caused by injuries or osteoporosis. Calcium-phosphate based ceramic are preferred as bone graft biomaterials in hard tissue surgery because their chemical composition is close to the composition of human bone. They also have a marked bioresorbability and bioactivity. In this work, we have developed methods for synthesis of β-tricalcium phosphate apatite (β-TCP). These products were characterized by different techniques such as X-ray diffraction, infrared spectroscopy, scanning electron microscopy and chemical analysis. Copyright © 2017 Elsevier Masson SAS. All rights reserved.

Synthesis and stereochemical investigation of potential saturated heterocyclic drugs Pt. 1

International Nuclear Information System (INIS)

Bernath, G.

1982-01-01

Studies of partially and fully saturated heterocyclic compounds with condensed skeleton containing two heteroatoms are presented. The synthesis, stereochemical and conformation analyses aimed at the synthesis of potential drugs. Dihydro- and tetrahydro-1,3-oxazines were prepared from alicyclic 1,3-amino-alcohols by ring closure with aldehydes or imide esters. 1,3-oxazine-4-one derivatives were prepared by reacting alicyclic cis- and trans-2-hydroxy-1-carboxamides with aliphatic or aromatic aldehides. The conformations of the compounds prepared were determined by means of NMR spectroscopy. The main results of the determination of the steric structure of some representatives of the above described families of compounds by means of X-ray diffraction analysis are also presented. (author)

A facile and fast approach for the synthesis of doped nanoparticles using a microfluidic device

International Nuclear Information System (INIS)

Singh, Akanksha; Limaye, Mukta; Singh, Shashi; Kulkarni, Sulabha; Lalla, Niranjan Prasad; Malek, Chantal Khan

2008-01-01

The microfluidic approach emerges as a new and promising technology for the synthesis of nanomaterials. A microreactor allows a variety of reaction conditions to be quickly scanned without consuming large amounts of raw material. In this study, we investigated the synthesis of water soluble 1-thioglycerol-capped Mn-doped ZnS nanocrystalline semiconductor nanoparticles (TG-capped ZnS:Mn) via a microfluidic approach. This is the first report for the successful doping of Mn in a ZnS semiconductor at room temperature as well as at 80 deg. C using a microreactor. Transmission electron microscopy and x-ray diffraction analysis show that the average particle size of Mn-doped ZnS nanoparticles is ∼3.0 nm with a zinc-blende structure. Photoluminescence, x-ray photoelectron spectroscopy, atomic absorption spectroscopy and electron paramagnetic resonance studies were carried out to confirm that the Mn 2+ dopants are present in the ZnS nanoparticles

Synthesis of Boron Nano wires, Nano tubes, and Nano sheets

International Nuclear Information System (INIS)

Patel, R.B.; Chou, T.; Iqbal, Z.

2014-01-01

The synthesis of boron nano wires, nano tubes, and nano sheets using a thermal vapor deposition process is reported. This work confirms previous research and provides a new method capable of synthesizing boron nano materials. The materials were made by using various combinations of MgB 2 , Mg(BH 4 ) 2 , MCM-41, NiB, and Fe wire. Unlike previously reported methods, a nanoparticle catalyst and a silicate substrate are not required for synthesis. Two types of boron nano wires, boron nano tubes, and boron nano sheets were made. Their morphology and chemical composition were determined through the use of scanning electron microscopy, transmission electron microscopy, and electron energy loss spectroscopy. These boron-based materials have potential for electronic and hydrogen storage applications.

Microwave-Assisted Synthesis of Alumina Nanoparticles Using Some Plants Extracts

Directory of Open Access Journals (Sweden)

Meisam Hasanpoor

2017-01-01

Full Text Available In present study we used five green plants for microwave assisted synthesis of Alumina nanoparticles from Aluminum nitrate. Structural characterization was studied using x-ray diffraction that showed semi- crystalline and possibly, amorphous structure. Fourier infrared spectroscopy was used to determine Al-O bond and functional groups responsible for synthesis of nanoparticles. FTIR confirmed existence of Al-O band and bio-functional groups, originated from plant extract. Morphology and size of nanoparticles were investigated using scanning electron microscopy, transmission electron microscopy and atomic force microscopy techniques. It was observed that nanoparticles have near-spherical shape. Average size of clusters of nanoparticles varied with different routes from of 60 nm to 300 nm. AFM images showed that Individual nanoparticles were less than 10 nm.

Synthesis of lucifensin by native chemical ligation and characteristics of its isomer having different disulfide bridge pattern

Czech Academy of Sciences Publication Activity Database

Stanchev, Stancho; Zawada, Zbigniew; Monincová, Lenka; Bednárová, Lucie; Slaninová, Jiřina; Fučík, Vladimír; Čeřovský, Václav

2014-01-01

Roč. 20, č. 9 (2014), s. 725-735 ISSN 1075-2617 Institutional support: RVO:61388963 Keywords : lucifensin * native chemical ligation * solid-phase peptide synthesis * antimicrobial activity * CD spectroscopy * DTT reduction Subject RIV: CE - Biochemistry Impact factor: 1.546, year: 2014

Spectroscopy

CERN Document Server

Walker, S

1976-01-01

The three volumes of Spectroscopy constitute the one comprehensive text available on the principles, practice and applications of spectroscopy. By giving full accounts of those spectroscopic techniques only recently introduced into student courses - such as Mössbauer spectroscopy and photoelectron spectroscopy - in addition to those techniques long recognised as being essential in chemistry teaching - sucha as e.s.r. and infrared spectroscopy - the book caters for the complete requirements of undergraduate students and at the same time provides a sound introduction to special topics for graduate students.

Synthesis of diamondlike carbon particles in/on a water substrate by laser irradiation

International Nuclear Information System (INIS)

Hidai, Hirofumi; Tokura, Hitoshi

2005-01-01

We proposed two-particle synthesis techniques using a liquid as a substrate. First, utilizing liquid instead of solid substrates, particle synthesis is expected on the liquid surface. Particles sink into the liquid before the particles grow into film, because of liquid fluidity. Second, the excitation of a gas dissolved in water was also attempted. An ArF excimer laser beam was focused in a chamber. The 60% volume of the chamber was filled with water, in which methane was dissolved and the remaining space of the chamber was filled with methane gas. As a result, diamondlike carbon particles could be synthesized in water. The particles synthesized from methane in the gas phase were 50-200 nm in diameter, and the particles synthesized from methane dissolved in water were 200-700 nm in diameter, and no structural differences were observed between the particles of two different diameters. Energy-dispersive spectroscopy, Raman spectroscopy analysis, and high-resolution transmission electron microscopy observations revealed that particles contained a diamondlike carbon component and that graphite was attached to them. These particles were harder than graphite particles

Green chemistry synthesis of nano-cuprous oxide.

Science.gov (United States)

Ceja-Romero, L R; Ortega-Arroyo, L; Ortega Rueda de León, J M; López-Andrade, X; Narayanan, J; Aguilar-Méndez, M A; Castaño, V M

2016-04-01

Green chemistry and a central composite design, to evaluate the effect of reducing agent, temperature and pH of the reaction, were employed to produce controlled cuprous oxide (Cu2O) nanoparticles. Response surface method of the ultraviolet-visible spectroscopy is allowed to determine the most relevant factors for the size distribution of the nanoCu2O. X-ray diffraction reflections correspond to a cubic structure, with sizes from 31.9 to 104.3 nm. High-resolution transmission electron microscopy reveals that the different shapes depend strongly on the conditions of the green synthesis.

Synthesis and optical spectroscopy of (hetero)-nanocrystals: An exciting interplay between Chemistry and Physics

NARCIS (Netherlands)

Groeneveld, E.

2012-01-01

This thesis describes the synthesis and study of the optical properties of various colloidal semiconductor (hetero)nanocrystals ((H)NCs). Before the experimental results are discussed in detail, the essential theoretical background on the chemical and physical aspects of this work is provided in

Electron spectroscopy

International Nuclear Information System (INIS)

Hegde, M.S.

1979-01-01

An introduction to the various techniques in electron spectroscopy is presented. These techniques include: (1) UV Photoelectron spectroscopy, (2) X-ray Photoelectron spectroscopy, (3) Auger electron spectroscopy, (4) Electron energy loss spectroscopy, (5) Penning ionization spectroscopy and (6) Ion neutralization spectroscopy. The radiations used in each technique, the basis of the technique and the special information obtained in structure determination in atoms and molecules by each technique are summarised. (A.K.)

Solvent-Free Synthesis of Quaternary Metal Sulfide Nanoparticles Derived from Thiourea

KAUST Repository

Bhunia, Manas Kumar

2017-08-09

The synthesis of metal sulfide (MS) materials with sizes in the sub-10 nm regime often requires capping agents with long hydrocarbon chains that affect their structures and properties. Herein, this study presents a molten-state synthesis method for a series of transition-MS nanoparticles using thiourea as a reactive precursor without capping agents. This study also reports the synthesis of MS with single metals (Fe, Co, Ni, Cu, and Zn) and quaternary CuGa2In3S8 using the same synthesis protocol. Thiourea first melts to form a molten-state condition to serve as the reaction medium at a relatively low temperature (<200 °C), followed by its thermal decomposition to induce a reaction with the metal precursor to form different MS. This synthesis protocol, owing to its dynamic characteristics, involves the formation of a variety of organic carbon nitride polymeric complexes around the MS particles. Dynamic nuclear polarization surface-enhanced nuclear magnetic resonance spectroscopy is effective to identify the polymeric compositions and structures as well as their interactions with the MS. These results provided thorough structural descriptions of the MS nanoparticles surrounded by the carbon nitride species derived from thiourea, which may find various applications, including photocatalytic water splitting.

Characterization of Colloidal Quantum Dot Ligand Exchange by X-ray Photoelectron Spectroscopy

Science.gov (United States)

Atewologun, Ayomide; Ge, Wangyao; Stiff-Roberts, Adrienne D.

2013-05-01

Colloidal quantum dots (CQDs) are chemically synthesized semiconductor nanoparticles with size-dependent wavelength tunability. Chemical synthesis of CQDs involves the attachment of long organic surface ligands to prevent aggregation; however, these ligands also impede charge transport. Therefore, it is beneficial to exchange longer surface ligands for shorter ones for optoelectronic devices. Typical characterization techniques used to analyze surface ligand exchange include Fourier-transform infrared spectroscopy, x-ray diffraction, transmission electron microscopy, and nuclear magnetic resonance spectroscopy, yet these techniques do not provide a simultaneously direct, quantitative, and sensitive method for evaluating surface ligands on CQDs. In contrast, x-ray photoelectron spectroscopy (XPS) can provide nanoscale sensitivity for quantitative analysis of CQD surface ligand exchange. A unique aspect of this work is that a fingerprint is identified for shorter surface ligands by resolving the regional XPS spectrum corresponding to different types of carbon bonds. In addition, a deposition technique known as resonant infrared matrix-assisted pulsed laser evaporation is used to improve the CQD film uniformity such that stronger XPS signals are obtained, enabling more accurate analysis of the ligand exchange process.

Capillary electrophoresis-driven synthesis of water-soluble CdTe quantum dots in nanoliter scale

Science.gov (United States)

Nejdl, Lukas; Hynek, David; Adam, Vojtech; Vaculovicova, Marketa

2018-04-01

‘Green nanotechnology’ is a term used for the design of nanomaterials and processes that reduce or eliminate the use and/or generation of hazardous substances. In this paper, a capillary electrophoresis (CE)-driven synthesis of CdTe quantum dots (QDs) and their subsequent conjugation with a metal-binding protein metallothionein (isofom MT1) is reported. Even though the toxic materials (cadmium and potassium borohydride) were used for synthesis, the proposed method can be labeled as ‘environmentally friendly’ because the whole process (synthesis of QDs and MT1 conjugation) was carried out under mild conditions: ultra-low volume (nanoliter scale), relatively low temperature (50 °C), atmospheric pressure, and completed in a short time (under 90 s). Prepared QDs were also characterized by classical fluorescence spectroscopy and transmission electron microscopy. This study opens up new possibilities for the utilization of classical CE in the synthesis of nanoparticles and on-line labeling of biomolecules in the nanoliter scale in short period of time.

Synthesis of hydroxyapatite nanoparticles by Sonochemistry Method

International Nuclear Information System (INIS)

Cota, L.F.; Pereira, L.C.; Licona, K.P.M.; Lunz, J.N.; Ribeiro, A.A.; Morejon, L.

2014-01-01

bone implant substitute due to a great chemical similarity with the biological calcified tissues. Among synthesis conventional methods, the acoustic cavitation, induced by the sonochemical method, allows formation of nano powders. This work aimed to synthesize HAp nano-sized powders by using CaCl2. 2H2O and Na3PO4. 12H2O as precursors, along with pH and temperature control. The sonochemical method was accomplished by using different amplitudes (20%, 60% e 100%). To optimize the process, another synthesis at 60% ultrasound amplitude was performed, with the use of a peristaltic pump for dripping control. The HAp nano powders achieved were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), BET analysis, Scanning Electron Microscope/Field Emission Gun (SEM/FEG) combined with EDS. The results indicated the influence of the sonochemical methodology and drip controlling, on the chemical composition, crystallinity and nanoparticles morphology. (author)

Synthesis of hydroxyapatite nanoparticles by Sonochemistry Method

Energy Technology Data Exchange (ETDEWEB)

Cota, L.F.; Pereira, L.C. [Coordenacao dos Programas de Pos-Graduacao em Engenharia (COPPE/UFRJ), Rio de Janeiro, RJ (Brazil); Licona, K.P.M.; Lunz, J.N.; Ribeiro, A.A. [Instituto Nacional de Tecnologia (DPCM/INT), Rio de Janeiro, RJ (Brazil); Morejon, L. [Universidad de La Habana (UH/BIOMAT), Habana (Cuba). Centro de Biomateriales

2014-07-01

bone implant substitute due to a great chemical similarity with the biological calcified tissues. Among synthesis conventional methods, the acoustic cavitation, induced by the sonochemical method, allows formation of nano powders. This work aimed to synthesize HAp nano-sized powders by using CaCl2. 2H2O and Na3PO4. 12H2O as precursors, along with pH and temperature control. The sonochemical method was accomplished by using different amplitudes (20%, 60% e 100%). To optimize the process, another synthesis at 60% ultrasound amplitude was performed, with the use of a peristaltic pump for dripping control. The HAp nano powders achieved were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), BET analysis, Scanning Electron Microscope/Field Emission Gun (SEM/FEG) combined with EDS. The results indicated the influence of the sonochemical methodology and drip controlling, on the chemical composition, crystallinity and nanoparticles morphology. (author)

A Better Understanding of Protein Structure and Function by the Synthesis and Incorporation of Selenium- and Tellurium Containing Tryptophan Analogs

Energy Technology Data Exchange (ETDEWEB)

Helmey, Sherif Samir [Los Alamos National Lab. (LANL), Los Alamos, NM (United States). Bioscience Division; Belmont Univ., Nashville, TN (United States). Dept. of Chemistry and Physics; Rice, Ambrose Eugene [Los Alamos National Lab. (LANL), Los Alamos, NM (United States). Bioscience Division; Belmont Univ., Nashville, TN (United States). Dept. of Chemistry and Physics; Hatch, Duane Michael [Los Alamos National Lab. (LANL), Los Alamos, NM (United States). Bioscience Division; Belmont Univ., Nashville, TN (United States). Dept. of Chemistry and Physics; Silks, Louis A. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States). Bioscience Division; Marti-Arbona, Ricardo [Los Alamos National Lab. (LANL), Los Alamos, NM (United States). Bioscience Division

2016-08-17

Unnatural heavy metal-containing amino acid analogs have shown to be very important in the analysis of protein structure, using methods such as X-ray crystallography, mass spectroscopy, and NMR spectroscopy. Synthesis and incorporation of selenium-containing methionine analogs has already been shown in the literature however with some drawbacks due to toxicity to host organisms. Thus synthesis of heavy metal tryptophan analogs should prove to be more effective since the amino acid tryptophan is naturally less abundant in many proteins. For example, bioincorporation of β-seleno[3,2-b]pyrrolyl-L-alanine ([4,5]SeTrp) and β-selenolo[2,3-b]pyrrolyl-L-alanine ([6,7]SeTrp) has been shown in the following proteins without structural or catalytic perturbations: human annexin V, barstar, and dihydrofolate reductase. The reported synthesis of these Se-containing analogs is currently not efficient for commercial purposes. Thus a more efficient, concise, high-yield synthesis of selenotryptophan, as well as the corresponding, tellurotryptophan, will be necessary for wide spread use of these unnatural amino acid analogs. This research will highlight our progress towards a synthetic route of both [6,7]SeTrp and [6,7]TeTrp, which ultimately will be used to study the effect on the catalytic activity of Lignin Peroxidase (LiP).

Synthesis and optical properties of polyurethane foam modified with silver nanoparticles

International Nuclear Information System (INIS)

Apyari, V V; Volkov, P A; Dmitrienko, S G

2012-01-01

This paper for the first time describes peculiarities of synthesis of polyurethane foam modified with silver nanoparticles as a potential material for optical sensors in analytical chemistry. We found that the unique sorptional properties of polyurethane foam gave an opportunity to perform such a synthesis by two different approaches. The first one was based on sorption of previously synthesized in-solution nanoparticles by polyurethane foam, the second one consisted in preparation of nanoparticles directly in polyurethane foam matrix. This possibility is novel and interesting for practical use because the nanoparticles in polyurethane foam are capable of surface plasmon resonance. The influence of different factors during the synthesis was investigated and the optimal conditions were found. The samples prepared were characterized by diffuse reflectance spectroscopy and scanning electron microscopy. On the basis of the results obtained we first suggested that this material is attractive from the viewpoint of analytical chemistry as a convenient analytical form for determination of oxidants and reductants

The role of magnetite in Fischer-Tropsch synthesis

International Nuclear Information System (INIS)

Rao, K.R.P.M.; Huggins, F.E.; Mahajan, V.; Huffman, G.P.; Rao, V.U.S.

1994-01-01

Moessbauer spectroscopy studies of iron catalysts from a Fischer-Tropsch (FT) Pilot Plant run at different time-on-stream periods were carried out. Magnetite Fe 3 O 4 was found to be active for the water-gas-shift (WGS) reaction which accompanies the FT synthesis reaction over Fe-based catalysts. A correlation between the ratio of the occupancy of octahedral sites to the tetrahedral sites in magnetite to the WGS activity was found. Cation-deficient magnetite gave higher WGS activity as compared to the stoichiometric phase. (orig.)

Adsorption and Deactivation Characteristics of Cu/ZnO-Based Catalysts for Methanol Synthesis from Carbon Dioxide

Energy Technology Data Exchange (ETDEWEB)

Natesakhawat, Sittichai; Ohodnicki, Paul R; Howard, Bret H; Lekse, Jonathan W; Baltrus, John P; Matranga, Christopher

2013-07-09

The adsorption and deactivation characteristics of coprecipitated Cu/ZnO-based catalysts were examined and correlated to their performance in methanol synthesis from CO₂ hydrogenation. The addition of Ga₂O₃ and Y₂O₃ promoters is shown to increase the Cu surface area and CO₂/H₂ adsorption capacities of the catalysts and enhance methanol synthesis activity. Infrared studies showed that CO₂ adsorbs spontaneously on these catalysts at room temperature as both monoand bi-dentate carbonate species. These weakly bound species desorb completely from the catalyst surface by 200 °C while other carbonate species persist up to 500 °C. Characterization using N₂O decomposition, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and transmission electron microscopy (TEM) with energy-dispersive X-ray spectroscopy (EDX) analysis clearly indicated that Cu sintering is the main cause of catalyst deactivation. Ga and Y promotion improves the catalyst stability by suppressing the agglomeration of Cu and ZnO particles under pretreatment and reaction conditions.

Eco-friendly and green synthesis of silver nanoparticles using leaf extract of Strychnos potatorum Linn.F. and their bactericidal activities

OpenAIRE

Kagithoju, Srikanth; Godishala, Vikram; Nanna, Rama Swamy

2014-01-01

Inspired green synthesis of metallic nanoparticles is evolving as an important branch of nanotechnology. Traditionally these are manufactured by wet chemical methods which require toxic and flammable chemicals. We report for the first time an economic and eco-friendly green synthesis of silver nanoparticles using Strychnos potatorum aqueous leaf extract from 3 mM silver nitrate solution. Nanoparticles thus formed are confirmed and characterized by using UV–Vis absorption spectroscopy, SEM and...

Hyperbranched Polyethylenebased Macromolecular Architectures: Synthesis, Characterization, and Selfassembly

KAUST Repository

Al-Sulami, Ahlam

2018-05-01

"Chain walking” catalytic polymerization CWCP is a powerful tool for the one-pot synthesis of a unique class of hyperbranched polyethylene HBPE-based macromolecules with a controllable molecular weight, topology, and composition. This dissertation focuses on new synthetic routes to prepare HBPE-based macromolecular architectures by combining the CWCP technique with ring opening polymerization ROP, atom–transfer radical polymerization ATRP, and “click” chemistry. Taking advantage of end-functionalized HBPE, and a new ethynyl-soketal star-shape agent, we were able to synthesize different types of the HBPE-based architectures including hyperbranched-on-hyperbranched core-shell nanostructure, and miktoarm-star-HBPE-based block copolymers. The first part of the dissertation provides a general introduction to the synthesis of polyethylene types with controllable structures. Well-defined polyethylene with different macromolecule architectures were synthesized either for academic or industrial purposes. In the second part, the HBPE with different topologies was synthesized by CWCP, using a α-diimine Pd (II) catalyst. The effect of the temperature and pressure on the catalyst activity and polymer properties, including branch content, molecular weight, distribution, and thermal properties were studied. Two series of samples were synthesized: a) serial samples (A) under pressures of 1, 5, and 27 atm at 5˚C, and b) serial samples (B) at temperatures of 5, 15, and 35 ˚C under 5 atm. Proton nuclear magnetic resonance spectroscopy, 1H NMR, and gel permeation chromatography, GPC, analysis were used to calculate the branching content, molecular weight, and distribution, whereas differential scanning calorimetry, DSC, was used to record the melting and glass transition temperatures as well as the degree of the crystallinity. Well-defined HBPE-based core diblock copolymers with predictable amphiphilic properties are studied in the third part of the project. Hyperbranched

Study of the influence of the silica source on the synthesis of the zeolite precursor MCM-22

International Nuclear Information System (INIS)

Barbosa, A.S.; Santos, E.R.F. dos; Leite, R.C.N.; Rodrigues, M.G.F.

2012-01-01

Zeolite MCM-22 precursors were synthesized under hydrothermal conditions in systems with hexamethyleneimine HMI as bulking agent (driver). Synthesis parameter, such as sources of silica (aerosil® and quartz) was modified to investigate the effects on the morphology and crystallization in precursor MCM-22 zeolite. The products were characterized by X-Ray Diffraction (XRD), Energy Dispersive Spectroscopy (EDX) and Scanning Electron Microscopy (SEM). According to, the X-ray diffraction showed the same characteristic peaks of zeolite MCM-22. It was found that the parameter in this work of synthesis, silica source, affects the hydrothermal synthesis of zeolite MCM-22 precursor. This can be evidenced by the different morphologies found using the different sources of silica. (author)

MZnFe{sub 2}O{sub 4} (M = Ni, Mn) cubic superparamagnetic nanoparticles obtained by hydrothermal synthesis

Energy Technology Data Exchange (ETDEWEB)

Freire, R. M. [Universidade Federal do Ceara-UFC, Grupo de Quimica de Materiais Avancados (GQMAT)- Departamento de Quimica Analitica e Fisico-Quimica (Brazil); Ribeiro, T. S.; Vasconcelos, I. F. [Universidade Federal do Ceara, Departamento de Engenharia Metalurgica e de Materiais (Brazil); Denardin, J. C. [Universidad de Santiago de Chile, USACH, Departamento de Fisica (Chile); Barros, E. B. [Universidade Federal do Ceara-UFC, Departamento de Fisica (Brazil); Mele, Giuseppe [Universita del Salento, Dipartimento di Ingegneria dell' Innovazione (Italy); Carbone, L. [IPCF-CNR, UOS Pisa (Italy); Mazzetto, S. E.; Fechine, P. B. A., E-mail: fechine@ufc.br [Universidade Federal do Ceara-UFC, Grupo de Quimica de Materiais Avancados (GQMAT)- Departamento de Quimica Analitica e Fisico-Quimica (Brazil)

2013-05-15

MZnFe{sub 2}O{sub 4} (M = Ni or Mn) cubic nanoparticles have been prepared by hydrothermal synthesis in mild conditions and short time without any procedure of calcinations. The structural and magnetic properties of the mixed ferrites were investigated by X-ray diffraction, Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, Moessbauer spectroscopy, vibrating sample magnetometer, and Transmission electron microscopy (TEM). X-ray analysis showed peaks characteristics of the spinel phase. The average diameter of the nanoparticles observed by TEM measurements was approximately between 4 and 10 nm. Spectroscopy study of the spinel structure was performed based on Group Theory. The predicted bands were observed in FTIR and Raman spectrum. The magnetic parameters and Moessbauer spectroscopy were measured at room temperature and superparamagnetic behavior was observed for mixed ferrites. This kind of nanoparticles can be used as precursor in drug delivery systems, magnetic hyperthermia, ferrofluids, or magnetic imaging contrast agents.

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.

Nucleus spectroscopy: extreme masses and deformations

International Nuclear Information System (INIS)

Theisen, Ch.

2009-12-01

The author proposes a synthesis of research activities performed since 1995 in the field of experimental nuclear physics, and more particularly in the investigation of two nucleus extreme states: deformation on the one hand, heavy and very heavy nuclei on the other hand. After a presentation of the context of investigations on deformation, rotation, and heavy nuclei, he gives an overview of developments regarding instruments (gamma spectrometers, detection of fission fragments, and detection at the focal plane of spectrometers or separators) and analysis techniques. Experiments and results are then reported and discussed, concerning super-deformed states with a high angular moment, spectroscopy of neutron-rich nuclei, very heavy nuclei close to nucleus map borders. He finally draws perspectives for middle and long term studies on the heaviest nuclei

Green synthesis of ZnO nanoparticles by Aspalathus linearis: Structural & optical properties

International Nuclear Information System (INIS)

Diallo, A.; Ngom, B.D.; Park, E.; Maaza, M.

2015-01-01

This contribution reports for the 1st time on the synthesis and the main physical properties of ZnO nanoparticles synthesized by an entirely green physical-chemistral process using Aspalathus linearis's natural extract as an efficient reduction/oxidizing agent. Their structural and optical properties by electron microscopy, X-rays diffraction, Raman and X-rays photoemission spectroscopies as well as room temperature photoluminescence are reported. - Highlights: • 1st time report on synthesis of ZnO nanoparticles by a green process via Aspalathus linearis extract. • A. linearis's natural extract was used as an effective reduction/oxidizing agent. • Wurtzite nature of ZnO nanoparticles was confirmed via XRD, Raman, XPS and PL

Green synthesis of ZnO nanoparticles by Aspalathus linearis: Structural & optical properties

Energy Technology Data Exchange (ETDEWEB)

Diallo, A.; Ngom, B.D. [UNESCO-UNISA Africa Chair in Nanosciences-Nanotechnology, College of Graduate Studies, University of South Africa, Muckleneuk Ridge, PO Box 392, Pretoria (South Africa); Nanosciences African Network (NANOAFNET), iThemba LABS-National Research Foundation, 1 Old Faure road, Somerset West 7129, PO Box 722, Somerset West, Western Cape (South Africa); Park, E. [UNESCO-UNISA Africa Chair in Nanosciences-Nanotechnology, College of Graduate Studies, University of South Africa, Muckleneuk Ridge, PO Box 392, Pretoria (South Africa); Nanosciences African Network (NANOAFNET), iThemba LABS-National Research Foundation, 1 Old Faure road, Somerset West 7129, PO Box 722, Somerset West, Western Cape (South Africa); Nelson Mandela African Institute for Science & Technology, Arusha (Tanzania, United Republic of); Maaza, M., E-mail: Maaza@tlabs.ac.za [UNESCO-UNISA Africa Chair in Nanosciences-Nanotechnology, College of Graduate Studies, University of South Africa, Muckleneuk Ridge, PO Box 392, Pretoria (South Africa); Nanosciences African Network (NANOAFNET), iThemba LABS-National Research Foundation, 1 Old Faure road, Somerset West 7129, PO Box 722, Somerset West, Western Cape (South Africa)

2015-10-15

This contribution reports for the 1st time on the synthesis and the main physical properties of ZnO nanoparticles synthesized by an entirely green physical-chemistral process using Aspalathus linearis's natural extract as an efficient reduction/oxidizing agent. Their structural and optical properties by electron microscopy, X-rays diffraction, Raman and X-rays photoemission spectroscopies as well as room temperature photoluminescence are reported. - Highlights: • 1st time report on synthesis of ZnO nanoparticles by a green process via Aspalathus linearis extract. • A. linearis's natural extract was used as an effective reduction/oxidizing agent. • Wurtzite nature of ZnO nanoparticles was confirmed via XRD, Raman, XPS and PL.

Microwave assisted scalable synthesis of titanium ferrite nanomaterials

Science.gov (United States)

Shukla, Abhishek; Bhardwaj, Abhishek K.; Singh, S. C.; Uttam, K. N.; Gautam, Nisha; Himanshu, A. K.; Shah, Jyoti; Kotnala, R. K.; Gopal, R.

2018-04-01

Titanium ferrite magnetic nanomaterials are synthesized by one-step, one pot, and scalable method assisted by microwave radiation. Effects of titanium content and microwave exposure time on size, shape, morphology, yield, bonding nature, crystalline structure, and magnetic properties of titanium ferrite nanomaterials are studied. As-synthesized nanomaterials are characterized by X-ray diffraction (XRD), ultraviolet-visible absorption spectroscopy (UV-Vis), attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR), Raman spectroscopy, transmission electron microscopy (TEM), and vibrating sample magnetometer measurements. XRD measurements depict the presence of two phases of titanium ferrite into the same sample, where crystallite size increases from ˜33 nm to 37 nm with the increase in titanium concentration. UV-Vis measurement showed broad spectrum in the spectral range of 250-600 nm which reveals that its characteristic peaks lie between ultraviolet and visible region; ATR-FTIR and Raman measurements predict iron-titanium oxide structures that are consistent with XRD results. The micrographs of TEM and selected area electron diffraction patterns show formation of hexagonal shaped particles with a high degree of crystallinity and presence of multi-phase. Energy dispersive spectroscopy measurements confirm that Ti:Fe compositional mass ratio can be controlled by tuning synthesis conditions. Increase of Ti defects into titanium ferrite lattice, either by increasing titanium precursor or by increasing exposure time, enhances its magnetic properties.

Comparison of Conventional and Microwave-assisted Synthesis of Benzimidazole Derivative from Citronellal in Kaffir lime oil (Citrus hystrix DC.)

Science.gov (United States)

Warsito, W.; Noorhamdani, A. S.; Suratmo; Dwi Sapri, R.; Alkaroma, D.; Azhar, A. Z.

2018-04-01

Simple method has been used for the synthesis of benzimidazole derivative from citronellal in kaffir lime oil under microwave irradiation. These compounds were synthesized also by conventional heating for comparison. In addtion, microwave-assited synthesis was also compared between using to dichloromethane and methanol solvents with variation of reaction time for 30 to 70 minutes and 4 to 12 h for conventional heating. The 2-citronellyl benzimidazole compound synthesized were characterised by FT-IR, GC-MS, 1H and 13C NMR spectroscopy. Comparison between conventional and microwave-assisted synthesis was done by comparing between correlation of reaction time and percentage yield. The time optimum of microwave-assisted and conventional synthesis using dichloromethane solvent respectively at 60 minutes (yield 19.23%) and 8 hours (yield 11.54%). In addition, microwave-assited synthesis increasing 157.81 times compared by conventional heating. While using methanol solvent tends to increase linearly however the percentage of yield only 0.77 times of synthesis using dichloromethane solvent.

Synthesis of nanofibrous ZnO by magnetron sputtering and its integration in dye-sensitized solar cells

International Nuclear Information System (INIS)

Ghimpu, L.; Tiginyanu, I.; Pauporte, T.; Guerin, V.M.; Lupan, O.

2013-01-01

This work demonstrates a cost-effective synthesis of nanofibrous ZnO layers by a magnetron sputtering. We present the results of layer characterization by scanning electron microscopy, X-ray diffraction, energy dispersive X-ray spectrometry, Raman spectroscopy, and photoluminescence which are indicative of good structural properties of the layers. The nanofibrous ZnO layers proves good structural properties offering a new nanomaterial for dye-sensitized solar cells (DSCs) application. Their successful integration in DSC for solar energy conversion is demonstrated by impedance spectroscopy, and photo-current-voltage (J-V) studies.

Experimental study by infrared spectroscopy of irradiation effects in silicates and ices, applied to astrophysics

International Nuclear Information System (INIS)

Rocard, F.

1986-05-01

This thesis presents the study of the radiation effects (erosion and synthesis) with ions of low energy (a few KeV/u) in silicates and ices. The erosion of the H 2 O ice is analysed by infrared spectroscopy versus different parameters: ion beam flux, mass and energy of the ions, and the thickness of the samples. The interpretation is that the erosion of the ice comes mainly from the dissociation, along the ion range, of the H 2 O molecules. A study of the synthesis in SiO 2 and H 2 O by carbon, nitrogen and hydrogen implantation leads to the characterization of the synthesized molecules and the determination of the yields. The irradiation of ices mixtures (H 2 O, CO 2 and NH 3 ) leads to the synthesis of a great variety of molecules which are identified. The experimental results are extrapolated to different astrophysical situations in the solar cavity (Moon, satellites of giant planets, comets) and in the interstellar medium (molecular clouds) [fr

Synthesis and characterization of polypyrrole and its application for solar cell

Science.gov (United States)

Almuntaser, Faisal M. A.; Majumder, Sutripto; Baviskar, Prashant K.; Sali, Jaydeep V.; Sankapal, B. R.

2017-08-01

In this report, the fabrication of a solar cell device with the structures FTO/PPy/PTh/ZnO/Al was performed using wet chemical synthesis methods in open environment. The cost-effective methods like CBD, SILAR, and spin coating have been used for the synthesis. The effect of thickness of PPy active layer on the device performance is investigated. Features such as structural, morphological, and chemical bonding of the layers have been investigated using X-ray diffraction, field emission scanning electron microscopy, and Fourier transform infrared spectroscopy and are discussed herein. Effects of PPy thickness on current-voltage characteristics have been studied under dark and illumination at 1 Sun (100 mW/cm2, AM 1.5 G) condition to study the solar cell performance.

Spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Hellman, Hal

1968-01-01

This booklet discusses spectroscopy, the study of absorption of radiation by matter, including X-ray, gamma-ray, microwave, mass spectroscopy, as well as others. Spectroscopy has produced more fundamental information to the study of the detailed structure of matter than any other tools.

Synthesis of C60(OH)18-20 in aqueous alkaline solution under O2-atmosphere

International Nuclear Information System (INIS)

Alves, Gustavo Catao; Ladeira, Luiz Orlando; Righi, Ariete; Krambrock, Klaus; Pinheiro, Mauricio Veloso B.; Calado, Hallen Daniel; Gil, Rossimiriam Pereira de Freitas

2006-01-01

In this work we report on an alternative synthesis of water-soluble fullerenes known as fullerols, aiming for biomedical applications. The synthesis is based on a process in which polyethylene glycol (PEG400) is used as phase-transfer catalyst between fullerene/benzene and aqueous NaOH solutions. The polyhydroxylation of the fullerenes occurs in the NaOH solution under a continuous flow of O 2 to enhance the reaction yield. The resulting compound was characterized with infrared spectroscopy, nuclear magnetic resonance, thermo-gravimetric analysis and optical absorption. The formation of C 60 (OH) 18-20 in high yields was confirmed. (author)

Green chemistry approach for the synthesis of biocompatible graphene

Science.gov (United States)

Gurunathan, Sangiliyandi; Han, Jae Woong; Kim, Jin-Hoi

2013-01-01

Background Graphene is a single-atom thick, two-dimensional sheet of hexagonally arranged carbon atoms isolated from its three-dimensional parent material, graphite. One of the most common methods for preparation of graphene is chemical exfoliation of graphite using powerful oxidizing agents. Generally, graphene is synthesized through deoxygenation of graphene oxide (GO) by using hydrazine, which is one of the most widespread and strongest reducing agents. Due to the high toxicity of hydrazine, it is not a promising reducing agent in large-scale production of graphene; therefore, this study focused on a green or sustainable synthesis of graphene and the biocompatibility of graphene in primary mouse embryonic fibroblast cells (PMEFs). Methods Here, we demonstrated a simple, rapid, and green chemistry approach for the synthesis of reduced GO (rGO) from GO using triethylamine (TEA) as a reducing agent and stabilizing agent. The obtained TEA reduced GO (TEA-rGO) was characterized by ultraviolet (UV)–visible absorption spectroscopy, X-ray diffraction (XRD), particle size dynamic light scattering (DLS), scanning electron microscopy (SEM), Raman spectroscopy, and atomic force microscopy (AFM). Results The transition of graphene oxide to graphene was confirmed by UV–visible spectroscopy. XRD and SEM were used to investigate the crystallinity of graphene and the surface morphologies of prepared graphene respectively. The formation of defects further supports the functionalization of graphene as indicated in the Raman spectrum of TEA-rGO. Surface morphology and the thickness of the GO and TEA-rGO were analyzed using AFM. The presented results suggest that TEA-rGO shows significantly more biocompatibility with PMEFs cells than GO. Conclusion This is the first report about using TEA as a reducing as well as a stabilizing agent for the preparation of biocompatible graphene. The proposed safe and green method offers substitute routes for large-scale production of graphene

The synthesis of a pyridine-: N -oxide isophthalamide rotaxane utilizing supplementary amide hydrogen bond interactions

OpenAIRE

Evans, Nicholas Henley; Gell, Charlie; Peach, Michael Joseph George

2016-01-01

The synthesis of a pyridine-N-oxide containing rotaxane, not requiring an additional ionic template, has been achieved in 32% yield. Successful rotaxane formation is dependent upon the structure of the isophthalamide macrocycle used, an observation which has been rationalised by a combination of NMR spectroscopy, X-ray crystallography and computational modelling.

Dihydroazulene Photochromism:Synthesis, Molecular Electronics and Hammett Correlations

DEFF Research Database (Denmark)

Broman, Søren Lindbæk

This thesis describes the development of a versatile synthetic protocol for preparation of a large selection of dihydroazulenes (DHAs) with both electron withdrawing and donating groups. By UV-Vis and NMR spectroscopies and even in a single-molecule junction, their ability to undergo a light...... will be discussed in detail. The second chapter describes the design and synthesis of DHA/VHFs intended for use in molecular electronics and their solution and single-molecule junction switching properties. By the expansion of the recently reported procedure for functionalization of this system by Suzuki cross...

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.

Low Temperature Solid-State Synthesis and Characterization of LaBO3

Directory of Open Access Journals (Sweden)

Azmi Seyhun KIPÇAK

2016-11-01

Full Text Available Rare earth (lanthanide series borates, possess high vacuum ultraviolet (VUV transparency, large electronic band gaps, chemical and environmental stability and exceptionally large optical damage thresholds and used in the development of plasma display panels (PDPs. In this study the synthesis of lanthanum borates via solid-state method is studied. For this purpose, lanthanum oxide (La2O3 and boric acid (H3BO3 are used for as lanthanum and boron sources, respectively. Different elemental molar ratios of La to B (between 3:1 to 1:6 as La2O3:H3BO3 were reacted by solid-state method at the reaction temperatures between 500°C - 700°C with the constant reaction time of 4 h. Following the synthesis, characterizations of the synthesized products are conducted by X-ray diffraction (XRD, Fourier transform infrared spectroscopy (FT-IR, Raman spectroscopy and scanning electron microscope (SEM. From the results of the experiments, three types of lanthanum borates of; La3BO6, LaBO3 and La(BO23 were observed at different reaction parameters. Among these three types of lanthanum borates LaBO3 phase were obtained as a major phase.

Large Scale Screening of Southern African Plant Extracts for the Green Synthesis of Gold Nanoparticles Using Microtitre-Plate Method

Directory of Open Access Journals (Sweden)

Abdulrahman M. Elbagory

2016-11-01

Full Text Available The preparation of gold nanoparticles (AuNPs involves a variety of chemical and physical methods. These methods use toxic and environmentally harmful chemicals. Consequently, the synthesis of AuNPs using green chemistry has been under investigation to develop eco-friendly nanoparticles. One approach to achieve this is the use of plant-derived phytochemicals that are capable of reducing gold ions to produce AuNPs. The aim of this study was to implement a facile microtitre-plate method to screen a large number of aqueous plant extracts to determine the optimum concentration (OC for the bio-synthesis of the AuNPs. Several AuNPs of different sizes and shapes were successfully synthesized and characterized from 17 South African plants. The characterization was done using Ultra Violet-Visible Spectroscopy, Dynamic Light Scattering, High Resolution Transmission Electron Microscopy and Energy-Dispersive X-ray Spectroscopy. We also studied the effects of temperature on the synthesis of the AuNPs and showed that changes in temperatures affect the size and dispersity of the generated AuNPs. We also evaluated the stability of the synthesized AuNPs and showed that some of them are stable in biological buffer solutions.

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)

Synthesis of borylated porphyrin and bromo- porphyrin as building blocks for light harvesting antenna molecule

Science.gov (United States)

Radzuan, Nuur Haziqah Mohd; Hassan, Nurul Izzaty; Bakar, Muntaz Abu

2018-04-01

The building blocks for synthesis of light harvesting antenna which are 5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolane)-10,20-diphenylporphyrin, 5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolane)-10,20-dihexylporphyrin and 5,10,15,20-tetra-(bromophenyl)porphyrin were synthesized. Borylated porphyrin was synthesized by Suzuki coupling reaction between A2BC bromo-porphyrin and pinacolborane. Whereas 5,10,15,20-tetra-(bromophenyl) porphyrin was synthesized by Lindsey condensation reaction between pyrrole and 4-bromobenzaldehyde. 1H-NMR, 13C-NMR spectroscopy and UV-visible spectroscopy confirmed the successful formation of all compounds.

Synthesis of mesogenic phthalocyanine-C60 donor–acceptor dyads designed for molecular heterojunction photovoltaic devices

Directory of Open Access Journals (Sweden)

Yves Henri Geerts

2009-10-01

Full Text Available A series of phthalocyanine-C60 dyads 2a–d was synthesized. Key steps in their synthesis are preparation of the low symmetry phthalocyanine intermediate by the statistical condensation of two phthalonitriles, and the final esterification of the fullerene derivative bearing a free COOH group. Structural characterization of the molecules in solution was performed by NMR spectroscopy, UV–vis spectroscopy and cyclic voltammetry. Preliminary studies suggest formation of liquid crystalline (LC mesophases for some of the prepared dyads. To the best of our knowledge, this is the first example of LC phthalocyanine-C60 dyads.

Synthesis and characterization of organic-inorganic hybrids formed between conducting polymers and crystalline antimonic acid

Directory of Open Access Journals (Sweden)

Beleze Fábio A.

2001-01-01

Full Text Available In this paper we report the synthesis and characterization of novel organic-inorganic hybrid materials between the crystalline antimonic acid (CAA and two conductive polymers: polypyrrole and polyaniline. The hybrids were obtained by in situ oxidative polymerization of monomers by the Sb(V present in the pyrochlore-like CAA structure. The materials were characterized by infrared and Raman spectroscopy, X-ray diffraction, cyclic voltammetry, CHN elemental analysis and electronic paramagnetic resonance spectroscopy. The results showed that both polymers were formed in their oxidized form, with the CAA structure acting as a counter anion.

Spin labeled amino acid nitrosourea derivatives--synthesis and antitumour activity.

Science.gov (United States)

Zheleva, A; Raikov, Z; Ilarionova, M; Todorov, D

1995-01-01

The synthesis of three spin labeled derivatives of N-[N'-(chloroethyl)-N'-nitrosocarbamoyl] amino acids is reported. The new nitrosoureas are obtained by condensation of the corresponding N-[N'-(2-chloroethyl)-N'-nitrosocarbamoyl] amino acid with 2,2,6,6-tetramethyl-1-oxyl-4-aminopiperidine using dicyclohexylcarbodiimide. Their chemical structures are confirmed by elemental analysis, IR, MS, and EPR spectroscopy. All newly synthesized compounds showed high antitumour activity against the lymphoid leukemia L1210 in BDF1 mice.

Novel metal complexes of mixed piperaquine-acetaminophen and piperaquine-acetylsalicylic acid: Synthesis, characterization and antimicrobial activities

Directory of Open Access Journals (Sweden)

Yusuf Oloruntoyin Ayipo

2016-11-01

Full Text Available Synthesis of coordination compounds of Zinc(II, Copper(II, Nickel(II, Cobalt(II and Iron(II with mixed piperaquine-acetaminophen and piperaquine-acetylsalicylic acid has been studied. The complexes were characterized via: solubility test, melting point determination, conductivity measurement, Atomic Absorption Spectroscopy, UV-Visible Spectroscopy, FTIR Spectroscopy and magnetic susceptibility. The complexes were proposed to have a stoichiometry ratio of 1:1:1 between each metal salt and the ligands with tetrahedral and octahedral geometry following the reaction pattern of MX.yH2O + L1L2/3 to give ML1L2/3X.yH2O. Biological activities of the synthesized complexes have been evaluated against Escherichia coli and Staphylococcus aureus.

Escherichia coli cell-free protein synthesis and isotope labeling of mammalian proteins.

Science.gov (United States)

Terada, Takaho; Yokoyama, Shigeyuki

2015-01-01

This chapter describes the cell-free protein synthesis method, using an Escherichia coli cell extract. This is a cost-effective method for milligram-scale protein production and is particularly useful for the production of mammalian proteins, protein complexes, and membrane proteins that are difficult to synthesize by recombinant expression methods, using E. coli and eukaryotic cells. By adjusting the conditions of the cell-free method, zinc-binding proteins, disulfide-bonded proteins, ligand-bound proteins, etc., may also be produced. Stable isotope labeling of proteins can be accomplished by the cell-free method, simply by using stable isotope-labeled amino acid(s) in the cell-free reaction. Moreover, the cell-free protein synthesis method facilitates the avoidance of stable isotope scrambling and dilution over the recombinant expression methods and is therefore advantageous for amino acid-selective stable isotope labeling. Site-specific stable isotope labeling is also possible with a tRNA molecule specific to the UAG codon. By the cell-free protein synthesis method, coupled transcription-translation is performed from a plasmid vector or a PCR-amplified DNA fragment encoding the protein. A milligram quantity of protein can be produced with a milliliter-scale reaction solution in the dialysis mode. More than a thousand solution structures have been determined by NMR spectroscopy for uniformly labeled samples of human and mouse functional domain proteins, produced by the cell-free method. Here, we describe the practical aspects of mammalian protein production by the cell-free method for NMR spectroscopy. © 2015 Elsevier Inc. All rights reserved.

Synthesis of multicomponent metallic layers during impulse plasma deposition

Directory of Open Access Journals (Sweden)

Nowakowska-Langier Katarzyna

2015-12-01

Full Text Available Pulsed plasma in the impulse plasma deposition (IPD synthesis is generated in a coaxial accelerator by strong periodic electrical pulses, and it is distributed in a form of energetic plasma packets. A nearly complete ionization of gas, in these conditions of plasma generation, favors the nucleation of new phase of ions and synthesis of metastable materials in a form of coatings which are characterized by amorphous and/or nanocrystalline structure. In this work, the Fe–Cu alloy, which is immiscible in the state of equilibrium, was selected as a model system to study the possibility of formation of a non-equilibrium phase during the IPD synthesis. Structural characterization of the layers was done by means of X-ray diffraction and conversion-electron Mössbauer spectroscopy. It was found that supersaturated solid solutions were created as a result of mixing and/or alloying effects between the layer components delivered to the substrate independently and separately in time. Therefore, the solubility in the Fe–Cu system was largely extended in relation to the equilibrium conditions, as described by the equilibrium phase diagram in the solid state.

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.

Synthesis of CuO-NiO core-shell nanoparticles by homogeneous precipitation method

International Nuclear Information System (INIS)

Bayal, Nisha; Jeevanandam, P.

2012-01-01

Highlights: ► CuO-NiO core-shell nanoparticles have been synthesized using a simple homogeneous precipitation method for the first time. ► Mechanism of the formation of core-shell nanoparticles has been investigated. ► The synthesis route may be extended for the synthesis of other mixed metal oxide core-shell nanoparticles. - Abstract: Core-shell CuO–NiO mixed metal oxide nanoparticles in which CuO is the core and NiO is the shell have been successfully synthesized using homogeneous precipitation method. This is a simple synthetic method which produces first a layered double hydroxide precursor with core-shell morphology which on calcination at 350 °C yields the mixed metal oxide nanoparticles with the retention of core-shell morphology. The CuO–NiO mixed metal oxide precursor and the core-shell nanoparticles were characterized by powder X-ray diffraction, FT-IR spectroscopy, thermal gravimetric analysis, elemental analysis, scanning electron microscopy, transmission electron microscopy, and diffuse reflectance spectroscopy. The chemical reactivity of the core-shell nanoparticles was tested using catalytic reduction of 4-nitrophenol with NaBH 4 . The possible growth mechanism of the particles with core-shell morphology has also been investigated.

Synthesis of hydroxyapatite nanoparticles onto modified polypropylene surface to be used in bone tissue engineering

International Nuclear Information System (INIS)

Cellet, Thelma Sley P.; Pereira, Guilherme M.; Fragal, Elizangela H.; Rubira, Adley F.; Companhoni, Mychelle V.P.; Nakamura, Celso V.; Ueda-Nakamura, Tania

2015-01-01

Chemical modification of polypropylene (PP) films can be explored to prepare innovative materials, for instance materials which can be used in tissue engineering application. The maleimide synthesis onto PP films was made for later polymerizes glycidyl methacrylate (GMA) and to grow up hydroxyapatite nanoparticles (n-HA) by biomimetization method (BM) in metastable simulated body fluid (SBF) for 7, 14 and 21 days. The modification steps were proved by infrared spectroscopy (FTIR) and the n-HA synthesis evidenced by X-ray diffractometry (XRD), scanning electronic microscopy (SEM) and energy dispersive spectroscopy (EDS). PP films exposed to SBF for 14 and 21 days showed n-HA on all over the films surface. The interaction of pre-osteoblasts with the films after 48 hours was evaluated by SEM. The results demonstrate that cells on the surface of n-HA films showed spreading, and number of filopodia similar to the control, wherein the films with greater amount of n-HA appear to have higher filopodia connections between the cells and appear to have its surface covered with higher cell density. (author)

Microwave-assisted synthesis of palladium nanocubes and nanobars

International Nuclear Information System (INIS)

Yu, Yanchun; Zhao, Yanxi; Huang, Tao; Liu, Hanfan

2010-01-01

Microwave was employed in the shape-controlled synthesis of palladium nanoparticles. Palladium nanocubes and nanobars with a mean size of about 23.8 nm were readily synthesized with H 2 PdCl 4 as a precursor, tetraethylene glycol (TEG) as both a solvent and a reducing agent in the presence of PVP and CTAB in 80 s under microwave irradiation. The structures of the as-prepared palladium nanoparticles were characterized by transmission electron microscopy (TEM), X-ray powder diffraction (XRD) and ultraviolet-visible (UV-vis) absorption spectroscopy. The formation of PdBr 4 2- due to the coordination replacement of the ligand Cl - ions in PdCl 4 2- ions by Br - ions in the presence of bromide was responsible for the synthesis of Pd nanocubes and nanobars. In addition, a milder reducing power, a higher viscosity and a stronger affinity of TEG were beneficial to the larger sizes of Pd nanocubes and nanobars.

Rapeseed Oil as Renewable Resource for Polyol Synthesis

Science.gov (United States)

Stirna, Uldis; Fridrihsone, Anda; Misane, Marija; Vilsone, Dzintra

2011-01-01

Vegetable oils are one of the most important platform chemicals due to their accessibility, specific structure of oils and low price. Rapeseed oil (RO) polyols were prepared by amidization of RO with diethanolamine (DEA). To determine the kinetics of amidization reaction, experiments were carried out. Fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), amine (NH) value was determined. Group contribution method by Fedor‵s was used to calculate solubility parameters, van der Waals volume was calculated by Askadskii. Obtained polyol‵s OH and NH value are from 304 up to 415 mg KOH/g. RO polyols synthesis meets the criteria of "green chemistry". In the present study, reaction of RO amidization with DEA was investigated, as well as optimum conditions for polyol synthesis was established to obtain polyols for polyurethane production. Calculations of solubility parameter and cohesion energy density were calculated, as RO polyols will be used as side chains in polymers, and solubility parameter will be used to explain properties of polymers.

Synthesis of Photochromic Oligophenylenimines: Optical and Computational Studies

Directory of Open Access Journals (Sweden)

Armando I. Martínez Pérez

2015-03-01

Full Text Available Phenyleneimine oligomers 4,4'-(((1E,1'E-(((1E,1'E-(1,4-phenylenebis-(azanylylidenebis(methanylylidenebis(2,5-bis(octyloxy-4,1-phenylenebis(methanylyl-idene-bis(azanylylidenedianiline (OIC1MS and 7,7'-(((1E,1'E-(((1E,1'E-((9H-fluorene-2,7-diylbis(azanylylidenebis(methanylylidenebis(2,5-bis(octyloxy-4,1phenylenebis- (methanylylidenebis(azanylylidenebis(9H-fluoren-2-amine (OIC2MS were prepared by means of conventional and mechanochemical synthesis and characterized by FT-IR, 1H- and 13C-NMR techniques. The optical properties of the compounds were studied in solution by using UV-visible spectroscopy, and the optical effects were analyzed as a function of solvent. The results show that OIC2MS exhibits interesting photochromic properties. Furthermore, the structural and electronic properties of the compounds were analyzed by TD-DFT. It was found that the mechanosynthesis is an efficient method for the synthesis of both tetraimines.

Shape- and Size-Controlled Synthesis of Silver Nanoparticles Using Aloe vera Plant Extract and Their Antimicrobial Activity

Science.gov (United States)

Logaranjan, Kaliyaperumal; Raiza, Anasdass Jaculin; Gopinath, Subash C. B.; Chen, Yeng; Pandian, Kannaiyan

2016-11-01

Biogenic synthesis of silver nanoparticles (AgNP) was performed at room temperature using Aloe vera plant extract in the presence of ammoniacal silver nitrate as a metal salt precursor. The formation of AgNP was monitored by UV-visible spectroscopy at different time intervals. The shape and size of the synthesized particle were visualized by scanning electron microscopy (SEM) and transmission electron microscopy (TEM) observations. These results were confirmed by X-ray powder diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) analyses and further supported by surface-enhanced Raman spectroscopy/Raman scattering (SERS) study. UV-visible spectrum has shown a sharp peak at 420 nm and further evidenced by FTIR peak profile (at 1587.6, 1386.4, and 1076 cm-1 with corresponding compounds). The main band position with SERS was noticed at 1594 cm-1 (C-C stretching vibration). When samples were heated under microwave radiation, AgNP with octahedron shapes with 5-50 nm were found and this method can be one of the easier ways to synthesis anisotropic AgNP, in which the plant extract plays a vital role to regulate the size and shape of the nanoparticles. Enhanced antibacterial effects (two- to fourfold) were observed in the case of Aloe vera plant protected AgNP than the routinely synthesized antibiotic drugs.

Unprecedented Carbonato Intermediates in Cyclic Carbonate Synthesis Catalysed by Bimetallic Aluminium(Salen) Complexes.

Science.gov (United States)

Castro-Osma, José A; North, Michael; Offermans, Willem K; Leitner, Walter; Müller, Thomas E

2016-04-21

The mechanism by which [Al(salen)]2 O complexes catalyse the synthesis of cyclic carbonates from epoxides and carbon dioxide in the absence of a halide cocatalyst has been investigated. Density functional theory (DFT) studies, mass spectrometry and (1) H NMR, (13) C NMR and infrared spectroscopies provide evidence for the formation of an unprecedented carbonato bridged bimetallic aluminium complex which is shown to be a key intermediate for the halide-free synthesis of cyclic carbonates from epoxides and carbon dioxide. Deuterated and enantiomerically-pure epoxides were used to study the reaction pathway. Based on the experimental and theoretical results, a catalytic cycle is proposed. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Green and Rapid Synthesis of Anticancerous Silver Nanoparticles by Saccharomyces boulardii and Insight into Mechanism of Nanoparticle Synthesis

Directory of Open Access Journals (Sweden)

Abhishek Kaler

2013-01-01

Full Text Available Rapidly developing field of nanobiotechnology dealing with metallic nanoparticle (MNP synthesis is primarily lacking control over size, shape, dispersity, yield, and reaction time. Present work describes an ecofriendly method for the synthesis of silver nanoparticles (AgNPs by cell free extract (CFE of Saccharomyces boulardii. Parameters such as culture age (stationary phase growth, cell mass concentration (400 mg/mL, temperature (35°C, and reaction time (4 h, have been optimized to exercise a control over the yield of nanoparticles and their properties. Nanoparticle (NP formation was confirmed by UV-Vis spectroscopy, elemental composition by EDX (energy dispersive X-rays analysis, and size and shape by transmission electron microscopy. Synthesized nanoparticles had the size range of 3–10 nm with high negative zeta potential (−31 mV indicating excellent stability. Role of proteins/peptides in NP formation and their stability were also elucidated. Finally, anticancer activity of silver nanoparticles as compared to silver ions was determined on breast cancer cell lines.

Trispyrazolylborate Complexes: An Advanced Synthesis Experiment Using Paramagnetic NMR, Variable-Temperature NMR, and EPR Spectroscopies

Science.gov (United States)

Abell, Timothy N.; McCarrick, Robert M.; Bretz, Stacey Lowery; Tierney, David L.

2017-01-01

A structured inquiry experiment for inorganic synthesis has been developed to introduce undergraduate students to advanced spectroscopic techniques including paramagnetic nuclear magnetic resonance and electron paramagnetic resonance. Students synthesize multiple complexes with unknown first row transition metals and identify the unknown metals by…

Synthesis, structural, X-ray photoelectron spectroscopy (XPS) studies and IR induced anisotropy of Tl{sub 4}HgI{sub 6} single crystals

Energy Technology Data Exchange (ETDEWEB)

Parasyuk, O.V. [Department of Inorganic and Physical Chemistry, Lesya Ukrainka Eastern European National University, Voli Ave. 13, Lutsk, 43025 (Ukraine); Khyzhun, O.Y. [Frantsevych Institute for Problems of Materials Science, National Academy of Sciences of Ukraine, 3 Krzhyzhanivsky St., 03142, Kyiv (Ukraine); Piasecki, M. [Institute of Physics, J. Dlugosz University Częstochowa, Armii Krajowej 13/15, Częstochowa (Poland); Kityk, I.V., E-mail: iwank74@gmail.com [Electrical Engineering Department, Czestochowa University Technology, Armii Krajowej 17, PL-42-217, Czestochowa (Poland); Lakshminarayana, G. [Wireless and Photonic Networks Research Centre, Faculty of Engineering, Universiti Putra Malaysia, 43400, Serdang, Selangor (Malaysia); Luzhnyi, I. [Frantsevych Institute for Problems of Materials Science, National Academy of Sciences of Ukraine, 3 Krzhyzhanivsky St., 03142, Kyiv (Ukraine); Fochuk, P.M. [Yuriy Fed’kovych Chernivtsi National University, 2 Kotziubynskoho Str., 58012, Chernivtsi (Ukraine); Fedorchuk, A.O. [Department of Inorganic and Organic Chemistry, Lviv National University of Veterinary Medicine and Biotechnologies, Pekarska Street 50, 79010, Lviv (Ukraine); Levkovets, S.I.; Yurchenko, O.M.; Piskach, L.V. [Department of Inorganic and Physical Chemistry, Lesya Ukrainka Eastern European National University, Voli Ave. 13, Lutsk, 43025 (Ukraine)

2017-02-01

In the present work, we report on the synthesis and structural properties including X-ray protoelectron spectroscopy (XPS) analysis of Tl{sub 4}HgI{sub 6} crystals that were grown by Bridgman-Stockbarger method up to 80 mm in length and 18 mm in diameter. The existence of the ternary compound Tl{sub 4}HgI{sub 6} that melts incongruently at 641 K was confirmed. Phase equilibria and structural properties for the TlI–HgI{sub 2} system were investigated by differential thermal analysis (DTA) and X-ray diffraction (XRD) methods. X-ray photoelectron spectra were measured for both pristine and Ar{sup +} ion-bombarded Tl{sub 4}HgI{sub 6} single crystal surfaces. The data reveal that the Tl{sub 4}HgI{sub 6} single crystal is sensitive with respect to Ar{sup +} ion-bombardment as 3.0 keV Ar{sup +} irradiation over 5 min at an ion current density 14 μA/cm{sup 2} induces changes to the elemental stoichiometry of the Tl{sub 4}HgI{sub 6} surface, leading to a decrease of the mercury content in the topmost surface layers. X-ray photoelectron spectroscopy (XPS) measurements indicate very low hygroscopic nature of the Tl{sub 4}HgI{sub 6} single crystal surface. The IR coherent bicolor laser treatment at wavelengths 10.6/5.3 μm has shown an occurrence of anisotropy at wavelengths 1540 nm of Er:glass laser. This may open the applications of Tl{sub 4}HgI{sub 6} as a material for IR laser triggering. - Highlights: • Phase diagram of the HgI{sub 2}–TlI system was built. • Tl{sub 4}HgI{sub 6} single crystals were grown by Bridgman Stockbarger method. • XRD, XPS analysis was done. • Ir induced anisotropy was established. • The compounds may be proposed as Ir laser operated polarizers.

Green Chemistry Approach for Synthesis of Effective Anticancer Palladium Nanoparticles.

Science.gov (United States)

Gurunathan, Sangiliyandi; Kim, EunSu; Han, Jae Woong; Park, Jung Hyun; Kim, Jin-Hoi

2015-12-15

The purpose of this study was to design and synthesize Palladium nanoparticles (PdNPs) using an environmentally friendly approach and evaluate the in vitro efficacy of PdNPs in human ovarian cancer A2780 cells. Ultraviolet-Visible (UV-Vis) spectroscopy was used to monitor the conversion of Pd(II) ions to Pd(0)NPs. X-ray diffraction (XRD) revealed the crystallinity of the as-synthesized PdNPs and Fourier transform infrared spectroscopy (FTIR) further confirmed the role of the leaf extract of Evolvulus alsinoides as a reducing and stabilizing agent for the synthesis of PdNPs. Dynamic light scattering (DLS) and transmission electron microscopy (TEM) showed that the average size of the NPs was 5 nm. After a 24-h exposure to PdNPs, cell viability and light microscopy assays revealed the dose-dependent toxicity of the PdNPs. Furthermore, the dose-dependent cytotoxicity of the PdNPs was confirmed by lactate dehydrogenase (LDH), increased reactive oxygen species (ROS) generation, activation of PdNPs-induced autophagy, impairment of mitochondrial membrane potential (MMP), enhanced caspase-3 activity, and detection of TUNEL-positive cells. Our study demonstrates a single, simple, dependable and green approach for the synthesis of PdNPs using leaf extracts of Evolvulus alsinoides. Furthermore, the in vitro efficacy of PdNPs in human ovarian cancer cells suggests that it could be an effective therapeutic agent for cancer therapy.

Photonic crystals based on opals and inverse opals: synthesis and structural features

International Nuclear Information System (INIS)

Klimonsky, S O; Abramova, Vera V; Sinitskii, Alexander S; Tretyakov, Yuri D

2011-01-01

Methods of synthesis of photonic crystals based on opals and inverse opals are considered. Their structural features are discussed. Data on different types of structural defects and their influence on the optical properties of opaline materials are systematized. The possibilities of investigation of structural defects by optical spectroscopy, electron microscopy, microradian X-ray diffraction, laser diffraction and using an analysis of Kossel ring patterns are described. The bibliography includes 253 references.

Spectroscopy of Kerr Black Holes with Earth- and Space-Based Interferometers.

Science.gov (United States)

Berti, Emanuele; Sesana, Alberto; Barausse, Enrico; Cardoso, Vitor; Belczynski, Krzysztof

2016-09-02

We estimate the potential of present and future interferometric gravitational-wave detectors to test the Kerr nature of black holes through "gravitational spectroscopy," i.e., the measurement of multiple quasinormal mode frequencies from the remnant of a black hole merger. Using population synthesis models of the formation and evolution of stellar-mass black hole binaries, we find that Voyager-class interferometers will be necessary to perform these tests. Gravitational spectroscopy in the local Universe may become routine with the Einstein Telescope, but a 40-km facility like Cosmic Explorer is necessary to go beyond z∼3. In contrast, detectors like eLISA (evolved Laser Interferometer Space Antenna) should carry out a few-or even hundreds-of these tests every year, depending on uncertainties in massive black hole formation models. Many space-based spectroscopical measurements will occur at high redshift, testing the strong gravity dynamics of Kerr black holes in domains where cosmological corrections to general relativity (if they occur in nature) must be significant.

Green Synthesis of Silver Nanoparticles Using Sodium Alginate and Lignosulphonic Acid Blends

Science.gov (United States)

Thakur, Amrita; Reddy, Giridhar

2017-08-01

A simple method based on the principles of green chemistry has been developed to synthesize stable silver nanoparticles (AgNP) for possible biomedical applications. Blend of sodium alginate (SA) and lignosulphonic acid (LS) prepared in the ratio of 80/20 mass percent respectively was used as reducing and stabilizing agent. This blend is biocompatible and has shown drug release ability under physiological conditions. Use of blend has an added advantage as LS has the ability to reduce silver while the blend matrix acts as a stabilizing agent. Effect of precursor concentration (AgNO3) and temperature was investigated. Progress of synthesis was monitored using UV-Vis spectroscopy. Higher temperature and lower silver nitrate concentration showed better synthesis of AgNP.

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.

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

The role of tannic acid and sodium citrate in the synthesis of silver nanoparticles

Science.gov (United States)

Ranoszek-Soliwoda, Katarzyna; Tomaszewska, Emilia; Socha, Ewelina; Krzyczmonik, Pawel; Ignaczak, Anna; Orlowski, Piotr; Krzyzowska, Małgorzata; Celichowski, Grzegorz; Grobelny, Jaroslaw

2017-08-01

We describe herein the significance of a sodium citrate and tannic acid mixture in the synthesis of spherical silver nanoparticles (AgNPs). Monodisperse AgNPs were synthesized via reduction of silver nitrate using a mixture of two chemical agents: sodium citrate and tannic acid. The shape, size and size distribution of silver particles were determined by UV-Vis spectroscopy, dynamic light scattering (DLS) and scanning transmission electron microscopy (STEM). Special attention is given to understanding and experimentally confirming the exact role of the reagents (sodium citrate and tannic acid present in the reaction mixture) in AgNP synthesis. The oxidation and reduction potentials of silver, tannic acid and sodium citrate in their mixtures were determined using cyclic voltammetry. Possible structures of tannic acid and its adducts with citric acid were investigated in aqueous solution by performing computer simulations in conjunction with the semi-empirical PM7 method. The lowest energy structures found from the preliminary conformational search are shown, and the strength of the interaction between the two molecules was calculated. The compounds present on the surface of the AgNPs were identified using FT-IR spectroscopy, and the results are compared with the IR spectrum of tannic acid theoretically calculated using PM6 and PM7 methods. The obtained results clearly indicate that the combined use of sodium citrate and tannic acid produces monodisperse spherical AgNPs, as it allows control of the nucleation, growth and stabilization of the synthesis process. [Figure not available: see fulltext.

Green synthesis of silver nanoparticles using a Melissa officinalis leaf extract with antibacterial properties

Directory of Open Access Journals (Sweden)

Álvaro de Jesús Ruíz-Baltazar

Full Text Available The exceptional properties of the silver nanoparticles offer several applications in the biomedicine field. The development of antibiotics which are clinically useful against bacteria and drug resistant microorganisms, it is one of the main approaches of silver nanoparticles. However, it is necessary to develop environmentally friendly methods for their synthesis. In this sense, the main objective of this work is focused on to propose a simplified and efficient green synthesis of silver nanoparticles with proven antibacterial properties. The green synthesis route is based on the use of the Melissa officinalis as reducing agent of the silver ions in aqueous solution at room temperature. Complementary, the antibacterial activity of the silver nanoparticles against Staphylococcus aureus and Escherichia coli was confirmed. The silver nanoparticles obtained were characterized by transmission electron microscopy, X-ray diffraction, UV–vis, Raman and FT-IR spectroscopy. The observed results suggested that using Melissa officinalis, it is possible to performed silver nanoparticles with controlled characteristics and with significant inhibitory activity against the Staphylococcus aureus and Escherichia coli. Keywords: Green synthesis, Nanoparticles, Antibacterial effect

Solvothermal synthesis of nanocrystalline KTaO.sub.3./sub. : Effect of solvent dielectric constant

Czech Academy of Sciences Publication Activity Database

Makarova, Marina; Bykov, Pavlo; Drahokoupil, Jan; Čerňanský, Marian; Dlabáček, Zdeněk; Dejneka, Alexandr; Jastrabík, Lubomír; Trepakov, Vladimír

2012-01-01

Roč. 47, č. 7 (2012), s. 1798-1773 ISSN 0025-5408 R&D Projects: GA AV ČR KAN301370701; GA ČR GAP108/12/1941 Institutional research plan: CEZ:AV0Z10100522; CEZ:AV0Z10100520 Keywords : nanostructures * chemical synthesis * Raman spectroscopy * X-ray diffraction Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.913, year: 2012

Synthesis of SiOC:H nanoparticles by electrical discharge in hexamethyldisilazane and water

KAUST Repository

Hamdan, Ahmad

2017-07-25

Nanoparticles have unique properties and are useful in many applications. Efficient synthesis of high yields of nanoparticles remains a challenge. Here, we synthesized SiOC:H, a low-dielectric-constant material, by electrical discharge at the interface of hexamethyldisilazane and water. The nanoparticle production rate of our technique was ∼17 mg per minute. We used Fourier transform infrared spectroscopy, scanning and transmission electron microscopy, and X-ray photoemission spectroscopy to characterize the synthesized material. Heating the nanoparticles to 500 °C for 2 h released hydrogen from CHx groups and evaporated volatile compounds. Our method to produce high yields of low-dielectric-constant nanoparticles for microelectronic applications is promising.

Synthesis of SiOC:H nanoparticles by electrical discharge in hexamethyldisilazane and water

KAUST Repository

Hamdan, Ahmad; Abdul Halim, Rasha; Anjum, Dalaver H.; Cha, Min

2017-01-01

Nanoparticles have unique properties and are useful in many applications. Efficient synthesis of high yields of nanoparticles remains a challenge. Here, we synthesized SiOC:H, a low-dielectric-constant material, by electrical discharge at the interface of hexamethyldisilazane and water. The nanoparticle production rate of our technique was ∼17 mg per minute. We used Fourier transform infrared spectroscopy, scanning and transmission electron microscopy, and X-ray photoemission spectroscopy to characterize the synthesized material. Heating the nanoparticles to 500 °C for 2 h released hydrogen from CHx groups and evaporated volatile compounds. Our method to produce high yields of low-dielectric-constant nanoparticles for microelectronic applications is promising.

Synthesis of eco-friendly silver nanoparticles from Morinda tinctoria leaf extract and its larvicidal activity against Culex quinquefasciatus.

Science.gov (United States)

Kumar, K Ramesh; Nattuthurai, N; Gopinath, Ponraj; Mariappan, Tirupathi

2015-02-01

Mosquitoes are the major vector for the transmission of malaria, dengue fever, yellow fever, filariasis, chikungunya and Japanese encephalitis, and they accounted for global mortality and morbidity with increased resistance to common insecticides. The aim of this study was to investigate the larvicidal potential of the acetone leaf extracts of Morinda tinctoria and synthesized silver nanoparticles against third instar larvae of Culex quinquefasciatus Say (Diptera: Culicidae). Nanoparticles are being used in many commercial applications. It was found that aqueous silver ions can be reduced by aqueous extract of plant parts to generate extremely stable silver nanoparticles in water. Synthesized AgNPs were characterized by ultraviolet-visible (UV-vis) spectroscopy, Atomic force microscopy (AFM) and Fourier transform infrared spectroscopy (FT-IR) analysis. The synthesized silver nanoparticles have also been tested against the third instar larvae of C. quinquefasciatus. The leaf extract and the AgNPs high mortality values were 50 % lethal concentration (LC50) = 8.088 and 1.442 ppm against C. quinquefasciatus, respectively. The results recorded from ultraviolet-visible spectroscopy, atomic force microscopy and Fourier transform infrared spectroscopy support the biosynthesis and characterization of silver nanoparticles. These results suggest that the leaf extract of M. tinctoria and synthesis of AgNPs have the potential to be used as an ideal eco-friendly approach for the control of C. quinquefasciatus. By this approach, it is suggestive that this rapid synthesis of nanoparticles would be proper for developing a biological process for mosquito control.

Terahertz spectroscopy

DEFF Research Database (Denmark)

Jepsen, Peter Uhd

2009-01-01

In this presentation I will review methods for spectroscopy in the THz range, with special emphasis on the practical implementation of the technique known ad THz time-domain spectroscopy (THz-TDS). THz-TDS has revived the old field of far-infrared spectroscopy, and enabled a wealth of new...... activities that promise commercial potential for spectroscopic applications in the THz range. This will be illustrated with examples of spectroscopy of liquids inside their bottles as well as sensitive, quantitative spectroscopy in waveguides....

Continuous microwave flow synthesis of mesoporous hydroxyapatite

International Nuclear Information System (INIS)

Akram, Muhammad; Alshemary, Ammar Z.; Goh, Yi-Fan; Wan Ibrahim, Wan Aini; Lintang, Hendrik O.; Hussain, Rafaqat

2015-01-01

We have successfully used continuous microwave flow synthesis (CMFS) technique for the template free synthesis of mesoporous hydroxyapatite. The continuous microwave flow reactor consisted of a modified 2.45 GHz household microwave, peristaltic pumps and a Teflon coil. This cost effective and efficient system was exploited to produce semi-crystalline phase pure nano-sized hydroxyapatite. Effect of microwave power, retention time and the concentration of reactants on the phase purity, degree of crystallinity and surface area of the final product was studied in detail. X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) were used to study the phase purity and composition of the product, while transmission electron microscopy (TEM) was used to study the effect of process parameters on the morphology of hydroxyapatite. The TEM analysis confirmed the formation of spherical particles at low microwave power; however the morphology of the particles changed to mesoporous needle and rod-like structure upon exposing the reaction mixture to higher microwave power and longer retention time inside the microwave. The in-vitro ion dissolution behavior of the as synthesized hydroxyapatite was studied by determining the amount of Ca 2+ ion released in SBF solution. - Highlights: • Continuous microwave flow synthesis method was used to prepare hydroxyapatite. • Increase in microwave power enhanced the degree of crystallinity. • TEM images confirmed the presence of mesopores on the surface of HA

Continuous microwave flow synthesis of mesoporous hydroxyapatite

Energy Technology Data Exchange (ETDEWEB)

Akram, Muhammad; Alshemary, Ammar Z.; Goh, Yi-Fan; Wan Ibrahim, Wan Aini [Department of Chemistry, Universiti Teknologi Malaysia, 81310 UTM Johor Bahru, Johor (Malaysia); Lintang, Hendrik O. [Centre for Sustainable Nanomaterials (CSNano), Ibnu Sina Institute for Scientific and Industrial Research, Universiti Teknologi Malaysia, 81310 UTM Johor Bahru, Johor (Malaysia); Hussain, Rafaqat, E-mail: rafaqat@kimia.fs.utm.my [Centre for Sustainable Nanomaterials (CSNano), Ibnu Sina Institute for Scientific and Industrial Research, Universiti Teknologi Malaysia, 81310 UTM Johor Bahru, Johor (Malaysia)

2015-11-01

We have successfully used continuous microwave flow synthesis (CMFS) technique for the template free synthesis of mesoporous hydroxyapatite. The continuous microwave flow reactor consisted of a modified 2.45 GHz household microwave, peristaltic pumps and a Teflon coil. This cost effective and efficient system was exploited to produce semi-crystalline phase pure nano-sized hydroxyapatite. Effect of microwave power, retention time and the concentration of reactants on the phase purity, degree of crystallinity and surface area of the final product was studied in detail. X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) were used to study the phase purity and composition of the product, while transmission electron microscopy (TEM) was used to study the effect of process parameters on the morphology of hydroxyapatite. The TEM analysis confirmed the formation of spherical particles at low microwave power; however the morphology of the particles changed to mesoporous needle and rod-like structure upon exposing the reaction mixture to higher microwave power and longer retention time inside the microwave. The in-vitro ion dissolution behavior of the as synthesized hydroxyapatite was studied by determining the amount of Ca{sup 2+} ion released in SBF solution. - Highlights: • Continuous microwave flow synthesis method was used to prepare hydroxyapatite. • Increase in microwave power enhanced the degree of crystallinity. • TEM images confirmed the presence of mesopores on the surface of HA.

Size-controlled one-pot synthesis of fluorescent cadmium sulfide semiconductor nanoparticles in an apoferritin cavity

International Nuclear Information System (INIS)

Iwahori, K; Yamashita, I

2008-01-01

A simple size-controlled synthesis of cadmium sulfide (CdS) nanoparticle (NP) cores in the cavity of apoferritin from horse spleen (HsAFr) was performed by a slow chemical reaction synthesis and a two-step synthesis protocol. We found that the CdS NP core synthesis was slow and that premature CdS NP cores were formed in the apoferritin cavity when the concentration of ammonia water was low. It was proven that the control of the ammonia water concentration can govern the CdS NP core synthesis and successfully produce size-controlled CdS NP cores with diameters from 4.7 to 7.1 nm with narrow size dispersion. X-ray powder diffraction (XRD), energy dispersive spectroscopy (EDS) analysis and high-resolution transmission electron microscopy (HR-TEM) observation characterized the CdS NP cores obtained as cubic polycrystalline NPs, which showed photoluminescence with red shifts depending on their diameters. From the research of CdS NP core synthesis in the recombinant apoferritins, the zeta potential of apoferritin is important for the biomineralization of CdS NP cores in the apoferritin cavity. These synthesized CdS NPs with different photoluminescence properties will be applicable in a wide variety of nano-applications.

Assessment of PVA/silver nanocomposite hydrogel patch as antimicrobial dressing scaffold: Synthesis, characterization and biological evaluation

International Nuclear Information System (INIS)

Bhowmick, Sirsendu; Koul, Veena

2016-01-01

A novel, elastic, non-adhesive and antimicrobial hydrogel PVA scaffold (loaded with AgNPs) synthesized using freeze-thaw method has been characterized in this study. The direct visualization of the as synthesized (one-pot green synthesis methodology) AgNPs using TEM shows particle size in the range of 7 ± 3 nm. The minimum inhibitory concentration (MIC) of AgNPs for Staphylococcus aureus and Escherichia coli was estimated to be 7.81 μg/mL, whereas for Pseudomonas aeruginosa (gram negative) it was around 3.90 μg/mL. The antimicrobial efficacy of AgNPs was further studied by protein leakage, ROS and LDH activity assay. The quantitative elemental analysis of silver was calculated before and after release in phosphate buffer (pH-7.4) by atomic absorption spectroscopy. The antimicrobial efficacy of the scaffold was retained even after 96 h of release of AgNPs which suggests that the scaffold can be used as a reservoir for AgNPs to maintain a moist and sterile environment for a long period of time. - Highlights: • Green synthesis of AgNPs and evaluation of its antimicrobial efficacy • Synthesis of PVA hydrogel by freeze thaw technique • Antimicrobial activity of AgNPs loaded PVA hydrogel by zone of inhibition • Release kinetics of AgNPs from hydrogel by atomic absorption spectroscopy

Insitu synthesis of self-assembled gold nanoparticles on glass or silicon substrates through reactive inkjet printing

KAUST Repository

Abulikemu, Mutalifu

2013-12-18

A facile and low cost method for the synthesis of self-assembled nanoparticles (NPs) with minimal size variation and chemical waste by using reactive inkjet printing was developed. Gold NPs with diameters as small as (8±2)nm can be made at low temperature (120 °C). The size of the resulting NPs can be readily controlled through the concentration of the gold precursor and oleylamine ink. The pure gold composition of the synthesized NPs was confirmed by energy-dispersive X-ray spectroscopy (EDXS) analysis. High-resolution SEM (HRSEM) and TEM (HRTEM), and X-ray diffraction revealed their size and face-centered cubic (fcc) crystal structure, respectively. Owing to the high density of the NP film, UV/Vis spectroscopy showed a red shift in the intrinsic plasmonic resonance peak. We envision the extension of this approach to the synthesis of other nanomaterials and the production of tailored functional nanomaterials and devices. Midas touch: The use of low-cost manufacturing approaches in the synthesis of nanoparticles is critical for many applications. Reactive inkjet printing, along with a judicious choice of precursor/solvent system, was used to synthesize a relatively uniform assembly of crystalline gold nanoparticles, with diameters as small as (8±2)nm, over a given substrate surface. © 2014 WILEY-VCH Verlag GmbH.

Harnessing the wine dregs: An approach towards a more sustainable synthesis of gold and silver nanoparticles.

Science.gov (United States)

González-Ballesteros, N; Rodríguez-González, J B; Rodríguez-Argüelles, M C

2018-01-01

In recent years, the management of food waste processing has emerged as a major concern. One such type of food waste, grape pomace, has been shown to be a great source of bioactive compounds which might be used for more environmentally - friendly processes for the synthesis of nanomaterials. In this study, grape pomace of Vitis vinifera has been used for the obtainment of an aqueous extract. Firstly, the reducing activity, total phenolic content and DPPH scavenging activity of the aqueous extract were determined. Then, the aqueous extract was used for the synthesis of gold and silver nanoparticles. The formation of spherical and stable nanoparticles with mean diameters of 35.3±5.2nm for Au@GP and 42.9±6.4nm for Ag@GP was confirmed by UV-vis spectroscopy and transmission electron microscopy. Furthermore, the functional group of biomolecules present in grape pomace extract, Au@GP and Ag@GP, were characterized by Fourier transform infrared spectroscopy prior to and after the synthesis, in order to obtain information about the biomolecules involved in the reducing and stabilization process. This study is the first to deal with the use of Vitis vinifera grape pomace in obtaining gold and silver nanoparticles through an eco-friendly, quick, one-pot synthetic route. Copyright © 2017 Elsevier B.V. All rights reserved.

Assessment of PVA/silver nanocomposite hydrogel patch as antimicrobial dressing scaffold: Synthesis, characterization and biological evaluation

Energy Technology Data Exchange (ETDEWEB)

Bhowmick, Sirsendu; Koul, Veena, E-mail: veenak@iitd.ac.in

2016-02-01

A novel, elastic, non-adhesive and antimicrobial hydrogel PVA scaffold (loaded with AgNPs) synthesized using freeze-thaw method has been characterized in this study. The direct visualization of the as synthesized (one-pot green synthesis methodology) AgNPs using TEM shows particle size in the range of 7 ± 3 nm. The minimum inhibitory concentration (MIC) of AgNPs for Staphylococcus aureus and Escherichia coli was estimated to be 7.81 μg/mL, whereas for Pseudomonas aeruginosa (gram negative) it was around 3.90 μg/mL. The antimicrobial efficacy of AgNPs was further studied by protein leakage, ROS and LDH activity assay. The quantitative elemental analysis of silver was calculated before and after release in phosphate buffer (pH-7.4) by atomic absorption spectroscopy. The antimicrobial efficacy of the scaffold was retained even after 96 h of release of AgNPs which suggests that the scaffold can be used as a reservoir for AgNPs to maintain a moist and sterile environment for a long period of time. - Highlights: • Green synthesis of AgNPs and evaluation of its antimicrobial efficacy • Synthesis of PVA hydrogel by freeze thaw technique • Antimicrobial activity of AgNPs loaded PVA hydrogel by zone of inhibition • Release kinetics of AgNPs from hydrogel by atomic absorption spectroscopy.

Synthesis and applications of 13C glycerol

International Nuclear Information System (INIS)

Stocking, E.; Khalsa, O.; Martinez, R.; Silks, L.A. III

1994-01-01

The authors are currently developing new synthetic routes to the various isotopomers of glycerol. Labeled glycerol is useful for 13 C enrichment of biomolecules. However, traditional methods of glycerol synthesis are not easily adapted for isotopic enrichment or have poor overall yields (12-15%). In addition, the use of glycerol for enrichment can be prohibitively expensive and its availability depends on the level of demand. The authors have developed a short de novo synthesis of [U- 13 C]glycerol from carbon dioxide (∼53% overall yield for four steps) and are currently examining the feasibility of synthesizing site-specific 13 C labeled glycerol and dihydroxyacetone (DHA) from methanol and carbon dioxide. The authors have examined the enzymatic conversion of [U- 13 C]glycerol to glyceraldehyde-3-monophosphate or dihydroxyacetone monophosphate (DHAP) with yields ranging from 25-50% (as determined by NMR spectroscopy). The authors are also pursuing the chemical conversion of 13 C labeled DHA to DHAP and the results are presented. Labeled DHAP is a possible enzymatic precursor for both labeled 2-deoxyribose and 2-deoxyribonucleic acids

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.

Synthesis of higher diamondoids by pulsed laser ablation plasmas in supercritical CO2

International Nuclear Information System (INIS)

Nakahara, Sho; Stauss, Sven; Kato, Toru; Terashima, Kazuo; Sasaki, Takehiko

2011-01-01

Pulsed laser ablation (wavelength 532 nm; fluence 18 J/cm 2 ; pulse width 7 ns; repetition rate 10 Hz) of highly oriented pyrolytic graphite was conducted in adamantane-dissolved supercritical CO 2 with and without cyclohexane as a cosolvent. Micro-Raman spectroscopy of the products revealed the presence of hydrocarbons possessing sp 3 -hybridized carbons similar to diamond structures. The synthesis of diamantane and other possible diamondoids consisting of up to 12 cages was confirmed by gas chromatography-mass spectrometry. Furthermore, gas chromatography-mass spectrometry measurements of samples before and after pyrolysis treatment indicate the synthesis of the most compact decamantane, namely, superadamantane. It is thought that oxidant species originating from CO 2 during pulsed laser ablation might lead to the selective dissociation of C-H bonds, enabling the synthesis of low H/C ratio molecules. Therefore, laser ablation in supercritical CO 2 is proposed as a practical method for synthesizing diamondoids.

Ergonomic Synthesis Suitable for Industrial Production of Silver-Festooned Zinc Oxide Nanorods

Science.gov (United States)

Khan, G. R.; Khan, R. A.

2015-07-01

For maximizing productivity, minimizing cost, time-boxing process and optimizing human effort, a single-step, cost-effective, ultra-fast and environmentally benign synthesis suitable for industrial production of nanocrystalline ZnO, and Ag-doped ZnO has been reported in this paper. The synthesis based on microwave-supported aqueous solution method used zinc acetate dehydrate and silver nitrate as precursors for fabrication of nanorods. The synthesized products were characterized by X-ray diffractometry (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Raman spectroscopy and UV-Vis-NIR spectroscopy. The undoped and Ag-doped ZnO nanorods crystallized in a hexagonal wurtzite structure having spindle-like morphology. The blue shift occurred at absorption edge of Ag-doped ZnO around 260 nm compared to 365 nm of bulk ZnO. The red shift occurred at Raman peak site of 434 cm-1 compared to characteristic wurtzite phase peak of ZnO (437 cm-1). The bandgap energies were found to be 3.10 eV, 3.11 eV and 3.18 eV for undoped, 1% Ag-doped, and 3% Ag-doped ZnO samples, respectively. The TEM results provided average particle sizes of 17 nm, 15 nm and 13 nm for undoped, and 1% and 3% Ag-doped ZnO samples, respectively.

Efficient Synthesis of Single-Chain Polymer Nanoparticles via Amide Formation

Directory of Open Access Journals (Sweden)

Ana Sanchez-Sanchez

2015-01-01

Full Text Available Single-chain technology (SCT allows the transformation of individual polymer chains to folded/collapsed unimolecular soft nanoparticles. In this work we contribute to the enlargement of the SCT toolbox by demonstrating the efficient synthesis of single-chain polymer nanoparticles (SCNPs via intrachain amide formation. In particular, we exploit cross-linking between active methylene groups and isocyanate moieties as powerful “click” chemistry driving force for SCNP construction. By employing poly(methyl methacrylate- (PMMA- based copolymers bearing β-ketoester units distributed randomly along the copolymer chains and bifunctional isocyanate cross-linkers, SCNPs were successfully synthesized at r.t. under appropriate reaction conditions. Characterization of the resulting SCNPs was carried out by means of a combination of techniques including size exclusion chromatography (SEC, infrared (IR spectroscopy, proton nuclear magnetic resonance (1H NMR spectroscopy, dynamic light scattering (DLS, and elemental analysis (EA.

Green Synthesis of Silver Nanoparticles and the Study of Optical Properties

Directory of Open Access Journals (Sweden)

Ramakrishna Vasireddy

2012-08-01

Full Text Available The synthesis of silver nanoparticles of varying size has been achieved using different molar concentrations of NaOH while the effect of changing the temperature has been studied. AgNO3, gelatine, glucose and NaOH are used as a silver precursor, stabilizer, reducing agent and accelerator respectively. The synthesized nanoparticles have been characterized by a FESEM study, X‐ray diffractometry, Raman spectroscopy and UV‐vis spectroscopy. The colloidal sols of the silver nanoparticles in a biopolymer gelatine show strong surface plasmon resonance absorption peaks. The visible photoluminescence emission from the synthesized silver nanocrystals has been recorded within the wavelength range of 400‐600 nm under UV excitation. The synthesized nanoparticles may be extremely useful in making biosensor devices as well as for other applications.

Synthesis of molybdenum oxide (MoO3) nanoparticles by hydrolysis method

International Nuclear Information System (INIS)

Alfons, M.; Manoj, V.; Karthika, M.; Karn, R.K.; John Bosco Balaguru, R.; Jeyadheepan, K.; Pandiyan, S.K.; Boomadevi, S.

2013-01-01

A pure crystalline MoO 3 nanoparticles were synthesized using Ammonium molybdate (NH 4 ) 6 Mo 7 O 24. 4H 2 O precursor and sodium carboxymethyl cellulose (CMC) capping agent. Various reaction parameters such as the additive/Mo molar ratio and temperature of the synthesis media were optimized to analyze the morphology and size of the nanoparticles. The prepared nanoparticles were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and Scanning Electron Microscopy (FESEM). (author)

Synthesis of Pt/rGO catalysts with two different reducing agents and their methanol electrooxidation activity

Energy Technology Data Exchange (ETDEWEB)

Vu, Thu Ha Thi, E-mail: ptntd2004@yahoo.fr [Key Laboratory for Petrochemical and Refinery Technologies, 2 Pham Ngu Lao street, Hanoi (Viet Nam); Tran, Thanh Thuy Thi, E-mail: tranthithanhthuygl@gmail.com [Key Laboratory for Petrochemical and Refinery Technologies, 2 Pham Ngu Lao street, Hanoi (Viet Nam); Le, Hong Ngan Thi; Tran, Lien Thi; Nguyen, Phuong Hoa Thi; Nguyen, Minh Dang [Key Laboratory for Petrochemical and Refinery Technologies, 2 Pham Ngu Lao street, Hanoi (Viet Nam); Quynh, Bui Ngoc [Institut de recherches sur la catalyse et l’environnement de Lyon, UMR5256, 2 avenue Albert Einstein, 69626 Villeurbanne cedex (France)

2016-01-15

Highlights: • Pt/rGO catalysts were successfully synthesized using either NaBH{sub 4} or ethylene glycol. • Synthesis using NaBH{sub 4} could improve electrocatalytic towards methanol oxidation of Pt/rGO catalyst. • 40%Pt/rGO synthesized using NaBH{sub 4} showed the best electrocatalytic performance. - Abstract: The synthesis processes of Platinum (Pt) on reduced graphene oxide (rGO) catalysts from graphene oxide (GO) using two reducing agents including sodium borohydride and ethylene glycol is reported. Structure and morphology of Pt/rGO catalysts are characterized by X-ray powder diffraction, transmission electron microscopy, Raman spectroscopy, and X-ray photoelectron spectroscopy. Electrocatalytic methanol oxidation properties of these catalysts are evaluated by cyclic voltammetry and chronoamperometry. The results show that catalyst synthesized using sodium borohydride has a higher metallic Pt content and an improved catalytic performance in comparison to catalyst synthesized using ethylene glycol. Moreover, effect of Pt loading amount on electrocatalytic methanol oxidation performance of catalysts synthesized using sodium borohydride is systematically investigated. The optimal Pt loading amount on graphene is determined to be 40%.

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.

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)

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

Microwave assisted synthesis of MnO2 on nickel foam-graphene for electrochemical capacitor

International Nuclear Information System (INIS)

Bello, A.; Fashedemi, O.O.; Fabiane, M.; Lekitima, J.N.; Ozoemena, K.I.; Manyala, N.

2013-01-01

Highlights: •Three-dimensional synthesis of graphene using CVD. •Hydrothermal deposition (microwave irradiation) of MnO 2 on graphene. •Morphologies of the composite reveals flower-like nanostructures of MnO 2 on graphene. •Composite exhibit excellent electrochemical performance. -- Abstract: A green chemistry approach (hydrothermal microwave irradiation) has been used to deposit manganese oxide on nickel foam-graphene. The 3D graphene was synthesized using nickel foam template by chemical vapor deposition (CVD) technique. Raman spectroscopy, X-ray diffraction (XRD), scanning electron and transmission electron microscopies (SEM and TEM) have been used to characterize structure and surface morphology of the composite, respectively. The Raman spectroscopy measurements on the samples reveal that 3D graphene consists of mostly few layers with low defect density. The composite was tested in a three electrode configuration for electrochemical capacitor, and exhibited a specific capacitance of 305 F g −1 at a current density of 1 A g −1 and showed excellent cycling stability. The obtained results demonstrate that microwave irradiation technique could be a promising approach to synthesis graphene based functional materials for electrochemical applications

Latex-mediated synthesis of ZnS nanoparticles: green synthesis approach

Energy Technology Data Exchange (ETDEWEB)

Hudlikar, Manish; Joglekar, Shreeram [University of Pune, Division of Biochemistry, Department of Chemistry (India); Dhaygude, Mayur [National Chemical Laboratory, Polymer Science and Engineering Division (India); Kodam, Kisan, E-mail: kodam@chem.unipune.ac.in [University of Pune, Division of Biochemistry, Department of Chemistry (India)

2012-05-15

A low-cost, green synthesis of ZnS nanoparticles is reported using 0.3 % latex solution prepared from Jatropha curcas L. ZnS nanoparticles were characterized by X-ray diffraction, selected area electron diffraction, transmission electron microscopy, energy dispersive analysis of X-rays, UV-vis optical absorption and photoluminescence techniques. Fourier Transform Infrared Spectroscopy was performed to find the role of cyclic peptides namely curcacycline A (an octapeptide), curcacycline B (a nonapeptide) and curcain (an enzyme) as a possible reducing and stabilizing agents present in the latex of J. curcas L. The average size of ZnS nanoparticles was found to be 10 nm. Latex of J. curcas L. itself acts as a source of sulphide (S{sup -2}) ions that are donated to Zn ions under present experimental conditions. Source of sulphide (S{sup -2}) ions is still unclear, but we speculate that cysteine or thiol residues present in enzyme curcain may be donating these sulphide (S{sup -2}) ions.

Latex-mediated synthesis of ZnS nanoparticles: green synthesis approach

Science.gov (United States)

Hudlikar, Manish; Joglekar, Shreeram; Dhaygude, Mayur; Kodam, Kisan

2012-05-01

A low-cost, green synthesis of ZnS nanoparticles is reported using 0.3 % latex solution prepared from Jatropha curcas L. ZnS nanoparticles were characterized by X-ray diffraction, selected area electron diffraction, transmission electron microscopy, energy dispersive analysis of X-rays, UV-vis optical absorption and photoluminescence techniques. Fourier Transform Infrared Spectroscopy was performed to find the role of cyclic peptides namely curcacycline A (an octapeptide), curcacycline B (a nonapeptide) and curcain (an enzyme) as a possible reducing and stabilizing agents present in the latex of J. curcas L. The average size of ZnS nanoparticles was found to be 10 nm. Latex of J. curcas L. itself acts as a source of sulphide (S-2) ions that are donated to Zn ions under present experimental conditions. Source of sulphide (S-2) ions is still unclear, but we speculate that cysteine or thiol residues present in enzyme curcain may be donating these sulphide (S-2) ions.

Latex-mediated synthesis of ZnS nanoparticles: green synthesis approach

International Nuclear Information System (INIS)

Hudlikar, Manish; Joglekar, Shreeram; Dhaygude, Mayur; Kodam, Kisan

2012-01-01

A low-cost, green synthesis of ZnS nanoparticles is reported using 0.3 % latex solution prepared from Jatropha curcas L. ZnS nanoparticles were characterized by X-ray diffraction, selected area electron diffraction, transmission electron microscopy, energy dispersive analysis of X-rays, UV–vis optical absorption and photoluminescence techniques. Fourier Transform Infrared Spectroscopy was performed to find the role of cyclic peptides namely curcacycline A (an octapeptide), curcacycline B (a nonapeptide) and curcain (an enzyme) as a possible reducing and stabilizing agents present in the latex of J. curcas L. The average size of ZnS nanoparticles was found to be 10 nm. Latex of J. curcas L. itself acts as a source of sulphide (S −2 ) ions that are donated to Zn ions under present experimental conditions. Source of sulphide (S −2 ) ions is still unclear, but we speculate that cysteine or thiol residues present in enzyme curcain may be donating these sulphide (S −2 ) ions.

Synthesis and characterization of silver nanoparticles: effect on phytopathogen Colletotrichum gloesporioides

Energy Technology Data Exchange (ETDEWEB)

Aguilar-Mendez, Miguel A., E-mail: maguilarme@ipn.mx; San Martin-Martinez, Eduardo; Ortega-Arroyo, Lesli [Instituto Politecnico Nacional, Centro de Investigacion en Ciencia Aplicada y Tecnologia Avanzada (Mexico); Cobian-Portillo, Georgina [Instituto Politecnico Nacional, Centro Interdisciplinario de Investigacion para el Desarrollo Integral Regional (Mexico); Sanchez-Espindola, Esther [Instituto Politecnico Nacional, Escuela Nacional de Ciencias Biologicas, Prolongacion Manuel M. Carpio s/n, esq. Plan de Ayala (Mexico)

2011-06-15

Colloidal silver nanoparticles were synthesized by reducing silver nitrate solutions with glucose, in the presence of gelatin as capping agent. The obtained nanoparticles were characterized by means of UV-Vis spectroscopy, transmission electron microscopy (TEM), and Fourier transform infrared (FTIR) spectroscopy. The response surface methodology (RSM) was also used to determine the influence of the variables on the size of the nanoparticles. The antifungal activity of the silver nanoparticles was evaluated on the phytopathogen Colletotrichum gloesporioides, which causes anthracnose in a wide range of fruits. The UV-Vis spectra indicated the formation of silver nanoparticles preferably spherical and of relatively small size (<20 nm). The above-mentioned was confirmed by TEM, observing a size distribution of 5-24 nm. According to RSM the synthesis variables influenced on the size of the silver nanoparticles. By means of FTIR spectroscopy it was determined that gelatin, through their amide and hydroxyl groups, interacts with nanoparticles preventing their agglomeration. The growth of C. gloesporioides in the presence of silver nanoparticles was significantly delayed in a dose dependent manner.

Facile synthesis of PdAgTe nanowires with superior electrocatalytic activity

Science.gov (United States)

Hong, Wei; Wang, Jin; Wang, Erkang

2014-12-01

In this work, ultrathin Te nanowires (NWs) with high-aspect-ratio are prepared by a simple hydrothermal method. By using Te NWs as the sacrificial template, we demonstrate a facile and efficient method for the synthesis of PdAgTe NWs with high-quality through the partly galvanic replacement between Te NWs and the corresponding noble metal salts precursors in an aqueous solution. The compositions of PdAgTe NWs can be tuned by simply altering the concentration of the precursors. After cyclic voltammetry treatment, multi-component PdAgTe NW with a highly active and stable surface can be obtained. The structure and composition of the as-prepared nanomaterials are analyzed by transmission electron microscope, X-ray diffraction, energy dispersive X-ray spectroscopy, inductively coupled plasma-mass spectroscopy and X-ray photoelectron spectroscopy. Electrochemical catalytic measurement results prove that the as synthesized PdAgTe NWs present superior catalytic activity toward ethanol electrooxidation in alkaline solution than the commercial Pd/C catalyst, which making them can be used as effective catalysts for the direct ethanol fuel cells.

Synthesis and characterization of silver nanoparticles: effect on phytopathogen Colletotrichum gloesporioides

International Nuclear Information System (INIS)

Aguilar-Méndez, Miguel A.; San Martín-Martínez, Eduardo; Ortega-Arroyo, Lesli; Cobián-Portillo, Georgina; Sánchez-Espíndola, Esther

2011-01-01

Colloidal silver nanoparticles were synthesized by reducing silver nitrate solutions with glucose, in the presence of gelatin as capping agent. The obtained nanoparticles were characterized by means of UV–Vis spectroscopy, transmission electron microscopy (TEM), and Fourier transform infrared (FTIR) spectroscopy. The response surface methodology (RSM) was also used to determine the influence of the variables on the size of the nanoparticles. The antifungal activity of the silver nanoparticles was evaluated on the phytopathogen Colletotrichum gloesporioides, which causes anthracnose in a wide range of fruits. The UV–Vis spectra indicated the formation of silver nanoparticles preferably spherical and of relatively small size (<20 nm). The above-mentioned was confirmed by TEM, observing a size distribution of 5–24 nm. According to RSM the synthesis variables influenced on the size of the silver nanoparticles. By means of FTIR spectroscopy it was determined that gelatin, through their amide and hydroxyl groups, interacts with nanoparticles preventing their agglomeration. The growth of C. gloesporioides in the presence of silver nanoparticles was significantly delayed in a dose dependent manner.

Streptomyces somaliensis mediated green synthesis of silver nanoparticles

Directory of Open Access Journals (Sweden)

Meysam Soltani Nejad

2015-07-01

Full Text Available Objective(s: The development of reliable and ecofriendly process for the synthesis of nano-metals is an important aspect in the field of nanotechnology. Nano-metals are a special group of materials with broad area of applications. Materials and Methods: In this study, extracellular synthesis of silver nanoparticles (SNPs performed by use of the gram positive soil Streptomycetes. Streptomycetes isolated from rice fields of Guilan Province, Iran (5 isolates. Initial characterization of SNPs was performed by visual change color. To determine the bacterium taxonomical identity, its colonies characterized morphologically by use of scanning electron microscope. The PCR molecular analysis of active isolate represented its identity partially. In this regard, 16S rDNA of isolate G was amplified using universal bacterial primers FD1 and RP2. The PCR products were purified and sequenced. Sequence analysis of 16S rDNA was then conducted using NCBI GenBank database using BLAST. Also SNPs were characterized by, transmission electron microscopy (TEM and X-ray diffraction spectroscopy (XRD. Results: From all 5 collected Streptomyces somaliensis isolates, isolate G showed highest extracellular synthesis of SNPs via in vitro. SNPs were formed immediately by the addition of (AgNO3 solution (1 mM. UV-visible spectrophotometry for measuring surface plasmon resonance showed a single absorption peak at 450 nm, which confirmed the presence of SNPs. TEM revealed the extracellular formation of spherical silver nanoparticles in the size range of 5-35 nm. Conclusions: The biological approach for the synthesis of metal nanoparticles offers an environmentally benign alternative to the traditional chemical and physical synthesis methods. So, a simple, environmentally friendly and cost-effective method has been developed to synthesize AgNPs using Streptomycetes.

Large influence of the synthesis conditions on the physico-chemical properties of nanostructured Fe3O4

International Nuclear Information System (INIS)

Franger, S.; Berthet, P.; Dragos, O.; Baddour-Hadjean, R.; Bonville, P.; Berthon, J.

2007-01-01

Magnetite synthesized via three different synthesis routes (coprecipitation process in aqueous media, electrochemical synthesis in presence of complexing agents and solid state reaction at high temperature) has been characterized by X-Ray diffraction, scanning electron microscopy, thermal analysis (TGA), FT-IR and Moessbauer spectroscopies. Although each procedure gave homogeneous magnetite powders, many differences could be seen in the physico-chemical properties of the samples mostly depending on the synthesis conditions. For instance, at least two factors seem to have a huge impact onto the Fe 3 O 4 behaviour: the presence of hydration water molecules and the particle size of the powders since a superparamagnetic behaviour was observed with the thinnest particles, at room temperature, on the Moessbauer spectra via the appearance of line broadening and a pronounced central doublet

Sum Frequency Generation Vibrational Spectroscopy of 1,3-Butadiene Hydrogenation on 4 nm Pt@SiO 2 , Pd@SiO 2 , and Rh@SiO 2 Core–Shell Catalysts

KAUST Repository

Krier, James M.; Michalak, William D.; Cai, Xiaojun; Carl, Lindsay; Komvopoulos, Kyriakos; Somorjai, Gabor A.

2015-01-01

NPs (Stöber encapsulation) prepared by colloidal synthesis. Sum frequency generation (SFG) vibrational spectroscopy was performed to correlate surface intermediates observed in situ with reaction selectivity. It is shown that calcination is effective

Synthesis of nanosilver on polyamide fabric using silver/ammonia complex

Energy Technology Data Exchange (ETDEWEB)

Montazer, Majid, E-mail: tex5mm@aut.ac.ir [Textile Department, Functional Fibrous Structures and Environmental Enhancement (FFSEE), Amirkabir University of Technology, Hafez Avenue, Tehran (Iran, Islamic Republic of); Shamei, Ali; Alimohammadi, Farbod [Young Researchers Club, Tehran South Branch, Islamic Azad University, Tehran (Iran, Islamic Republic of)

2014-05-01

In this paper, a novel synthesis method for nanosilver has been introduced on or within the polymeric chains of polyamide 6 fabric by using silver/ammonia complex [Ag(NH{sub 3}){sub 2}]{sup +}. The silver complex was reduced directly by functional groups of polyamide chains without using any additional chemical reducing agents. The polyamide fabric was also stabilized with formation of new linkages between the polymeric chains of the nylon fabric through silver nanoparticle synthesis. The presence of nanosilver on the fabric was confirmed by UV–vis spectra, EDX patterns and XRD patterns. In addition, X-ray photoelectron spectroscopy (XPS) was utilized to identify the chemical state of silver in a range of silver oxide and silver metal. The SEM images confirmed the presence of nanosilver on the polyamide within the size of 20 and 150 nm. Excellent antibacterial properties were achieved with the treated fabrics against Staphylococcus aureus and Escherichia coli. Further, the antibacterial properties of the polyamide fabric treated with 35 mg/L silver/ammonia were durable against washing as they only decreased to 98.6% after 20 washes. In addition, some other properties of the treated fabrics including color changes, dimensional stability, water droplet adsorption, and reflectance spectrum are reported and thoroughly discussed. - Highlights: • Novel in situ synthesis of nanosilver on polyamide 6 • Synthesis of nanosilver without using external stabilizing and reducing agent • Synthesis of nanosilver particles within molecular chains of polyamide 6 • Producing antibacterial polyamide 6 using 35 mg/L Ag/ammonia complex • Obtaining durable antibacterial properties on polyamide 6 by this method.

Synthesis of nanosilver on polyamide fabric using silver/ammonia complex

International Nuclear Information System (INIS)

Montazer, Majid; Shamei, Ali; Alimohammadi, Farbod

2014-01-01

In this paper, a novel synthesis method for nanosilver has been introduced on or within the polymeric chains of polyamide 6 fabric by using silver/ammonia complex [Ag(NH 3 ) 2 ] + . The silver complex was reduced directly by functional groups of polyamide chains without using any additional chemical reducing agents. The polyamide fabric was also stabilized with formation of new linkages between the polymeric chains of the nylon fabric through silver nanoparticle synthesis. The presence of nanosilver on the fabric was confirmed by UV–vis spectra, EDX patterns and XRD patterns. In addition, X-ray photoelectron spectroscopy (XPS) was utilized to identify the chemical state of silver in a range of silver oxide and silver metal. The SEM images confirmed the presence of nanosilver on the polyamide within the size of 20 and 150 nm. Excellent antibacterial properties were achieved with the treated fabrics against Staphylococcus aureus and Escherichia coli. Further, the antibacterial properties of the polyamide fabric treated with 35 mg/L silver/ammonia were durable against washing as they only decreased to 98.6% after 20 washes. In addition, some other properties of the treated fabrics including color changes, dimensional stability, water droplet adsorption, and reflectance spectrum are reported and thoroughly discussed. - Highlights: • Novel in situ synthesis of nanosilver on polyamide 6 • Synthesis of nanosilver without using external stabilizing and reducing agent • Synthesis of nanosilver particles within molecular chains of polyamide 6 • Producing antibacterial polyamide 6 using 35 mg/L Ag/ammonia complex • Obtaining durable antibacterial properties on polyamide 6 by this method

Microwave-assisted synthesis and micellization behavior of soy-based copoly(2-oxazoline)s

OpenAIRE

Hoogenboom, Richard; Leenen, Mark A. M.; Huang, Haiying; Fustin, Charles-Andr?; Gohy, Jean-Fran?ois; Schubert, Ulrich S.

2006-01-01

Polymers based on renewable resources are promising candidates for replacing common organic polymers, and thus, for reducing oil consumption. In this contribution we report the microwave-assisted synthesis of block and statistical copolymers from 2-ethyl-2-oxazoline and 2-?soy alkyl?-2-oxazoline via a cationic ring-opening polymerization mechanism. The synthesized copolymers were characterized by gel permeation chromatography and 1H-NMR spectroscopy. The micellization of these amphiphilic cop...

Melanin-Like Pigment Synthesis by Soil Bacillus weihenstephanensis Isolates from Northeastern Poland.

Directory of Open Access Journals (Sweden)

Justyna M Drewnowska

Full Text Available Although melanin is known for protecting living organisms from harmful physical and chemical factors, its synthesis is rarely observed among endospore-forming Bacillus cereus sensu lato. Here, for the first time, we reported that psychrotolerant Bacillus weihenstephanensis from Northeastern Poland can produce melanin-like pigment. We assessed physicochemical properties of the pigment and the mechanism of its synthesis in relation to B. weihenstephanensis genotypic and phenotypic characteristics. Electron paramagnetic resonance (EPR spectroscopy displayed a stable free radical signal of the pigment from environmental isolates which are consistent with the commercial melanin. Fourier transform infrared spectroscopy (FT-IR and physicochemical tests indicated the phenolic character of the pigment. Several biochemical tests showed that melanin-like pigment synthesis by B. weihenstephanensis was associated with laccase activity. The presence of the gene encoding laccase was confirmed by the next generation whole genome sequencing of one B. weihenstephanensis strain. Biochemical (API 20E and 50CHB tests and genetic (Multi-locus Sequence Typing, 16S rRNA sequencing, and Pulsed-Field Gel Electrophoresis characterization of the isolates revealed their close relation to the psychrotrophic B. weihenstephanensis DSMZ 11821 reference strain. The ability to synthesize melanin-like pigment by soil B. weihenstephanensis isolates and their psychrotrophic character seemed to be a local adaptation to a specific niche. Detailed genetic and biochemical analyses of melanin-positive environmental B. weihenstephanensis strains shed some light on the evolution and ecological adaptation of these bacteria. Moreover, our study raised new biotechnological possibilities for the use of water-soluble melanin-like pigment naturally produced by B. weihenstephanensis as an alternative to commercial non-soluble pigment.

Gamma Spectroscopy

NARCIS (Netherlands)

Niemantsverdriet, J.W.; Butz, Tilman; Ertl, G.; Knözinger, H.; Schüth, F.

2008-01-01

No abstract. The sections in this article are 1 Introduction 2 Mössbauer Spectroscopy 3 Time-Differential Perturbed Angular Correlations (TDPAC) 4 Conclusions and Outlook Keywords: Mössbauer spectroscopy; gamma spectroscopy; perturbed angular correlation; TDPAC

Sedimentation in Particulate Aqueous Suspensions as studied by means of Dielectric Time Domain Spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Pettersen, Bjoernar Hauknes

1997-12-31

Many problems in offshore oil production and multiphase transport are related to surface and colloid chemistry. This thesis applies dielectric spectroscopy as an experimental technique to study the behaviour of particle suspensions in polar media. The thesis opens with an introduction to suspensions and time domain dielectric spectroscopy. It then investigates the dielectric properties of silica and alumina dispersed in polar solvents. It is found that theoretical models can be used to calculate the volume fraction disperse phase in the suspension and that the particle sedimentation depends on the wetting of the particles, charge on the particle surface and viscosity of the solvent, and that this dependency can be measured by time domain dielectric spectroscopy. When the surface properties of silica and alumina particles were modified by coating them with a non-ionic polymer and a non-ionic surfactant, then different degrees of packing in the sedimented phase at the bottom of the sedimentation vessel occurred. Chemometrical methods on the synthesis of monodisperse silica particles were used to investigate what factors influence the particle size. It turned out that it is insufficient to consider only main variables when discussing the results of the synthesis. By introducing interaction terms, the author could explain the variation in the size of particles synthesized. The difference in the sedimentation rate of monodisperse silica particles upon variation of volume fraction particles, pH, salinity, amount of silanol groups at the particle surface and temperature was studied. The cross interactions play an important role and a model explaining the variation in sedimentation is introduced. Finally, magnetic particles dispersed in water and in an external magnetic field were used to study the impact on the sedimentation due to the induced flocculation. 209 refs., 90 figs., 9 tabs.

ASSESSMENT OF TECHNETIUM LEACHABILITY IN CEMENT-STABILIZED BASIN 43 GROUNDWATER BRINE

International Nuclear Information System (INIS)

Duncan, J.B.; Cooke, G.A.; Lockrem, L.L.

2009-01-01

This report documents the effort to sequester technetium by the use of getters, reductants (tin(II) apatite and ferrous sulfate), sorbents (A530E and A532E ion exchange resins), and cementitious waste form. The pertechnetate form of technetium is highly soluble and mobile in aerobic (oxidizing) environments.

Synthesis, characteristics and antimicrobial activity of ZnO nanoparticles

Science.gov (United States)

Janaki, A. Chinnammal; Sailatha, E.; Gunasekaran, S.

2015-06-01

The utilization of various plant resources for the bio synthesis of metallic nano particles is called green technology and it does not utilize any harmful protocols. Present study focuses on the green synthesis of ZnO nano particles by Zinc Carbonate and utilizing the bio-components of powder extract of dry ginger rhizome (Zingiber officinale). The ZnO nano crystallites of average size range of 23-26 nm have been synthesized by rapid, simple and eco friendly method. Zinc oxide nano particles were characterized by using X-ray diffraction (XRD), Scanning Electron Microscope (SEM), Energy Dispersive X-ray spectroscopy (EDX). FTIR spectra confirmed the adsorption of surfactant molecules at the surface of ZnO nanoparticles and the presence of ZnO bonding. Antimicrobial activity of ZnO nano particles was done by well diffusion method against pathogenic organisms like Klebsiella pneumonia, Staphylococcus aureus and Candida albicans and Penicillium notatum. It is observed that the ZnO synthesized in the process has the efficient antimicrobial activity.

Synthesis and Spectral Evaluation of Some Unsymmetrical Mesoporphyrinic Complexes

Directory of Open Access Journals (Sweden)

Rica Boscencu

2012-06-01

Full Text Available Synthesis and spectral evaluation of new zinc and copper unsymmetrical mesoporphyrinic complexes are reported. Zn(II-5-(4-acetoxy-3-methoxyphenyl-10,15,20-tris-(4-carboxymethylphenylporphyrin, Zn(II-5-[(3,4-methylenedioxyphenyl]-10,15,20-tris-(4-carboxymethylphenylporphyrin, Cu(II-5-(4-acetoxy-3-methoxyphenyl-10,15,20-tris-(4-carboxymethylphenylporphyrin and Cu(II-5-[(3,4-methylenedioxyphenyl]-10,15,20-tris-(4-carboxymethylphenylporphyrin were synthesized using microwave-assisted synthesis. The complexes were characterized by elemental analysis, FT-IR, UV-Vis, EPR and NMR spectroscopy, which fully confirmed their structure. The spectral absorption properties of the porphyrinic complexes were studied in solvents with different polarities. Fluorescence emission and singlet oxygen formation quantum yields were evaluated for the compounds under study, revealing high yields for the zinc derivatives. The copper complexes are not emissive and only display residual capacity for singlet oxygen formation.

Study of barium bismuth titanate prepared by mechanochemical synthesis

Directory of Open Access Journals (Sweden)

Lazarević Z.Ž.

2009-01-01

Full Text Available Barium-bismuth titanate, BaBi4Ti4O15 (BBT, a member of Aurivillius bismuth-based layer-structure perovskites, was prepared from stoichiometric amounts of barium titanate and bismuth titanate obtained via mechanochemical synthesis. Mechanochemical synthesis was performed in air atmosphere in a planetary ball mill. The reaction mechanism of BaBi4Ti4O15 and the preparation and characteristics of BBT ceramic powders were studied using XRD, Raman spectroscopy, particle analysis and SEM. The Bi-layered perovskite structure of BaBi4Ti4O15 ceramic forms at 1100 °C for 4 h without a pre-calcination step. The microstructure of BaBi4Ti4O15 exhibits plate-like grains typical for the Bi-layered structured material and spherical and polygonal grains. The Ba2+ addition leads to changes in the microstructure development, particularly in the change of the average grain size.

Synthesis of Silver nanoparticles (AgNPs) with Antibacterial Activity

Science.gov (United States)

Campillo Gloria, E.; Ederley, Vélez; Gladis, Morales; César, Hincapié; Jaime, Osorio; Oscar, Arnache; Uribe José, Ignacio; Franklin, Jaramillo

2017-06-01

The synthesis of nanomaterials is currently one of the most active in nanoscience branches; especially those help improve the human quality life. Silver nanoparticles (AgNPs) are an example of this as it is known to have inhibitory and bactericidal effects. In this work, we report the synthesis of silver nanoparticles by chemical reduction method of silver nitrate (AgNO3) from aqueous solution, using a mix of polivinyl pyrrolidone (PVP) - Aloe Vera as reducing agent and for stabilization and control of particle size. Silver nanoparticles obtained were characterized by Scanning Electron Microscopy (SEM), UV-visible spectroscopy and measurements using Zetasizer Nano ZS were applied to size estimation. The existence of surface plasmon resonance peak at λmax ~ 420 nm is evidence of silver nanoparticles formation. It was possible to standardize an appropriate protocol for the evaluation of bactericidal activity of the nanoparticles, for mesophilic microorganisms. Bactericidal activity above 90% against these kinds of bacteria was demonstrated.

Synthesis of Silver nanoparticles (AgNPs) with Antibacterial Activity

International Nuclear Information System (INIS)

Gloria, E. Campillo; Ederley, Vélez; César, Hincapié; Gladis, Morales; Jaime, Osorio; Oscar, Arnache; José, Ignacio Uribe; Franklin, Jaramillo

2017-01-01

The synthesis of nanomaterials is currently one of the most active in nanoscience branches; especially those help improve the human quality life. Silver nanoparticles (AgNPs) are an example of this as it is known to have inhibitory and bactericidal effects. In this work, we report the synthesis of silver nanoparticles by chemical reduction method of silver nitrate (AgNO 3 ) from aqueous solution, using a mix of polivinyl pyrrolidone (PVP) – Aloe Vera as reducing agent and for stabilization and control of particle size. Silver nanoparticles obtained were characterized by Scanning Electron Microscopy (SEM), UV–visible spectroscopy and measurements using Zetasizer Nano ZS were applied to size estimation. The existence of surface plasmon resonance peak at λ max ∼ 420 nm is evidence of silver nanoparticles formation. It was possible to standardize an appropriate protocol for the evaluation of bactericidal activity of the nanoparticles, for mesophilic microorganisms. Bactericidal activity above 90% against these kinds of bacteria was demonstrated. (paper)

Solid-phase synthesis of compounds of europium and terbium with nitrogen-containing heterocyclic compounds under mechanical activation

International Nuclear Information System (INIS)

Kalinovskaya, I.V.; Karasev, V.E.

2000-01-01

Effect of solvents and parameters of mechanical treatment on basic regularities of synthesis of rare earth compounds with nitrogen-containing heterocyclic compounds is studied. It is shown that interaction on europium (3) and terbium (3) nitrates with nitrogen-containing heterocyclic compounds leads to formation of compounds of Ln(NO 3 )·2D composition, where Ln=Eu, Tb; D=2,2-dipyridyl, 1,10-phenanthroline, diphenylguanidine. Effect of conditions of mechanical treatment and different additions on process and yield of products is studied. Compounds prepared are characterized by the methods of chemical element analysis, IR spectroscopy and luminescent spectroscopy [ru

Synthesis of nickel nanoparticles by hydrazine reduction: mechanistic study and continuous flow synthesis

International Nuclear Information System (INIS)

Eluri, Ravi; Paul, Brian

2012-01-01

The continuous synthesis of nickel nanoparticles (NiNPs) in a static microchannel T-mixer by the reduction of NiCl 2 ·6H 2 O in the presence of ethylene glycol without a stabilizing/capping agent was investigated. The nanoparticles were formed in accordance with the modified polyol process with hydrazine used as a reducing agent and NaOH as a catalyst for nanoparticle formation. The reaction mechanism for NiNP formation was investigated in batch with the help of Fourier transform infrared spectroscopy and X-ray diffraction (XRD) techniques. Parameters were found for reducing reaction times from 60 to 1 min. The effects of temperature (60–120 °C) and NaOH concentration (0.1 and 0.5 M) on batch-processed particle characteristics were also studied using XRD, transmission electron microscope and electron microprobe analysis. Average particle size was reduced from 9.2 ± 2.9 to 5.4 ± 0.9 nm at higher temperature and NaOH concentration. Adaptation of this chemistry to a static microchannel T-mixer for continuous synthesis resulted in smooth, spherical particles. Increases in the reaction temperature from 120 to 130 °C resulted in a narrow size distribution of 5.3 ± 1 nm and also resulted in magnetic properties of 5.1 emu/g (saturation magnetization), 1.1 emu/g (remanent magnetization), and 62 Oe (coercivity).

Optical Waveguide Lightmode Spectroscopy (OWLS) as a Sensor for Thin Film and Quantum Dot Corrosion

OpenAIRE

Yu, Hao; Eggleston, Carrick M.; Chen, Jiajun; Wang, Wenyong; Dai, Qilin; Tang, Jinke

2012-01-01

Optical waveguide lightmode spectroscopy (OWLS) is usually applied as a biosensor system to the sorption-desorption of proteins to waveguide surfaces. Here, we show that OWLS can be used to monitor the quality of oxide thin film materials and of coatings of pulsed laser deposition synthesized CdSe quantum dots (QDs) intended for solar energy applications. In addition to changes in data treatment and experimental procedure, oxide- or QD-coated waveguide sensors must be synthesized. We synthesi...

Ambient template synthesis of multiferroic MnWO4 nanowires and nanowire arrays

International Nuclear Information System (INIS)

Zhou Hongjun; Yiu Yuen; Aronson, M.C.; Wong, Stanislaus S.

2008-01-01

The current report describes the systematic synthesis of polycrystalline, multiferroic MnWO 4 nanowires and nanowire arrays with controllable chemical composition and morphology, using a modified template-directed methodology under ambient room-temperature conditions. We were able to synthesize nanowires measuring 55±10, 100±20, and 260±40 nm in diameter, respectively, with lengths ranging in the microns. Extensive characterization of as-prepared samples has been performed using X-ray diffraction, scanning electron microscopy, transmission electron microscopy (TEM), high-resolution TEM, and energy-dispersive X-ray spectroscopy. Magnetic behavior in these systems was also probed. - Graphical abstract: Systematic synthesis of crystalline, multiferroic MnWO4 nanowires and nanowire arrays with controllable chemical composition and morphology, using a modified template-directed methodology under ambient room-temperature conditions

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.

Synthesis, radiometric determination of functional groups, complexation

International Nuclear Information System (INIS)

Pompe, S.; Bubner, M.; Schmeide, K.; Heise, K.H.; Bernhard, G.; Nitsche, H.

2000-01-01

The interaction behavior of humic acids with uranium(VI) and the influence of humic substances on the migration behavior of uranium was investigated. A main focus of this work was the synthesis of four different humic acid model substances and their characterization and comparison to the natural humic acid from Aldrich. A radiometric method for the determination of humic acid functional groups was applied in addition to conventional methods for the determination of the functionality of humic acids. The humic acid model substances show functional and structural properties comparable to natural humic acids. Modified humic acids with blocked phenolic OH were synthesized to determine the influence of phenolic OH groups on the complexation behavior of humic acids. A synthesis method for 14 C-labeled humic acids with high specific activity was developed. The complexation behavior of synthetic and natural humic acids with uranium(VI) was investigated by X-ray absorption spectroscopy, laser-induced fluorescence spectroscopy and FTIR spectroscopy. The synthetic model substances show an interaction behavior with uranium(VI) that is comparable to natural humic acids. This points to the fact that the synthetic humic acids simulate the functionality of their natural analogues very well. For the first time the influence of phenolic OH groups on the complexation behavior of humic acids was investigated by applying a modified humic acid with blocked phenolic OH groups. The formation of a uranyl hydroxy humate complex was identified by laserspectroscopic investigations of the complexation of Aldrich humic acid with uranium(VI) at pH 7. The migration behavior of uranium in a sandy aquifer system rich is humic substances was investigated in column experiments. A part of uranium migrates non-retarded through the sediment, bound to humic colloids. The uranium migration behavior is strongly influenced by the kinetically controlled interaction processes of uranium with the humic colloids

Nyctanthes arbortristis mediated synthesis of silver nanoparticles: Cytotoxicity assay against THP-1 human leukemia cell lines

Science.gov (United States)

Kumari, Priti; Kumari, Niraj; Jha, Anal K.; Singh, K. P.; Prasad, K.

2018-05-01

Green synthesis, characterizations and applications of nanoparticles have become an important branch of nanotechnology now a day. In this paper, green synthesis of silver nanoparticles (AgNPs) using the aqueous extract of Nyctanthes arbortristis as a reducing and stabilizing agent, has been discussed. Present synthetic method is very handy, cost-effective and reproducible. Formation of AgNPs was characterized by X-ray diffraction, dynamic light scattering, scanning electron microscopy and UV-visible spectroscopy techniques. The phytochemicals responsible for nano-transformation were principally flavonoids, phenols and glycosides present in the leaves. Further, the dose dependent cytotoxicity assay of biosynthesized AgNPs against THP-1 human leukemia cell lines showed the encouraging results.

Efficient synthesis of silver nanoparticles from Prosopis juliflora leaf extract and its antimicrobial activity using sewage

Science.gov (United States)

Raja, K.; Saravanakumar, A.; Vijayakumar, R.

2012-11-01

In this paper, aqueous extract of fresh leaves of Prosopis juliflora was used for the synthesis of silver (Ag) nanoparticles. UV-Vis spectroscopy studies were carried out to asses silver nanoparticles formation within 5 min, scanning electron microscopic was used to characterize shape of the Ag nanoparticles, X-ray diffraction analysis confirms the nanoparticles as crystalline silver and facecentered cubic type and Fourier transform infra-red assed that shows biomolecule compounds which are responsible for reduction and capping material of silver nanoparticles. The anti microbial activity of silver nanoparticle was performed using sewage. The approach of plant-mediated synthesis appears to be cost efficient, eco-friendly and easy methods.

Sol-gel synthesis of hydroxyapatite; Sintese de hidroxiapatita via sol-gel

Energy Technology Data Exchange (ETDEWEB)

Zupanski, M.D.; Lucena, M.P.P.; Bergmann, C.P., E-mail: michelledunin@yahoo.com.b [Universidade Federal do Rio Grande do Sul (UFRGS), Porto Alegre, RS (Brazil)

2010-07-01

Hydroxyapatite (HAp) has been established as the calcium phosphate based compound with most applications in the biological field. Among the numerous techniques for synthesis of HAp, the sol-gel processing route affords great control over purity and formed phases using low processing temperatures. In addition, the sol-gel approach offers an option for homogeneous HAp coating on metal substrates, as well as the ability to generate nanocrystalline powders. In this work, the sol-gel synthesis of HAp was investigated employing triethyl phosphate and calcium nitrate tetrahydrate as phosphorous and calcium precursors, respectively. The aging effect on phase composition and powder morphology of the final product was studied in terms of temperature and aging time. The powders were studied by using X-ray diffraction, Fourier transform infrared spectroscopy, particle size distribution by laser diffraction and scanning electron microscopy. (author)

One step paired electrochemical synthesis of iron and iron oxide nanoparticles

Directory of Open Access Journals (Sweden)

Ordoukhanian Juliet

2016-09-01

Full Text Available In this study, a new one step paired electrochemical method is developed for simultaneous synthesis of iron and iron oxide nanoparticles. iron and iron oxide are prepared as cathodic and anodic products from iron (ii sulfate aqueous solution in a membrane divided electrolytic cell by the pulsed current electrosynthesis. Because of organic solvent-free and electrochemical nature of the synthesis, the process could be considered as green and environmentally friendly. The reduction of energy consumption and low cost are the other significant advantages of this new method that would have a great application potential in the chemical industry. The nanostructure of prepared samples was characterized by Fourier transform infrared spectroscopy (FT-IR, X-ray diffraction (XRD, scanning electron microscopy (SEM and transmission electron microscopy (TEM. The magnetic properties were studied by vibrating sample magnetometer (VsM.

Prospects of Fe/MCM-41 as a Catalyst for Hydrocarbon Synthesis

International Nuclear Information System (INIS)

Cagnoli, Maria V.; Gallegos, Norma G.; Bengoa, Jose F.; Alvarez, Ana M.; Marchetti, Sergio G.; Moreno, Sergio M. J.; Roig, Anna; Mercader, Roberto C.

2005-01-01

We report the synthesis of cylindrical nanoparticles of metallic Fe entirely included in MCM-41 pores. Their dimensions are approx.3 nm diameter and approx. 3.8 nm length. We show that a coherent analysis of the results yielded by the various techniques is essential to obtain a catalyst supported on an MCM-41 matrix of ≅ 3 nm average pore diameter, which is active and selective toward olefins. The solids were characterized by low-angle x-ray diffraction, high-resolution transmission electron microscopy, high-resolution scanning transmission electron microscopy equipped with a high-angle annular dark-field, CO chemisorption, volumetric oxidation, and Moessbauer spectroscopy (in controlled atmosphere for the reduced catalysts). Catalytic results in the Fischer-Tropsch synthesis, as well as some unexpected results --like the inhomogeneous pore filling and discontinuous Fe particles-- are also discussed

Sub-Doppler spectroscopy

International Nuclear Information System (INIS)

Hansch, T.W.

1983-01-01

This chapter examines Doppler-free saturation spectroscopy, tunable cw sources, and Doppler-free two-photon spectroscopy. Discusses saturation spectroscopy; continuous wave saturation spectroscopy in the ultraviolet; and two-photon spectroscopy of atomic hydrogen 1S-2S. Focuses on Doppler-free laser spectroscopy of gaseous samples. Explains that in saturation spectroscopy, a monochromatic laser beam ''labels'' a group of atoms within a narrow range of axial velocities through excitation or optical pumping, and a Doppler-free spectrum of these selected atoms is observed with a second, counterpropagating beam. Notes that in two-photon spectroscopy it is possible to record Doppler-free spectra without any need for velocity selection by excitation with two counterpropagating laser beams whose first order Doppler shifts cancel

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.

Bark extract mediated green synthesis of silver nanoparticles: Evaluation of antimicrobial activity and antiproliferative response against osteosarcoma.

Science.gov (United States)

Nayak, Debasis; Ashe, Sarbani; Rauta, Pradipta Ranjan; Kumari, Manisha; Nayak, Bismita

2016-01-01

In the current investigation we report the biosynthesis potentials of bark extracts of Ficus benghalensis and Azadirachta indica for production of silver nanoparticle without use of any external reducing or capping agent. The appearance of dark brown color indicated the complete nanoparticle synthesis which was further validated by absorbance peak by UV-vis spectroscopy. The morphology of the synthesized particles was characterized by Field emission- scanning electron microscopy (Fe-SEM) and atomic force microscopy (AFM). The X-ray diffraction (XRD) patterns clearly illustrated the crystalline phase of the synthesized nanoparticles. ATR-Fourier Transform Infrared (ATR-FTIR) spectroscopy was performed to identify the role of various functional groups in the nanoparticle synthesis. The synthesized nanoparticles showed promising antimicrobial activity against Gram negative (Escherichia coli, Pseudomonas aeruginosa and Vibrio cholerae) and Gram positive (Bacillus subtilis) bacteria. The synthesized nano Ag also showed antiproliferative activity against MG-63 osteosarcoma cell line in a dose dependent manner. Thus, these synthesized Ag nanoparticles can be used as a broad spectrum therapeutic agent against osteosarcoma and microorganisms. Copyright © 2015 Elsevier B.V. All rights reserved.

Decoding Nucleation and Growth of Zeolitic Imidazolate Framework Thin Films with Atomic Force Microscopy and Vibrational Spectroscopy.

Science.gov (United States)

Öztürk, Zafer; Filez, Matthias; Weckhuysen, Bert M

2017-08-10

The synthesis of metal-organic framework (MOF) thin films has garnered significant attention during the past decade. By better understanding the parameters governing the nucleation and growth of such thin films, their properties can be rationally tuned, empowering their application as (reactive) membranes. Here, a combined AFM-vibrational spectroscopy research strategy is employed to detail the chemistries governing the nucleation and growth of zeolitic imidazolate framework (ZIF) thin films, in particular isostructural Co-ZIF-67 and Zn-ZIF-8. First, a single step direct synthesis approach is used to investigate the influence of different synthesis parameters -metal/linker ratio, temperature, and metal type- on the thin film nucleation and growth behaviour. While the metal/linker ratio has a pronounced effect on the thin film nucleation rate, the temperature mainly influences the growth kinetics of nuclei forming the thin film. In addition, the nucleation and growth of ZIF thin films is shown to be highly dependent on the electronegativity of the metal type. Thin-film thickness control can be achieved by using a multistep synthesis strategy, implying repetitive applications of single step deposition under identical synthesis conditions, for which a growth mechanism is proposed. This study provides insight into the influence of synthesis parameters on the ZIF thin film properties, using tools at hand to rationally tune MOF thin film properties. © 2017 The Authors. Published by Wiley-VCH Verlag GmbH & Co. KGaA.

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)

Effect of reducing agents on low-temperature synthesis of nanostructured LiFePO4

Science.gov (United States)

Kulka, Andrzej; Walczak, Katarzyna; Zając, Wojciech; Molenda, Janina

2017-09-01

Simple co-precipitation synthesis procedure yielding nanometric LiFePO4 with enhanced electrochemical properties without any post-synthesis heat treatment is presented. XRD, SEM and TEM analysis of the obtained powders revealed platelet crystallites and well crystalized bulk structure. Effective way of decreasing amount of Fe3+ containing phases by addition of reducing agents (KI, (NH4)2S2O3, glucose and the atmosphere of 5%H2-95%Ar) during low-temperature (107 °C) synthesis is described. The traditional analytical chemistry methods or the Mӧssbauer spectroscopy methods revealed that utilization of selected reducing agents diminished Fe3+ concentration from 25 to 12 at%. The constructed cells with optimized LiFePO4 as a cathode material showed superior electrochemical performances, including high reversible capacity up to 162 mAh/g at C/10 current discharge rate, flat voltage plateau with a value close to 3.45 V vs. Li0/+.

Sonochemical synthesis of manganese (II) hydroxide for supercapacitor applications

International Nuclear Information System (INIS)

Anandan, Sambandam; Gnana Sundara Raj, Balasubramaniam; Lee, Gang-Juan; Wu, Jerry J.

2013-01-01

Graphical abstract: - Highlights: • Octahedral Mn(OH) 2 nanoparticles were prepared by sonochemical process. • TEM images indicates the formation of octahedral Mn(OH) 2 nanoparticles. • Octahedral Mn(OH) 2 nanoparticles are evaluated as a supercapacitor material. - Abstract: In this research, a rapid and controllable synthesis of octahedral Mn(OH) 2 nanoparticles with a size range from 140 to 200 nm has been done by a sonochemial irradiation method for the energy storage applications. Transmission electron microscopic images, energy disperse X-ray spectroscopy (EDX), X-ray photo electron spectroscopy (XPS), X-ray diffraction (XRD), and Fourier transform infrared (FTIR) analyses clearly indicate the formation of octahedral Mn(OH) 2 nanoparticles. Octahedral Mn(OH) 2 nanoparticles were evaluated as a supercapacitor material that exhibits specific capacitance 127 F g −1 at a current density of 0.5 mA cm −2 in the potential range from −0.1 to 0.8 V in 1 M Na 2 SO 4 solution

Synthesis, characterization and magnetic properties of Fe-Al nanopins

International Nuclear Information System (INIS)

Zhang, W.S.; Brueck, E.; Li, W.F.; Si, P.Z.; Geng, D.Y.; Zhang, Z.D.

2005-01-01

We report the synthesis of Fe-Al nanopins using arc discharge. The morphology and chemical composition of the Fe-Al nanopins were studied by means of X-ray diffraction, X-ray photoelectron spectroscopy (XPS), energy dispersive X-ray spectroscopy (EDX), and high-resolution transmission electron microscopy (HRTEM). The nanopins are composed of a spherical base of about 20-100 nm and a needle-like tip of about several hundred nanometers. EDX and HRTEM studies indicate that the spherical base is mainly composed of α-Fe and FeAl core coated with a thin Al 2 O 3 layer, while the needle-like part contains only Al and O and corresponds to Al 2 O 3 . The formation mechanism of the nanopins is suggestive of a vapor-liquid-solid (VLS) growth process. The as-prepared Fe-Al nanopins show ferromagnetic properties. The temperature dependence of the magnetization at high temperatures indicates the existence of some phase transformations

Green Chemistry Approach for Synthesis of Effective Anticancer Palladium Nanoparticles

Directory of Open Access Journals (Sweden)

Sangiliyandi Gurunathan

2015-12-01

Full Text Available The purpose of this study was to design and synthesize Palladium nanoparticles (PdNPs using an environmentally friendly approach and evaluate the in vitro efficacy of PdNPs in human ovarian cancer A2780 cells. Ultraviolet-Visible (UV-Vis spectroscopy was used to monitor the conversion of Pd(II ions to Pd(0NPs. X-ray diffraction (XRD revealed the crystallinity of the as-synthesized PdNPs and Fourier transform infrared spectroscopy (FTIR further confirmed the role of the leaf extract of Evolvulus alsinoides as a reducing and stabilizing agent for the synthesis of PdNPs. Dynamic light scattering (DLS and transmission electron microscopy (TEM showed that the average size of the NPs was 5 nm. After a 24-h exposure to PdNPs, cell viability and light microscopy assays revealed the dose-dependent toxicity of the PdNPs. Furthermore, the dose-dependent cytotoxicity of the PdNPs was confirmed by lactate dehydrogenase (LDH, increased reactive oxygen species (ROS generation, activation of PdNPs-induced autophagy, impairment of mitochondrial membrane potential (MMP, enhanced caspase-3 activity, and detection of TUNEL-positive cells. Our study demonstrates a single, simple, dependable and green approach for the synthesis of PdNPs using leaf extracts of Evolvulus alsinoides. Furthermore, the in vitro efficacy of PdNPs in human ovarian cancer cells suggests that it could be an effective therapeutic agent for cancer therapy.

Comparison of in vivo postexercise phosphocreatine recovery and resting ATP synthesis flux for the assessment of skeletal muscle mitochondrial function

NARCIS (Netherlands)

Broek, van den N.M.A.; Ciapaite, J.; Nicolay, K.; Prompers, J.J.

2010-01-01

31P magnetic resonance spectroscopy (MRS) has been used to assess skeletal muscle mitochondrial function in vivo by measuring 1) phosphocreatine (PCr) recovery after exercise or 2) resting ATP synthesis flux with saturation transfer (ST). In this study, we compared both parameters in a rat model of

Study On The Synthesis Of Disida Derivatives For Labeling With 99mTc

International Nuclear Information System (INIS)

Pham Ngoc Dien; Duong Van Dong; Nguyen Thi Thu; Bui Van Cuong; Mai Phuoc Tho; Vo Cam Hoa

2007-01-01

This study describes the synthesis method and characterization of 2,6-Diisopropyl acetanilide iminodiacetic acid (DISIDA). DISIDA is synthesized by replacement reaction of two Clo atoms in chloroacetyl chloride molecule. The synthesis process has two steps. Step1: The synthesis of 2,6-diisopropylacetanilide; Step 2: The synthesis of DISIDA. The good result obtained in the step 1 reaction, it was carried out in the low pH i.e acid medium. The synthesis reaction achieved high performance at room temperature for 2 hours. The product was crystallized completely while adding in mixture reaction amount sodium acetate by drop wise and stir slowly. The step 2 reaction was carried out in medium of alkali (pH = 10-12), reaction temperature was 50 o C - 60 o C, reaction time during 8 hours. After that EtOH was evaporated by vacuum and compound was crystallized with pH = 2-3, in cool medium ( o C ). Raw material was recrystallized many time by cool EtOH. Pure product (DISIDA ) was characterized by IR, LC/MS, HPLC spectroscopy, melting point, crystal picture. Synthesized DISIDA, when tagged with diagnostic radionuclides such as 99m Tc are quite good, 99m Tc-DISIDA Complexes with RC purity and labeling efficiency >98% and above could be prepared by ordinary reaction condition, that reason can apply for valuation of possibility and reality on different purposes. (author)

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.

Synthesis and Characterization of Mercaptoacetic Acid Capped Cadmium Sulphide Quantum Dots.

Science.gov (United States)

Wageh, S; Maize, Mai; Donia, A M; Al-Ghamdi, Ahmed A; Umar, Ahmad

2015-12-01

This paper reports the facile synthesis and detailed characterization of mercaptoacetic acid capped cadmium sulphide (CdS) quantum dots using various cadmium precursors. The mercaptoacetic acid capped CdS quantum dots were prepared by facile and simple wet chemical method and characterized by several techniques such as energy dispersive spectroscopy (EDS), X-ray diffraction, Fourier transform infrared (FTIR) spectroscopy, UV-vis. spectroscopy, photoluminescence spectroscopy, high-resolution transmission microscopy (HRTEM) and thremogravimetric analysis. The EDS studies revealed that the prepared quantum dots possess higher atomic percentage of sulfur compared to cadmium due to the coordination of thiolate to the quantum dots surfaces. The X-ray and absorption analyses exhibited that the size of quantum dots prepared by cadmium acetate is larger than the quantum dots prepared by cadmium chloride and cadmium nitrate. The increase in size can be attributed to the low stability constant of cadmium acetate in comparison with cadmium chloride and cadmium nitrate. The FTIR and thermogravimetric analysis showed that the nature of capping molecule on the surface of quantum dots are different depending on the cadmium precursors which affect the emission from CdS quantum dots. Photoemission spectroscopy revealed that the emission of quantum dots prepared by cadmium acetate has high intensity band edge emission along with low intensity trapping state emission. However the CdS quantum dots prepared by cadmium chloride and cadmium nitrate produced only trapping state emissions.

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.

Journal of Chemical Sciences | Indian Academy of Sciences

Indian Academy of Sciences (India)

Home; Journals; Journal of Chemical Sciences. Sujit Roy. Articles written in Journal of Chemical Sciences. Volume 114 Issue 4 August 2002 pp 277-283. Transition metal catalysed Grignard-like allylic activation across tetragonal tin(II) oxide · Pradipta Sinha Moloy Banerjee Abhijit Kundu Sujit Roy · More Details Abstract ...

Biological synthesis of ZnO nanoparticles using C. albicans and studying their catalytic performance in the synthesis of steroidal pyrazolines

Directory of Open Access Journals (Sweden)

Shamsuzzaman

2017-05-01

Full Text Available In this study, we describe a green and simple procedure for biosynthesis of ZnO nanoparticles using Candida albicans as eco-friendly reducing and capping agent. The synthesized ZnO nanoparticles were characterized by UV–vis spectroscopy, powder X-ray diffraction, scanning electron microscopy (SEM, transmission electron microscopy (TEM, photoluminescence (PL, thermo gravimetric analysis (TGA and differential thermal analysis (DTA. The prepared nano-particles were used as catalyst for the fast and efficient synthesis of steroidal pyrazolines (4–9 from α, β-unsaturated steroidal ketones (1–3. The target molecules were obtained in good to excellent yields applying the current method.

Study of Chemical Intermediates by Means of ATR-IR Spectroscopy and Hybrid Hard- and Soft-Modelling Multivariate Curve Resolution-Alternating Least Squares

Directory of Open Access Journals (Sweden)

Junxiu Ma

2017-01-01

Full Text Available 3,5-Diamino-1,2,4-triazole (DAT became a significant energetic materials intermediate, and the study of its reaction mechanism has fundamental significance in chemistry. The aim of this study is to investigate the ability of online attenuated total reflection infrared (ATR-IR spectroscopy combined with the novel approach of hybrid hard- and soft-modelling multivariate curve resolution-alternating least squares (HS-MCR analysis to monitor and detect changes in structural properties of compound during 3,5-diamino-1,2,4-triazole (DAT synthesis processes. The subspace comparison method (SCM was used to obtain the principal components number, and then the pure IR spectra of each substance were obtained by independent component analysis (ICA and HS-MCR. The extent of rotation ambiguity was estimated from the band boundaries of feasible solutions calculated using the MCR-BANDS procedure. There were five principal components including two intermediates in the process in the results. The reaction rate constants of DAT formation reaction were also obtained by HS-MCR. HS-MCR was used to analyze spectroscopy data in chemical synthesis process, which not only increase the information domain but also reduce the ambiguities of the obtained results. This study provides the theoretical basis for the optimization of synthesis process and technology of energetic materials and provides a strong technical support of research and development of energy material with extraordinary damage effects.

Study of Chemical Intermediates by Means of ATR-IR Spectroscopy and Hybrid Hard- and Soft-Modelling Multivariate Curve Resolution-Alternating Least Squares.

Science.gov (United States)

Ma, Junxiu; Qi, Juan; Gao, Xinyu; Yan, Chunhua; Zhang, Tianlong; Tang, Hongsheng; Li, Hua

2017-01-01

3,5-Diamino-1,2,4-triazole (DAT) became a significant energetic materials intermediate, and the study of its reaction mechanism has fundamental significance in chemistry. The aim of this study is to investigate the ability of online attenuated total reflection infrared (ATR-IR) spectroscopy combined with the novel approach of hybrid hard- and soft-modelling multivariate curve resolution-alternating least squares (HS-MCR) analysis to monitor and detect changes in structural properties of compound during 3,5-diamino-1,2,4-triazole (DAT) synthesis processes. The subspace comparison method (SCM) was used to obtain the principal components number, and then the pure IR spectra of each substance were obtained by independent component analysis (ICA) and HS-MCR. The extent of rotation ambiguity was estimated from the band boundaries of feasible solutions calculated using the MCR-BANDS procedure. There were five principal components including two intermediates in the process in the results. The reaction rate constants of DAT formation reaction were also obtained by HS-MCR. HS-MCR was used to analyze spectroscopy data in chemical synthesis process, which not only increase the information domain but also reduce the ambiguities of the obtained results. This study provides the theoretical basis for the optimization of synthesis process and technology of energetic materials and provides a strong technical support of research and development of energy material with extraordinary damage effects.

Synthesis of glycinamides using protease immobilized magnetic nanoparticles

Directory of Open Access Journals (Sweden)

Abha Sahu

2016-12-01

Full Text Available In the present investigation, Bacillus subtilis was isolated from slaughterhouse waste and screened for the production of protease enzyme. The purified protease was successfully immobilized on magnetic nanoparticles (MNPs and used for the synthesis of series of glycinamides. The binding and thermal stability of protease on MNPs was confirmed by FTIR spectroscopy and TGA analysis. The surface morphology of MNPs before and after protease immobilization was carried out using SEM analysis. XRD pattern revealed no phase change in MNPs after enzyme immobilization. The processing parameters for glycinamides synthesis viz. temperature, pH, and time were optimized using Response Surface Methodology (RSM by using Design Expert (9.0.6.2. The maximum yield of various amides 2 butyramidoacetic acid (AMD-1,83.4%, 2-benzamidoacetic acid (AMD-2,80.5% and 2,2′((carboxymethyl amino-2-oxoethyl-2-hydroxysuccinylbis(azanediyldiacetic acid (AMD-3,80.8% formed was observed at pH-8, 50 °C and 30 min. The synthesized immobilized protease retained 70% of the initial activity even after 8 cycles of reuse.

Two-directional synthesis as a tool for diversity-oriented synthesis: Synthesis of alkaloid scaffolds

Directory of Open Access Journals (Sweden)

Kieron M. G. O’Connell

2012-06-01

Full Text Available Two-directional synthesis represents an ideal strategy for the rapid elaboration of simple starting materials and their subsequent transformation into complex molecular architectures. As such, it is becoming recognised as an enabling technology for diversity-oriented synthesis. Herein, we provide a thorough account of our work combining two-directional synthesis with diversity-oriented synthesis, with particular reference to the synthesis of polycyclic alkaloid scaffolds.

SYNTHESIS OF AMPHIPHILIC COMB-SHAPED COPOLYMERS USED FOR SURFACE MODIFICATION OF PVDF MEMBRANES

Institute of Scientific and Technical Information of China (English)

徐又一

2009-01-01

The synthesis of a novel amphiphilic comb-shaped copolymer consisting of a main chain of styrene-(N-(4- hydroxyphenyl) maleimide)(SHMI) copolymer and poly(ethylene glycol) methyl ether methacrylate(PEGMA) side groups was achieved by atom transfer radical polymerization(ATRP).The amphiphilic copolymers were characterized by ~1H-NMR, Fourier transform infrared(FTIR) spectroscopy and gel permeation chromatography(GPC).From thermogravimetric analysis (TGA),the decomposition temperature of SHMI-g-PEGMA is low...

Simple, mild, and highly efficient synthesis of 2-substituted benzimidazoles and bis-benzimidazoles

OpenAIRE

Eren,Bilge; Bekdemir,Yunus

2014-01-01

A new convenient method for preparation of 2-substituted benzimidazoles and bis-benzimidazoles is presented. In this method, o-phenylenediamines were condensed with bisulfite adducts of various aldehydes and di-aldehydes under neat conditions by microwave heating. The results were also compared with results of synthesis by conventional heating under reflux. Structures of the products were confirmed by infrared, ¹H- and 13C-NMR spectroscopy. Short reaction times, good yields, easy purification...

One-pot multi-component green synthesis of highly substituted piperidines

Directory of Open Access Journals (Sweden)

Ravi Bansal

2017-05-01

Full Text Available An effective and expeditious method of the synthesis of a highly functionalized piperidines, catalyzed by nontoxic, recyclable and environment friendly sodium lauryl sulfate (SLS, via one-pot multi-component condensation of aldehydes, amines and β-ketoesters in water at room temperature, has been developed. This new protocol has advantages such as moderate to high yields of products obtained after simple post reaction workup. Structure of the synthesized compounds 4a–4j have been elucidated based on the 1H NMR, 13C NMR, FT-IR spectroscopy and elemental analysis.

Synthesis of Carbon Nanomaterials from Rice Husk via Microwave Oven

Directory of Open Access Journals (Sweden)

Muhammad Asnawi

2018-01-01

Full Text Available Microwave oven was utilized to fabricate carbon nanostructure, specifically CNTs, from waste RH powders. It has been shown that the use of carbon source, catalyst, and commercial microwave oven to induce plasma is necessary to carry on this synthesis. The plasma enhances and speeds up the catalytic decomposition of RH in presence of ferrocene. FESEM, TGA, and Raman spectroscopy were utilized to confirm the presence and quality of produced carbon nanomaterials. In addition, these results suggest the conversion of ferrocene to iron(II, III oxide with notable conversion rate.

Molecular spectroscopy

International Nuclear Information System (INIS)

Kokh, Eh.; Zonntag, B.

1981-01-01

The latest investigation results on molecular spectroscopy with application of synchrotron radiation in the region of vacuum ultraviolet are generalized. Some results on investigation of excited, superexcited and ionized molecule states with the use of adsorption spectroscopy, photoelectron spectroscopy, by fluorescent and mass-spectrometric methods are considered [ru

Synthesis and characterization of the polystyrene - asphaltene graft copolymer BY FT-IR spectroscopy

International Nuclear Information System (INIS)

Leo, Adan Yovani; Salazar Ramiro

2008-01-01

The creation of new polymer compounds to be added to asphalt has drawn considerable attention because these substances have succeeded in modifying the asphalt rheological characteristics and physical properties for the enhancement of its behavior during the time of use. This work explains the synthesis of a new graft copolymer based on an asphalt fraction called asphaltene, modified with maleic anhydride. Polystyrene functionalization is conducted in a parallel fashion in order to obtain polybenzylamine resin with an amine - NH2 free group that reacts with the anhydride graft groups in the asphaltene, thus obtaining the new Polystyrene/Asphaltene graft copolymer

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

Directory of Open Access Journals (Sweden)

Mohammed Rafi Shaik

2016-11-01

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

Synthesis of thermoplastic poly(ester-olefin elastomers

Directory of Open Access Journals (Sweden)

Tanasijević Branka

2004-01-01

Full Text Available A series of thermoplastic poly(ester-olefin elastomers, based on poly(ethylene-stat-butylene, HO-PEB-OH, as the soft segment and poly (butylene terephthalate, PBT, as the hard segment, were synthesized by a catalyzed transesterification reaction in solution. The incorporation of soft hydrogenated poly(butadiene segments into the copolyester backbone was accomplished by the polycondensation of α, ω-dihydroxyl telechelic HO-PEB-OH, (PEB Mn = 3092 g/mol with 1,4-butanediol (BD and dimethyl terephthalate (DMT in the presence of a 50 wt-% high boiling solvent i.e., 1,2,4-trichlorobenzene. The molar ratio of the starting comonomers was selected to result in a constant hard to soft weight ratio of 60:40. The synthesis was optimized in terms of both the concentration of catalyst, tetra-n-butyl-titanate (Ti(OBu4, and stabilizer, N,N'-diphenyl-p-phenylenediamine (DPPD, as well as the reaction time. It was found that the optimal catalyst concentration (Ti(OBu4 for the synthesis of these thermoplastic elastomers was 1.0 mmol/mol ester and the optimal DPPD concentration was 1.0 wt-%. The extent of the reaction was followed by measuring the inherent viscosity of the reaction mixture. The effectiveness of the incorporation of the soft segments into the copolymer chains was proved by Soxhlet extraction with chloroform. The molecular structures, composition and the size of the synthesized poly(ester-butylenes were verified by 1H NMR spectroscopy, viscometry of dilute solutions and the complex dynamic melt viscosity. The thermal properties of poly(ester-olefins were investigated by differential scanning calorimetry (DSC. The degree of crystallinity was also determined by DSC. The thermal and thermo-oxidative stability were investigated by thermogravimetric analysis (TGA. The rheological properties of poly(ester-olefins were investigated by dynamic mechanical spectroscopy in the melt and solid state.

Synthesis of alumina-metal nanocomposites by mechanical alloying

International Nuclear Information System (INIS)

Osso, D.; Caer, G. le; Begin-Colin, S.; Mocellin, A.; Matteazzi, P.

1993-01-01

The synthesis of nanometer-sized α-Al 2 O 3 -metal composites can be performed by room temperature ball-milling of mixtures of metal-oxides and aluminium as shown by Matteazzi and Le Caer. The average crystallite size of the alumina-metal composite so obtained is in general about 10nm. Such composites may also be prepared by direct grinding of a mixture of α-Al 2 O 3 and of a metal or an alloy. The present work is devoted to the study of the reaction mechanisms by X-Ray diffraction and 57 Fe Moessbauer spectroscopy for the α-Al 2 O 3 -Cr, α-Al 2 O 3 -Fe, α-Al 2 O 3 -(Fe-Cr) and α-Al 2 O 3 -Ti systems. Moessbauer spectroscopy shows that non-completely reduced Fe, partly in the form of Fe 2+ , still exists at the end of the synthesis and belongs to a ternary Al-Fe-O oxide in α-Al 2 O 3 -Fe composites although it cannot be indexed by X-Ray diffraction. The Fe 2+ component is mainly associated with iron environments in or similar to those of hercynite. Species like Fe 3+ in Al 2 O 3 or in grain boundaries are observed, Fe 4+ and Fe 0 cannot be excluded. Differences are obtained by reactive milling and by direct milling the reaction products. Reactive milling of Al-TiO 2 (anatase) yields α-Al 2 O 3 -Ti nanocomposites. The transient formation of a high-pressure orthorhombic form of TiO 2 of the α-PbO 2 type is observed. (orig.)

Optical nanoparticles: synthesis and biomedical application

International Nuclear Information System (INIS)

Nhung Tran, Hong; Lien Nghiem, Thi Ha; Duong Vu, Thi Thuy; Ha Chu, Viet; Hoa Do, Quang; Vu, Duong; Nghia Nguyen, Trong; Tan Pham, Minh; Son Vu, Van; Nguyen, Thi Thuy; Ngoc Nguyen, Thi Bich; Duc Tran, Anh; Trinh, Thi Thuong; Huan Le, Quang; Thuan Tong, Kim; Thuy Tran, Thanh; Hoang, Thi My Nhung; Thanh Nguyen, Lai; Nguyen Duong, Cao; Minh Pham, Duc

2015-01-01

This paper presents a summary of our results on studies of synthesis and biomedical application of optical nanoparticles. Gold, dye-doped silica based and core–shell multifunctional multilayer (SiO_2/Au, Fe_3O_4/SiO_2, Fe_3O_4/SiO_2/Au) water-monodispersed nanoparticles were synthesized by chemical route and surface modified with proteins and biocompatible chemical reagents. The particles were conjugated with antibody or aptamer for specific detecting and imaging bacteria and cancer cells. The photothermal effects of gold nanoshells (SiO_2/Au and Fe_3O_4/SiO_2/Au) on cells and tissues were investigated. The nano silver substrates were developed for surface enhanced Raman scattering (SERS) spectroscopy to detect melamine. (review)

Vibrational spectroscopy

Science.gov (United States)

Umesh P. Agarwal; Rajai Atalla

2010-01-01

Vibrational spectroscopy is an important tool in modern chemistry. In the past two decades, thanks to significant improvements in instrumentation and the development of new interpretive tools, it has become increasingly important for studies of lignin. This chapter presents the three important instrumental methods-Raman spectroscopy, infrared (IR) spectroscopy, and...

Synthesis of highly stable and biocompatible gold nanoparticles for use as a new X-ray contrast agent.

Science.gov (United States)

Iranpour, Pooya; Ajamian, Maral; Safavi, Afsaneh; Iranpoor, Nasser; Abbaspour, Abdolkarim; Javanmardi, Sanaz

2018-04-18

This work reports a novel reduction procedure for the synthesis of Gum Arabic (GA) capped-gold nanoparticles (AuNPs) in glucosammonium formate as a new ionic liquid. The GA coated AuNPs show good stability in physiological media. The synthesized AuNPs were characterized by UV-Vis spectroscopy, transmission electron microscopy, dynamic light scattering and X-ray diffraction analysis. These stable AuNPs are introduced as a new contrast agent for X-ray Computed Tomography (X-ray CT). These nanoparticles have higher contrasting properties than the commercial contrast agent, Visipaque. The precursors used (Gum Arabic and glucose based-ionic liquid) for synthesis of AuNPs are biocompatible and non-toxic.

Synthesis of pure monetite by heterogeneous acid-base reaction

Directory of Open Access Journals (Sweden)

Luis Carlos Moreno Aldana

2017-01-01

Full Text Available Five variations of the monetite (M synthesis were evaluated modifying the stirring, the phosphoric acid addition rate, the homogeneity and the drying temperature. Products were assessed by means of XRD, FTIR, SEM-EDS analysis and chemical assay of Ca/P (calcium by titration with potassium permanganate and phosphorus by colorimetric assessment of the molybdenum blue complex. X-ray diffraction, infrared spectroscopy and Ca/P ratio indicate that the synthesized phosphate corresponds to pure monetite. It was found that the most influential factors affecting composition, crystal size and Ca/P were stoichiometry and ballmilling mechanoactivation.

Modern spectroscopy

CERN Document Server

Hollas, J Michael

2013-01-01

The latest edition of this highly acclaimed title introduces the reader to a wide range of spectroscopies, and includes both the background theory and applications to structure determination and chemical analysis.  It covers rotational, vibrational, electronic, photoelectron and Auger spectroscopy, as well as EXAFs and the theory of lasers and laser spectroscopy. A  revised and updated edition of a successful, clearly written book Includes the latest developments in modern laser techniques, such as cavity ring-down spectroscopy and femtosecond lasers Provides numerous worked examples, calculations and questions at the end of chapters.

Synthesis of reduced graphene oxide-anatase TiO2 nanocomposite and its improved photo-induced charge transfer properties.

Science.gov (United States)

Wang, Ping; Zhai, Yueming; Wang, Dejun; Dong, Shaojun

2011-04-01

The construction of reduced graphene oxide or graphene oxide with semiconductor has gained more and more attention due to its unexpected optoelectronic and electronic properties. The synthesis of reduced graphene oxide (RGO) or graphene oxide-semiconductor nanocomposite with well-dispersed decorated particles is still a challenge now. Herein, we demonstrate a facile method for the synthesis of graphene oxide-amorphous TiO(2) and reduced graphene oxide-anatase TiO(2) nanocomposites with well-dispersed particles. The as-synthesized samples were characterized by transmission electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy, UV-Vis absorption spectroscopy, Fourier transform infrared spectrometry, and thermogravimetric analysis. The photovoltaic properties of RGO-anatase TiO(2) were also compared with that of similar sized anatase TiO(2) by transient photovoltage technique, and it was interesting to find that the combination of reduced graphene oxide with anatase TiO(2) will significantly increase the photovoltaic response and retard the recombination of electron-hole pairs in the excited anatase TiO(2).

Microwave-assisted green synthesis of superparamagnetic nanoparticles using fruit peel extracts: surface engineering, T2 relaxometry, and photodynamic treatment potential

Directory of Open Access Journals (Sweden)

Bano S

2016-08-01

Full Text Available Shazia Bano,1–3 Samina Nazir,2 Alia Nazir,1 Saeeda Munir,3 Tariq Mahmood,2 Muhammad Afzal,1 Farzana Latif Ansari,4 Kehkashan Mazhar3 1Department of Physics, The Islamia University of Bahawalpur, Bahawalpur, 2Nanosciences and Technology Department, National Centre for Physics, 3Institute of Biomedical and Genetic Engineering (IBGE, 4Pakistan Council for Science and Technology, Islamabad, Pakistan Abstract: Superparamagnetic iron oxide nanoparticles (SPIONs have the potential to be used as multimodal imaging and cancer therapy agents due to their excellent magnetism and ability to generate reactive oxygen species when exposed to light. We report the synthesis of highly biocompatible SPIONs through a facile green approach using fruit peel extracts as the biogenic reductant. This green synthesis protocol involves the stabilization of SPIONs through coordination of different phytochemicals. The SPIONs were functionalized with polyethylene glycol (PEG-6000 and succinic acid and were extensively characterized by X-ray diffraction analysis, field emission scanning electron microscopy, energy-dispersive X-ray spectroscopy, atomic force microscopy, Rutherford backscattering spectrometry, diffused reflectance spectroscopy, fluorescence emission, Fourier-transform infrared spectroscopy, ultraviolet-visible spectroscopy, and magnetization analysis. The developed SPIONs were found to be stable, almost spherical with a size range of 17–25 nm. They exhibited excellent water dispersibility, colloidal stability, and relatively high R2 relaxivity (225 mM-1 s-1. Cell viability assay data revealed that PEGylation or carboxylation appears to significantly shield the surface of the particles but does not lead to improved cytocompatibility. A highly significant increase of reactive oxygen species in light-exposed samples was found to play an important role in the photokilling of human cervical epithelial malignant carcinoma (HeLa cells. The bio-SPIONs developed

The quantitative monitoring of mechanochemical reaction between solid L-tartaric acid and sodium carbonate monohydrate by terahertz spectroscopy

Science.gov (United States)

Liu, Xiaohong; Liu, Guifeng; Zhao, Hongwei; Zhang, Zengyang; Wei, Yongbo; Liu, Min; Wen, Wen; Zhou, Xingtai

2011-11-01

The solid-state reaction of chiral tartaric acid and alkali carbonate was studied by terahertz time-domain spectroscopy (THz-TDS). The sodium tartrate dihydrate was synthesized with high efficiency by mechanical grinding in the solid-state without waste that is particularly sustainable and environmentally benign. Distinct THz absorptions were observed for reactants and products. It indicates that THz spectroscopy is sensitive to different materials and crystal structures. The characteristic THz absorption peak at 1.09 THz of L (+)-Tartaric acid was selected for quantitative analysis. The reaction kinetics could be expressed by the Second-order equation and the Jander equation, which is consistent with a three-dimensional diffusion mechanism. The combination of multi-techniques including synchrotron radiation X-ray powder diffraction (SRXRPD), Fourier transform infrared (FT-IR) and scanning electron microscopy (SEM) was used to investigate the grinding process and presented supporting evidences. The results demonstrate that THz spectroscopy technique has great potential applications in process monitoring and analysis in pharmaceutical and chemical synthesis industry.

Atom spectroscopy

International Nuclear Information System (INIS)

Kodling, K.

1981-01-01

Experiments on atom photoabsorption spectroscopy using synchrotron radiation in the 10-1000 eV range are reviewed. Properties of the necessary synchrotron radiation and the experiment on absorption spectroscopy are briefly described. Comparison with other spectroscopy methods is conducted. Some data on measuring photoabsorption, photoelectron emission and atom mass spectra are presented [ru

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.

Greener synthesis of magnetite nanoparticles using green tea extract and their magnetic properties

Science.gov (United States)

Karade, V. C.; Waifalkar, P. P.; Dongle, T. D.; Sahoo, Subasa C.; Kollu, P.; Patil, P. S.; Patil, P. B.

2017-09-01

The facile green synthesis method has been employed for the synthesis of biocompatible Fe3O4 magnetic nanoparticles (MNPs) using green tea extract. The effective reduction of ferric ions (Fe3+) were done using an aqueous green tea extract where it acts as reducing as well as capping agent. The effect of iron precursor to green tea extract ratio and reaction temperature was studied. The MNPs were characterized by x-ray diffraction, Fourier transform infrared spectroscopy, field-emission scanning electron microscopy, dynamic light scattering and vibrating sample magnetometer. It was observed that the reaction temperature strongly affects the magnetic and structural properties of MNPs. The magnetic measurements study showed that Fe3O4 MNPs are superparamagnetic at 300 K, while at 60 K have ferromagnetic as well as superparamagnetic contributions.

Use of deuterium labelled glucose in evaluating the pathway of hepatic glycogen synthesis

International Nuclear Information System (INIS)

Goodman, M.N.; Masuoka, L.K.; deRopp, J.S.; Jones, A.D.

1989-01-01

Deuterium labelled glucose has been used to study the pathway of hepatic glycogen synthesis during the fasted-refed transition in rats. Deuterium enrichment of liver glycogen was determined using nuclear magnetic resonance as well as mass spectroscopy. Sixty minutes after oral administration of deuterated glucose to fasted rats, the portal vein blood was fully enriched with deuterated glucose. Despite this, less than half of the glucose molecules incorporated into liver glycogen contained deuterium. The loss of deuterium label from glucose is consistent with hepatic glycogen synthesis by an indirect pathway requiring prior metabolism of glucose. The use of deuterium labelled glucose may prove to be a useful probe to study hepatic glycogen metabolism. Its use may also find application in the study of liver glycogen metabolism in humans by a noninvasive means

Low temperature synthesis of InP nanocrystals

International Nuclear Information System (INIS)

Ung Thi Dieu Thuy; Tran Thi Thuong Huyen; Nguyen Quang Liem; Reiss, Peter

2008-01-01

We present a simple method for the chemical synthesis of InP nanocrystals, which comprises several advantages: (i) the use of simple reagents, namely InCl 3 .4H 2 O and yellow P as the In and P precursors, respectively, and NaBH 4 as the reducing agent in a mixed solvent of ethanol and toluene; (ii) a short reaction time (1-5 h) and low temperature (<75 deg. C); (iii) a high reaction yield approaching 100%. InP NCs in the zinc-blende structure have been obtained as confirmed by powder X-ray diffraction and Raman scattering measurements. Their mean size of 4 nm has been determined by transmission electron microscopy, Raman scattering and absorption spectroscopy

Synthesis of antihydrogen atoms in a CUSP trap

Energy Technology Data Exchange (ETDEWEB)

Kuroda, Naofumi, E-mail: kuroda@phys.c.u-tokyo.ac.jp [University of Tokyo, Graduate School of Arts and Sciences (Japan); Enomoto, Yoshinori [RIKEN Advanced Science Institute (Japan); Michishio, Koji [Tokyo University of Science, Department of Physics (Japan); Kim, Chanhyoun [University of Tokyo, Graduate School of Arts and Sciences (Japan); Higaki, Hiroyuki [Hiroshima University, Graduate School of Advanced Science of Matter (Japan); Nagata, Yugo; Kanai, Yasuyuki [RIKEN Advanced Science Institute (Japan); Torii, Hiroyuki A. [University of Tokyo, Graduate School of Arts and Sciences (Japan); Corradini, Maurizzio; Leali, Marco; Lodi-Rizzini, Evandro; Mascagna, Valerio; Venturelli, Luca; Zurlo, Nicola [Universita di Brescia and Instituto Nazionale di Fisica Nucleare, Dipartimento di Chimica e Fisica per l' Ingegneria e per i Materiali (Italy); Fujii, Koki; Ohtsuka, Miki; Tanaka, Kazuo [University of Tokyo, Graduate School of Arts and Sciences (Japan); Imao, Hiroshi [RIKEN Nishina Center for Accelerator-Based Science (Japan); Nagashima, Yasuyuki [Tokyo University of Science, Department of Physics (Japan); Matsuda, Yasuyuki [University of Tokyo, Graduate School of Arts and Sciences (Japan); and others

2012-05-15

ASACUSA collaboration has been making a path to realize high precision microwave spectroscopy of ground-state hyperfine transitions of antihydrogen atom in flight for stringent test of the CPT symmetry. Recently, we have succeeded in synthesizing our first cold antihydrogen atoms employing a CUSP trap. It is expected that synthesized antihydrogen atoms in the low-field-seeking states are preferentially focused along the cusp magnetic field axis whereas those in the high-field-seeking states are not focused, resulting in the formation of a spin-polarized antihydrogen beam. We report the recent results of antihydrogen atom synthesis and beam production developed with the CUSP trap.

Synthesis of antihydrogen atoms in a CUSP trap

International Nuclear Information System (INIS)

Kuroda, Naofumi; Enomoto, Yoshinori; Michishio, Koji; Kim, Chanhyoun; Higaki, Hiroyuki; Nagata, Yugo; Kanai, Yasuyuki; Torii, Hiroyuki A.; Corradini, Maurizzio; Leali, Marco; Lodi-Rizzini, Evandro; Mascagna, Valerio; Venturelli, Luca; Zurlo, Nicola; Fujii, Koki; Ohtsuka, Miki; Tanaka, Kazuo; Imao, Hiroshi; Nagashima, Yasuyuki; Matsuda, Yasuyuki

2012-01-01

ASACUSA collaboration has been making a path to realize high precision microwave spectroscopy of ground-state hyperfine transitions of antihydrogen atom in flight for stringent test of the CPT symmetry. Recently, we have succeeded in synthesizing our first cold antihydrogen atoms employing a CUSP trap. It is expected that synthesized antihydrogen atoms in the low-field-seeking states are preferentially focused along the cusp magnetic field axis whereas those in the high-field-seeking states are not focused, resulting in the formation of a spin-polarized antihydrogen beam. We report the recent results of antihydrogen atom synthesis and beam production developed with the CUSP trap.

Synthesis and applications of 13C glycerol

International Nuclear Information System (INIS)

Stocking, E.; Khalsa, O.; Martinez, R.A.; Silks, L.A. III

1994-01-01

Due in part to the use of labeled glycerol for the 13 C enrichment of biomolecules, we are currently developing new synthetic routes to various isotopomers of glycerol. Judging from our experience, traditional methods of glycerol synthesis are not easily adapted for isotopic enrichment and/or have poor overall yields (12 to 15%). Furthermore, the use of glycerol for enrichment can be prohibitively expensive and its availability is limited by the level of demand. We are presently developing a short de novo synthesis of glycerol from carbon dioxide (∼53% overall yield for four steps) and are examining the feasibility of synthesizing site-specific 13 C-labeled glycerol and dihydroxyacetone (DHA) from labeled methanol and carbon dioxide. One application of 13 C glycerol we have examined is enzymatic conversion of glycerol to glyceraldehyde-3-monophosphate or dihydroxyacetone monophosphate (DHAP) with yields ranging from 25 to 50% (as determined by NMR spectroscopy). We are also pursuing the chemical conversion of 13 C-labeled DHA to DHAP. We are especially interested in 13 C-labeled DHAP because we are investigating its use as a chemo-enzymatic precursor for both labeled 2-deoxyribose and 2-deoxyribonucleic acids

Synthesis and optical properties of novel organic-inorganic hybrid nanolayer structure semiconductors

International Nuclear Information System (INIS)

Zhang Sanjun; Lanty, Gaetan; Lauret, Jean-Sebastien; Deleporte, Emmanuelle; Audebert, Pierre; Galmiche, Laurent

2009-01-01

We report on the synthesis of some novel organic-inorganic hybrid 2D perovskite semiconductors (R-(CH 2 ) n NH 3 ) 2 PbX 4 . These semiconductors are self-assembled intercalation nanolayers and have a multi-quantum-well energy level structure. We systematically vary the characteristic of organic groups (R-(CH 2 ) n NH 3 + ) to study the relationship between their structures and the optical properties of (R-(CH 2 ) n NH 3 ) 2 PbX 4 . From optical absorption and photoluminescence spectroscopy experiments performed on series of samples, we find some trends of choosing the organic groups to improve the optical performance of (R-(CH 2 ) n NH 3 ) 2 PbX 4 . A new organic group, which allows synthesis of nanolayer perovskite semiconductors with quite high photoluminescence efficiency and better long-term stability, has been found.

Rapid synthesis of single-phase bismuth ferrite by microwave-assisted hydrothermal method

Energy Technology Data Exchange (ETDEWEB)

Cao, Wenqian [College of Materials Science and Engineering, China Jiliang University, 258 Xueyuan Street, Xiasha Higher Education District, Hangzhou 310018, Zhejiang Province (China); Chen, Zhi, E-mail: zchen0@gmail.com [College of Materials Science and Engineering, China Jiliang University, 258 Xueyuan Street, Xiasha Higher Education District, Hangzhou 310018, Zhejiang Province (China); Gao, Tong; Zhou, Dantong; Leng, Xiaonan; Niu, Feng [College of Materials Science and Engineering, China Jiliang University, 258 Xueyuan Street, Xiasha Higher Education District, Hangzhou 310018, Zhejiang Province (China); Zhu, Yuxiang [College of Materials Science and Engineering, China Jiliang University, 258 Xueyuan Street, Xiasha Higher Education District, Hangzhou 310018, Zhejiang Province (China); Tianjin Key Laboratory of Marine Resources and Chemistry, Tianjin University of Science and Technology, Tianjin (China); Qin, Laishun, E-mail: qinlaishun@yeah.net [College of Materials Science and Engineering, China Jiliang University, 258 Xueyuan Street, Xiasha Higher Education District, Hangzhou 310018, Zhejiang Province (China); Wang, Jiangying; Huang, Yuexiang [College of Materials Science and Engineering, China Jiliang University, 258 Xueyuan Street, Xiasha Higher Education District, Hangzhou 310018, Zhejiang Province (China)

2016-06-01

This paper describes on the fast synthesis of bismuth ferrite by the simple microwave-assisted hydrothermal method. The phase transformation and the preferred growth facets during the synthetic process have been investigated by X-ray diffraction. Bismuth ferrite can be quickly prepared by microwave hydrothermal method by simply controlling the reaction time, which is further confirmed by Fourier Transform infrared spectroscopy and magnetic measurement. - Graphical abstract: Single-phase BiFeO{sub 3} could be realized at a shortest reaction time of 65 min. The reaction time has strong influences on the phase transformation and the preferred growth facets. - Highlights: • Rapid synthesis (65 min) of BiFeO{sub 3} by microwave-assisted hydrothermal method. • Reaction time has influence on the purity and preferred growth facets. • FTIR and magnetic measurement further confirm the pure phase.

Rapid synthesis of single-phase bismuth ferrite by microwave-assisted hydrothermal method

International Nuclear Information System (INIS)

Cao, Wenqian; Chen, Zhi; Gao, Tong; Zhou, Dantong; Leng, Xiaonan; Niu, Feng; Zhu, Yuxiang; Qin, Laishun; Wang, Jiangying; Huang, Yuexiang

2016-01-01

This paper describes on the fast synthesis of bismuth ferrite by the simple microwave-assisted hydrothermal method. The phase transformation and the preferred growth facets during the synthetic process have been investigated by X-ray diffraction. Bismuth ferrite can be quickly prepared by microwave hydrothermal method by simply controlling the reaction time, which is further confirmed by Fourier Transform infrared spectroscopy and magnetic measurement. - Graphical abstract: Single-phase BiFeO_3 could be realized at a shortest reaction time of 65 min. The reaction time has strong influences on the phase transformation and the preferred growth facets. - Highlights: • Rapid synthesis (65 min) of BiFeO_3 by microwave-assisted hydrothermal method. • Reaction time has influence on the purity and preferred growth facets. • FTIR and magnetic measurement further confirm the pure phase.

Synthesis of ZnO Nanostructures for Low Temperature CO and UV Sensing

Directory of Open Access Journals (Sweden)

Nazar Abbas Shah

2012-10-01

Full Text Available In this paper, synthesis and results of the low temperature sensing of carbon monoxide (CO gas and room temperature UV sensors using one dimensional (1-D ZnO nanostructures are presented. Comb-like structures, belts and rods, and needle-shaped nanobelts were synthesized by varying synthesis temperature using a vapor transport method. Needle-like ZnO nanobelts are unique as, according to our knowledge, there is no evidence of such morphology in previous literature. The structural, morphological and optical characterization was carried out using X-ray diffraction, scanning electron microscopy and diffused reflectance spectroscopy techniques. It was observed that the sensing response of comb-like structures for UV light was greater as compared to the other grown structures. Comb-like structure based gas sensors successfully detect CO at 75 °C while other structures did not show any response.

Green Synthesis of Gold nanoparticles with Starch-glucose and Application in Bioelectrochemistry

DEFF Research Database (Denmark)

Engelbrekt, Christian; Sørensen, Karsten Holm; Zhang, Jingdong

2009-01-01

and basic solution. The starch concentration, temperature and chemical nature of the buffers are key factors in the AuNP formation. Glucose and starch are reducing and protecting agents, respectively. Among several inorganic and biological Good's buffers, phosphate and MES buffers give the best results...... MES is also a synergist with more composite function. AuNPs prepared by this method are stable in solution even after 17 months at room temperature. TEM confirms the crystalline structure of the AuNPs, meaning that the AuNP surfaces are low-index single-crystal facets such as (100), (110) and (111......A method for gold nanoparticle (AuNP) synthesis from buffered glucose and starch solution has been developed and the particles investigated by UV-Vis spectroscopy, transmission electron microscopy (TEM), atomic force microscopy (AFM) and electrochemistry. The synthesis proceeds smoothly in neutral...

Switching from Reactant to Substrate Engineering in the Selective Synthesis of Graphene Nanoribbons.

Science.gov (United States)

Merino-Díez, Néstor; Lobo-Checa, Jorge; Nita, Pawel; Garcia-Lekue, Aran; Basagni, Andrea; Vasseur, Guillaume; Tiso, Federica; Sedona, Francesco; Das, Pranab K; Fujii, Jun; Vobornik, Ivana; Sambi, Mauro; Pascual, José Ignacio; Ortega, J Enrique; de Oteyza, Dimas G

2018-04-27

The challenge of synthesizing graphene nanoribbons (GNRs) with atomic precision is currently being pursued along a one-way road, based on the synthesis of adequate molecular precursors that react in predefined ways through self-assembly processes. The synthetic options for GNR generation would multiply by adding a new direction to this readily successful approach, especially if both of them can be combined. We show here how GNR synthesis can be guided by an adequately nanotemplated substrate instead of by the traditionally designed reactants. The structural atomic precision, unachievable to date through top-down methods, is preserved by the self-assembly process. This new strategy's proof-of-concept compares experiments using 4,4''-dibromo-para-terphenyl as a molecular precursor on flat Au(111) and stepped Au(322) substrates. As opposed to the former, the periodic steps of the latter drive the selective synthesis of 6 atom-wide armchair GNRs, whose electronic properties have been further characterized in detail by scanning tunneling spectroscopy, angle resolved photoemission, and density functional theory calculations.

Room temperature chemical synthesis of Cu(OH)2 thin films for supercapacitor application

International Nuclear Information System (INIS)

Gurav, K.V.; Patil, U.M.; Shin, S.W.; Agawane, G.L.; Suryawanshi, M.P.; Pawar, S.M.; Patil, P.S.; Lokhande, C.D.; Kim, J.H.

2013-01-01

Highlights: •Cu(OH) 2 is presented as the new supercapacitive material. •The novel room temperature method used for the synthesis of Cu(OH) 2 . •The hydrous, nanograined Cu(OH) 2 shows higher specific capacitance of 120 F/g. -- Abstract: Room temperature soft chemical synthesis route is used to grow nanograined copper hydroxide [Cu(OH) 2 ] thin films on glass and stainless steel substrates. The structural, morphological, optical and wettability properties of Cu(OH) 2 thin films are studied by means of X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), field emission scanning electron microscopy (FESEM), UV–vis spectrophotometer and water contact angle measurement techniques. The results showed that, room temperature chemical synthesis route allows to form the nanograined and hydrophilic Cu(OH) 2 thin films with optical band gap energy of 3.0 eV. The electrochemical properties of Cu(OH) 2 thin films are studied in an aqueous 1 M NaOH electrolyte using cyclic voltammetry. The sample exhibited supercapacitive behavior with 120 F/g specific capacitance

An Innovative Electrolysis Approach for the Synthesis of Metal Matrix Bulk Nanocomposites: A Case Study on Copper-Niobium System

Science.gov (United States)

Shokrvash, Hussein; Rad, Rahim Yazdani; Massoudi, Abouzar

2018-04-01

Design and synthesis of a prototype Cu-Nb nanocomposite are presented. Oxygen-free Cu-Nb nanocomposites were prepared using an electrolysis facility with special emphasis on the cathodic deoxidation of Cu and nanometric Nb2O5 blends in a molten NaCl-CaCl2 electrolyte. The as-prepared nanocomposites were characterized by X-ray diffraction and energy-dispersive X-ray spectroscopy. The elemental analysis of the Cu matrix and Nb phase revealed the high solubility of Nb in the Cu structure (0.85 at. pct) and Cu in the Nb structure (10.59 at. pct) over short synthesis times (4-5 hours). Furthermore, precise analysis using field emission scanning electron microscopy and transmission electron microscopy confirmed the unique structure and nanocomposite morphology of the Cu-Nb nanocomposite. The successful synthesis of Cu-Nb nanocomposites offers a new conceptual and empirical outlook on the generation of bulk nanostructures of immiscible bimetals using electro-synthesis.

Biological sensing with surface-enhanced Raman spectroscopy (SERS) using a facile and rapid silver colloid-based synthesis technique

Science.gov (United States)

Smyth, C.; Mehigan, S.; Rakovich, Y. P.; Bell, S. E. J.; McCabe, E. M.

2011-03-01

Optical techniques towards the realisation of sensitive and selective biosensing platforms have received a considerable amount of attention in recent times. Techniques based on interferometry, surface plasmon resonance, field-effect transistors and waveguides have all proved popular, and in particular, spectroscopy offers a large range of options. Raman spectroscopy has always been viewed as an information rich technique in which the vibrational frequencies reveal a lot about the structure of a compound. The issue with Raman spectroscopy has traditionally been that its rather low cross section leads to poor limits-of-detection. In response to this problem, Surface-enhanced Raman Scattering (SERS), which increases sensitivity by bringing the sample in contact with many types of enhanceing substrates, has been developed. Here we discuss a facile and rapid technique for the detection of pterins using colloidal silver suspensions. Pteridine compounds are a family of biochemicals, heterocyclic in structure, and employed in nature as components of colour pigmentation and also as facilitators for many metabolic pathways, particularly those relating to the amino acid hydroxylases. In this work, xanthopterin, isoxanthopterin and 7,8- dihydrobiopterin have been examined whilst absorbed to SERS-active silver colloids. SERS, while far more sensitive than regular Raman spectroscopy, has its own issues relating to the reproducibility of substrates. In order to obtain quantitative data for the pteridine compounds mentioned above, exploratory studies of methods for introducing an internal standard for normalisation of the signals have been carried out.e

Synthesis, growth and characterization of organic nonlinear optical material: N-benzyl-2-methyl-4-nitroaniline (BNA)

Science.gov (United States)

Kalaivanan, R.; Srinivasan, K.

2017-05-01

Synthesis of the organic nonlinear optical compound N-benzyl-2-methyl-4-nitroaniline (BNA) was carried out in a newer chemical environment using the mixture of benzyl chloride and 2-methl-4-nitroaniline by a preferred laboratory synthesis process. The synthesized BNA compound was separated by column chromatography (CC) with low pressure silica gell using petrollium benzine and purity of the separated resultant product was confirmed by thin layer chromatography (TLC). Further, the material was recrystallized atleast four times in methanol and the highly purified BNA was used for the growth of single crystals from solutions with selected solvents by slow evaporation method at room temperature. Single crystals having natural growth morphology were harvested and their different growth faces were identified by optical goniometry. The grown crystals were subjected to different characterization techniques such as powder x-ray diffraction (PXRD), fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC) and UV-vis-Near IR spectroscopy. Further, the second harmonic generation (SHG) efficiency of the grown BNA crystal was studied by Kurtz and Perry powder technique using Nd:YAG laser as fundamental source and found to be twice that of inorganic standard KDP.

High yield and facile microwave-assisted synthesis of conductive H_2SO_4 doped polyanilines

International Nuclear Information System (INIS)

Gizdavic-Nikolaidis, Marija R.; Jevremovic, Milutin M.; Milenkovic, Maja; Allison, Morgan C.; Stanisavljev, Dragomir R.; Bowmaker, Graham A.; Zujovic, Zoran D.

2016-01-01

The microwave-assisted synthesis of polyaniline (PANI) was performed using ammonium persulphate (APS) as oxidizing agent in 0.5 M–2.5 M concentration range of aqueous sulphuric acid (H_2SO_4) at 93 W applied microwave power of 10 min duration. The microwave (MW) synthesized PANIs had 3 times higher yield in comparison to PANI samples prepared using a classical method, CS (0 W MW power) at the same temperature for 10 min synthesis duration period. Fourier Transform Infrared (FTIR) and UV–Vis spectroscopies confirmed the formation of PANI structure in all products. The influence of H_2SO_4 acid dopant on the spin concentration of MW and CS H_2SO_4 doped PANI samples were examined by EPR spectroscopy, while the morphological characteristics were investigated by using scanning electron microscopy (SEM). XRD results showed amorphous phases in both MW and CS H_2SO_4 doped PANI samples. Conductivity measurements revealed ∼1.5 times higher conductivity values for MW H_2SO_4 doped PANI samples in comparison with PANI samples prepared by the CS method under same condition. The influence of sulfate anion in comparison to chloride anion as a dopant on morphological, dopant levels and conductivity properties of MW PANI samples were also investigated. - Highlights: • Nanoporous microwave synthesized doped polyanilines as chemical sensor material. • Morphology and physical properties of polyanilines depend on acid concentration. • Spin concentration is determined by the nature of the polyaniline synthesis.

Synthesis and characterization of oxidic semiconductor alloys; Synthese und Charakterisierung oxidischer Halbleiterlegierungen

Energy Technology Data Exchange (ETDEWEB)

Merita, S.

2007-02-15

In the present thesis the possibility for the synthesis of the mixed systems ZnO{sub 1-x}Te{sub x} and Cu{sub 2}O{sub 1-x}S{sub x} by means of reactive RF sputtering deposition is studied. The layers deposed on glass, sapphire, and GaN substrateswere analyzed by X-ray diffraction, optical transmission and reflection measurements, energy-dispersive X-ray analysis, secondary-ion mass spectroscopy, Hall measurements, X-ray reflectometry, scanning electron and scanning force microscopy.

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)

Synthesis and evaluation of optical and antimicrobial properties of Ag-SnO2 nanocomposites

Science.gov (United States)

Kumar Nair, Kishore; Kumar, Promod; Kumar, Vinod; Harris, R. A.; Kroon, R. E.; Viljoen, Bennie; Shumbula, P. M.; Mlambo, M.; Swart, H. C.

2018-04-01

We report on the sol-gel based room temperature synthesis of undoped SnO2 and Ag-SnO2 nanostructures. The synthesized nanostructures were characterized by Fourier transform infrared spectroscopy, X-ray diffraction (XRD), Raman spectroscopy, High-resolution transmission electron microscopy (HR-TEM) and UV-visible spectroscopy. The XRD pattern confirmed that the obtained nanostructures have a tetragonally rutile structure. No extra phase changes were observed after Ag doping. UV-visible spectroscopy measurements indicated that the band gap of 3.59 eV for pure SnO2 nanostructures, decreased to 3.39 eV after doping. TEM analysis showed that no regular shape morphology existed and some rod-shaped particles were also detected in the nanostructures. The antibacterial activity of the nanostructures against E. coli was evaluated and a continuous decrease of microbial count was observed. The microbial population decreased from 6 × 105 cfu/ml to 7 × 104 cfu/ml and 5 × 104 cfu/ml on SnO2 and Ag-SnO2 treatments, respectively. Thus, the nanostructures can be used for the biorational management of E. coli for waste water treatment before discharge.

Synthesis and characterization of NiO nanoparticles by thermal decomposition of nickel linoleate and their optical properties

Energy Technology Data Exchange (ETDEWEB)

Kalam, Abul, E-mail: abul_k33@yahoo.com [Department of Chemistry, Faculty of Science, King Khalid University, Abha 61413, P.O. Box 9004 (Saudi Arabia); Al-Sehemi, Abdullah G.; Al-Shihri, Ayed S. [Department of Chemistry, Faculty of Science, King Khalid University, Abha 61413, P.O. Box 9004 (Saudi Arabia); Du Gaohui [Zhejiang Key Laboratory for Reactive Chemistry on Solid Surfaces, Institute of Physical Chemistry, Zhejiang Normal University, Jinhua 321004 (China); Ahmad, Tokeer [Nanochemistry Laboratory, Department of Chemistry, Jamia Millia Islamia, New Delhi 110025 (India)

2012-06-15

Well dispersed nickel oxide nanoparticles have been synthesized successfully by direct calcination of nickel linoleate. The structure, morphology and properties of the nanoparticles were characterized by X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy, transmission electron microscopy, high-resolution transmission electron microscopy and ultraviolet-visible spectroscopy. Transmission electron microscopic studies show that nickel oxide nanoparticles are uniform with an average size of 14-20 nm. The optical band gap of 3.8 eV is obtained using UV-Visible spectroscopy which exhibits the red shift compared with the bulk counterpart. - Highlights: Black-Right-Pointing-Pointer Synthesis of metal oxide nanoparticles by using metal complexes as precursors. Black-Right-Pointing-Pointer Characterization of isolated nanoparticles using XRD, FTIR, SEM, TEM and HRTEM data. Black-Right-Pointing-Pointer The expected optical properties of these nanoparticles are clarified.

Efficient synthesis of silver nanoparticles from Prosopis juliflora leaf extract and its antimicrobial activity using sewage.

Science.gov (United States)

Raja, K; Saravanakumar, A; Vijayakumar, R

2012-11-01

In this paper, aqueous extract of fresh leaves of Prosopis juliflora was used for the synthesis of silver (Ag) nanoparticles. UV-Vis spectroscopy studies were carried out to asses silver nanoparticles formation within 5 min, scanning electron microscopic was used to characterize shape of the Ag nanoparticles, X-ray diffraction analysis confirms the nanoparticles as crystalline silver and facecentered cubic type and Fourier transform infra-red assed that shows biomolecule compounds which are responsible for reduction and capping material of silver nanoparticles. The anti microbial activity of silver nanoparticle was performed using sewage. The approach of plant-mediated synthesis appears to be cost efficient, eco-friendly and easy methods. Copyright © 2012 Elsevier B.V. All rights reserved.

Synthesis of new 3-(2-aminothiazol-4-yl-4-hydroxy-2H-chromen-2-one derivatives

Directory of Open Access Journals (Sweden)

S. SUKDOLAK

2006-06-01

Full Text Available Aminothiazole derivatives of 4-hydroxy-2H-chromen-2-one were prepared by the Hantzsch reaction1 using 3-(2-bromoacetyl-4-hydroxy-2H-chromen-2-one and thiourea derivatives. Starting compound for this synthesis 3-(2-bromoacetyl-4-hydroxy- 2H-chromen-2-one (1 was prepared previously.2 Also, for this synthesis we used thiourea derivatives (2a–j as compounds which possess groups with biological activity. Reactions are carried out in refluxing ethanol for a period of 30 – 45 min. Final products (3a–j are obtained in a high yield. Chemical structure of the obtained compounds was confirmed by elemental and structural analysis (IR and 1H NMR spectroscopy.

Al-doped MgB_2 materials studied using electron paramagnetic resonance and Raman spectroscopy

International Nuclear Information System (INIS)

Bateni, Ali; Somer, Mehmet; Erdem, Emre; Repp, Sergej; Weber, Stefan

2016-01-01

Undoped and aluminum (Al) doped magnesium diboride (MgB_2) samples were synthesized using a high-temperature solid-state synthesis method. The microscopic defect structures of Al-doped MgB_2 samples were systematically investigated using X-ray powder diffraction, Raman spectroscopy, and electron paramagnetic resonance. It was found that Mg-vacancies are responsible for defect-induced peculiarities in MgB_2. Above a certain level of Al doping, enhanced conductive properties of MgB_2 disappear due to filling of vacancies or trapping of Al in Mg-related vacancy sites.

Selective synthesis of FAU-type zeolites

Science.gov (United States)

Garcia, Gustavo; Cabrera, Saúl; Hedlund, Jonas; Mouzon, Johanne

2018-05-01

In the present work, parameters influencing the selectivity of the synthesis of FAU-zeolites from diatomite were studied. The final products after varying synthesis time were characterized by scanning electron microscopy, energy dispersive spectroscopy, X-ray diffraction and gas adsorption. It was found that high concentrations of NaCl could completely inhibit the formation of zeolite P, which otherwise usually forms as soon as maximum FAU crystallinity is reached. In the presence of NaCl, the FAU crystals were stable for extended time after completed crystallization of FAU before formation of sodalite. It was also found that addition of NaCl barely changed the crystallization kinetics of FAU zeolite and only reduced the final FAU particle size and SiO2/Al2O3 ratio slightly. Other salts containing either Na or Cl were also investigated. Our results suggest that there is a synergistic effect between Na+ and Cl-. This is attributed to the formation of (Na4Cl)3+ clusters that stabilize the sodalite cages. This new finding may be used to increase the selectivity of syntheses leading to FAU-zeolites and avoid the formation of undesirable by-products, especially if impure natural sources of aluminosilica are used.

Bioinspired synthesis and self-assembly of hybrid organic–inorganic nanomaterials

Energy Technology Data Exchange (ETDEWEB)

Zhang, Honghu [Iowa State Univ., Ames, IA (United States)

2016-12-17

Nature is replete with complex organic–inorganic hierarchical materials of diverse yet specific functions. These materials are intricately designed under physiological conditions through biomineralization and biological self-assembly processes. Tremendous efforts have been devoted to investigating mechanisms of such biomineralization and biological self-assembly processes as well as gaining inspiration to develop biomimetic methods for synthesis and self-assembly of functional nanomaterials. In this work, we focus on the bioinspired synthesis and self-assembly of functional inorganic nanomaterials templated by specialized macromolecules including proteins, DNA and polymers. The in vitro biomineralization process of the magnetite biomineralizing protein Mms6 has been investigated using small-angle X-ray scattering. Templated by Mms6, complex magnetic nanomaterials can be synthesized on surfaces and in the bulk. DNA and synthetic polymers have been exploited to construct macroscopic two- and three-dimensional (2D and 3D) superlattices of gold nanocrystals. Employing X-ray scattering and spectroscopy techniques, the self-assembled structures and the self-assembly mechanisms have been studied, and theoretical models have been developed. Our results show that specialized macromolecules including proteins, DNA and polymers act as effective templates for synthesis and self-assembly of nanomaterials. These bottom-up approaches provide promising routes to fabricate hybrid organic–inorganic nanomaterials with rationally designed hierarchical structures, targeting specific functions.

Synthesis of new oxovanadium (IV) complexes of potential insulinmimetic activity with coumarin-3-carboxylic acid ligands and substituted derivatives

International Nuclear Information System (INIS)

Salas Fernandez, Paloma; Alvino de la Sota, Nora; Galli Rigo-Righi, Carla

2013-01-01

This work comprises the design and synthesis of four new oxovanadium (IV) complexes, a metal which possesses insulin-mimetic action. Coumarin-3-carboxylic acid and three of its 6 -and 6,8- derivatives were used as ligands. Coumarins are of interest due to their well-known biological properties and pharmacological applications; these include the insulino-sensibilizing effect of certain alcoxy-hydroxy-derivatives which might lead to the eventual existence of a synergetic effect with the active metal center. The synthesis of the vanadyl complexes was preceded by the synthesis of the coumarin-3-carboxylic acid and its 6-bromo- derivative, as well as the syntheses of three derivatives not previously reported: 6-bromo-8-metoxi-, 6-bromo-8-nitro-, and 6-bromo-8-hydroxy-, which were prepared by a Knoevenagel condensation reaction. The complexes, on their part, were prepared by a metathesis reaction between VOSO 4 and the corresponding ligands, on the basis of methods reported for other vanadyl complexes and under strict pH control. The coumarin-3-carboxylic ligands and the derivatives were characterized by 1 H-NMR-, FTIR- and UV-Vis-spectroscopy. In the case of the complexes, their paramagnetic character did not allow for NMR characterization, being thus identified by FT-IR-spectroscopy and by the quantitative determination of their vanadium contents. (author)

Bark extract mediated green synthesis of silver nanoparticles: Evaluation of antimicrobial activity and antiproliferative response against osteosarcoma

Energy Technology Data Exchange (ETDEWEB)

Nayak, Debasis; Ashe, Sarbani; Rauta, Pradipta Ranjan; Kumari, Manisha; Nayak, Bismita, E-mail: nayakb@nitrkl.ac.in

2016-01-01

In the current investigation we report the biosynthesis potentials of bark extracts of Ficus benghalensis and Azadirachta indica for production of silver nanoparticle without use of any external reducing or capping agent. The appearance of dark brown color indicated the complete nanoparticle synthesis which was further validated by absorbance peak by UV–vis spectroscopy. The morphology of the synthesized particles was characterized by Field emission- scanning electron microscopy (Fe-SEM) and atomic force microscopy (AFM). The X-ray diffraction (XRD) patterns clearly illustrated the crystalline phase of the synthesized nanoparticles. ATR-Fourier Transform Infrared (ATR-FTIR) spectroscopy was performed to identify the role of various functional groups in the nanoparticle synthesis. The synthesized nanoparticles showed promising antimicrobial activity against Gram negative (Escherichia coli, Pseudomonas aeruginosa and Vibrio cholerae) and Gram positive (Bacillus subtilis) bacteria. The synthesized nano Ag also showed antiproliferative activity against MG-63 osteosarcoma cell line in a dose dependent manner. Thus, these synthesized Ag nanoparticles can be used as a broad spectrum therapeutic agent against osteosarcoma and microorganisms. - Highlights: • Rapid, cost effective, benign synthesis of AgNPs using novel bark extracts • Color change and absorbance peak observed at 426 and 420 nm due to SPR phenomenon • Crystalline and spherical nanoparticles having average size of ~ 40 and ~ 50 nm each • Highly enhanced antimicrobial activity against human nosocomial strains • Demonstrated dose dependent toxicity towards osteosarcoma MG-63 cell lines.

Bark extract mediated green synthesis of silver nanoparticles: Evaluation of antimicrobial activity and antiproliferative response against osteosarcoma

International Nuclear Information System (INIS)

Nayak, Debasis; Ashe, Sarbani; Rauta, Pradipta Ranjan; Kumari, Manisha; Nayak, Bismita

2016-01-01

In the current investigation we report the biosynthesis potentials of bark extracts of Ficus benghalensis and Azadirachta indica for production of silver nanoparticle without use of any external reducing or capping agent. The appearance of dark brown color indicated the complete nanoparticle synthesis which was further validated by absorbance peak by UV–vis spectroscopy. The morphology of the synthesized particles was characterized by Field emission- scanning electron microscopy (Fe-SEM) and atomic force microscopy (AFM). The X-ray diffraction (XRD) patterns clearly illustrated the crystalline phase of the synthesized nanoparticles. ATR-Fourier Transform Infrared (ATR-FTIR) spectroscopy was performed to identify the role of various functional groups in the nanoparticle synthesis. The synthesized nanoparticles showed promising antimicrobial activity against Gram negative (Escherichia coli, Pseudomonas aeruginosa and Vibrio cholerae) and Gram positive (Bacillus subtilis) bacteria. The synthesized nano Ag also showed antiproliferative activity against MG-63 osteosarcoma cell line in a dose dependent manner. Thus, these synthesized Ag nanoparticles can be used as a broad spectrum therapeutic agent against osteosarcoma and microorganisms. - Highlights: • Rapid, cost effective, benign synthesis of AgNPs using novel bark extracts • Color change and absorbance peak observed at 426 and 420 nm due to SPR phenomenon • Crystalline and spherical nanoparticles having average size of ~ 40 and ~ 50 nm each • Highly enhanced antimicrobial activity against human nosocomial strains • Demonstrated dose dependent toxicity towards osteosarcoma MG-63 cell lines

Plasma-polymerized alkaline anion-exchange membrane: Synthesis and structure characterization

International Nuclear Information System (INIS)

Hu Jue; Meng Yuedong; Zhang Chengxu; Fang Shidong

2011-01-01

After-glow discharge plasma polymerization was developed for alkaline anion-exchange membranes synthesis using vinylbenzyl chloride as monomer. X-ray photoelectron spectroscopy and attenuated total reflection Fourier transform infrared spectroscopy were used to characterize the chemical structure properties of plasma-polymerized membranes. Ion-exchange capacities of quaternized poly(vinylbenzyl chloride) (QPVBC) membranes were measured to evaluate their capability of hydroxyl ion transport. A mechanism of plasma polymerization using VBC as monomer that accounts for the competitive effects of free radicals polymerization and plasma ablation in the plasma polymerization process was proposed. Our results indicate that plasma discharge power influences the contents of functional groups and the structure of the plasma polymer membranes, which attribute to the coactions of polymerization and ablation. The properties of uniform morphology, good adhesion to the substrate, high thermal stability and satisfying anion conduction level suggest the potential application of QPVBC membrane deposited at discharge power of 20 W in alkaline direct methanol fuel cells.

Ultrasound irradiation based in-situ synthesis of star-like Tragacanth gum/zinc oxide nanoparticles on cotton fabric.

Science.gov (United States)

Ghayempour, Soraya; Montazer, Majid

2017-01-01

Application of natural biopolymers for green and safe synthesis of zinc oxide nanoparticles on the textiles is a novel and interesting approach. The present study offers the use of natural biopolymer, Tragacanth gum, as the reducing, stabilizing and binding agent for in-situ synthesis of zinc oxide nanoparticles on the cotton fabric. Ultrasonic irradiation leads to clean and easy synthesis of zinc oxide nanoparticles in short-time at low-temperature. FESEM/EDX, XRD, FT-IR spectroscopy, DSC, photocatalytic activities and antimicrobial assay are used to characterize Tragacanth gum/zinc oxide nanoparticles coated cotton fabric. The analysis confirmed synthesis of star-like zinc oxide nanoparticles with hexagonal wurtzite structure on the cotton fabric with the average particle size of 62nm. The finished cotton fabric showed a good photocatalytic activity on degradation of methylene blue and 100% antimicrobial properties with inhibition zone of 3.3±0.1, 3.1±0.1 and 3.0±0.1mm against Staphylococcus aureus, Escherichia coli and Candida albicans. Copyright © 2016 Elsevier B.V. All rights reserved.

Synthesis and characterization of Ag-Ni bimetallic nanoparticles by laser-induced plasma

International Nuclear Information System (INIS)

Xiao Qingmei; Yao Zhi; Liu Jiahong; Hai Ran; Oderji, Hassan Yousefi; Ding Hongbin

2011-01-01

We present an approach in which laser ablation deposition is used to synthesize silver-nickel bimetallic nanoparticles. A variety of techniques, including scanning electron microscopy, energy disperse spectroscopy and X-ray photoelectron spectroscopy have been used to characterize the morphology, composition and construction of synthesized bimetallic nanoparticles, respectively. The formation mechanism of bimetallic nanoparticles has been discussed. The Raman spectra of silver-nickel bimetallic nanoparticles have been analyzed. Time-of-flight mass spectrometry has been applied to directly measure intermediate species. The results indicate that diatomic AgNi is the most abundant species and suggest that the AgNi is the most stable intermediate which may play an important role in the synthesis process. Emission spectra demonstrate that the electron temperature is in the range of 6000-10000 K during the ablation process and increases with the laser power density.

A Comparative Study of the Effect of MgO and CaCO3 as Support Materials in the Synthesis of Carbon Nanotubes with Fe/Co as Catalyst

Directory of Open Access Journals (Sweden)

Ezekiel D. Dikio

2014-01-01

Full Text Available A comparative study of the effect of magnesium oxide and calcium carbonate as support material in the synthesis of carbon nanotubes using the catalyst Fe/Co is presented. The synthesized carbon nanotubes were characterized with Raman spectroscopy, scanning electron spectroscopy (SEM, high-resolution transmission electron microscopy (HRTEM, X-ray diffraction spectroscopy (XRD, and energy dispersive spectroscopy (EDS. The morphology of the carbon nanotubes synthesized with magnesium oxide as support material gives rise to carbon nanotubes with consistent and well-defined structure unlike that synthesized with calcium carbonate. The ID/IG ratio of synthesized carbon nanotubes (CNTs was 0.8544 for magnesium oxide supported compared to 0.8501 for calcium carbonate supported carbon nanotube.

Self-assembled 3-D flower-shaped SnO2 nanostructures with improved electrochemical performance for lithium storage

International Nuclear Information System (INIS)

Yang Rong; Gu Yingan; Li Yaoqi; Zheng Jie; Li Xingguo

2010-01-01

Flower-shaped SnO 2 nanoplates were successfully synthesized via a simple hydrothermal treatment of a mixture of tin(II) dichloride dihydrate (SnCl 2 .2H 2 O) and sodium citrate (Na 3 C 6 H 5 O 7 .2H 2 O) in alkali solution. The obtained SnO 2 nanoplates were less than 5 nm thick and self-assembled into flower-shaped nanostructures. The introduction of citrate was essential for the preparation of the SnO 2 nanoplates. The nanoscale shape and self-assembled architecture of SnO 2 nanoparticles were mainly controlled by the alkalinity of the solution. When the self-assembled SnO 2 nanostructures were used as anode materials in Li-ion batteries, they exhibit a reversible capacity of 670 mA h g -1 after 30 cycles and an average capacity fading of 0.95% per cycle after the second cycle. The good electrochemical performance of the SnO 2 sample prepared via the hydrothermal synthesis indicates the possibility of fabricating specific self-assembled three-dimensional nanostructures for Li-ion batteries.

Different catalysts for new polyols for rigid PUR-PIR foams

Directory of Open Access Journals (Sweden)

Liszkowska Joanna

2015-12-01

Full Text Available New polyols were synthesized with 2-hydroxypropane-1.2.3-tricarboxylic acid and butane-1,4-diol (1.4-BD. The synthesis was performed using different catalysts in the amount of 0.1%. Used catalyst: Tyzor TPT, tin(II acetate, sulfuric(IV acid. The fourth reaction was conducted without the use of a catalyst. The polyols’ properties were evaluated with regards to the usefulness in rigid polyurethane-polyisocyanurate (PUR-PIR foams (acid value, density, pH and solubility, FTIR spectra. Based on the research, it was evaluated that only the polyol synthesized using Tyzor TPT (E6 was useful in production of rigid PUR-PIR foams. Its hydroxyl number was 496 mgKOH/g and its viscosity was about 14 552 mPa · s. A series of five foams P6.1–P6.5 was produced with this polyol. Rigid foams test results indicated that the amount of this compound in the foam substantially affects its compressive strength, density and their retention. The foams have low brittleness values.

Synthesis of C{sub 60}(OH){sub 18-20} in aqueous alkaline solution under O{sub 2}-atmosphere

Energy Technology Data Exchange (ETDEWEB)

Alves, Gustavo Catao; Ladeira, Luiz Orlando; Righi, Ariete; Krambrock, Klaus; Pinheiro, Mauricio Veloso B. [Minas Gerais Univ., Belo Horizonte, MG (Brazil). Dept. de Fisica; Calado, Hallen Daniel; Gil, Rossimiriam Pereira de Freitas [Minas Gerais Univ., Belo Horizonte, MG (Brazil). Dept. de Quimica]. E-mail: gustavo.catao@terra.com.br

2006-09-15

In this work we report on an alternative synthesis of water-soluble fullerenes known as fullerols, aiming for biomedical applications. The synthesis is based on a process in which polyethylene glycol (PEG400) is used as phase-transfer catalyst between fullerene/benzene and aqueous NaOH solutions. The polyhydroxylation of the fullerenes occurs in the NaOH solution under a continuous flow of O{sub 2} to enhance the reaction yield. The resulting compound was characterized with infrared spectroscopy, nuclear magnetic resonance, thermo-gravimetric analysis and optical absorption. The formation of C{sub 60}(OH){sub 18-20} in high yields was confirmed. (author)

Synthesis and characterization of bimetallic metal-organic framework Cu-Ru-BTC with HKUST-1 structure.

Science.gov (United States)

Gotthardt, Meike A; Schoch, Roland; Wolf, Silke; Bauer, Matthias; Kleist, Wolfgang

2015-02-07

The bimetallic metal-organic framework Cu-Ru-BTC with the stoichiometric formula Cu2.75Ru0.25(BTC)2·xH2O, which is isoreticular to HKUST-1, was successfully prepared in a direct synthesis using mild reaction conditions. The partial substitution of Cu(2+) by Ru(3+) centers in the paddlewheel structure and the absence of other Ru-containing phases was proven using X-ray absorption spectroscopy.

Synthesis of lanthanum tungstate interconnecting nanoparticles by high voltage electrospinning

Energy Technology Data Exchange (ETDEWEB)

Keereeta, Yanee, E-mail: ynkeereeta@gmail.com [Department of Physics and Materials Science, Faculty of Science, Chiang Mai University, Chiang Mai 50200 (Thailand); Thongtem, Titipun, E-mail: ttpthongtem@yahoo.com [Department of Chemistry, Faculty of Science, Chiang Mai University, Chiang Mai 50200 (Thailand); Materials Science Research Center, Faculty of Science, Chiang Mai University, Chiang Mai 50200 (Thailand); Thongtem, Somchai [Department of Physics and Materials Science, Faculty of Science, Chiang Mai University, Chiang Mai 50200 (Thailand); Materials Science Research Center, Faculty of Science, Chiang Mai University, Chiang Mai 50200 (Thailand)

2015-10-01

Graphical abstract: - Highlights: • La{sub 2}(WO{sub 4}){sub 3} as one of semiconducting materials. • H.V. electrospinning was used to synthesize La{sub 2}(WO{sub 4}){sub 3} interconnecting nanoparticles. • A promising material for photoemission. - Abstract: Lanthanum tungstate (La{sub 2}(WO{sub 4}){sub 3}) interconnecting nanoparticles in the shape of fibers were successfully synthesized by electrospinning in combination with high temperature calcination. In this research, calcination temperature for the synthesis of the fibers evidently influenced the diameter, morphology and crystalline degree. The crystalline monoclinic La{sub 2}(WO{sub 4}){sub 3} fibers with 200–700 nm in diameter, two main Raman peaks at 945 and 927 cm{sup −1}, FTIR stretching modes at 936 and 847 cm{sup −1}, 2.02 eV energy gap and 415–430 nm blue emission were synthesized by calcination of inorganic/organic hybrid fibers at 750 °C for 5 h, characterized by X-ray diffraction, scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED), thermogravimetric analysis (TGA), Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, UV–visible spectroscopy and photoluminescence (PL) spectroscopy. The surface of the composite fibers before calcination was very smooth. Upon calcination the composite fibers at 750 °C for 5 h, they were transformed into nanoparticles join together in the shape of fibers with rough surface.

Synthesis and extracellular accumulation of silver nanoparticles by employing radiation-resistant Deinococcus radiodurans, their characterization, and determination of bioactivity

Directory of Open Access Journals (Sweden)

Kulkarni RR

2015-01-01

Full Text Available Rasika R Kulkarni, Nayana S Shaiwale, Dileep N Deobagkar, Deepti D Deobagkar Molecular Biology Research Laboratory, Center of Advanced Studies, Department of Zoology, University of Pune, Pune, India Abstract: There has been rapid progress in exploring microorganisms for green synthesis of nanoparticles since microbes show extraordinary diversity in terms of species richness and niche localization. Microorganisms are easy to culture using relatively inexpensive and simple nutrients under varied conditions of temperature, pressure, pH, etc. In this work, Deinococcus radiodurans that possesses the ability to withstand extremely high radiation and desiccation stress has been employed for the synthesis of silver nanoparticles (AgNPs. D. radiodurans was able to accumulate AgNPs in medium under various conditions, and process optimization was carried out with respect to time, temperature, pH, and concentration of silver salt. AgNPs were characterized using UV/vis spectroscopy, scanning electron microscopy, transmission electron microscopy, X-ray diffraction, energy-dispersive X-ray spectroscopy, and Fourier transform infrared spectroscopy. The microbially synthesized AgNPs exhibited good antimicrobial activity against both Gram-negative and Gram-positive organisms and anti-biofouling activity. Their ability to inhibit growth and proliferation of cancer cell line was also examined, and it could be seen that AgNPs synthesized using D. radiodurans exhibited excellent anticancer activity. Keywords: Deinococcus radiodurans, silver nanoparticles, anticancer, radiation resistance, antibacterial, anti-biofouling 

In situ synthesis of carbon nanotubes decorated with palladium nanoparticles using arc-discharge in solution method

International Nuclear Information System (INIS)

Bera, Debasis; Kuiry, Suresh C.; McCutchen, Matthew; Seal, Sudipta; Heinrich, Helge; Slane, Grady C.

2004-01-01

A unique, simple, inexpensive, and one-step synthesis route to produce carbon nanotubes (CNTs) decorated with palladium nanoparticles using a simplified dc arc-discharge in solution is reported. Zero-loss energy filtered transmission electron microscopy and scanning transmission electron microscopy confirm the presence of 3 nm palladium nanoparticles. Such palladium nanoparticles form during the reduction of palladium tetra-chloro-square-planar complex. The deconvoluted x-ray photoelectron spectroscopy envelope shows the presence of palladium on the decorated CNTs. The energy dispersive spectroscopy suggests no functionalization of atomic chlorine to the sidewall of the CNTs. The presence of dislodged graphene sheets with wavy morphology supports the formation of CNTs through the 'scroll mechanism'

Effect of synthesis method on the preparation of lanthanum chromite for using as ceramic pigment

International Nuclear Information System (INIS)

Dantas, G.C.B.; Ferreira, K.M.B.; Pimentel, P.M.; Melo, D.M.A.; Gomes, D.K.S.; Costa, A.F.

2016-01-01

In this paper, LaCrO3 perovskites were synthesized by two synthesis methods, in order to compare these methods in function of microstructure and optical properties. The synthesis routes employed were a method that use gelatin as organic precursor and microwave assisted auto-combustion. The resulting powders were calcined at 800 ° C and 1000 ° C for obtaining the perovskite phase. Then, they were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM); UV-Visible spectroscopy and colorimetric analysis for color identification. No significant changes were observed in the powders synthesized by two routes. The oxides presented orthorhombic perovskite structure. The powders synthesized by the gelatin method were single phase. Chromite lanthanide presented grayish hue being darker in perovskites calcined at higher temperatures. (author)

Design, Synthesis, and Mechanistic Evaluation of Iron-Based Catalysis for Synthesis Gas Conversion to Fuels and Chemicals. Technical Progress Report

International Nuclear Information System (INIS)

Akio Ishikawa; Manuel Ojeda; Nan Yao; Enrique Iglesia

2006-01-01

This project extends previously discovered Fe-based catalysts to hydrogen-poor synthesis gas streams derived from coal and biomass sources. These catalysts have shown unprecedented Fischer-Tropsch synthesis rate, selectivity for feedstocks consisting of synthesis gas derived from methane. During the first reporting period, we certified a microreactor, installed required analytical equipment, and reproduced synthetic protocols and catalytic results previously reported. During the second reporting period, we prepared several Fe-based compositions for Fischer-Tropsch synthesis and tested the effects of product recycle under both subcritical and supercritical conditions. During the third and fourth reporting periods, we improved the catalysts preparation method, which led to Fe-based FT catalysts with the highest FTS reaction rates and selectivities so far reported, a finding that allowed their operation at lower temperatures and pressures with high selectivity to desired products (C 5+ , olefins). During this fifth reporting period, we have studied the effects of different promoters on catalytic performance, specifically how their sequence of addition dramatically influences the performance of these materials in the Fischer-Tropsch synthesis. The resulting procedures have been optimized to improve further upon the already unprecedented rates and C 5+ selectivities of the Fe-based catalysts that we have developed as part of this project. During this fifth reporting period, we have also continued our studies of optimal activation procedures, involving reduction and carburization of oxide precursors during the early stages of contact with synthesis gas. We have completed the analysis of the evolution of oxide, carbide, and metal phases of the active iron components during initial contact with synthesis gas using advanced synchrotron techniques based on X-ray absorption spectroscopy. We have confirmed that the Cu or Ru compensates for inhibitory effects of Zn, a surface

Characterization of bimetallic Fe/Pd nanoparticles by grape leaf aqueous extract and identification of active biomolecules involved in the synthesis

Energy Technology Data Exchange (ETDEWEB)

Luo, Fang; Yang, Die; Chen, Zuliang, E-mail: Zuliang.chen@newcastle.edu.au; Megharaj, Mallavarapu; Naidu, Ravi

2016-08-15

This paper reports the detailed composition and morphology of one-step green synthesized bimetallic Fe/Pd nanoparticles (NPs) using grape leaf aqueous extract and identification of active biomolecules involved in the synthesis employing various techniques. Transmission Electron Microscopy (TEM) and Scanning Electron Microscopy (SEM) revealed that Fe/Pd NPs were polydispersed and quasi-spherical with a diameter ranging from 2 to 20 nm. X-ray Photoelectron Spectroscopy (XPS) and Energy Dispersive X-ray Spectroscopy (EDS) provided evidence for the composition of Fe and Pd and for their species existing on the surface of Fe/Pd NPs. In addition, biomolecules in the grape leaf aqueous extract were identified but their functions are still unclear. Biomolecules in the aqueous extract such as methoxy-phenyl-oxime, N-benzoyl-2-cyano-histamine, 2-ethyl-phenol, 1,2-benzenediol, β-hydroxyquebracamine, hydroquinone, 2-methoxy-4-vinylphenol, 5-methyl-2-furancarboxaldehyde, 4-(3-hydroxybutyl)-3,5,5-trimethyl-2-cyclohexen and some polyphenolic compounds were identified as reducing and capping agents, which were studied by Chromatography-Mass Spectroscopy (GC–MS), XPS and Fourier Transform Infrared Spectroscopy (FTIR). Our finding suggests a new insight into cost-effective, simple, and environmentally benign production of bimetallic Fe/Pd NPs. - Graphical abstract: TEM image for the Fe/Pd NPs synthesized by grape leaf aqueous extract. - Highlights: • The one-step green synthesis of Fe/Pd nanoparticles has been systematically characterized. • TEM showed that the Fe/Pd NPs were polydispersed with a diameter ranging from 2 to 20 nm. • Active biomolecules in the grape extract were identified.

Characterization of bimetallic Fe/Pd nanoparticles by grape leaf aqueous extract and identification of active biomolecules involved in the synthesis

International Nuclear Information System (INIS)

Luo, Fang; Yang, Die; Chen, Zuliang; Megharaj, Mallavarapu; Naidu, Ravi

2016-01-01

This paper reports the detailed composition and morphology of one-step green synthesized bimetallic Fe/Pd nanoparticles (NPs) using grape leaf aqueous extract and identification of active biomolecules involved in the synthesis employing various techniques. Transmission Electron Microscopy (TEM) and Scanning Electron Microscopy (SEM) revealed that Fe/Pd NPs were polydispersed and quasi-spherical with a diameter ranging from 2 to 20 nm. X-ray Photoelectron Spectroscopy (XPS) and Energy Dispersive X-ray Spectroscopy (EDS) provided evidence for the composition of Fe and Pd and for their species existing on the surface of Fe/Pd NPs. In addition, biomolecules in the grape leaf aqueous extract were identified but their functions are still unclear. Biomolecules in the aqueous extract such as methoxy-phenyl-oxime, N-benzoyl-2-cyano-histamine, 2-ethyl-phenol, 1,2-benzenediol, β-hydroxyquebracamine, hydroquinone, 2-methoxy-4-vinylphenol, 5-methyl-2-furancarboxaldehyde, 4-(3-hydroxybutyl)-3,5,5-trimethyl-2-cyclohexen and some polyphenolic compounds were identified as reducing and capping agents, which were studied by Chromatography-Mass Spectroscopy (GC–MS), XPS and Fourier Transform Infrared Spectroscopy (FTIR). Our finding suggests a new insight into cost-effective, simple, and environmentally benign production of bimetallic Fe/Pd NPs. - Graphical abstract: TEM image for the Fe/Pd NPs synthesized by grape leaf aqueous extract. - Highlights: • The one-step green synthesis of Fe/Pd nanoparticles has been systematically characterized. • TEM showed that the Fe/Pd NPs were polydispersed with a diameter ranging from 2 to 20 nm. • Active biomolecules in the grape extract were identified.

Niobium-Doped Hydroxyapatite Bioceramics: Synthesis, Characterization and In Vitro Cytocompatibility

Directory of Open Access Journals (Sweden)

Nádia S. V. Capanema

2015-07-01

Full Text Available Doping calcium phosphates with ionic species can play an important role in biological responses promoting alkaline phosphatase activity, and, therefore inducing the generation of new bone. Thus, in this study, the synthesis of niobium-doped hydroxyapatite (Nb-HA nanosize particles obtained by the precipitation process in aqueous media followed by thermal treatment is presented. The bioceramics were extensively characterized by X-ray diffraction, wavelength dispersive X-ray fluorescence spectrometry, Fourier transform infrared spectroscopy, scanning electron microscopy/energy dispersive X-ray spectroscopy analysis, transmission electron microscopy, atomic force microscopy and thermal analysis regarding their chemical composition, structure and morphology. The results showed that the precipitate dried at 110 °C was composed of amorphous calcium phosphate and HA, with polidisperse particles ranging from micro to nano dimensions. After the thermal treatment at 900 °C, the bioceramic system evolved predominantly to HA crystalline phase, with evident features of particle sintering and reduction of surface area. Moreover, the addition of 10 mol% of niobium salt precursor during the synthesis indicated the complete incorporation of the Nb(V species in the HA crystals with detectable changes in the original lattice parameters. Furthermore, the incorporation of Nb ions caused a significant refinement on the average particle size of HA. Finally, the preliminary cytocompatibility response of the biomaterials was accessed by human osteoblast cell culture using MTT and resazurin assays, which demonstrated no cytotoxicity of the Nb-alloyed hydroxyapatite. Thus, these findings seem promising for developing innovative Nb-doped calcium phosphates as artificial biomaterials for potential use in bone replacements and repair.

Analytical applications of spectroscopy

International Nuclear Information System (INIS)

Creaser, C.S.

1988-01-01

This book provides an up to date overview of recent developments in analytical spectroscopy, with a particular emphasis on the common themes of chromatography - spectroscopy combinations, Fourier transform methods, and data handling techniques, which have played an increasingly important part in the development of all spectroscopic techniques. The book contains papers originally presented at a conference entitled 'Spectroscopy Across The Spectrum' held jointly with the first 'International Near Infrared Spectroscopy Conference' at the University of East Anglia, Norwich, UK, in July 1987, which have been edited and rearranged with some additional material. Each section includes reviews of key areas of current research as well as short reports of new developments. The fields covered are: Near Infrared Spectroscopy; Infrared Spectroscopy; Mass Spectroscopy; NMR Spectroscopy; Atomic and UV/Visible Spectroscopy; Chemometrics and Data Analysis. (author)

Tin dioxide sol-gel derived films doped with platinum and antimony deposited on porous silicon

NARCIS (Netherlands)

Savaniu, C.; Arnautu, A.; Cobianu, C.; Craciun, G.; Flueraru, C.; Zaharescu, M.; Parlog, C.; Paszti, F.; van den Berg, Albert

1999-01-01

SnO2 sol-gel derived thin films doped simultaneously with Pt and Sb are obtained and reported for the first time. The Sn sources were tin(IV) ethoxide or tin(II) ethylhexanoate, while hexachloroplatinic acid (H2PtCl6) and antimony chloride (SbCl3) were used as platinum and antimony sources,

Triblock copolymer-mediated synthesis of catalytically active gold nanostructures

Science.gov (United States)

Santos, Douglas C.; de Souza, Viviane C.; Vasconcelos, Diego A.; Andrade, George R. S.; Gimenez, Iara F.; Teixeira, Zaine

2018-04-01

The design of nanostructures based on poly(ethylene oxide)-poly(propylene)-poly(ethylene oxide) (PEO-PPO-PEO) and metal nanoparticles is becoming an important research topic due to their multiple functionalities in different fields, including nanomedicine and catalysis. In this work, water-soluble gold nanoparticles have been prepared through a green aqueous synthesis method using Pluronic F127 as both reducing and stabilizing agents. The size dependence (varying from 2 to 70 nm) and stability of gold nanoparticles were systematically studied by varying some parameters of synthesis, which were the polymer concentration, temperature, and exposure to UV-A light, being monitored by UV-Vis spectroscopy and TEM. Also, an elaborated study regarding to the kinetic of formation (nucleation and growth) was presented. Finally, the as-prepared Pluronic-capped gold nanoparticles have shown excellent catalytic activity towards the reduction of 4-nitrophenol to 4-aminophenol with sodium borohydride, in which a higher catalytic performance was exhibited when compared with gold nanoparticles prepared by classical reduction method using sodium citrate. [Figure not available: see fulltext.

Enzymatic Synthesis of Fatty Hydroxamic Acid Derivatives Based on Palm Kernel Oil

Directory of Open Access Journals (Sweden)

Sidik Silong

2011-08-01

Full Text Available Fatty hydroxamic acid derivatives were synthesized using Lipozyme TL IM catalyst at biphasic medium as the palm kernel oil was dissolved in hexane and hydroxylamine derivatives were dissolved in water: (1 N-methyl fatty hydroxamic acids (MFHAs; (2 N-isopropyl fatty hydroxamic acids (IPFHAs and (3 N-benzyl fatty hydroxamic acids (BFHAs were synthesized by reaction of palm kernel oil and N-methyl hydroxylamine (N-MHA, N-isopropyl hydroxylamine (N-IPHA and N-benzyl hydroxylamine (N-BHA, respectively. Finally, after separation the products were characterized by color testing, elemental analysis, FT-IR and 1H-NMR spectroscopy. For achieving the highest conversion percentage of product the optimum molar ratio of reactants was obtained by changing the ratio of reactants while other reaction parameters were kept constant. For synthesis of MFHAs the optimum mol ratio of N-MHA/palm kernel oil = 6/1 and the highest conversion was 77.8%, for synthesis of IPFHAs the optimum mol ratio of N-IPHA/palm kernel oil = 7/1 and the highest conversion was 65.4% and for synthesis of BFHAs the optimum mol ratio of N-BHA/palm kernel oil = 7/1 and the highest conversion was 61.7%.

Urea-assisted low temperature green synthesis of graphene nanosheets for transparent conducting film

Science.gov (United States)

Chamoli, Pankaj; Das, Malay K.; Kar, Kamal K.

2018-02-01

Present work demonstrates the fabrication of graphene nanosheet (GN) based transparent conducting film (TCF) using spray coating. Green synthesis of GN is carried out by reduction of graphene oxide (GO) using urea as green reducing agent. The reductive ability of urea with varied concentration is studied for GO at low temperature (i.e., 90 °C). As synthesized graphene nanosheets (GNs) are characterized by Raman spectroscopy, Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), UV-visible spectroscopy, field emission scanning electron microscopy (FESEM), atomic force microscope (AFM), and X-ray Photon spectroscopy (XPS). Raman analysis confirms that the maximum reduction of oxygen species is noticed using 30 mg/ml urea concentration at 90 °C from GO, and found Raman D to G band ratio (ID/IG) of ∼1.30. XPS analysis validates the Raman signature of removal of oxygen functional groups from GO, and obtained C/O ratio of ∼5.28. Further, transparent conducting films (TCFs) are fabricated using synthesized GNs. Thermal graphitization is carried out to enhance the optical and electrical properties of TCFs. TCF shows best performance when it is annealed at 900 °C for 1 h in vacuum, and obtained sheet resistance is ∼1.89 kΩ/□ with transmittance of ∼62.53%.

Facile synthesis of carbon-ZnO nanocomposite with enhanced visible light photocatalytic performance

Energy Technology Data Exchange (ETDEWEB)

Akir, Sana [Univ. Lille, CNRS, Centrale Lille, ISEN, Univ. Valenciennes, UMR 8520 − IEMN, F-59000, Centrale Lille (France); Laboratoire de Physique des Matériaux Lamellaires et Nano-Matériaux Hybrides, Faculté des Sciences de Bizerte, Université de Carthage, 7021, Bizerte (Tunisia); Laboratoire de Physico-chimie des Matériaux Minéraux et leurs Applications, Centre National des Recherches en Sciences des Matériaux, Technopôle de Bordj Cedria, BP73, 8027, Soliman (Tunisia); Hamdi, Abderrahmane [Univ. Lille, CNRS, Centrale Lille, ISEN, Univ. Valenciennes, UMR 8520 − IEMN, F-59000, Centrale Lille (France); Laboratoire de Physique des Matériaux Lamellaires et Nano-Matériaux Hybrides, Faculté des Sciences de Bizerte, Université de Carthage, 7021, Bizerte (Tunisia); Laboratory of Semi-conductors, Nano-structures and Advanced Technologies, Research and Technology Centre of Energy, Borj-Cedria Science and Technology Park, BP 95, 2050, Hammam-Lif (Tunisia); Addad, Ahmed [UMET, UMR CNRS 8207, Université Lille 1, 59655 Villeneuve d' Ascq Cédex (France); Coffinier, Yannick [Univ. Lille, CNRS, Centrale Lille, ISEN, Univ. Valenciennes, UMR 8520 − IEMN, F-59000, Centrale Lille (France); Boukherroub, Rabah, E-mail: rabah.boukherroub@iemn.univ-lille1.fr [Univ. Lille, CNRS, Centrale Lille, ISEN, Univ. Valenciennes, UMR 8520 − IEMN, F-59000, Centrale Lille (France); and others

2017-04-01

Highlights: • C-ZnO nanocomposite was successfully prepared via a facile and eco-friendly process. • C-ZnO NPs have excellent photocatalytic activity for RhB dye degradation under visible light irradiation compared with literature. • The visible photocatalytic properties originate from injection e{sup −} in CB of ZnO from RhB. - Abstract: The present study describes a facile route for synthesis of carbon-ZnO nanocomposites (C-ZnO) via hydrothermal process in presence of glucose as carbon precursor. The samples were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDX), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), UV–vis diffuse reflectance spectroscopy (DRS) and photoluminescence (PL) measurements. The results showed carbon uniformly coated on the surface of the ZnO nanoparticles to form the C-ZnO nanocomposites. Further investigation revealed that carbon could significantly protect ZnO NPs against the coalescence during high temperature treatment. The obtained C-ZnO nanocomposite showed excellent photocatalytic activity for the degradation of rhodamine B (RhB) under visible light irradiation, which was attributed to the repressed charge carrier recombination in the nanocomposite. Quenching experiments and photocurrent measurements revealed a photocatalytic mechanism occurring through photosensitization.

Green Synthesis and Antibacterial Activities of Silver Nanoparticles Using Extracellular Laccase of Lentinus edodes

Directory of Open Access Journals (Sweden)

Agbaje LATEEF

2015-12-01

Full Text Available This study reports the multi-step mutagenesis of Lentinus edodes towards optimization of the production of laccase and novel application of laccase in the biosynthesis of silver nanoparticles (AgNPs which could be used to develop an eco-friendly method for the rapid biosynthesis of AgNPs. The wild strain of L. edodes was subjected to UV irradiation at 254 nm and the resultant viable mutant was further treated with acridine orange, a chemical mutagen. The strains were evaluated for the production of laccase and the crude laccase of the UV mutant (UV10 was used for the green synthesis of AgNPs. The particles were characterized by UV-Visible spectroscopy, Fourier transform infrared (FTIR spectroscopy and scanning electron microscopy (SEM. Laccase activities of wild, UV10 and UV10ACR8 strains of L. edodes were obtained as 2.6, 10.6 and 2.8 U/ml/min respectively after 7 days of fermentation, showing laccase yield improvement of 4.08-fold for UV10 mutant. UV-Visible spectroscopy indicated the formation of AgNPs at absorption band of 430 nm. FTIR result indicated that proteins were responsible for AgNP synthesis, while SEM analysis confirmed the formation of walnut-shaped nanoparticles with size range of 50-100 nm. The biosynthesized nanoparticles revealed effective inhibition against clinical isolates of Escherichia coli, Pseudomonas aeruginosa and Klebsiella pneumoniae. To the best of the authors’ knowledge, this result represents the first report on the biosynthesis of AgNPs using L. edodes metabolite. The report adds to the growing relevance of L. edodes as potential industrially viable organism, used for diverse biotechnological applications.

Extracellular synthesis of silver nanoparticles using the leaf extract of Coleus amboinicus Lour

Energy Technology Data Exchange (ETDEWEB)

Narayanan, Kannan Badri [Department of Biotechnology, School of Life Sciences, Pondicherry University, Kalapet, Puducherry 605014 (India); Sakthivel, Natarajan, E-mail: puns2005@gmail.com [Department of Biotechnology, School of Life Sciences, Pondicherry University, Kalapet, Puducherry 605014 (India)

2011-10-15

Highlights: {yields} Synthesis of AgNPs using the leaf extract of Coleus amboinicus L. was described. {yields} UV-vis absorption spectra showed the formation of isotrophic AgNPs at 437 nm in 6 h. {yields} XRD analysis showed intense peaks corresponding to fcc structure of AgNPs. {yields} HR-TEM analysis revealed the formation of stable anisotrophic and isotrophic AgNPs. -- Abstract: In the present investigation, Coleus amboinicus Lour. leaf extract-mediated green chemistry approach for the synthesis of silver nanoparticles was described. The nanoparticles were characterized by ultraviolet-visible (UV-Vis) spectroscopy, X-ray diffraction (XRD), energy dispersive X-ray analysis (EDAX), Fourier transform infrared spectroscopy (FTIR) and transmission electron microscopy (TEM). The influence of leaf extract on the control of size and shape of silver nanoparticles is reported. Upon an increase in the concentration of leaf extract, there was a shift in the shape of nanoparticles from anisotrophic nanostructures like triangle, decahedral and hexagonal to isotrophic spherical nanoparticles. Crystalline nature of fcc structured nanoparticles was confirmed by XRD spectrum with peaks corresponding to (1 1 1), (2 0 0), (2 2 0) and (3 1 1) planes and bright circular spots in the selected-area electron diffraction (SAED). Such environment friendly and sustainable methods are non-toxic, cheap and alternative to hazardous chemical procedures.

Synthesis of carbon nanofibres from waste chicken fat for field electron emission applications

Energy Technology Data Exchange (ETDEWEB)

Suriani, A.B., E-mail: absuriani@yahoo.com [Nanotechnology Research Centre, Faculty of Science and Mathematics, Universiti Pendidikan Sultan Idris, Tanjung Malim, Perak 35900 (Malaysia); Department of Physics, Faculty of Science and Mathematics, Universiti Pendidikan Sultan Idris, Tanjung Malim, Perak 35900 (Malaysia); Dalila, A.R. [Nanotechnology Research Centre, Faculty of Science and Mathematics, Universiti Pendidikan Sultan Idris, Tanjung Malim, Perak 35900 (Malaysia); Department of Physics, Faculty of Science and Mathematics, Universiti Pendidikan Sultan Idris, Tanjung Malim, Perak 35900 (Malaysia); Mohamed, A.; Isa, I.M.; Kamari, A.; Hashim, N. [Nanotechnology Research Centre, Faculty of Science and Mathematics, Universiti Pendidikan Sultan Idris, Tanjung Malim, Perak 35900 (Malaysia); Department of Chemistry, Faculty of Science and Mathematics, Universiti Pendidikan Sultan Idris, Tanjung Malim, Perak 35900 (Malaysia); Soga, T.; Tanemura, M. [Department of Frontier Materials, Nagoya Institute of Technology, Gokiso-cho, Showa-ku, Nagoya 466-8555 (Japan)

2015-10-15

Highlights: • Waste chicken fat is used as a starting material to produce CNFs via TCVD method. • High heating rate applied resulted in aggregation of catalyst particles. • Aggregated catalyst produced sea urchin-like CNFs with amorphous nature. • The as-grown CNFs presented a potential for field electron emission applications. - Abstract: Carbon nanofibres (CNFs) with sea urchin-like morphology were synthesised from waste chicken fat precursor via catalytic thermal chemical vapour deposition method at 750 °C. The CNFs showed amorphous structures under high-resolution transmission electron microscopy, micro-Raman spectroscopy and X-ray diffraction examination. X-ray photoelectron spectroscopy analysis confirmed that the core of the sea urchin-like CNFs was composed of Fe{sub 3}C formed within the first 20 min of synthesis time. The growth of amorphous CNFs from agglomerated Fe{sub 3}C particles was favourable due to the high heating rate applied during the synthesis. Field electron emission examination of the CNFs indicated turn-on and threshold field values of 5.4 and 6.6 V μm{sup −1} at current density of 1 and 10 μA cm{sup −2}, respectively. This study demonstrates that waste chicken fat, a low-cost and readily available resource, can be used as an inexpensive carbon source for the production of CNFs with a potential application in field electron emitters.

Controlled Synthesis of Au@AgAu Yolk-Shell Cuboctahedra with Well-Defined Facets.

Science.gov (United States)

Londono-Calderon, Alejandra; Bahena, Daniel; Yacaman, Miguel J

2016-08-02

The synthesis of Au@AgAu yolk-shell cuboctahedra nanoparticles formed by galvanic replacement in a seed-mediated method is described. Initially, single-crystal Au seeds are used for the formation of Au@Ag core-shell nanocubes, which serve as the template material for the deposition of an external Au layer. The well-controlled synthesis yields the formation of cuboctahedra nanoparticles with smooth inner and outer Au/Ag surfaces. The deposition/oxidation process is described to understand the formation of cuboctahedra and octahedra nanoparticles. The Au core maintains the initial morphology of the seed and remains static at the center of the yolk-shell because of residual Ag. Structural analysis of the shell indicates intrinsic stacking faults (SFs) near the surface. Energy dispersive X-ray spectroscopy (EDS) and X-ray photoelectron spectroscopy (XPS) compositional analysis show an Au-Ag nonordered alloy forming the shell. The three-dimensional structure of the nanoparticles presented open facets on the [111] as observed by electron tomography SIRT reconstruction over a stack of high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) images. The geometrical model was validated by analyzing the direction of streaks in coherent nanobeam diffraction (NBD). The catalytic activity was evaluated using a model reaction based on the reduction of 4-nitrophenol (4-NTP) by NaBH4 in the presence of Au@AgAu yolk-shell nanoparticles.

Synthesis of carbon nanofibres from waste chicken fat for field electron emission applications

International Nuclear Information System (INIS)

Suriani, A.B.; Dalila, A.R.; Mohamed, A.; Isa, I.M.; Kamari, A.; Hashim, N.; Soga, T.; Tanemura, M.

2015-01-01

Highlights: • Waste chicken fat is used as a starting material to produce CNFs via TCVD method. • High heating rate applied resulted in aggregation of catalyst particles. • Aggregated catalyst produced sea urchin-like CNFs with amorphous nature. • The as-grown CNFs presented a potential for field electron emission applications. - Abstract: Carbon nanofibres (CNFs) with sea urchin-like morphology were synthesised from waste chicken fat precursor via catalytic thermal chemical vapour deposition method at 750 °C. The CNFs showed amorphous structures under high-resolution transmission electron microscopy, micro-Raman spectroscopy and X-ray diffraction examination. X-ray photoelectron spectroscopy analysis confirmed that the core of the sea urchin-like CNFs was composed of Fe 3 C formed within the first 20 min of synthesis time. The growth of amorphous CNFs from agglomerated Fe 3 C particles was favourable due to the high heating rate applied during the synthesis. Field electron emission examination of the CNFs indicated turn-on and threshold field values of 5.4 and 6.6 V μm −1 at current density of 1 and 10 μA cm −2 , respectively. This study demonstrates that waste chicken fat, a low-cost and readily available resource, can be used as an inexpensive carbon source for the production of CNFs with a potential application in field electron emitters

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

Synthesis and characterization of strontium carboxylates at room temperature and at high temperature in autoclave vessels

DEFF Research Database (Denmark)

Christgau, Stephan; Ståhl, Kenny; Andersen, Jens Enevold Thaulov

2006-01-01

A novel method was developed for synthesis of strontium coordination compounds in high yields. The synthesis proceeded along three pathways that provided strontium salts in high purity and high yields, close to 100%, as confirmed by flame atomic absorption spectroscopy (FAAS) and powder x......-ray crystallography. Optimum conditions were found at T = 120-1400C, a base-to-acid ratio of 1.2 and 15 min. of reaction-time in an autoclave vessel. Large crystals were readily obtained within a time period of hours. The crystal structures of strontium D-glutamate hexahydrate (I) and strontium di-(hydrogen L......-glutamate) pentahydrate (II) were confirmed by X-ray powder diffraction at 295 K and Rietveld refinements (I: Space group P212121, Z=4, a=7.3519(2), b=8.7616(2), c=20.2627(5) Å, and II: Space group P21, Z=2, a=8.7243(1), b=7.2635(1), c=14.6840(2) Å, β=100.5414(7) °). Synthesis at room temperature provided four additional...

Green synthesis, characterization and catalytic activity of natural bentonite-supported copper nanoparticles for the solvent-free synthesis of 1-substituted 1H-1,2,3,4-tetrazoles and reduction of 4-nitrophenol

Directory of Open Access Journals (Sweden)

Akbar Rostami-Vartooni

2015-12-01

Full Text Available In this study, Cu nanoparticles were immobilized on the surface of natural bentonite using Thymus vulgaris extract as a reducing and stabilizing agent. The natural bentonite-supported copper nanoparticles (Cu NPs/bentonite were characterized by FTIR spectroscopy, X-ray diffraction (XRD, X-ray fluorescence (XRF, field emission scanning electron microscopy (FE-SEM, energy dispersive X-ray spectroscopy (EDS, transmission electron microscopy (TEM, selected area electron diffraction (SAED and Brunauer–Emmett–Teller (BET analysis. Afterward, the catalytic performance of the prepared catalyst was investigated for the solvent-free synthesis of 1-substituted 1H-1,2,3,4-tetrazoles and reduction of 4-nitrophenol (4-NP in water. It was found that the Cu NPs/bentonite is a highly active and recyclable catalyst for related reactions.

Oxovanadium(IV) complexes of non-steroidal anti-inflammatory drugs: synthesis, spectroscopy, and antimicrobial activity

International Nuclear Information System (INIS)

Muhammad, N.; Ali, S.; Shahzadi, S.; Khan, A.N.

2008-01-01

Oxovanadium(IV) complexes with four different non-steroidal anti-inflammatory drugs have been synthesized. These complexes were characterized by different analytical techniques such as CHN, IR, UV-Vis spectroscopy, and mass spectrometry. The IR data show the bidentate nature of the ligands and reveal hexacoordinate geometry in the solid state. The complexes were tested for their biological activity against six different bacterial strains and plant pathogens, and all complexes showed good biological activity with few exceptions [ru

Piper betle-mediated synthesis, characterization, antibacterial and rat splenocyte cytotoxic effects of copper oxide nanoparticles.

Science.gov (United States)

Praburaman, Loganathan; Jang, Jum-Suk; Muthusamy, Govarthanan; Arumugam, Sengottaiyan; Manoharan, Koildhasan; Cho, Kwang-Min; Min, Cho; Kamala-Kannan, Seralathan; Byung-Taek, Oh

2016-09-01

The study reports a simple, inexpensive, and eco-friendly synthesis of copper oxide nanoparticles (CuONPs) using Piper betle leaf extract. Formation of CuONPs was confirmed by UV-visible spectroscopy at 280 nm. Transmission electron microscopy (TEM) images showed that the CuONPs were spherical, with an average size of 50-100 nm. The scanning electron microscopy (SEM)-energy dispersive spectroscopy (EDS) peak was observed approximately at 1 and 8 keV. The X-ray diffraction (XRD) studies indicated that the particles were crystalline in nature. CuONPs effectively inhibited the growth of phytopathogens Ralstonia solanacearum and Xanthomonas axonopodis. The cytotoxic effect of the synthesized CuONPs was analyzed using rat splenocytes. The cell viability was decreased to 94% at 300 μg/mL.

Admittance spectroscopy or deep level transient spectroscopy: A contrasting juxtaposition

Science.gov (United States)

Bollmann, Joachim; Venter, Andre

2018-04-01

A comprehensive understanding of defects in semiconductors remains of primary importance. In this paper the effectiveness of two of the most commonly used semiconductor defect spectroscopy techniques, viz. deep level transient spectroscopy (DLTS) and admittance spectroscopy (AS) are reviewed. The analysis of defects present in commercially available SiC diodes shows that admittance spectroscopy allows the identification of deep traps with reduced measurement effort compared to deep Level Transient Spectroscopy (DLTS). Besides the N-donor, well-studied intrinsic defects were detected in these diodes. Determination of their activation energy and defect density, using the two techniques, confirm that the sensitivity of AS is comparable to that of DLTS while, due to its well defined peak shape, the spectroscopic resolution is superior. Additionally, admittance spectroscopy can analyze faster emission processes which make the study of shallow defects more practical and even that of shallow dopant levels, possible. A comparative summary for the relevant spectroscopic features of the two capacitance methods are presented.

Room temperature chemical synthesis of Cu(OH){sub 2} thin films for supercapacitor application

Energy Technology Data Exchange (ETDEWEB)

Gurav, K.V. [Thin Film Photonic and Electronics Lab, Department of Materials Science and Engineering, Chonnam National University, 300 Yongbong-dong, Puk-Gu, Gwangju 500-757 (Korea, Republic of); Patil, U.M. [Thin Film Physics Laboratory, Department of Physics, Shivaji University, Kolhapur 416 007 (M.S.) (India); Shin, S.W.; Agawane, G.L.; Suryawanshi, M.P.; Pawar, S.M.; Patil, P.S. [Thin Film Photonic and Electronics Lab, Department of Materials Science and Engineering, Chonnam National University, 300 Yongbong-dong, Puk-Gu, Gwangju 500-757 (Korea, Republic of); Lokhande, C.D. [Thin Film Physics Laboratory, Department of Physics, Shivaji University, Kolhapur 416 007 (M.S.) (India); Kim, J.H., E-mail: jinhyeok@chonnam.ac.kr [Thin Film Photonic and Electronics Lab, Department of Materials Science and Engineering, Chonnam National University, 300 Yongbong-dong, Puk-Gu, Gwangju 500-757 (Korea, Republic of)

2013-10-05

Highlights: •Cu(OH){sub 2} is presented as the new supercapacitive material. •The novel room temperature method used for the synthesis of Cu(OH){sub 2}. •The hydrous, nanograined Cu(OH){sub 2} shows higher specific capacitance of 120 F/g. -- Abstract: Room temperature soft chemical synthesis route is used to grow nanograined copper hydroxide [Cu(OH){sub 2}] thin films on glass and stainless steel substrates. The structural, morphological, optical and wettability properties of Cu(OH){sub 2} thin films are studied by means of X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), field emission scanning electron microscopy (FESEM), UV–vis spectrophotometer and water contact angle measurement techniques. The results showed that, room temperature chemical synthesis route allows to form the nanograined and hydrophilic Cu(OH){sub 2} thin films with optical band gap energy of 3.0 eV. The electrochemical properties of Cu(OH){sub 2} thin films are studied in an aqueous 1 M NaOH electrolyte using cyclic voltammetry. The sample exhibited supercapacitive behavior with 120 F/g specific capacitance.

Synthesis and Characterization of Monometallic (Ag, Cu and Bimetallic Ag-Cu Particles for Antibacterial and Antifungal Applications

Directory of Open Access Journals (Sweden)

Marta Paszkiewicz

2016-01-01

Full Text Available In this paper, the experimental studies are concerned with the effect of the synthesis parameters on the formation of monometallic Ag and Cu nanoparticles (NPs. We consider the synthesis strategies verification for the bimetallic core-shell and alloy particles preparation. It was successfully obtained by chemical reduction method. The obtained colloidal solution is characterized by the transmission electron microscopy (TEM with energy-dispersive X-ray spectroscopy (EDX data, UV-Vis spectra, particle size distribution, and zeta potential. This work presents a comprehensive overview of experimental studies of the most stable colloidal solutions to impregnate fabrics that will exhibit a bactericidal and fungicidal activity against Candida albicans, Escherichia coli, and Staphylococcus aureus.

Polymer-assisted synthesis of water-soluble PbSe quantum dots

International Nuclear Information System (INIS)

Melnig, V.; Apostu, M.-O.; Foca, N.

2008-01-01

Stable PbSe quantum dots were synthesised in water-based media using poly(amidehydroxyurethane) water-soluble polymer. The polymer acts like a precursor carrier, blocks the particles aggregation and assures their solubility. Atomic force microscopy data show that the particle radius is smaller than the Bohr radius of PbSe. Interactions studies, performed by Fourier transform IR spectroscopy, show that the quantum dots are capped with poly(amidehydroxyurethane). The proposed synthesis was realised in the absence of any organic solvent. As a result, the produced particles have good water solubility, stability and good arguments to be biologically compatible.

High-Yield Synthesis of Zinc Oxide Nanoparticles from Bicontinuous Microemulsions

Directory of Open Access Journals (Sweden)

S. López-Cuenca

2011-01-01

Full Text Available The high-yield synthesis of zinc oxide (ZnO primary nanoparticles with high purity and with diameters between 6 and 22 nm using bicontinuous microemulsions is reported in this work. The ZnO nanoparticles were made by hydrolysis of Zn(NO32 with NaOH aqueous solution and precipitation, followed by calcination of the precipitate. Higher yields and productivities of ZnO nanoparticles were obtained compared to values produced with w/o micremulsions reported in the literature. Particles were characterized by transmission electronic microscopy (TEM, X-ray diffraction, and atomic absorption spectroscopy.

Synthesis of microsphere silicon carbide/nanoneedle manganese oxide composites and their electrochemical properties as supercapacitors

Science.gov (United States)

Kim, Myeongjin; Yoo, Youngjae; Kim, Jooheon

2014-11-01

Synthesis of microsphere silicon carbide/nanoneedle MnO2 (SiC/N-MnO2) composites for use as high-performance materials in supercapacitors is reported herein. The synthesis procedure involves the initial treatment of silicon carbide (SiC) with hydrogen peroxide to obtain oxygen-containing functional groups to provide anchoring sites for connection of SiC and the MnO2 nanoneedles (N-MnO2). MnO2 nanoneedles are subsequently formed on the SiC surface. The morphology and microstructure of the as-prepared composites are characterized via X-ray diffractometry, field-emission scanning electron microscopy, thermogravimetric analysis, and X-ray photoelectron spectroscopy. The characterizations indicate that MnO2 nanoneedles are homogeneously formed on the SiC surface in the composite. The capacitive properties of the as-prepared SiC/N-MnO2 electrodes are evaluated using cyclic voltammetry, galvanostatic charge/discharge testing, and electrochemical impedance spectroscopy in a three-electrode experimental setup using a 1-M Na2SO4 aqueous solution as the electrolyte. The SiC/N-MnO2(5) electrode, for which the MnO2/SiC feed ratio is 5:1, displays a specific capacitance as high as 273.2 F g-1 at 10 mV s-1.

Nanostructured Samarium Doped Fluorapatites and Their Catalytic Activity towards Synthesis of 1,2,4-Triazoles

Directory of Open Access Journals (Sweden)

Kranthi Kumar Gangu

2016-09-01

Full Text Available An investigation was conducted into the influence of the amino acids as organic modifiers in the facile synthesis of metal incorporated fluorapatites (FAp and their properties. The nanostructured Sm doped fluorapatites (Sm-FAp were prepared by a co-precipitation method using four different amino acids, namely glutamic acid, aspartic acid, glycine and histidine. The materials were characterized by various techniques including X-ray diffraction (XRD, Fourier transform infra-red spectroscopy (FT-IR, field emission scanning electron microscopy (FE-SEM, energy-dispersive X-ray spectroscopy (EDX, high resolution transmission electron microscopy (HR-TEM, N2-adsorption/desorption isotherm, temperature programmed desorption (TPD and fluorescence spectrophotometry. Under similar conditions, Sm-FAp prepared using different amino acids exhibited distinctly different morphological structures, surface area and pore properties. Their activity as catalysts was assessed and Sm-FAp/Glycine displayed excellent efficiency in the synthesis of 1,2,4-triazole catalyzing the reaction between 2-nitrobenzaldehyde and thiosemicarbazide with exceptional selectivity and 98% yield in a short time interval (10 min. The study provides an insight into the role of organic modifiers as controllers of nucleation, growth and aggregation which significantly influence the nature and activity of the catalytic sites on Sm-FAp. Sm-FAp could also have potential as photoactive material.

Tin-Assisted Synthesis of ɛ -Ga2O3 by Molecular Beam Epitaxy

Science.gov (United States)

Kracht, M.; Karg, A.; Schörmann, J.; Weinhold, M.; Zink, D.; Michel, F.; Rohnke, M.; Schowalter, M.; Gerken, B.; Rosenauer, A.; Klar, P. J.; Janek, J.; Eickhoff, M.

2017-11-01

The synthesis of ɛ -Ga2O3 and β -Ga2O3 by plasma-assisted molecular beam epitaxy on (001 )Al2O3 substrates is studied. The growth window of β -Ga2O3 in the Ga-rich regime, usually limited by the formation of volatile gallium suboxide, is expanded due to the presence of tin during the growth process, which stabilizes the formation of gallium oxides. X-ray diffraction, transmission electron microscopy, time-of-flight secondary-ion mass spectrometry, Raman spectroscopy, and atomic force microscopy are used to analyze the influence of tin on the layer formation. We demonstrate that it allows the synthesis of phase-pure ɛ -Ga2O3 . A growth model based on the oxidation of gallium suboxide by reduction of an intermediate sacrificial tin oxide is suggested.

Morphology Changes of Co Catalyst Nanoparticles at the Onset of Fischer-Tropsch Synthesis

DEFF Research Database (Denmark)

Høydalsvik, Kristin; Fløystad, Jostein B.; Voronov, Alexey

2014-01-01

Cobalt nanoparticles play an important role as catalysts for the Fischer-Tropsch synthesis, which is an attractive route for production of synthetic fuels. It is of particular interest to understand the varying conversion rate during the first hours after introducing synthesis gas (H-2 and CO......) to the system. To this end, several in situ characterization studies have previously been done on both idealized model systems and commercially relevant catalyst nanoparticles, using bulk techniques, such as X-ray powder diffraction and X-ray absorption spectroscopy. Since catalysis takes place at the surface...... of the cobalt particles, it is important to develop methods to gain surface-specific structural information under realistic processing conditions. We addressed this challenge using small-angle X-ray scattering (SAXS), a technique exploiting the penetrating nature of X-rays to provide information about particle...

Low-temperature synthesis and characterization of anatase TiO2 nanoparticles by an acid assisted sol–gel method

International Nuclear Information System (INIS)

Leyva-Porras, C.; Toxqui-Teran, A.; Vega-Becerra, O.; Miki-Yoshida, M.; Rojas-Villalobos, M.; García-Guaderrama, M.

2015-01-01

The synthesis of anatase TiO 2 nanoparticles by an acid-assisted sol–gel method at 25 and 80 °C is described. Specifically, acetic acid (AA) was used and the evolution of the anatase phase with the amount of AA was observed. The results of X-ray diffraction (XRD) and transmission electron microscopy (TEM) both showed that a pure anatase phase was obtained with particle size smaller than 5 nm. Structural refinements and quantitative determination of phase composition was achieved by using the Rietveld method. The particle size distribution became slightly narrower as the amount of AA was increased. Raman spectroscopy showed that when the amount of AA was increased a small amount of brookite was present at the contamination level. The anatase phase was studied by differential thermal analysis (DTA), providing phase stability up to 600 °C. These and other results were discussed in terms of particle size and structure. Likewise, the formation of the anatase phase under these synthesis conditions was explained. - Highlights: • Synthesis of anatase TiO 2 nanoparticles by an acid assisted sol–gel method at mild conditions. • Microstructure characterization by XRD, TEM and Raman spectroscopy. • Observation of the formation and evolution of the anatase phase as acetic acid was increased. • Anatase thermal stability up to 600 °C and band gap range between 3.2 and 3.5 eV. • A simplified method which can be considered as a green chemistry process

Preliminary Study of Fermented Tapioca for Synthesis of Carbon Nano tubes

International Nuclear Information System (INIS)

Nurulhuda Ismail; Ying, P.Y.

2011-01-01

Carbon nano tubes had been produced by various precursor such as gas (methane, carbon dioxide), oil (camphor oil, olive oil, and cooking oil) and alcohol. Different methods used for carbon nano tubes synthesis like arc discharge method, laser ablation method and chemical vapour deposition method. In this experiment, thermal chemical vapour deposition method was selected for carbon nano tubes synthesis. Starting material of fermented tapioca was used as carbon source for the process. Argon gas flow were controlled at around 10-15 bubbles per minute and deposition time around 20 to 30 minute. Others parameters such as temperature of furnace 1 and 2, amount of inoculum and catalyst have been studied. The asThermogravimetri (TGA) was used to determine the volatile temperature of the mixing catalyst and fermented tapioca extract. The grown carbon nano tubes morphology was characterized through Raman spectroscopy, scanning and Field Emission Scanning Electron Microscopy (FESEM) techniques. The surface morphology and uniformity of carbon nano tubes are reliant to parameters used. (author)

Reduced graphene oxide and inorganic nanoparticles composites – synthesis and characterization

Directory of Open Access Journals (Sweden)

Onyszko Magdalena

2015-12-01

Full Text Available Graphene – novel 2D material, which possesses variety of fascinating properties, can be considered as a convenient support material for the nanoparticles. In this work various methods of synthesis of reduced graphene oxide with metal or metal oxide nanoparticles will be presented. The hydrothermal approach for deposition of platinum, palladium and zirconium dioxide nanoparticles in ethylene glycol/water solution was applied. Here, platinum/reduced graphene oxide (Pt/RGO, palladium/reduced graphene oxide (Pd/RGO and zirconium dioxide/reduced graphene oxide (ZrO2/RGO nanocomposites were prepared. Additionally, manganese dioxide/reduced graphene oxide nanocomposite (MnO2/RGO was synthesized in an oleic-water interface. The obtained nanocomposites were investigated by transmission electron microscopy (TEM, X-ray diffraction analysis (XRD, Raman spectroscopy and thermogravimetric analysis (TGA. The results shows that GO can be successfully used as a template for direct synthesis of metal or metal oxide nanoparticles on its surface with a homogenous distribution.

Sacha inchi (Plukenetia volubilis L. shell biomass for synthesis of silver nanocatalyst

Directory of Open Access Journals (Sweden)

Brajesh Kumar

2017-01-01

Full Text Available This article describes a new approach for synthesis of silver nanostructured particles by using a Sacha inchi shell biomass (SISB. Sacha inchi shell biomass should be considered as an important source of phytochemicals for the synthesis and stabilization of silver nanoparticles (AgNPs. The characterization of AgNPs was performed by UV–vis spectroscopy, Transmission Electron Microscopy and Selected Area Electron Diffraction, indicating that AgNps were synthesized successfully with an average size of 7.2 nm. Infrared spectrum measurements were carried out to hypothesize the possible biomolecules responsible for stabilization and capping of the silver nanoparticles. Then, AgNps were used as a catalyst in the presence of sunlight for the removal of methyl orange dye (MO, anionic dye from aqueous solution. The results implied AgNps to be effective photocatalyst for the decomposition of MO (∼60%, pH 2.0 from aqueous solution.

New synthesis method for the growth of epitaxial graphene

Energy Technology Data Exchange (ETDEWEB)

Yu, X.Z. [Materials Sciences Division, Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States); Laboratory of Condensed Matter Spectroscopy and Opto-Electronic Physics, Department of Physics, Shanghai Jiao Tong University, 1954 Hua Shan Road, Shanghai 200030 (China); Hwang, C.G.; Jozwiak, C.M.; Koehl, A. [Materials Sciences Division, Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States); Schmid, A.K. [National Center for Electron Microscopy, Lawrence Berkeley National Laboratory, Berkeley, CA 94709 (United States); Lanzara, A., E-mail: ALanzara@lbl.gov [Materials Sciences Division, Lawrence Berkeley National Laboratory, Berkeley, CA 94720 (United States); Department of Physics, University of California, Berkeley, CA 94720 (United States)

2011-04-15

Highlights: {yields} We report a new straightforward method for the synthesis of micrometer scale graphene sheets. {yields} The process is based on a face to face mehtod in which two SiC substrates are placed one on top of the other and are heated simultaneously, leading to highly homogeneous samples. {yields} The number of graphene layers is determined by the annealing temperature. - Abstract: As a viable candidate for an all-carbon post-CMOS electronics revolution, epitaxial graphene has attracted significant attention. To realize its application potential, reliable methods for fabricating large-area single-crystalline graphene domains are required. A new way to synthesize high quality epitaxial graphene, namely 'face-to-face' method, has been reported in this paper. The structure and morphologies of the samples are characterized by low-energy electron diffraction, atomic force microscopy, angle-resolved photoemission spectroscopy and Raman spectroscopy. The grown samples show better quality and larger length scales than samples grown through conventional thermal desorption. Moreover, the graphene thickness can be easily controlled by changing annealing temperature.

Structure, reactivity and synthesis of piramidines and their derivates (dihidroperimidines and perimidinones); Estructura, reactividad y sintesis de perimidinas y de sus derivados (dihidroperimidinas y perimifinonas)

Energy Technology Data Exchange (ETDEWEB)

Claramunt, R.M.; Dotor, J.; Elguero, J. [Departamento de Quimica Organica, Facultad de Ciencias, UNED, Madrid (Spain)

1995-12-01

This review reports 346 references dealing with structure, reactivity and synthesis of pyrimidines and their derivatives (mainly 2,3-dihidroperimidines, 2-perimidinones and perimidinium salts). Special emphasis has been made on spectroscopy and structural properties as well as on reactivity. 346 refs.

Mulberry leaf extract mediated synthesis of gold nanoparticles and its anti-bacterial activity against human pathogens

International Nuclear Information System (INIS)

Adavallan, K; Krishnakumar, N

2014-01-01

Gold nanoparticles (Au-NPs) were synthesized at room temperature using Morus alba (mulberry) leaf extract as reducing and stabilizing agent. The development of plant mediated synthesis of nanoparticles is gaining importance due to its simplicity, low cost, non-toxicity, eco-friendliness, long term stability and reproducible aqueous synthesis method to obtain a self-assembly of nearly monodispersed Au-NPs. The formation and morphology of biosynthesized nanoparticles are investigated with the help of UV-Vis spectroscopy, dynamic light scattering (DLS), transmission electron microscopy (TEM), atomic force microscopy (AFM), x-ray diffraction (XRD), and Fourier transform infrared spectroscopy (FT-IR) techniques. Au-NPs formation was screened by UV-Vis spectroscopy through color conversion due to surface plasmon resonance band at 538 nm for Au-NPs. DLS studies revealed that the average size of Au-NPs was 50 nm. TEM studies showed the particles to be nearly spherical with few irregular shapes and particle size ranges 15−53 nm. The AFM image clearly shows the surface morphology of the well-dispersed Au-NPs with less than 50 nm. The high crystallinity of nanoparticles is evident from bright circular spots in the selected area electron diffraction (SAED) pattern. X-ray diffraction pattern showed high purity and face-centered cubic structure of Au-NPs. The FT-IR results indicate the presence of different functional groups present in the biomolecule capping the nanoparticles. Further, biosynthesized Au-NPs show strong zone of inhibition against Vibrio cholera (gram-negative) and Staphylococcus aureus (gram-positive) whereas, chemically synthesized Au-NPs and mulberry leaf extract exhibit a fair zone of inhibition. (papers)

Mulberry leaf extract mediated synthesis of gold nanoparticles and its anti-bacterial activity against human pathogens

Science.gov (United States)

Adavallan, K.; Krishnakumar, N.

2014-06-01

Gold nanoparticles (Au-NPs) were synthesized at room temperature using Morus alba (mulberry) leaf extract as reducing and stabilizing agent. The development of plant mediated synthesis of nanoparticles is gaining importance due to its simplicity, low cost, non-toxicity, eco-friendliness, long term stability and reproducible aqueous synthesis method to obtain a self-assembly of nearly monodispersed Au-NPs. The formation and morphology of biosynthesized nanoparticles are investigated with the help of UV-Vis spectroscopy, dynamic light scattering (DLS), transmission electron microscopy (TEM), atomic force microscopy (AFM), x-ray diffraction (XRD), and Fourier transform infrared spectroscopy (FT-IR) techniques. Au-NPs formation was screened by UV-Vis spectroscopy through color conversion due to surface plasmon resonance band at 538 nm for Au-NPs. DLS studies revealed that the average size of Au-NPs was 50 nm. TEM studies showed the particles to be nearly spherical with few irregular shapes and particle size ranges 15-53 nm. The AFM image clearly shows the surface morphology of the well-dispersed Au-NPs with less than 50 nm. The high crystallinity of nanoparticles is evident from bright circular spots in the selected area electron diffraction (SAED) pattern. X-ray diffraction pattern showed high purity and face-centered cubic structure of Au-NPs. The FT-IR results indicate the presence of different functional groups present in the biomolecule capping the nanoparticles. Further, biosynthesized Au-NPs show strong zone of inhibition against Vibrio cholera (gram-negative) and Staphylococcus aureus (gram-positive) whereas, chemically synthesized Au-NPs and mulberry leaf extract exhibit a fair zone of inhibition.

Investigation of Sm(3) and Eu(3) coordination compounds with pyrazolones by IR spectroscopy method

International Nuclear Information System (INIS)

Panyushkin, V.T.; Grishenko, T.V.; Afanas'ev, Yu.A.; Garnovskij, A.D.; Osipov, O.A.

1978-01-01

The synthesis is described of the coordination nitrate compounds of Sm(3) and Eu(3) with pyrazolones: 4-aminoantipyrine (A), 1-ethylpyridyl- 3-phenyl-pyrazolone-5(B); 1-(3'-ethylpyridyl)-3(phenylamine-n)-pyrazolone-5(C). It has been determined by the infrared spectroscopy method that exocyclic oxygen atom is the place of coordination bond localization in the pentioned compounds. The infrared spectra analysis of complexes in the 1700-1800 cm -1 region makes it possible to mention bidentate character of NO 3 -groups in the studied complex compounds

Al-doped MgB{sub 2} materials studied using electron paramagnetic resonance and Raman spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Bateni, Ali; Somer, Mehmet, E-mail: emre.erdem@physchem.uni-freiburg.de, E-mail: msomer@ku.edu.tr [Department of Chemistry, Koç University, Rumelifeneri Yolu, Sariyer, Istanbul (Turkey); Erdem, Emre, E-mail: emre.erdem@physchem.uni-freiburg.de, E-mail: msomer@ku.edu.tr; Repp, Sergej [Institut für Physikalische Chemie, Universität Freiburg, Albertstr. 21, Freiburg (Germany); Weber, Stefan [Institut für Physikalische Chemie, Universität Freiburg, Albertstr. 21, Freiburg (Germany); Freiburg Institute for Advanced Studies (FRIAS), Universität Freiburg, Albertstr. 19, Freiburg (Germany)

2016-05-16

Undoped and aluminum (Al) doped magnesium diboride (MgB{sub 2}) samples were synthesized using a high-temperature solid-state synthesis method. The microscopic defect structures of Al-doped MgB{sub 2} samples were systematically investigated using X-ray powder diffraction, Raman spectroscopy, and electron paramagnetic resonance. It was found that Mg-vacancies are responsible for defect-induced peculiarities in MgB{sub 2}. Above a certain level of Al doping, enhanced conductive properties of MgB{sub 2} disappear due to filling of vacancies or trapping of Al in Mg-related vacancy sites.

Facile synthesis of water-soluble curcumin nanocrystals

Directory of Open Access Journals (Sweden)

Marković Zoran M.

2015-01-01

Full Text Available In this paper, facile synthesis of water soluble curcumin nanocrystals is reported. Solvent exchange method was applied to synthesize curcumin nanocrystals. Different techniques were used to characterize the structural and photophysical properties of curcumin nanocrystals. We found that nanocurcumin prepared by this method had good chemical and physical stability, could be stored in the powder form at room temperature, and was freely dispersible in water. It was established that the size of curcumin nanocrystals was varied in the range of 20-500 nm. Fourier transform infrared spectroscopy and UV-Vis analyses showed the presence of tetrahydrofuran inside the curcumin nanocrystals. Also, it was found that nanocurcumin emitted photoluminescencewith yellow-green colour. [Projekat Ministarstva nauke Republike Srbije, br. 172003

Low temperature synthesis of InP nanocrystals

Energy Technology Data Exchange (ETDEWEB)

Ung Thi Dieu Thuy [Institute of Materials Science (IMS), Vietnamese Academy of Science and Technology (VAST), 18 Hoang Quoc Viet, Cau Giay, Hanoi (Viet Nam); Tran Thi Thuong Huyen [Institute of Materials Science (IMS), Vietnamese Academy of Science and Technology (VAST), 18 Hoang Quoc Viet, Cau Giay, Hanoi (Viet Nam); National University of Thai Nguyen, 2 Luong Ngoc Quyen, Thai Nguyen (Viet Nam); Nguyen Quang Liem [Institute of Materials Science (IMS), Vietnamese Academy of Science and Technology (VAST), 18 Hoang Quoc Viet, Cau Giay, Hanoi (Viet Nam)], E-mail: liemnq@ims.vast.ac.vn; Reiss, Peter [DSM/INAC/SPrAM, UMR 5819 CEA-CNRS-Universite Joseph Fourier/LEMOH, CEA Grenoble, 17 rue des Martyrs, 38054 Grenoble Cedex 9 (France)

2008-12-20

We present a simple method for the chemical synthesis of InP nanocrystals, which comprises several advantages: (i) the use of simple reagents, namely InCl{sub 3}.4H{sub 2}O and yellow P as the In and P precursors, respectively, and NaBH{sub 4} as the reducing agent in a mixed solvent of ethanol and toluene; (ii) a short reaction time (1-5 h) and low temperature (<75 deg. C); (iii) a high reaction yield approaching 100%. InP NCs in the zinc-blende structure have been obtained as confirmed by powder X-ray diffraction and Raman scattering measurements. Their mean size of 4 nm has been determined by transmission electron microscopy, Raman scattering and absorption spectroscopy.

Green synthesis of silver nanoparticle using Bambusa arundinacea leaves

Science.gov (United States)

Kataria, Bharat; Shyam, Vasvani; Kaushik, Babiya; Vasoya, Jaydeep; Joseph, Joyce; Savaliya, Chirag; Kumar, Sumit; Parikh, Sachin P.; Thakar, C. M.; Pandya, D. D.; Ravalia, A. B.; Markna, J. H.; Shah, N. A.

2017-05-01

The synthesis of nanoparticles using ecofriendly way is an interesting area in advance nanotechnology. Silver (Ag) nanoparticles are usually synthesized by chemicals route, which are quite flammable and toxic in nature. This study deals with a biosynthesis process (environment friendly) of silver nanoparticles using Bambusa arundinacea leaves for its antibacterial activity. The formation and characterization of AgNPs was confirmed by UV-Vis spectroscopy. Silver nanoparticles were successfully synthesized from AgNO3 through a simple green route using the latex of Bambusa arundinacea leaves as reducing as well as capping agent. Scanning Electron Microscopy (SEM) study indicates the formation of grains (particles) with different size and shape.

Improved synthesis of glycine, taurine and sulfate conjugated bile acids as reference compounds and internal standards for ESI-MS/MS urinary profiling of inborn errors of bile acid synthesis.

Science.gov (United States)

Donazzolo, Elena; Gucciardi, Antonina; Mazzier, Daniela; Peggion, Cristina; Pirillo, Paola; Naturale, Mauro; Moretto, Alessandro; Giordano, Giuseppe

2017-04-01

Bile acid synthesis defects are rare genetic disorders characterized by a failure to produce normal bile acids (BAs), and by an accumulation of unusual and intermediary cholanoids. Measurements of cholanoids in urine samples by mass spectrometry are a gold standard for the diagnosis of these diseases. In this work improved methods for the chemical synthesis of 30 BAs conjugated with glycine, taurine and sulfate were developed. Diethyl phosphorocyanidate (DEPC) and diphenyl phosphoryl azide (DPPA) were used as coupling reagents for glycine and taurine conjugation. Sulfated BAs were obtained by sulfur trioxide-triethylamine complex (SO 3 -TEA) as sulfating agent and thereafter conjugated with glycine and taurine. All products were characterized by NMR, IR spectroscopy and high resolution mass spectrometry (HRMS). The use of these compounds as internal standards allows an improved accuracy of both identification and quantification of urinary bile acids. Copyright © 2017 Elsevier B.V. All rights reserved.

Basic molecular spectroscopy

CERN Document Server

Gorry, PA

1985-01-01

BASIC Molecular Spectroscopy discusses the utilization of the Beginner's All-purpose Symbolic Instruction Code (BASIC) programming language in molecular spectroscopy. The book is comprised of five chapters that provide an introduction to molecular spectroscopy through programs written in BASIC. The coverage of the text includes rotational spectra, vibrational spectra, and Raman and electronic spectra. The book will be of great use to students who are currently taking a course in molecular spectroscopy.

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.

Changing vacancy balance in ZnO by tuning synthesis between zinc/oxygen lean conditions

Science.gov (United States)

Venkatachalapathy, Vishnukanthan; Galeckas, Augustinas; Zubiaga, Asier; Tuomisto, Filip; Kuznetsov, Andrej Yu.

2010-08-01

The nature of intrinsic defects in ZnO films grown by metal organic vapor phase epitaxy was studied by positron annihilation and photoluminescence spectroscopy techniques. The supply of Zn and O during the film synthesis was varied by applying different growth temperatures (325-485 °C), affecting decomposition of the metal organic precursors. The microscopic identification of vacancy complexes was derived from a systematic variation in the defect balance in accordance with Zn/O supply trends.

The Green Synthesis and Evaluation of Silver Nanoparticles and Zinc Oxide Nanoparticles

Science.gov (United States)

Gebear-Eigzabher, Bellsabel

Nanoparticle (NP) research has received exceptional attention as the field of study that contributes to transforming the world of materials science. When implementing NPs in consumer and industrial products, their unique properties improve technologies to the extent of significant game-changing breakthroughs. Conversely, the increased production of NPs, their use, their disposal or inadvertent release in the environment drove the need for processes and policies that ensures consumer and environmental safety. Mitigation of any harmful effects that NPs could potentially have combines methods of safe preparation, safe handling and safe disposal as well as containment of any inadvertent release. Our focus is in safe preparation of nanomaterials and we report green and energy efficient synthesis methods for metal NPs and metal oxide NPs of two popular materials: silver (Ag) and zinc oxide (ZnO). The thesis explained: 1) The impact of NPs in nowadays' world; 2) Synthesis methods that were designed to include environmentally-friendly staring materials and energy-saving fabrication processes, with emphasis on maintaining NPs final size and morphology when compared with existing methods; and 3) Nanoparticles characterization and data collection which allowed us to determine and/or validate their properties. Nanoparticles were studied using transmission electron microscope (TEM), X-Ray powder diffraction (XRD), low-voltage (5 keV) transmission electron microscopy (LV EM 5), Fourier-Transform Infrared Spectroscopy (FT-IR), and Ultraviolet-Visible (UV-Vis) spectroscopy. We developed an aqueous-based preparation of zinc oxide nanoparticles (ZnO NPs) using microwave-assisted chemistry to render a well-controlled particle size distribution within each set of reaction conditions in the range of 15 nm to 75 nm. We developed a scalable silver nanoparticles synthesis by chemical reduction methods. The NPs could be used in consumer products. The measurement tools for consumer products

Synthesis and physicochemical properties of 7,8-dicarba-nido-undecarborane(11) adducts with pyridine bases

International Nuclear Information System (INIS)

Volkov, O.V.; Il'inchik, E.A.; Volkov, V.V.; Voronina, G.S.; Yur'eva, O.P.; Polyanskaya, T.M.

1993-01-01

Synthesis of some 7,8-C 2 B 9 H 11 adducts in conducted via 7.8-C 2 B 9 H 12 ion interaction with iron (3) chloride at presence of pyridine derivatives and their study is carried out using IR, NMR 12 B, PMR, X-ray phase, UV spectroscopy techniques. Character of bond between heterocycle and carborane holyhedron is discussed. Luminescent properties of the prepared compounds under UV radiation are detected

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.

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

Synthesis and applications of {sup 13}C glycerol

Energy Technology Data Exchange (ETDEWEB)

Stocking, E.; Khalsa, O.; Martinez, R.A.; Silks, L.A. III [Los Alamos National Laboratory, NM (United States)

1994-12-01

Due in part to the use of labeled glycerol for the {sup 13}C enrichment of biomolecules, we are currently developing new synthetic routes to various isotopomers of glycerol. Judging from our experience, traditional methods of glycerol synthesis are not easily adapted for isotopic enrichment and/or have poor overall yields (12 to 15%). Furthermore, the use of glycerol for enrichment can be prohibitively expensive and its availability is limited by the level of demand. We are presently developing a short de novo synthesis of glycerol from carbon dioxide ({approximately}53% overall yield for four steps) and are examining the feasibility of synthesizing site-specific {sup 13}C-labeled glycerol and dihydroxyacetone (DHA) from labeled methanol and carbon dioxide. One application of {sup 13}C glycerol we have examined is enzymatic conversion of glycerol to glyceraldehyde-3-monophosphate or dihydroxyacetone monophosphate (DHAP) with yields ranging from 25 to 50% (as determined by NMR spectroscopy). We are also pursuing the chemical conversion of {sup 13}C-labeled DHA to DHAP. We are especially interested in {sup 13}C-labeled DHAP because we are investigating its use as a chemo-enzymatic precursor for both labeled 2-deoxyribose and 2-deoxyribonucleic acids.

Study of strontium- and magnesium-doped lanthanum gallate solid electrolyte surface by X-ray photoelectron spectroscopy

International Nuclear Information System (INIS)

Datta, Pradyot; Majewski, Peter; Aldinger, Fritz

2008-01-01

The chemical states of the surface of the oxygen ion conducting solid electrolyte La 0.9 Sr 0.1 Ga 0.85 Mg 0.15 O 3-δ (LSGM 1015) as prepared by solid-state synthesis was analyzed by X-ray photoelectron spectroscopy. It was found that adventitious carbon did not interact with any of the constituent elements of LSGM 1015. Ga and La were found to exist in trivalent states. But, due to ionic bombardment presence of Mg could not be detected in the electrolyte surface

Curcumin coated gold nanoparticles: synthesis, characterization, cytotoxicity, antioxidant activity and its comparison with citrate coated gold nanoparticles

Directory of Open Access Journals (Sweden)

Elnaz Shaabani

2017-04-01

Full Text Available Objective(s: Biological applications of gold nanoparticles have limitations because of the toxic chemicals used in their synthesis. Curcumin can be used as reducing as well as capping agent in synthesis of GNPs to eliminate the cytotoxicity. Conjugation of curcumin to gold also helps in increasing its solubility and bioavailability. Materials and Methods: Here we report synthesis of gold nanoparticles coated with citrate and curcumin and of two different sizes via chemical routes. UV-Vis absorbance spectroscopy, Dynamic Light Scattering and Transmission Electron Microscopy were applied to study the average particle size, size stability of the samples and zeta potential. Fourier transform infrared, Raman Spectroscopy and Fluorescence Spectroscopy were applied for detection of curcumin on the surface of GNPs. The antioxidant activity was evaluated using DPPH assay and Cytotoxicity was evaluated by MTT assay.Results: Particles were synthesized of 6 and 16 nm size. The average particle size was found to be 21.7 ± 5.7 by TEM. The zeta potential on the surface of Cur-GNPs was negative and larger than 25 mV which is a sign of their high stability. The stability of these particles (with different coatings but with similar sizes at different time intervals (up to 3 months and also in different media like cell culture medium, different buffers, glucose and at different pH conditions have been investigated thoroughly. Appearance of functional groups assigned to curcumin in FTIR and SERS spectra are sign of presence of curcumin in the sample. The quenching of the fluorescence in the presence of GNPs reveals the clear indication of the capping and binding of curcumin with GNPs. Cur-GNP1 (16 nm were found to exhibit highest antioxidant activity than other gold nanoparticles. Cytotoxicity evaluation using MTT assay on L929 cell line proved curcumin coated gold nanoparticles were non-toxic up to 40 ppm.Conclusion: The results revealed that larger curcumin

Good use of fruit wastes: eco-friendly synthesis of silver nanoparticles, characterization, BSA protein binding studies.

Science.gov (United States)

Sreekanth, T V M; Ravikumar, Sambandam; Lee, Yong Rok

2016-06-01

A simple and eco-friendly methodology for the green synthesis of silver nanoparticles (AgNPs) using a mango seed extract was evaluated. The AgNPs were characterized by ultraviolet-visible spectrophotometry, Fourier transform infrared spectroscopy, transmission electron microscopy, energy dispersive X-ray spectroscopy, and X-ray diffraction. The interaction between the green synthesized AgNPs and bovine serum albumin (BSA) in an aqueous solution at physiological pH was examined by fluorescence spectroscopy. The results confirmed that the AgNPs quenched the fluorophore of BSA by forming a ground state complex in aqueous solution. This fluorescence quenching data were also used to determine the binding sites and binding constants at different temperatures. The calculated thermodynamic parameters (ΔG°, ΔH° and ΔS°) suggest that the binding process occurs spontaneously through the involvement of electrostatic interactions. The synchronous fluorescence spectra showed a blue shift, indicating increasing hydrophobicity. Copyright © 2015 John Wiley & Sons, Ltd. Copyright © 2015 John Wiley & Sons, Ltd.

Instant synthesis of gold nanoparticles at room temperature and SERS applications

International Nuclear Information System (INIS)

Britto Hurtado, R.; Cortez-Valadez, M.; Ramírez-Rodríguez, L.P.; Larios-Rodriguez, Eduardo; Alvarez, Ramón A.B.; Rocha-Rocha, O.; Delgado-Beleño, Y.; Martinez-Nuñez, C.E.; Arizpe-Chávez, H.; Hernández-Martínez, A.R.; Flores-Acosta, M.

2016-01-01

Nowadays, gold nanoparticles (AuNps) can be used in a variety of applications, thus efficient methods to produce them are necessary. Several methods have been proposed in this area, but NPs production time is one limitation of these approaches. In this study, we propose a high competitive method to synthesize gold colloidal nanoparticles, instantaneously, using no-toxic reducing agents. These substances allow the instantaneous synthesis at room temperature, even without magnetic stirrers, ovens or ultrasonic baths. Optic analysis showed two absorption bands, associated with surface Plasmon as function of HAuCl_4 concentration. The nanoparticles synthesized have a 10–20 nm size, seen by the transmission electron microscopy (TEM). Therefore, it was possible to obtain several geometric patterns of AuNps, and the synthesis was performed reducing significantly processing time. Additionally, Mie and Fuchs theories were used to predict the location of the absorption bands linked to the plasmon surface in gold nanoparticles. The Surface Enhanced Raman Spectroscopy (SERS) effect was analyzed considering natural zeolite (Chabazite) as analyte, in order to determinate its possible application in soil analysis. - Highlights: • Cubic and spherical morphologies in AuNp. • Surface plasmon prediction in cubic and spherical AuNp. • Instant synthesis of AuNp. • SERS applications in soil analysis.

Instant synthesis of gold nanoparticles at room temperature and SERS applications

Energy Technology Data Exchange (ETDEWEB)

Britto Hurtado, R. [Departamento de Investigación en Física, Universidad de Sonora, Apdo. Postal 5-88, 83190, Hermosillo, Sonora (Mexico); Cortez-Valadez, M., E-mail: jose.cortez@unison.mx [CONACYT-Departamento de Investigación en Física, Universidad de Sonora, Apdo. Postal 5-88, 83190, Hermosillo, Sonora (Mexico); Ramírez-Rodríguez, L.P. [Departamento de Física, Universidad de Sonora, Apdo. Postal 5-88, 83190, Hermosillo, Sonora (Mexico); Larios-Rodriguez, Eduardo [Departamento de Ingeniería Química y Metalurgia, Universidad de Sonora, Rosales y Luis Encinas S/N, Hermosillo, Sonora (Mexico); Alvarez, Ramón A.B.; Rocha-Rocha, O.; Delgado-Beleño, Y.; Martinez-Nuñez, C.E.; Arizpe-Chávez, H. [Departamento de Investigación en Física, Universidad de Sonora, Apdo. Postal 5-88, 83190, Hermosillo, Sonora (Mexico); Hernández-Martínez, A.R. [Centro de Física Aplicada y Tecnología Avanzada (CFATA), Universidad Nacional Autónoma de México, Campus Juriquilla, Querétaro C.P. 76130 (Mexico); Flores-Acosta, M. [Departamento de Investigación en Física, Universidad de Sonora, Apdo. Postal 5-88, 83190, Hermosillo, Sonora (Mexico)

2016-08-06

Nowadays, gold nanoparticles (AuNps) can be used in a variety of applications, thus efficient methods to produce them are necessary. Several methods have been proposed in this area, but NPs production time is one limitation of these approaches. In this study, we propose a high competitive method to synthesize gold colloidal nanoparticles, instantaneously, using no-toxic reducing agents. These substances allow the instantaneous synthesis at room temperature, even without magnetic stirrers, ovens or ultrasonic baths. Optic analysis showed two absorption bands, associated with surface Plasmon as function of HAuCl{sub 4} concentration. The nanoparticles synthesized have a 10–20 nm size, seen by the transmission electron microscopy (TEM). Therefore, it was possible to obtain several geometric patterns of AuNps, and the synthesis was performed reducing significantly processing time. Additionally, Mie and Fuchs theories were used to predict the location of the absorption bands linked to the plasmon surface in gold nanoparticles. The Surface Enhanced Raman Spectroscopy (SERS) effect was analyzed considering natural zeolite (Chabazite) as analyte, in order to determinate its possible application in soil analysis. - Highlights: • Cubic and spherical morphologies in AuNp. • Surface plasmon prediction in cubic and spherical AuNp. • Instant synthesis of AuNp. • SERS applications in soil analysis.

Synthesis, characterization and magnetic properties of highly monodispersed PtNi nanoparticles

International Nuclear Information System (INIS)

Du, Juan-Juan; Yang, Yi; Zhang, Rong-Hua; Zhou, Xin-Wen

2015-01-01

In this paper, we report the controlled-synthesis of PtNi nanoparticles through galvanic displacement reaction and chemical reduction. The size, composition and morphology of the products are characterized by transmission electron microscopy (TEM), powder X-ray diffraction (XRD), energy dispersed X-ray spectroscopy (EDS) and X-ray photoelectron spectroscopy (XPS) analyses. The structure and composition of the PtNi nanoparticles can be controlled by adjusting the synthetic conditions. The possible formation mechanism is obtained from the academic analysis and experimental studies. The results of the magnetic measurement illustrate that the PtNi nanoparticles show a superparamagnetic behavior with a blocking temperature (T B ) about 8.0 K. - Highlights: • Highly monodispersed PtNi nanoparticles were synthesized by galvanic displacement reaction. • The formation of Pt nanocrystals was the foremost step because of its self-catalysis effect. • The PtNi nanoparticles show a superparamagnetic behavior with a T B about 8.0 K

Synthesis, Characterization, and Self-Assembly of a Tetrathiafulvalene (TTF–Triglycyl Derivative

Directory of Open Access Journals (Sweden)

Sónia Pérez-Rentero

2018-04-01

Full Text Available In this work, we describe the synthesis, characterization, and self-assembly properties of a new tetrathiafulvalene (TTF–triglycyl low-molecular-weight (LMW gelator. Supramolecular organogels were obtained in various solvents via a heating–cooling cycle. Critical gelation concentrations (CGC (range ≈ 5–50 g/L and thermal gel-to-sol transition temperatures (Tgel (range ≈ 36–51 °C were determined for each gel. Fourier transform infrared (FT-IR spectroscopy suggested that the gelator is also aggregated in its solid state via a similar hydrogen-bonding pattern. The fibrillar microstructure and viscoelastic properties of selected gels were demonstrated by means of field-emission electron microscopy (FE-SEM and rheological measurements. As expected, exposure of a model xerogel to I2 vapor caused the oxidation of the TTF unit as confirmed by UV-vis-NIR analysis. However, FT-IR spectroscopy showed that the oxidation was accompanied with concurrent alteration of the hydrogen-bonded network.

Synthesis and characterization of iron nano particles for the arsenic removal in water; Sintesis y caracterizacion de nanoparticulas de hierro para la remocion de arsenico en agua

Energy Technology Data Exchange (ETDEWEB)

Gutierrez M, O. E.

2011-07-01

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)

Hydrogel-Embedded Model Photocatalytic System Investigated by Raman and IR Spectroscopy Assisted by Density Functional Theory Calculations and Two-Dimensional Correlation Analysis.

Science.gov (United States)

Geitner, Robert; Götz, Stefan; Stach, Robert; Siegmann, Michael; Krebs, Patrick; Zechel, Stefan; Schreyer, Kristin; Winter, Andreas; Hager, Martin D; Schubert, Ulrich S; Gräfe, Stefanie; Dietzek, Benjamin; Mizaikoff, Boris; Schmitt, Michael; Popp, Jürgen

2018-03-15

The presented study reports the synthesis and the vibrational spectroscopic characterization of different matrix-embedded model photocatalysts. The goal of the study is to investigate the interaction of a polymer matrix with photosensitizing dyes and metal complexes for potential future photocatalytic applications. The synthesis focuses on a new rhodamine B derivate and a Pt(II) terpyridine complex, which both contain a polymerizable methacrylate moiety and an acid labile acylhydrazone group. The methacrylate moieties are afterward utilized to synthesize functional model hydrogels mainly consisting of poly(ethylene glycol) methacrylate units. The pH-dependent and temperature-dependent behavior of the hydrogels is investigated by means of Raman and IR spectroscopy assisted by density functional theory calculations and two-dimensional correlation spectroscopy. The spectroscopic results reveal that the Pt(II) terpyridine complex can be released from the polymer matrix by cleaving the C═N bond in an acid environment. The same behavior could not be observed in the case of the rhodamine B dye although it features a comparable C═N bond. The temperature-dependent study shows that the water evaporation has a significant influence neither on the molecular structure of the hydrogel nor on the model photocatalytic moieties.

Green coconut ( Cocos nucifera Linn) shell extract mediated size controlled green synthesis of polyshaped gold nanoparticles and its application in catalysis

Science.gov (United States)

Paul, Koushik; Bag, Braja Gopal; Samanta, Kousik

2014-08-01

The shell extract of green coconut ( Cocos nucifera Linn) has been utilized for the synthesis of gold nanoparticles at room temperature under very mild condition without any extra stabilizing or capping agents. The size of the synthesized gold nanoparticles could be controlled by varying the concentration of the shell extract. The stabilized gold nanoparticles were analyzed by surface plasmon resonance spectroscopy, HRTEM, Energy dispersive X-ray spectroscopy and X-ray diffraction studies. The catalytic activity of the freshly synthesized gold nanoparticles was studied for the sodium borohydride reduction of 4-nitrophenol and the kinetics of the reduction reaction were studied spectrophotometrically.

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