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Sample records for butylamine

  1. Development of solvent washing process using butylamine compounds

    International Nuclear Information System (INIS)

    A new solvent washing process using normal butylamine compounds as salt-free washing reagents has been developed. The washing behaviors of plutonium, zirconium, ruthenium and di-n-butylphosphoric acid (HDBP) are examined in the new solvent-washing process with n-butylamine oxalate and n-butylamine bicarbonate. In low pH condition, the oxalate washed plutonium and zirconium effectively in solvent by making oxalate complexes. In high pH condition, the oxalate an bicarbonate washed plutonium, zirconium, and ruthenium by replacing a nitrate ion with a hydroxide ion and HDBP by dissociation with the hydroxide ion. The destruction of butylamine has been studied using a silver catalyzed electrochemical oxidation technique. The destruction rate of n-butylamine was measured as functions of the concentrations of butylamine, silver and nitric acid in aqueous solutions, anode potential and temperature. More than 99% of n-butylamine in nitric acid was destructed within 240 min by electrochemical oxidation at 1.6 V versus a reference saturated calomel electrode (SCE). (J.P.N.)

  2. N-butylamine functionalized graphene oxide for detection of iron(III) by photoluminescence quenching.

    Science.gov (United States)

    Gholami, Javad; Manteghian, Mehrdad; Badiei, Alireza; Ueda, Hiroshi; Javanbakht, Mehran

    2016-02-01

    An N-butylamine functionalized graphene oxide nanolayer was synthesized and characterized by ultraviolet (UV)-visible spectrometry, Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, and transmission electron microscopy. Detection of iron(III) based on photoluminescence spectroscopy was investigated. The N-butylamine functionalized graphene oxide was shown to specifically interact with iron (III), compared with other cationic trace elements including potassium (I), sodium (I), calcium (II), chromium (III), zinc (II), cobalt (II), copper (II), magnesium (II), manganese (II), and molybdenum (VI). The quenching effect of iron (III) on the luminescence emission of N-butylamine functionalized graphene oxide layer was used to detect iron (III). The limit of detection (2.8 × 10(-6)  M) and limit of quantitation (2.9 × 10(-5)  M) were obtained under optimal conditions. PMID:26016610

  3. Washing properties of n-butylamine oxalate in degraded solvent (Joint study between JNC and JAERI)

    International Nuclear Information System (INIS)

    Washing properties of n-butylamine compounds, which are decomposable by burning or electrolysis, for dibutylphosphoric acid (DBP) and Zr in real and simulated degraded solvents have been investigated. In experiments with simulated degraded solvents, basic properties of n-butylamine compounds for washing DBP and Zr were examined and optimum condition was obtained. It was confirmed from the simulated degraded solvent washing tests that 0.25 mol/dm3 n-butylamine oxalate of pH 2 could effectively remove Zr from the degraded solvent and the solution of pH 4 was effective for DBP, 95% removal of Zr and DBP were obtained by batch washing. The validity of n-butylamine as a degraded solvent wash reagent was shown by the washing test for real degraded solvent that was performed by continuous counter current flow using a miniature mixer-settler. The present study was carried out as a part of the joint study 'Research and Development of Process Elements in an Advanced Aqueous Reprocessing' between Japan Nuclear Cycle Development Institute and JAERI. (author)

  4. Highly enhanced vapor sensing of multiwalled carbon nanotube network sensors by n-butylamine functionalization

    OpenAIRE

    P. Slobodian; Riha, P.; Cavallo, P.; Barbero, C. A.; R. Benlikaya; Cvelbar, U.; Petras, D.; Saha, P.

    2014-01-01

    The sensing of volatile organic compounds by multiwall carbon nanotube networks of randomly entangled pristine nanotubes or the nanotubes functionalized by n-butylamine, which were deposited on polyurethane supporting electrospinned nonwoven membrane, has been investigated. The results show that the sensing of volatile organic compounds by functionalized nanotubes considerably increases with respect to pristine nanotubes. The increase is highly dependent on used vapor polarity. For the cas...

  5. Highly Enhanced Vapor Sensing of Multiwalled Carbon Nanotube Network Sensors by n-Butylamine Functionalization

    Directory of Open Access Journals (Sweden)

    P. Slobodian

    2014-01-01

    Full Text Available The sensing of volatile organic compounds by multiwall carbon nanotube networks of randomly entangled pristine nanotubes or the nanotubes functionalized by n-butylamine, which were deposited on polyurethane supporting electrospinned nonwoven membrane, has been investigated. The results show that the sensing of volatile organic compounds by functionalized nanotubes considerably increases with respect to pristine nanotubes. The increase is highly dependent on used vapor polarity. For the case of highly polar methanol, the functionalized MWCNT network exhibits even more than eightfold higher sensitivity in comparison to the network prepared from pristine nanotubes.

  6. Determination of Total Acid in Palygorskite Chemically Modified by N-Butylamine Thermodesorption

    Directory of Open Access Journals (Sweden)

    Ruiz Juan A.C.

    2002-01-01

    Full Text Available The acid properties of palygorskite clay (R1 were studied using n-butylamine as probe molecule. A comparison was made of these properties in palygorskite clay (R1, in an acidified palygorskite (R2 and in acid palygorskite loaded with 2% of lanthanum (R3. The total acid properties were determined by FTIR (Fourier Transform Infrared and TG-DTA (thermogravimetry. The acidity increased as follows: R3>R2>R1. The acid strength sites were classified as physisorbed, weak, medium and strong. The acid treatment did not change the site distribution, apparently only removing channel impurities. The introduction of lanthanum created many more acid sites and increased the specific area. Both weak and strong sites, which increased significantly, were considered new active acid sites produced by the lanthanum.

  7. Experimental determination of the isothermal (vapour + liquid) equilibria of binary aqueous solutions of sec-butylamine and cyclohexylamine at several temperatures

    International Nuclear Information System (INIS)

    Highlights: → Vapour pressures of sec-butylamine or cyclohexylamine and their aqueous solutions. → The investigated temperatures are 273 K and 363 K. → The (cyclohexylamine + water) mixture shows positive azeotropic behaviour. → The (sec-butylamine + water) or (cyclohexylamine + water) exhibit positive GE. - Abstract: The vapour pressures of (sec-butylamine + water), (cyclohexylamine + water) binary mixtures, and of pure sec-butylamine and cyclohexylamine components were measured by means of two static devices at temperatures between 293 (or 273) K and 363 K. The data were correlated with the Antoine equation. From these data, excess Gibbs functions (GE) were calculated for several constant temperatures and fitted to a fourth-order Redlich-Kister equation using the Barker's method. The (cyclohexylamine + water) system shows positive azeotropic behaviour for all investigated temperatures. The two binary mixtures exhibit positive deviations in GE for all investigated temperatures over the whole composition range.

  8. Experimental determination of the isothermal (vapour + liquid) equilibria of binary aqueous solutions of sec-butylamine and cyclohexylamine at several temperatures

    Energy Technology Data Exchange (ETDEWEB)

    Chiali-Baba Ahmed, Nouria [LATA2M, Laboratoire de Thermodynamique Appliquee et Modelisation Moleculaire, University AbouBekr Belkaid of Tlemcen, Post Office Box 119, Tlemcen 13000 (Algeria); Negadi, Latifa, E-mail: latifanegadi@yahoo.fr [LATA2M, Laboratoire de Thermodynamique Appliquee et Modelisation Moleculaire, University AbouBekr Belkaid of Tlemcen, Post Office Box 119, Tlemcen 13000 (Algeria); Mokbel, Ilham [LSA, Laboratoire des Sciences Analytiques, CNRS-UMR 5280, Universite Claude Bernard - Lyon I, 43, Bd du 11 Novembre 1918, Villeurbanne Cedex 69622 (France); Kaci, Ahmed Ait [Laboratoire de Thermodynamique et Modelisation Moleculaire, Universite des Sciences et de la Technologie Houari Boumediene, Post Office Box 32, El Alia 16111, Bab Ezzouar (Algeria); Jose, Jacques [LSA, Laboratoire des Sciences Analytiques, CNRS-UMR 5280, Universite Claude Bernard - Lyon I, 43, Bd du 11 Novembre 1918, Villeurbanne Cedex 69622 (France)

    2012-01-15

    Highlights: > Vapour pressures of sec-butylamine or cyclohexylamine and their aqueous solutions. > The investigated temperatures are 273 K and 363 K. > The (cyclohexylamine + water) mixture shows positive azeotropic behaviour. > The (sec-butylamine + water) or (cyclohexylamine + water) exhibit positive G{sup E}. - Abstract: The vapour pressures of (sec-butylamine + water), (cyclohexylamine + water) binary mixtures, and of pure sec-butylamine and cyclohexylamine components were measured by means of two static devices at temperatures between 293 (or 273) K and 363 K. The data were correlated with the Antoine equation. From these data, excess Gibbs functions (G{sup E}) were calculated for several constant temperatures and fitted to a fourth-order Redlich-Kister equation using the Barker's method. The (cyclohexylamine + water) system shows positive azeotropic behaviour for all investigated temperatures. The two binary mixtures exhibit positive deviations in G{sup E} for all investigated temperatures over the whole composition range.

  9. cis-Bis(butylamine-κNbis[sulfadiazine(1−-κ2N,N′]copper(II pentahydrate

    Directory of Open Access Journals (Sweden)

    Orhan Büyükgüngör

    2008-09-01

    Full Text Available In the title compound {systematic name: cis-bis[4-amino-N-(pyrimidin-2-ylbenzenesulfonamidato-κ2N,N′]bis(butylamine-κNcopper(II pentahydrate}, [Cu(C10H9N4O2S2(C4H11N2]·5H2O or [Cu(sdz2(ba2]·5H2O [ba is butylamine and sdz = sulfadiazine(1−], the copper(II cation is six-coordinated by four N atoms of two sulfadiazine ligands and two N atoms of butylamine ligands. The copper(II ion and one of the water molecules lie on twofold rotation axes. One of the butyl groups is disordered over two sites, with occupancies of 0.395 (8 and 0.605 (8. The geometry around the S atom is distorted tetrahedral. The crystal structure involves intermolecular N—H...N and N—H...O hydrogen bonds. N—H...N hydrogen bonds between sdz ligands lead to a sheet structure parallel to the ab plane.

  10. Recovery of Pyruvic Acid using Tri-n-butylamine Dissolved in Non-Toxic Diluent (Rice Bran Oil)

    Science.gov (United States)

    Pal, Dharm; Keshav, Amit

    2016-04-01

    An attempt has been made to investigate the effectiveness of the vegetable oil based biocompatible solvent for the separation of pyruvic acid from fermentation broth, by using rice bran oil as natural, non-toxic diluent. Reactive extraction of pyruvic acid (0.1-0.5 k mol/m3) from aqueous solutions has been studied using tri-n-butylamine (TBA; 10-70 %) as an extractant dissolved in non toxic rice bran oil at T = 30 ± 1 °C. Results were presented in terms of distribution coefficient (Kd), extraction efficiency (E %), loading ratio (Z), and complexation constant (\\varphi_{α β }). Extraction equilibrium was interpreted using mass action modeling approach. Based on the extent of loading (Z < 0.5) only (1:1), pyruvic acid: TBA complex was proposed. Equilibrium complexation constant was evaluated to 1.22 m3/k mol. Results obtained are useful in understanding the extraction mechanism.

  11. Solution-Processed Inorganic Thin Film Transistors Fabricated from Butylamine-Capped Indium-Doped Zinc Oxide Nanocrystals

    Energy Technology Data Exchange (ETDEWEB)

    Pham, Hien Thu; Jeong, Hyundam [Chonnam National Univ., Gwangju (Korea, Republic of)

    2014-02-15

    Indium-doped zinc oxide nanocrystals (IZO NCs), capped with stearic acid (SA) of different sizes, were synthesized using a hot injection method in a noncoordinating solvent 1-octadecene (ODE). The ligand exchange process was employed to modify the surface of IZO NCs by replacing the longer-chain ligand of stearic acid with the shorter-chain ligand of butylamine (BA). It should be noted that the ligand-exchange percentage was observed to be 75%. The change of particle size, morphology, and crystal structures were obtained using a field emission scanning electron microscope (FE-SEM) and X-ray diffraction pattern results. In our study, the 5 nm and 10 nm IZO NCs capped with stearic acid (SA-IZO) were ligand-exchanged with butylamine (BA), and were then spin-coated on a thermal oxide (SiO{sub 2}) gate insulator to fabricate a thin film transistor (TFT) device. The films were then annealed at various temperatures: 350 .deg. C, 400 .deg. C, 500 .deg. C, and 600 .deg. C. All samples showed semiconducting behavior and exhibited n-channel TFT{sup -} Curing temperature dependent on mobility was observed. Interestingly, mobility decreases with the increasing size of NCs from 5 to 10 nm. Miller-Abrahams hopping formalism was employed to explain the hopping mechanism insight our IZO NC films. By focusing on the effect of size, different curing temperatures, electron coupling, tunneling rate, and inter-NC separation, we found that the decrease in electron mobility for larger NCs was due to smaller electronic coupling.

  12. Solution-Processed Inorganic Thin Film Transistors Fabricated from Butylamine-Capped Indium-Doped Zinc Oxide Nanocrystals

    International Nuclear Information System (INIS)

    Indium-doped zinc oxide nanocrystals (IZO NCs), capped with stearic acid (SA) of different sizes, were synthesized using a hot injection method in a noncoordinating solvent 1-octadecene (ODE). The ligand exchange process was employed to modify the surface of IZO NCs by replacing the longer-chain ligand of stearic acid with the shorter-chain ligand of butylamine (BA). It should be noted that the ligand-exchange percentage was observed to be 75%. The change of particle size, morphology, and crystal structures were obtained using a field emission scanning electron microscope (FE-SEM) and X-ray diffraction pattern results. In our study, the 5 nm and 10 nm IZO NCs capped with stearic acid (SA-IZO) were ligand-exchanged with butylamine (BA), and were then spin-coated on a thermal oxide (SiO2) gate insulator to fabricate a thin film transistor (TFT) device. The films were then annealed at various temperatures: 350 .deg. C, 400 .deg. C, 500 .deg. C, and 600 .deg. C. All samples showed semiconducting behavior and exhibited n-channel TFT- Curing temperature dependent on mobility was observed. Interestingly, mobility decreases with the increasing size of NCs from 5 to 10 nm. Miller-Abrahams hopping formalism was employed to explain the hopping mechanism insight our IZO NC films. By focusing on the effect of size, different curing temperatures, electron coupling, tunneling rate, and inter-NC separation, we found that the decrease in electron mobility for larger NCs was due to smaller electronic coupling

  13. Evaluation of drug-carrier interactions in quaternary powder mixtures containing perindopril tert-butylamine and indapamide.

    Science.gov (United States)

    Voelkel, Adam; Milczewska, Kasylda; Teżyk, Michał; Milanowski, Bartłomiej; Lulek, Janina

    2016-04-30

    Interactions occurring between components in the quaternary powder mixtures consisting of perindopril tert-butylamine, indapamide (active pharmaceutical ingredients), carrier substance and hydrophobic colloidal silica were examined. Two grades of lactose monohydrate: Spherolac(®) 100 and Granulac(®) 200 and two types of microcrystalline cellulose: M101D+ and Vivapur(®) 102 were used as carriers. We determined the size distribution (laser diffraction method), morphology (scanning electron microscopy) and a specific surface area of the powder particles (by nitrogen adsorption-desorption). For the determination of the surface energy of powder mixtures the method of inverse gas chromatography was applied. Investigated mixtures were characterized by surface parameters (dispersive component of surface energy, specific interactions parameters, specific surface area), work of adhesion and cohesion as well as Flory-Huggins parameter χ23('). Results obtained for all quaternary powder mixtures indicate existence of interactions between components. The strongest interactions occur for both blends with different types of microcrystalline cellulose (PM-1 and PM-4) while much weaker ones for powder mixtures with various types of lactose (PM-2 and PM-3). PMID:26924356

  14. Use of 15N Label in Organic Synthesis and Spectroscopy. Part I: Preparation of 15N-Labeled tert-Butylamine

    Science.gov (United States)

    Talaty, Erach R.; Boese, Christopher A.; Adewale, Sanni M.; Ismail, Mohammed S.; Provenzano, Frank A.; Utz, Melissa J.

    2002-02-01

    The preparation of 15N-labeled tert-butylamine involves the conversion of the correspondingly labeled potassium cyanide into the 15N-labeled tert-butylformamide via the Ritter reaction in 85% yield, followed by hydrolysis with either aqueous sodium hydroxide or hydrochloric acid. The NMR spectra of the compounds provide a valuable opportunity for discussing several important topics in NMR spectroscopy, such as cis-trans isomerism due to restricted rotation and 15N coupling. Comparison of the IR spectra of the labeled and unlabeled compounds permits a forum for discussing the theory of vibrational frequencies.

  15. Structural properties of a family of hydrogen-bonded co-crystals formed between gemfibrozil and hydroxy derivatives of t-butylamine, determined directly from powder X-ray diffraction data

    International Nuclear Information System (INIS)

    We report the formation and structural properties of co-crystals containing gemfibrozil and hydroxy derivatives of t-butylamine H2NC(CH3)3-n (CH2OH) n , with n=0, 1, 2 and 3. In each case, a 1:1 co-crystal is formed, with transfer of a proton from the carboxylic acid group of gemfibrozil to the amino group of the t-butylamine derivative. All of the co-crystal materials prepared are polycrystalline powders, and do not contain single crystals of suitable size and/or quality for single crystal X-ray diffraction studies. Structure determination of these materials has been carried out directly from powder X-ray diffraction data, using the direct-space Genetic Algorithm technique for structure solution followed by Rietveld refinement. The structural chemistry of this series of co-crystal materials reveals well-defined structural trends within the first three members of the family (n=0, 1, 2), but significantly contrasting structural properties for the member with n=3. - Graphical abstract: Structural properties of a family of co-crystals containing gemfibrozil and hydroxy derivatives of t-butylamine are discussed and rationalized

  16. The influence of conventional heating and microwave irradiation on the resolution of (RS)-sec-butylamine catalyzed by free or immobilized lipases

    International Nuclear Information System (INIS)

    The lipases CAL-B, PSL, PSL-C, PSL-D, and A. niger lipase, free or immobilized in starch (obtained from two types of yam, known in Brazil as 'cara' (Discorea alata L.) and 'inhame' (Colocasia esculenta (L.) Schott) or gelatin films, were used in the acylation of (RS)-sec-butylamine with different acyl donors in various organic solvents applying conventional heating (CH) or microwave (MW) irradiation. In the case of free A. niger lipase, the conversion degrees were three times higher using MW irradiation when compared to conventional heating at 35 deg C. Using free A. niger lipase, the (R)-amide was obtained with a conversion degree of 21%, resulting in eep> 99% and E-value (enantioselectivity value) > 200, in 1 min of reaction under MW irradiation. When the A. niger lipase was immobilized in yam starch films, the (R)-amide was obtained in moderate conversions of 8-25% after 3 or 5 min of reaction under MW irradiation, but with higher selectivity (eep > 99% and E > 200) in comparison with the free form (conversion degree of 45%, eep 81% and E value of 18). (author)

  17. The influence of conventional heating and microwave irradiation on the resolution of (RS)-sec-butylamine catalyzed by free or immobilized lipases

    Energy Technology Data Exchange (ETDEWEB)

    Pilissao, Cristiane; Nascimento, Maria da Graca, E-mail: maria.nascimento@ufsc.br [Departamento de Quimica, Universidade Federal de Santa Catarina, Florianopolis,SC (Brazil); Carvalho, Patricia de Oliveira [Curso de Farmacia, Universidade Sao Francisco, Braganca Paulista, SP (Brazil)

    2012-09-15

    The lipases CAL-B, PSL, PSL-C, PSL-D, and A. niger lipase, free or immobilized in starch (obtained from two types of yam, known in Brazil as 'cara' (Discorea alata L.) and 'inhame' (Colocasia esculenta (L.) Schott) or gelatin films, were used in the acylation of (RS)-sec-butylamine with different acyl donors in various organic solvents applying conventional heating (CH) or microwave (MW) irradiation. In the case of free A. niger lipase, the conversion degrees were three times higher using MW irradiation when compared to conventional heating at 35 deg C. Using free A. niger lipase, the (R)-amide was obtained with a conversion degree of 21%, resulting in ee{sub p}> 99% and E-value (enantioselectivity value) > 200, in 1 min of reaction under MW irradiation. When the A. niger lipase was immobilized in yam starch films, the (R)-amide was obtained in moderate conversions of 8-25% after 3 or 5 min of reaction under MW irradiation, but with higher selectivity (eep > 99% and E > 200) in comparison with the free form (conversion degree of 45%, eep 81% and E value of 18). (author)

  18. Synthesis, characterization, crystal structure and HSA binding of two new N,O,O-donor Schiff-base ligands derived from dihydroxybenzaldehyde and tert-butylamine

    Science.gov (United States)

    Khosravi, Iman; Hosseini, Farnaz; Khorshidifard, Mahsa; Sahihi, Mehdi; Rudbari, Hadi Amiri

    2016-09-01

    Two new o-hydroxy Schiff-bases compounds, L1 and L2, were derived from the 1:1 M condensation of 2,3-dihydroxybenzaldehyde and 2,4-dihydroxybenzaldehyde with tert-butylamine and were characterized by elemental analysis, FT-IR, 1H and 13C NMR spectroscopies. The crystal structure of L2 was also determined by single crystal X-ray analysis. The crystal structure of L2 showed that the compound exists as a zwitterionic form in the solid state, with the H atom of the phenol group being transferred to the imine N atom. It adopts an E configuration about the central Cdbnd N double bond. Furthermore, binding of these Schiff base ligands to Human Serum Albumin (HSA) was investigated by fluorescence quenching, absorption spectroscopy, molecular docking and molecular dynamics (MD) simulation methods. The fluorescence emission of HSA was quenched by ligands. Also, suitable models were used to analyze the UV-vis absorption spectroscopy data for titration of HSA solution by various amounts of Schiff bases. The spectroscopic studies revealed that these Schiff bases formed 1:1 complex with HSA. Energy transfer mechanism of quenching was discussed and the values of 3.35 and 1.57 nm as the mean distances between the bound ligands and the HSA were calculated for L1 and L2, respectively. Molecular docking results indicated that the main active binding site for these Schiff bases ligands is in subdomain IB. Moreover, MD simulation results suggested that this Schiff base complex can interact with HSA, with a slight modification of its tertiary structure.

  19. Structural properties of a family of hydrogen-bonded co-crystals formed between gemfibrozil and hydroxy derivatives of t-butylamine, determined directly from powder X-ray diffraction data

    Science.gov (United States)

    Cheung, Eugene Y.; David, Sarah E.; Harris, Kenneth D. M.; Conway, Barbara R.; Timmins, Peter

    2007-03-01

    We report the formation and structural properties of co-crystals containing gemfibrozil and hydroxy derivatives of t-butylamine H 2NC(CH 3) 3-n(CH 2OH) n, with n=0, 1, 2 and 3. In each case, a 1:1 co-crystal is formed, with transfer of a proton from the carboxylic acid group of gemfibrozil to the amino group of the t-butylamine derivative. All of the co-crystal materials prepared are polycrystalline powders, and do not contain single crystals of suitable size and/or quality for single crystal X-ray diffraction studies. Structure determination of these materials has been carried out directly from powder X-ray diffraction data, using the direct-space Genetic Algorithm technique for structure solution followed by Rietveld refinement. The structural chemistry of this series of co-crystal materials reveals well-defined structural trends within the first three members of the family ( n=0, 1, 2), but significantly contrasting structural properties for the member with n=3.

  20. Laboratory study on new particle formation from the reaction OH + SO2: influence of experimental conditions, H2O vapour, NH3 and the amine tert-butylamine on the overall process

    Directory of Open Access Journals (Sweden)

    J. Curtius

    2010-08-01

    Full Text Available Nucleation experiments starting from the reaction of OH radicals with SO2 have been performed in the IfT-LFT flow tube under atmospheric conditions at 293±0.5 K for a relative humidity of 13–61%. The presence of different additives (H2, CO, 1,3,5-trimethylbenzene for adjusting the OH radical concentration and resulting OH levels in the range (4–300 ×105 molecule cm−3 did not influence the nucleation process itself. The number of detected particles as well as the threshold H2SO4 concentration needed for nucleation was found to be strongly dependent on the counting efficiency of the used counting devices. High-sensitivity particle counters allowed the measurement of freshly nucleated particles with diameters down to about 1.5 nm. A parameterization of the experimental data was developed using power law equations for H2SO4 and H2O vapour. The exponent for H2SO4 from different measurement series was in the range of 1.7–2.1 being in good agreement with those arising from analysis of nucleation events in the atmosphere. For increasing relative humidity, an increase of the particle number was observed. The exponent for H2O vapour was found to be 3.1 representing an upper limit. Addition of 1.2×1011 molecule cm−3 or 1.2×1012 molecule cm−3 of NH3 (range of atmospheric NH3 peak concentrations revealed that NH3 has a measureable, promoting effect on the nucleation rate under these conditions. The promoting effect was found to be more pronounced for relatively dry conditions, i.e. a rise of the particle number by 1–2 orders of magnitude at RH = 13% and only by a factor of 2–5 at RH = 47% (NH3 addition: 1.2×1012 molecule cm−3. Using the amine tert-butylamine instead of NH3, the enhancing impact of the base for nucleation and particle growth appears to be stronger. Tert-butylamine addition of about 1010 molecule cm−3 at RH = 13% enhances particle formation by about two orders of magnitude, while for NH3 only a small or negligible

  1. Electric Field Assisted Hopping of Tert-Butylamine on Cu(111)Surface%隧道结电场辅助下叔丁胺分子在Cu(111)表面跳跃

    Institute of Scientific and Technical Information of China (English)

    许逾群; 仉君; 袁秉凯; 邓珂; 杨蓉; 裘晓辉

    2010-01-01

    The lateral hopping of tert-butylamine (t-BA) molecules on a Cu(lll) surface was studied by scanning tunneling microscopy (STM) at 78K.The hopping probabilities of the molecules in the tunneling junction were found to depend linearly on the applied tunneling current,indicating a single electron-induced process.Hopping probabilities under an electric field of opposite polarity was found to be different.This non-equivalence is attributed to an electric field assisted diffusion where the adsorption energy and the diffusion barrier of the t-BA molecule are different when the polar molecule is subjected to opposite electric fields.%采用扫描隧道显微镜(STM)于78K研究了单个叔丁胺分子在Cu(111)表面的横向跃迁现象.研究发现叔丁胺分子的跳跃几率随隧道电流的增加而线性增加,这表明该过程是单电子激发过程;在不同极性的隧道结电场作用下,叔丁基胺分子跳跃行为发生的几率不同,这种现象可以用电场辅助的扩散过程解释.在不同极性电场作用下叔丁胺分子在Cu(111)表面的吸附能和扩散势垒不同,从而表现出不同的跳跃几率.

  2. 培哚普利精氨酸盐治疗轻中度原发性高血压患者的疗效观察%Efficacy comparison between 5 mg perindopril arginine salt and 4 mg perindopril tert-butylamine salt for patients with mild to moderate essential hypertension

    Institute of Scientific and Technical Information of China (English)

    齐丽彤; 赵水平; 黎辉; 郭莹; 徐耕; 葛均波; 吴士尧; 缪培智; 金艳

    2015-01-01

    目的 比较培哚普利精氨酸盐与培哚普利叔丁胺盐两种剂型治疗原发性轻中度高血压患者的疗效和安全性.方法 采用多中心、随机、双盲、活性药物平行对照设计.入选2010年7月至2011年5月北京大学第一医院等全国共19家中心的轻中度高血压患者524例,经过2周安慰剂导入期,最终369例入选,随机接受培哚普利精氨酸盐5 mg(试验组,186例)或培哚普利叔丁胺盐4 mg(对照组,183例)治疗.随机顺序由施维雅国际研究中心的生物统计部生成,在各中心内进行了平衡.经过8周双盲治疗后,根据血压达标情况调整服药剂量,对于血压未达标者,即坐位收缩压≥140 mmHg(1 mmHg =0.133 kPa)和(或)坐位舒张压≥90 mmHg,上调剂量至精氨酸盐10 mg或者叔丁胺盐8 mg,继续双盲治疗4周.同时观察两组患者药物治疗的安全性指标.结果 治疗8周时,试验组和对照组患者坐位收缩压分别下降了(19.9±17.2)和(18.5±14.7) mmHg(P=0.0005),舒张压分别下降了(12.0±10.0)和(11.0±8.9) mmHg(P<0.000 1).治疗12周时两组收缩压及舒张压的降低幅度依然类似.试验组和对照组组间血压达标率和治疗有效率均相当[8周达标率38.5%比31.3%,95% CI(-2.6 ~ 16.9),12周达标率36.3%比35.7%,95% CI(-9.3 ~10.4);8周有效率64.3%比63.2%,95%CI(-8.8~11.0),12周有效率65.9%比64.8%,95% CI(-8.7~ 10.9)].两组患者不良事件发生率均较低.结论 对于原发性轻中度高血压患者,培哚普利精氨酸盐的降压疗效与培哚普利叔丁胺盐相当,且安全性良好.%Objective To compare the efficacy and safety of 5 mg perindopril arginine salt and 4 mg perindopril tert-butylamine salt for patients with mild to moderate essential hypertension.Methods The study was designed as multicenter, randomized, double-blind, active controlled trial with two parallel groups enrolling 524 participants with mild to moderate essential hypertension

  3. DNA interacions of new antitumor platinum complexes with trans geometry activated by a 2-metylbutylamine or sec-butylamine ligand

    Czech Academy of Sciences Publication Activity Database

    Prokop, Radim; Kašpárková, Jana; Nováková, Olga; Marini, Victoria; Pizarro, A. M.; Navarro-Ranninger, C.; Brabec, Viktor

    2004-01-01

    Roč. 67, č. 6 (2004), s. 1097-1109. ISSN 0006-2952 R&D Projects: GA ČR GA305/02/1552; GA AV ČR KJB5004301; GA AV ČR IBS5004107 Grant ostatní: Ministry of Science and Technology (ES) SAF00-0029; CICYT(ES) SAF 03-01700 Institutional research plan: CEZ:AV0Z5004920 Keywords : cisplatin * transplatin * antitumor drugs Subject RIV: BO - Biophysics Impact factor: 3.436, year: 2004

  4. Highly enhanced vapor sensing of multi-walled carbon nanotube network sensors by n-butylamine functionalization

    Czech Academy of Sciences Publication Activity Database

    Slobodian, P.; Říha, Pavel; Cavallo, P.; Barbero, C.A.; Cvelbar, U.; Benlikaya, R.; Petras, D.; Sáha, P.

    2014-01-01

    Roč. 2014, August (2014), Article ID 589627. ISSN 1687-4110 R&D Projects: GA MŠk(CZ) 7AMB13AR019 Grant ostatní: UTB Zlín(CZ) IGA/FT/2014/013; GA MŠk(CZ) ED2.1.00/03.0111 Institutional support: RVO:67985874 Keywords : carbon nanotube (CNT) * multiwall carbon nanotube (MWCNT) * nanotube networks * volatile organic compounds (VOC) Subject RIV: BK - Fluid Dynamics Impact factor: 1.644, year: 2014

  5. DNA interacions of new antitumor platinum complexes with trans geometry activated by a 2-metylbutylamine of sec-butylamine ligand

    Czech Academy of Sciences Publication Activity Database

    Prokop, Radim; Kašpárková, Jana; Nováková, Olga; Marini, Victoria; Pizarro, A. M.; Navarro-Ranninger, C.; Brabec, Viktor

    2004-01-01

    Roč. 67, č. 6 (2004), s. 1097-1109. ISSN 0006-2952 R&D Projects: GA ČR GA305/02/1552; GA AV ČR KJB5004301; GA AV ČR IBS5004107 Institutional research plan: CEZ:AV0Z5004920 Keywords : cisplatin * transplatin * antitumor drugs Subject RIV: BO - Biophysics Impact factor: 3.436, year: 2004

  6. 旋光法测定培哚普利叔丁胺盐及培哚普利片含量%Determination of the content of perindopril tert-butylamine salt and perindopril tablets by polarimetric analysis

    Institute of Scientific and Technical Information of China (English)

    李雅茹; 李朝晖

    2006-01-01

    目的:建立培哚普利叔丁胺盐及培哚普利片含量测定方法.方法:以乙醇为溶剂,采用旋光法测定培哚普利叔丁胺盐及培哚普利片含量.结果:培哚普利叔丁胺盐在1.2~15 mg/ml范围内浓度与旋光度呈良好线性关系,回归方程C=0.005 4+1.468 8 X, r=1.000 0,平均回收率99.6%,RSD为0.19%(n=9).结论:本法简便易行,结果准确,可作为培哚普利叔丁胺盐及培哚普利片的质控方法.

  7. 一氧化碳共吸附法确定叔丁胺分子在Cu(111)表面的吸附位%Determination of the Adsorption Sites of tert-Butylamine Molecules on a Cu(111)Surface with a Co-Adsorbed CO Monolayer

    Institute of Scientific and Technical Information of China (English)

    陈毓敏; 邓珂; 裘晓辉; 王琛

    2009-01-01

    采用扫描隧道显微镜(STM)和密度泛函理论(DFT)研究了78 K时单个叔丁胺分子在Cu(111)表面的吸附位.我们提出以共吸附的一氧化碳(3)×(3)超结构为基底铜原子的标识方法,确定了低覆盖度的叔丁胺分子在Cu(111)表面的吸附位为顶位.而采用单个一氧化碳分子标识基底铜原子的位置,同样得出了叔丁胺分子的吸附位为顶位.此外,还采用DFT计算叔丁胺分子在Cu(111)表面的优势吸附构型.理论计算结果表明顶位吸附构型为能量最稳定的构型,与实验结果相吻合.

  8. Heck Arylation of Acrylonitrile with Aryl Iodides Catalyzed by a Silica-bound Arsine Palladium(0) Complex

    Institute of Scientific and Technical Information of China (English)

    Ming Zhong CAI; Hong ZHAO; Rong Li ZHANG

    2005-01-01

    Acrylonitrile reacts with aryl iodides in the presence of tri-n-butylamine and a catalytic amount of a silica-bound arsine palladium(0) complex to afford stereoselectively (E)-cinnamonitriles in high yields.

  9. cis-Bis(butyl­amine-κN)bis­[sulfa­diazine(1−)-κ2 N,N′]copper(II) penta­hydrate

    OpenAIRE

    Orhan Büyükgüngör; Zerrin Heren; Gökhan Kaştaş; Hümeyra Paşaoğlu

    2008-01-01

    In the title compound {systematic name: cis-bis[4-amino-N-(pyrimidin-2-yl)benzenesulfonamidato-κ2N,N′]bis(butylamine-κN)copper(II) pentahydrate}, [Cu(C10H9N4O2S)2(C4H11N)2]·5H2O or [Cu(sdz)2(ba)2]·5H2O [ba is butylamine and sdz = sulfadiazine(1−)], the copper(II) cation is six-coordinated by four N atoms of two sulfadiazine ligands and two N atoms of butylamine ligands. The copper(II) ion and one of the water molecules lie on twofold rotation axes. One of the b...

  10. Preparation of lamellar compounds: synthesis of the crystalline zirconium hydrogenphosphate and its intercalation with amines. An experiment for undergraduate students

    International Nuclear Information System (INIS)

    The present paper describes the synthesis of crystalline zirconium hydrogen phosphate by direct precipitation and its intercalation with pyridine and n-butylamine. The simple experiment was tested in the undergraduate inorganic chemistry laboratory course for chemistry students at IQ-UNICAMP using inexpensive reagents. The materials were characterized by powder X-ray diffraction and infrared analyses in order to obtain detailed information of the solid structure changes as a result of the intercalation process. Pyridine and n-butylamine are focused in this work as clear and elucidative examples leading to acid-base interactive processes that result in the well-formed infinite sequence of inorganic lamellar structures. (author)

  11. Derivatives of 1,3-oxazolidines on the base of diamino-alcohols

    International Nuclear Information System (INIS)

    In this article authors investigated the reaction of 1-cyclohexyl amino-3-diethyl amino-2-propanol, 1-butylamine-3-diethyl amino-2-propanol. By authors was determined that reaction of initial diamino-alcohols with furfural passing at molar correlation of reagents 1:1 at temperature 20-22digC at presence dehydrating medium-potash during 36 hours

  12. Guide On Analysis Of Dangerous And Harmful Object

    International Nuclear Information System (INIS)

    This book lists the dangerous and harmful object, which are Acetaldehyde, Acetic acid, Acetone, Acrolein, Aldrin Ammonia, Arsenic, Asphalt, Barium, Benzene, Benzyl chloride, Butane, Butylamine, Butyl mercaptan, Cadmium, Cadmium chloride, Cadmium nitrate, Cadmium sulfate, Calcium, Calcium carbonate, Calcium chloride, Calcium cyanamide, Calcium oxide, Captan, Carbon black, Carbon dioxide, Carbon disulfide, Catechol, Chlordane, Chlorine, Chlorine dioxide, Chlorine trifluoride and Chloroacetic acid.

  13. New adducts of Lapachol with primary amines

    Energy Technology Data Exchange (ETDEWEB)

    Santos, Mirelly D.F.; Litivack-Junior, Jose T.; Antunes, Roberto V.; Silva, Tania M.S.; Camara, Celso A., E-mail: ccelso@dq.ufrpe.b [Universidade Federal Rural de Pernambuco (UFRPE), Recife, PE (Brazil). Dept. de Quimica

    2011-07-01

    New adducts of lapachol with neat primary aliphatic amines were obtained in a solvent-free reaction in good to reasonable yields (52 to 88%), at room temperature. The new compounds containing a phenazine moiety were obtained from suitable functionalized aminoalkyl compounds, including ethanolamine, 3-propanolamine, 2-methoxy-ethylamine, 3-methoxy-propylamine, n-butylamine and 2-phenetylamine. (author)

  14. A volumetric and viscosity study for the binary mixtures of 1-hexyl-3-methylimidazolium tetrafluoroborate with some molecular solvents

    International Nuclear Information System (INIS)

    Research highlights: → Excess molar volumes and excess logarithm viscosities for the binary mixtures of 1-hexyl-3-methylimidazolium tetrafluroborate were determined. → The absolute values of VmE follow the sequence: THF > butanone > ethyl acetate > butylamine for the binary systems. → The values of (lnη)E decrease in the order: THF > butylamine > ethyl acetate > butanone. → Ion-dipole interaction, the hydrogen bond, the packing efficiency and the ion-pairs exist in the ionic liquid are believed to influence the excess properties of the related systems. → The information obtained in this work allows us to show how physical properties of molecular solvents affect their interaction with the ionic liquid. - Abstract: Information on the interactions between ionic liquids and molecular solvents are essential for the understanding of the function of ionic liquids in related procedures, and excess properties are sensitive probe for these interactions. In this work, excess molar volume (VmE) and excess logarithmic viscosity ((ln η)E) for the binary mixtures of 1-hexyl-3-methylimidazolium tetrafluoroborate ([C6mim][BF4]) with butanone, ethyl acetate, butylamine, and tetrahydrofuran have been determined from density and viscosity measurements in the whole composition range at the temperature of 298.15 K. It is found that for the studied systems, the values of VmE are negative but those of (ln η)E are positive in the whole concentration range. The VmE values show their minimum at the ionic liquid mole fraction of 0.3, and (ln η)E values exhibit a maximum at the same composition. The absolute values of VmE follow the sequence: tetrahydrofuran > butanone > ethyl acetate > butylamine for the binary systems, whereas the values of (ln η)E decrease in the order: tetrahydrofuran > butylamine > ethyl acetate > butanone. The results have been analyzed through the ion-dipole interaction, the hydrogen bonding, the packing efficiency and the ion-pairs exist in the ionic

  15. Study on Solution Properties of Binary Mixtures of Some Industrially Important Solvents with Cyclohexylamine and Cyclohexanone at 298.15 K

    Science.gov (United States)

    Roy, Mahendra Nath; Das, Rajesh Kumar; Chanda, Riju

    2010-03-01

    Densities and viscosities were measured for the binary mixtures of cyclohexylamine and cyclohexanone with butyl acetate, butanone, butylamine, tert-butylamine, and 2-butoxyethanol at 298.15 K over the entire composition range. From density data, the values of the excess molar volume ( V E) have been calculated. The experimental viscosity data were correlated by means of the equation of Grunberg-Nissan. The density and viscosity data have been analyzed in terms of some semiempirical viscosity models. The results are discussed in terms of molecular interactions and structural effects. The excess molar volume is found to be either negative or positive depending on the molecular interactions and the nature of the liquid mixtures and is discussed in terms of molecular interactions and structural changes.

  16. Preparation and permeability of ZSM-35 zeolite membranes on porous stainless steel tubes

    Institute of Scientific and Technical Information of China (English)

    ZHU Gang; WANG Jinqu; ZHANG Yan; LU Jinming; XIU Jinghai

    2007-01-01

    ZSM-35 zeolite membranes were prepared on porous stainless steel tubes with silica sol and tetraethoxysilane as silica source,and with 1-butylamine and ethylenediamine as templates,respectively.The characterization of X-ray diffraction(XRD)and scanning electron microscopy (SEM)showed that the membranes prepared with ethylene-diamine as the template displayed growth orientation with their crystal planes(h00)parallel to the support surface.The single-component permeability tests of H2,N2 and C3H8 showed that me membranes synthesized with ethylene-diamine as the template,compared with those witb 1-butylamine as the template,showed relatively higher permeation rates and ideal separation factors,and above their corresponding ideal Knudsen diflusion factors,Which might be attributed to the different growth orientation of zeolite membranes synthesized with different templates.

  17. Hydroquinone-O,O'-diacetic acid ('Q-linker') as a replacement for succinyl and oxalyl linker arms in solid phase oligonucleotide synthesis.

    OpenAIRE

    Pon, R T; Yu, S.

    1997-01-01

    When hydroquinone-O,Ooffiacetic acid is used as a linker arm in solid phase oligonucleotide synthesis, the time for NH4OH cleavage of oligodeoxy- or oligoribonucleotides is reduced to only 2 min. This allows increased productivity on automated DNA synthesizers without requiring any other modifications to existing reagents or synthesis and deprotection methods. The Q-linker may also be rapidly cleaved by milder reagents such as 5% NH4OH, potassium carbonate, anhydrous ammonia, t-butylamine or ...

  18. 40 CFR 261.33 - Discarded commercial chemical products, off-specification species, container residues, and spill...

    Science.gov (United States)

    2010-07-01

    ... 100-02-7 p-Nitrophenol U171 79-46-9 2-Nitropropane (I,T) U172 924-16-3 N-Nitrosodi-n-butylamine U173... described in § 261.2(a)(2)(i), when they are mixed with waste oil or used oil or other material and applied...-08-2 Acetamide, N-(aminothioxomethyl)- P057 640-19-7 Acetamide, 2-fluoro- P058 62-74-8 Acetic...

  19. Study on Synthesis and Intercalation Behavior of Layered Zirconium Proline-N-methylphosphonate-phosphate

    Institute of Scientific and Technical Information of China (English)

    Xiao Ping RAO; Xiang Kai FU; Kai RAO

    2004-01-01

    Zirconium proline-N-methylphosphonate-phosphate (α-ZPMPP) was prepared in the presence of HF for the first time. The α-ZPMPP sample is highly crystallized with interlayer distance of 1.52 nm. The interlayer distance of complex of α-ZPMPP with n-butylamine (α-ZPMPP-BA) is in 0.45 nm larger than that of α-ZPMPP. The α-ZPMPP possesses different intercalation behavior of host-guest compound from α-ZP.

  20. Evidence for covalent binding of epicocconone with proteins from synchronous fluorescence spectra and fluorescence lifetimes

    Indian Academy of Sciences (India)

    Debashis Panda; Anindya Datta

    2007-03-01

    Synchronous fluorescence and time-resolved fluorescence spectroscopic studies that reveal the interaction of epicocconone with human serum albumin is significantly different from its interaction with surfactant assemblies. This observation, along with steady-state fluorescence data, indicates groundstate interaction between the fluorophore epicocconone and the protein. Similarity in fluorescence properties with the adduct of the fluorophore with -butylamine indicates that bonding occurs at the Nterminus of the protein.

  1. Palladium-catalysed reactions of 8-hydroxy- and 8-benzyloxy-5,7-diiodoquinoline under aminocarbonylation conditions

    OpenAIRE

    Takács, Attila; Szilágyi, Antal; Ács, Péter; Márk, László; Peixoto, Andreia F.; Mariette M. Pereira; Kollár, László

    2011-01-01

    Various 5-carboxamido-7-iodo-8-benzyloxyquinolines were synthesised via selective aminocarbonylation of 5,7-diiodo-8-benzyloxyquinoline in the presence of ‘in situ’ generated palladium(0) catalysts. Under similar conditions (50 °C, 80 bar CO), 5,7-bis(N-tert-butyl-glyoxylamido)-8-hydroxyquinoline was obtained using tert-butylamine as N-nucleophile. The unprotected 5,7-diiodo-8-hydroxyquinoline underwent dehydroiodination resulting in 8-hydroxyquinoline as the major product.

  2. Adsorption of certain surface-active organic substances on lead, and their effect on hydrogen evolution kinetics in sulfuric acid

    Energy Technology Data Exchange (ETDEWEB)

    Sherstobitova, I.N.; Iskhakov, R.N.

    1988-02-01

    The adsorption of tetrabutylammonium sulfate, n-butyl, n-amyl, isoamyl, n-hexyl alcohol, butyric acid, butylamine, antipyrine and diantipyrylmethane was measured by differential-capacitance at a frequency of 10 kHz at smooth lead electrodes under cathodic polarization. Isotherms were determined by logarithms. Parameters in the Frumkin equation for adsorption of certain organic substances on lead were also determined and tabulated.

  3. The pharmacokinetics of perindopril in patients with liver cirrhosis.

    OpenAIRE

    Thiollet, M; Funck-Brentano, C.; Grangé, J D; Midavaine, M; Resplandy, G; Jaillon, P

    1992-01-01

    Perindopril is a non-sulphydryl angiotensin converting enzyme (ACE) inhibitor which requires hydrolysis to its active metabolite, perindoprilat, to produce its effects. Ten cirrhotic patients with mild to severe disease were studied after oral administration of a single 8 mg dose of perindopril as its tert-butylamine salt. Compared with a historical control group of young healthy volunteers receiving the same single oral dose of perindopril, mean AUC values of the prodrug perindopril were dou...

  4. Secondary organic aerosol formation from primary aliphatic amines with NO3 radical

    OpenAIRE

    Q. G. J. Malloy; Li Qi; B. Warren; Cocker III, D. R.; M. E. Erupe; Silva, P J

    2009-01-01

    Primary aliphatic amines are an important class of nitrogen containing compounds emitted from automobiles, waste treatment facilities and agricultural animal operations. A series of experiments conducted at the UC-Riverside/CE-CERT Environmental Chamber is presented in which oxidation of methylamine, ethylamine, propylamine, and butylamine with O3 and NO3 have been investigated. Very little aerosol formation is observed in the presence of O3 only. However, after addition of ...

  5. Secondary organic aerosol formation from primary aliphatic amines with NO3 radical

    OpenAIRE

    M. E. Erupe; Cocker III, D. R.; B. Warren; Li Qi; Q. G. J. Malloy; Silva, P J

    2008-01-01

    Primary aliphatic amines are an important class of nitrogen containing compounds found to be emitted from automobiles, waste treatment facilities and agricultural animal operations. A series of experiments conducted at the UC-Riverside/CE-CERT Environmental Chamber is presented in which oxidation of methylamine, ethylamine, propylamine, and butylamine with NO3 has been investigated. Very little aerosol formation is observed in the presence of O3 only. However, after addition of NO, and by ext...

  6. Secondary Organic Aerosol Formation from Primary Aliphatic Amines with Nitrate Radical

    OpenAIRE

    Q. G. J. Malloy; Qi, L; B. Warren; Cocker III, D. R.; M. E. Erupe; Silva, P J

    2009-01-01

    Primary aliphatic amines are an important class of nitrogen containing compounds emitted from automobiles, waste treatment facilities and agricultural animal operations. A series of experiments conducted at the UC-Riverside/CECERT Environmental Chamber is presented in which oxidation of methylamine, ethylamine, propylamine, and butylamine with O3 and NO3 have been investigated. Very little aerosol formation is observed in the presence of O3 only. However, after addition of NO, and by extensio...

  7. Electrochemical Characterization of Protein Adsorption onto YNGRT-Au and VLGXE-Au Surfaces

    Directory of Open Access Journals (Sweden)

    Hanna Trzeciakiewicz

    2015-08-01

    Full Text Available The adsorption of the proteins CD13, mucin and bovine serum albumin on VLGXE-Au and YNGRT-Au interfaces was monitored by electrochemical impedance spectroscopy in the presence of [Fe(CN6]3−/4−. The hydrophobicity of the Au surface was tailored using specific peptides, blocking agents and diluents. The combination of blocking agents (ethanolamine or n-butylamine and diluents (hexanethiol or 2-mercaptoethanol was used to prepare various peptide-modified Au surfaces. Protein adsorption onto the peptide-Au surfaces modified with the combination of n-butylamine and hexanethiol produced a dramatic decrease in the charge transfer resistance, Rct, for all three proteins. In contrast, polar peptide-surfaces induced a minimal change in Rct for all three proteins. Furthermore, an increase in Rct was observed with CD13 (an aminopeptidase overexpressed in certain cancers in comparison to the other proteins when the VLGXE-Au surface was modified with n-butylamine as a blocking agent. The electrochemical data indicated that protein adsorption may be modulated by tailoring the peptide sequence on Au surfaces and that blocking agents and diluents play a key role in promoting or preventing protein adsorption. The peptide-Au platform may also be used for targeting cancer biomarkers with designer peptides.

  8. Electrochemical Characterization of Protein Adsorption onto YNGRT-Au and VLGXE-Au Surfaces.

    Science.gov (United States)

    Trzeciakiewicz, Hanna; Esteves-Villanueva, Jose; Soudy, Rania; Kaur, Kamaljit; Martic-Milne, Sanela

    2015-01-01

    The adsorption of the proteins CD13, mucin and bovine serum albumin on VLGXE-Au and YNGRT-Au interfaces was monitored by electrochemical impedance spectroscopy in the presence of [Fe(CN)6](3-/4-). The hydrophobicity of the Au surface was tailored using specific peptides, blocking agents and diluents. The combination of blocking agents (ethanolamine or n-butylamine) and diluents (hexanethiol or 2-mercaptoethanol) was used to prepare various peptide-modified Au surfaces. Protein adsorption onto the peptide-Au surfaces modified with the combination of n-butylamine and hexanethiol produced a dramatic decrease in the charge transfer resistance, Rct, for all three proteins. In contrast, polar peptide-surfaces induced a minimal change in Rct for all three proteins. Furthermore, an increase in Rct was observed with CD13 (an aminopeptidase overexpressed in certain cancers) in comparison to the other proteins when the VLGXE-Au surface was modified with n-butylamine as a blocking agent. The electrochemical data indicated that protein adsorption may be modulated by tailoring the peptide sequence on Au surfaces and that blocking agents and diluents play a key role in promoting or preventing protein adsorption. The peptide-Au platform may also be used for targeting cancer biomarkers with designer peptides. PMID:26262621

  9. Variations in product in reactions of naphthoquinone with primary amines

    OpenAIRE

    Barooah Nilotpal; Karmakar Anirban; Singh Marjit W; Baruah Jubaraj B

    2007-01-01

    Abstract Reaction of 1,2-naphthoquinone with primary amines gives a 2-amino-1,4-naphthoquinone derivative which is equivalent to 1,2 to 1,4 carbonyl transposition. For example the reaction of 1,2-naphthoquinone with 4-methoxyaniline gives 2-(4-methoxyanilino)-naphthoquinone-1,4-(4-methoxyanil) (1) and with n-butylamine gives 2-(butylamino)-naphthoquinone-1,4-butylimine (2) respectively. The compounds 1 and 2 are characterized by X-ray crystallography; they have hydrogen-bonded dimeric structu...

  10. Synthesis of deuterated clenbuterol

    Energy Technology Data Exchange (ETDEWEB)

    Joergensen, Ole [Risoe National Lab., Roskilde (Denmark). Solid State Physics Dept.; Egsgaard, Helge; Larsen, Elfinn [Risoe National Lab., Roskilde (Denmark). Science and Technology Dept.

    1996-11-01

    The synthesis of D{sub 9}-clenbuterol (I) and D{sub 3}-clenbuterol (II) is described. D{sub 9}-clenbuterol (I) was prepared from 4-amino-{alpha}-bromo-3, 5-dichloroacetophenone by reaction with D{sub 9}-tert-butylamine followed by reduction of the keto group with NaBH{sub 4}. D{sub 3}-clenbuterol (II) was prepared from 4-amino-{alpha}-tert-butylamino-3, 5-dichloroacetophenone by an exchange reaction of the {alpha}-hydrogens with deuterium followed by reduction of the keto group with NaBD{sub 4}. The eventual products were characterized by mass spectrometry and NMR. (author).

  11. Synthesis, Spectroscopic, and Antimicrobial Studies of Binuclear Metallocene (M = Ti, Zr, or Hf) Derivatives of Bis(mercaptoazoles)

    OpenAIRE

    Akhilesh Kumar Srivastava; Chandra Mohan Tripathi; Om Prakash Pandey; Soumitra Kumar Sengupta; Shilpi Sinha

    2007-01-01

    The reactions of (η5−C5H5)2MCl2 (M = Ti, Zr, or Hf) with mercaptoazoles (LH2), namely, bis(mercaptotriazoles), bis(mercap-tooxadiazoles), and bis(mercaptothiadiazoles) in 2 : 1 molar ratio, respectively, have been studied in dry tetrahydrofuran in the presence of n-butylamine and the binuclear complexes of the type [{(η−C5H5)2M}2(L)] (M = Ti/Zr/Hf) are obtained. Tentative structural conclusions are drawn for the reaction products based upon elemental analysis, elec...

  12. Quantitation of buried contamination by use of solvents

    Science.gov (United States)

    Pappas, S. P.; Hsiao, P.; Hill, L. W.

    1972-01-01

    An investigation was made to determine (1) sporicidal properties of amine solvents that solubilize silicon resins, (2) recovery properties of a silicon potting compound (RTV 41) used in spacecraft, and (3) viability of spores during chemical curing of the potting compound. Results show that: (1) spores do remain viable during RTV 41 silicon potting chemical curing, and (2) spore recovery from cured silicon potting compound RTV 41 is very high when silicon rubber is dissolved in butylamine and series dilution with benzene prior to plate curing.

  13. Electrochemical Characterization of Protein Adsorption onto YNGRT-Au and VLGXE-Au Surfaces

    OpenAIRE

    Hanna Trzeciakiewicz; Jose Esteves-Villanueva; Rania Soudy; Kamaljit Kaur; Sanela Martic-Milne

    2015-01-01

    The adsorption of the proteins CD13, mucin and bovine serum albumin on VLGXE-Au and YNGRT-Au interfaces was monitored by electrochemical impedance spectroscopy in the presence of [Fe(CN)6]3−/4−. The hydrophobicity of the Au surface was tailored using specific peptides, blocking agents and diluents. The combination of blocking agents (ethanolamine or n-butylamine) and diluents (hexanethiol or 2-mercaptoethanol) was used to prepare various peptide-modified Au surfaces. Protein adsorption onto t...

  14. Synthesis of deuterated clenbuterol

    International Nuclear Information System (INIS)

    The synthesis of D9-clenbuterol (I) and D3-clenbuterol (II) is described. D9-clenbuterol (I) was prepared from 4-amino-α-bromo-3, 5-dichloroacetophenone by reaction with D9-tert-butylamine followed by reduction of the keto group with NaBH4. D3-clenbuterol (II) was prepared from 4-amino-α-tert-butylamino-3, 5-dichloroacetophenone by an exchange reaction of the α-hydrogens with deuterium followed by reduction of the keto group with NaBD4. The eventual products were characterized by mass spectrometry and NMR. (author)

  15. Time-resolved energy transfer from single chloride terminated nanocrystals to graphene

    CERN Document Server

    Ajayi, O A; Cotlet, M; Petrone, N; Gu, T; Wolcott, A; Gesuele, F; Hone, J; Owen, J S; Wong, C W

    2014-01-01

    We examine the time-resolved resonance energy transfer of excitons from single n-butyl amine-bound, chloride-terminated nanocrystals to two-dimensional graphene through time-correlated single photon counting. The radiative biexponential lifetime kinetics and blinking statistics of the individual surface-modified nanocrystal elucidate the non-radiative decay channels. Blinking modification as well as a 4 times reduction in spontaneous emission were observed with the short chloride and n-butylamine ligands, probing the energy transfer pathways for the development of graphene-nanocrystal nanophotonic devices.

  16. Isomorphous Substitution of Framework Atoms by Titanium in VPI-5 Aluminophosphate Molecular Sieve

    OpenAIRE

    Novak Tušar, Nataša; Zabukovec Logar, Nataša; Arčon, Iztok; Thibault-Starzyk, Frederic; Kaučič, Venčeslav

    2001-01-01

    Extra-large pore aluminophosphate molecular sieve TiVPI-5 was synthesised hydrothermally in the presence of di-n-butylamine and transformed by the calcination process at 500 °C to a large pore TAPO-8. Incorporation of titanium(IV) into VPI-5 framework was studied by elemental and thermogravimetric analyses, combined with X-ray Absorption Near Edge Structure (XANES) spectroscopy and UV-VIS absorption spectroscopy. We found that titanium(IV) incorporated in TiVPI-5 isomorphously substitutes fra...

  17. Investigations of (acid+base) equilibria in systems modelling interactions occurring in biomolecules

    International Nuclear Information System (INIS)

    By using the potentiometric microtitration method, acidity constants, Ka, anionic, KAHA-, and cationic, KBHB+, homoconjugation constants, as well as molecular heteroconjugation, KBHA, constants have been determined in (acid+base) systems formed by the following compounds: acetic acid, phenol, n-butylamine, imidazole, and 4(5)-methylimidazole. These compounds constitute fragments of the side chains of amino acids capable of proton exchange in active sites of enzymes. The (acid+base) equilibria were studied in five polar solvents of different properties, namely in aprotic protophobic acetonitrile, acetone and propylene carbonate, in aprotic protophilic dimethyl sulfoxide and in amphiprotic methanol. The lowest values of the acidity constants of the molecular and cationic acids have been found in aprotic protophobic polar solvents - acetonitrile, propylene carbonate and acetone. Their acid strength have been found to depend on solvent basicity expressed as donor numbers, DN. These media, in particular acetonitrile and acetone, are also favourable for establishing molecular homo- and heteroconjugation equilibria. The most stable homocomplexes are formed in the case of acetic acid (KAHA- values range from 2.26 to 3.56 in these media, being more than an order of magnitude higher than those for the remaining compounds). The magnitudes of lgKBHA reveal that the most stable heterocomplexes are formed by n-butylamine and acetic acid that are characterized by the smallest differences in pKa values

  18. Amphiphilic cellulose nanocrystals from acid-free oxidative treatment: physicochemical characteristics and use as an oil-water stabilizer.

    Science.gov (United States)

    Visanko, Miikka; Liimatainen, Henrikki; Sirviö, Juho Antti; Heiskanen, Juha Pentti; Niinimäki, Jouko; Hormi, Osmo

    2014-07-14

    A chemical pretreatment for producing cellulose nanocrystals (CNCs) with periodate oxidation and reductive amination is reported. This new functionalization of cellulose fibers dispenses an alternative method for fabricating individual CNCs without the widely used acid hydrolysis process. CNCs can be directly modified during the pretreatment step, and no additional post-treatments are required to tune the surface properties. Three butylamine isomers were tested to fabricate CNCs with amphiphilic features. After mechanical homogenization, CNCs occurred as individual crystallinities without aggregation where high uniformity in terms of shape and size was obtained. The elemental analysis and (1)H NMR measurement show that iso- and n-butylamine attach the highest number of butylamino groups to the cellulose fibers. Linking the alkyl groups increases the hydrophobic nature of the CNCs, where water contact angles from self-standing films up to 110.5° are reported. Since these butylamino-functionalized CNCs have hydrophobic characteristics in addition to the hydrophilic backbone of cellulose, the stabilization impact on oil/water emulsions is demonstrated as a potential application. PMID:24946006

  19. Pyrolytic synthesis and characterization of N-doped carbon nanoflakes for electrochemical applications

    Energy Technology Data Exchange (ETDEWEB)

    Savilov, S.V., E-mail: savilov@chem.msu.ru [M.V. Lomonosov Moscow State University, Department of Chemistry, Leninskie gory, 1-3, Moscow 119991 (Russian Federation); N.S. Kurnakov Institute of General and Inorganic Chemistry Of Russian Academy of Sciences, Leninsky avenue, 31, Moscow 119991 (Russian Federation); Arkhipova, E.A. [M.V. Lomonosov Moscow State University, Department of Chemistry, Leninskie gory, 1-3, Moscow 119991 (Russian Federation); N.S. Kurnakov Institute of General and Inorganic Chemistry Of Russian Academy of Sciences, Leninsky avenue, 31, Moscow 119991 (Russian Federation); Ivanov, A.S.; Maslakov, K.I [M.V. Lomonosov Moscow State University, Department of Chemistry, Leninskie gory, 1-3, Moscow 119991 (Russian Federation); Shen, Z. [Nanyang Technological University, Centre for Disruptive Photonic Technologies, 637371 Singapore (Singapore); Aldoshin, S.M.; Lunin, V.V. [M.V. Lomonosov Moscow State University, Department of Chemistry, Leninskie gory, 1-3, Moscow 119991 (Russian Federation)

    2015-09-15

    Highlights: • Carbon nanoflakes doped with nitrogen were produced by a pyrolytic technique. • Quarternary, pyrrolic and pyridinic types of nitrogen are confirmed by XPS. • Nitrogen content depends on precursor used and temperature processed. • Specific surface area values decrease with increasing of synthesis duration. • N-doped carbon nanoflakes may be suitable for electrochemical applications. - Abstract: Nitrogen doped carbon nanoflakes, which are very important for many electrochemical applications, were synthesized by pyrolysis of nitrogen containing organic compounds over metal oxide template. Acetonitrile, pyridine and butylamine, which are of different volatility were tested as N-containing precursors. Morphology, structure and chemical composition of the as-synthesized materials were investigated by scanning electron microscopy (SEM), high resolution transmission electron microscopy (TEM), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS). It was found that materials are highly defective and consist of a few malformed graphene layers. X-ray photoelectron spectra reflect the dominant graphitic and pyridinic N-bonding configuration. It was also noted that specific surface area depends on the duration and temperature of the reaction. Increase in duration and temperature led to decrease of the specific surface area from 1000 to 160 m{sup 2}/g, 1170 to 210 m{sup 2}/g and 1180 to 480 m{sup 2}/g for acetonitrile, butylamine and pyridine precursors, respectively.

  20. Neighboring Hetero-Atom Assistance of Sacrificial Amines to Hydrogen Evolution Using Pt-Loaded TiO2-Photocatalyst

    Directory of Open Access Journals (Sweden)

    Masahide Yasuda

    2014-05-01

    Full Text Available Photocatalytic H2 evolution was examined using Pt-loaded TiO2-photocatalyst in the presence of amines as sacrificial agents. In the case of amines with all of the carbon attached to the hetero-atom such as 2-aminoethanol, 1,2-diamonoethane, 2-amino-1,3-propanediol, and 3-amino-1,2-propanediol, they were completely decomposed into CO2 and water to quantitatively evolve H2. On the other hand, the amines with both hetero-atoms and one methyl group at the β-positions (neighboring carbons of amino group such as 2-amino-1-propanol and 1,2-diaminopropane were partially decomposed. Also, the photocatalytic H2 evolution using amines without the hetero-atoms at the β-positions such as ethylamine, propylamine, 1-butylamine, 1,3-diaminopropane, 2-propylamine, and 2-butylamine was inefficient. Thus, it was found that the neighboring hetero-atom strongly assisted the degradation of sacrificial amines. Moreover, rate constants for H2 evolution were compared among amines. In conclusion, the neighboring hetero-atom did not affect the rate constants but enhanced the yield of hydrogen evolution.

  1. Secondary organic aerosol formation from primary aliphatic amines with NO3 radical

    Directory of Open Access Journals (Sweden)

    M. E. Erupe

    2008-07-01

    Full Text Available Primary aliphatic amines are an important class of nitrogen containing compounds found to be emitted from automobiles, waste treatment facilities and agricultural animal operations. A series of experiments conducted at the UC-Riverside/CE-CERT Environmental Chamber is presented in which oxidation of methylamine, ethylamine, propylamine, and butylamine with NO3 has been investigated. Very little aerosol formation is observed in the presence of O3 only. However, after addition of NO, and by extension NO3, large yields of aerosol mass loadings (~44% for butylamine are seen. Aerosol generated was determined to be organic in nature due to the small fraction of NO and NO2 in the total signal (<17% for all amines tested as detected by an aerosol mass spectrometer (AMS. We propose a reaction mechanism between carbonyl containing species and the parent amine leading to formation of particulate imine products. These findings can have significant impacts on rural communities and lead to elevated nighttime PM loadings, when significant levels on NO3 exist.

  2. Enhancing hyaluronan pseudoplasticity via 4-(4,6-dimethoxy-1,3,5-triazin-2-yl)-4-methylmorpholinium chloride-mediated conjugation with short alkyl moieties.

    Science.gov (United States)

    Petta, Dalila; Eglin, David; Grijpma, Dirk W; D'Este, Matteo

    2016-10-20

    Hyaluronan (HA) is widely used in the clinical practice and in biomedical research. Through chemical modification, HA shear-thinning properties, essential for injectability and additive manufacturing, can be optimized. In this study, we employed 4-(4,6-dimethoxy-1,3,5-triazin-2-yl)-4-methylmorpholinium chloride (DMTMM) for grafting propylamine and butylamine to HA. A parametric study was performed to identify the optimal reaction conditions. Results showed that DMTMM amidation gives reproducible and accurate control over a range of degrees of substitution (DS) from 1% to 50% and proved reliable to tune viscoelasticity. At DS=3.0% for HA-propylamine and 3.7% for HA-butylamine a maximum for storage modulus and pseudoplasticity was found, whereas above or below this DS, rheological features go back to baseline values of pristine HA. Due to their singular rheological profiles, these derivatives are valuable biomaterials candidates for preparing bioinks and hydrogels for drug delivery and regenerative medicine. PMID:27474602

  3. Role of surface functionalization in ZnO:Fe nanostructures

    International Nuclear Information System (INIS)

    Graphical abstract: - Highlights: • The ex-situ surface functionalization in ZnO:Fe nanostructures by Tri-n-butylamine. • Enhancement of ferromagnetism in ZnO:Fe by amine capping. • The amine capping treatment induced zinc vacancies. - Abstract: In this work, we have explored the effect of surface functionalization in ZnO:Fe nanostructures. The ZnO:Fe nanostructures (NS), synthesized through hydrothermal route, have been surface functionalized (capped) by Tri-n-butylamine (amine). These samples have been characterized by X-ray diffraction (XRD), photoluminescence (PL) and Fourier transform infrared spectroscopy (FTIR). Field emission scanning electron microscopy (FESEM) and transmission electron microscope (TEM) illustrate that obtained nanostructures are high aspect ratio nanorods. Room temperature Mössbauer spectra (MS) of the samples indicate the presence of paramagnetic iron state i.e. Fe3+ in ZnO host. The ferromagnetic (FM) behavior of the samples was investigated by vibrating sample magnetometer (VSM) which shows that the significant enhancement of saturation magnetization in amine capped ZnO:Fe samples. This observed/enhanced ferromagnetism has been explained in terms of modification in the ZnO conduction band. The enhanced ferromagnetism due to surface functionalization has been justified by XRD, PL, FTIR and MS

  4. Pyrolytic synthesis and characterization of N-doped carbon nanoflakes for electrochemical applications

    International Nuclear Information System (INIS)

    Highlights: • Carbon nanoflakes doped with nitrogen were produced by a pyrolytic technique. • Quarternary, pyrrolic and pyridinic types of nitrogen are confirmed by XPS. • Nitrogen content depends on precursor used and temperature processed. • Specific surface area values decrease with increasing of synthesis duration. • N-doped carbon nanoflakes may be suitable for electrochemical applications. - Abstract: Nitrogen doped carbon nanoflakes, which are very important for many electrochemical applications, were synthesized by pyrolysis of nitrogen containing organic compounds over metal oxide template. Acetonitrile, pyridine and butylamine, which are of different volatility were tested as N-containing precursors. Morphology, structure and chemical composition of the as-synthesized materials were investigated by scanning electron microscopy (SEM), high resolution transmission electron microscopy (TEM), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS). It was found that materials are highly defective and consist of a few malformed graphene layers. X-ray photoelectron spectra reflect the dominant graphitic and pyridinic N-bonding configuration. It was also noted that specific surface area depends on the duration and temperature of the reaction. Increase in duration and temperature led to decrease of the specific surface area from 1000 to 160 m2/g, 1170 to 210 m2/g and 1180 to 480 m2/g for acetonitrile, butylamine and pyridine precursors, respectively

  5. Effects of synthetic conditions on the structure and morphology of open-ended vanadium oxide nanotubes and study of their growth mechanism

    Institute of Scientific and Technical Information of China (English)

    WEI Jia; ZHU Ying; ZHANG JingChang

    2007-01-01

    Vanadium oxide nanotubes (Vox-NTs) have been synthesized by using n-butylamine as structure- directing template and V2O5 as precursor under hydrothermal conditions. XRD, FTIR, SEM, TEM, BET and TG-DTA characterizations have been performed to both optimize the synthetic conditions and understand the growth mechanism of Vox-NTs. The results showed that open-ended Vox-NTs were obtained under the optimized conditions (hydrothermal temperature: 150-160°C, hydrothermal time: 5-7 d, the molar ratio of V2O5 to n-butylamine is 1:1) with diameters ranging from about 30 to 100 nm and several micrometers in length. The BET surface area and the desorption cumulative pore volume of pores of the as-synthesized sample were about 27.4609 m2/g and 0.191087 cm3/g, respectively. The result presents that the synthesis of Vox-NTs is controlled by the "rolling" mechanism and temperature is primary driving force for rolling.

  6. Utility of copper(II) oxide as a packed reactor in flow injection assembly for rapid analysis of some angiotensin converting enzyme inhibitors

    Energy Technology Data Exchange (ETDEWEB)

    Emara, Samy; El-Gindy, Alaa; El-Shorbagi, Abdel-Nasser; Hadad, Ghada

    2003-08-11

    A new simple, sensitive, rapid and precise flow injection (FI) procedure based on the formation of copper complexes with some angiotensin converting enzyme (ACE) inhibitors has been developed and evaluated for the analysis of lisinopril (LN), enalapril maleate (EP), ramipril (RP) and perindopril tert-butylamine (PD). In this method, samples were injected into a flowing stream of distilled-deionized water, carried through the packed reactor of CuO for derivatization followed by ultraviolet (UV) detection. The flow rate was 1.5 ml min{sup -1} and column temperature was ambient (25 deg. C). Lisinopril was injected directly into the flowing stream and the detector response was measured at 262 nm. The hydrolysis products of enalapril maleate, ramipril and perindopril tert-butylamine in 0.2N NaOH were injected after neutralization with 1N HCl and the detector response was measured at 272, 265 and 252 nm, respectively. The developed method was successfully applied to the determination of tested drugs in pharmaceutical preparations at a sampling rate of 60 samples h{sup -1} and a recovery near 100% for all compounds.

  7. Simultaneous determination of nine anticoagulant rodenticides in soil and water by LC-ESI-MS.

    Science.gov (United States)

    Hernández, Alma M; Bernal, José; Bernal, José L; Martín, María T; Caminero, Constantino; Nozal, María J

    2013-08-01

    A new and sensitive analytical method is presented to determine nine anticoagulant rodenticide (chlorophacinone, bromadiolone, pindone, diphacinone, warfarin, coumatetralyl, brodifacoum, floucomafen, and difenacoum) residues in water and soil samples by LC-ESI-MS. Rodenticides were extracted from soil using a methanol and ammonium formate 30 mM mixture, while ethyl acetate was employed in the water samples. A Gemini 5 μm C18 column was employed, and a mobile phase comprising a mixture of ammonium formate 30 mM and di-n-butylamine 30 mM in water (pH 3.5), ammonium formate 30 mM and di-n-butylamine 20 mM in water (pH 4.4), ammonium formate 30 mM in water (pH 6.5), and methanol in a gradient elution mode was selected. The method was fully validated and it was found to be selective and precise in terms of linearity and accuracy. Extraction recoveries ranged from 90 to 104% for the compounds studied, while the detection and quantification limits were between 0.09 and 2.2 μg/kg in soil or 0.08 and 1.7 μg/L in water. The method was applied to simultaneously measure these compounds in water and soil samples. PMID:23733735

  8. Secondary organic aerosol formation from primary aliphatic amines with NO3 radical

    Directory of Open Access Journals (Sweden)

    P. J. Silva

    2009-03-01

    Full Text Available Primary aliphatic amines are an important class of nitrogen containing compounds emitted from automobiles, waste treatment facilities and agricultural animal operations. A series of experiments conducted at the UC-Riverside/CE-CERT Environmental Chamber is presented in which oxidation of methylamine, ethylamine, propylamine, and butylamine with O3 and NO3 have been investigated. Very little aerosol formation is observed in the presence of O3 only. However, after addition of NO, and by extension NO3, large aerosol mass yields (~44% for butylamine are seen. Aerosol generated was determined to be organic in nature due to the small fraction of NO and NO2 in the total signal (<1% for all amines tested as detected by an aerosol mass spectrometer (AMS. We propose a reaction mechanism between carbonyl containing species and the parent amine leading to formation of particulate imine products. These findings can have significant impacts on rural communities with elevated nighttime PM loadings, when significant levels of NO3 exist.

  9. Self-Assembled PbSe Nanowire:Perovskite Hybrids

    KAUST Repository

    Yang, Zhenyu

    2015-12-02

    © 2015 American Chemical Society. Inorganic semiconductor nanowires are of interest in nano- and microscale photonic and electronic applications. Here we report the formation of PbSe nanowires based on directional quantum dot alignment and fusion regulated by hybrid organic-inorganic perovskite surface ligands. All material synthesis is carried out at mild temperatures. Passivation of PbSe quantum dots was achieved via a new perovskite ligand exchange. Subsequent in situ ammonium/amine substitution by butylamine enables quantum dots to be capped by butylammonium lead iodide, and this further drives the formation of a PbSe nanowire superlattice in a two-dimensional (2D) perovskite matrix. The average spacing between two adjacent nanowires agrees well with the thickness of single atomic layer of 2D perovskite, consistent with the formation of a new self-assembled semiconductor nanowire:perovskite heterocrystal hybrid.

  10. Porous Silicates Modified with Zirconium Oxide and Sulfate Ions for Alcohol Dehydration Reactions

    Directory of Open Access Journals (Sweden)

    Heriberto Esteban Benito

    2015-01-01

    Full Text Available Porous silicates were synthesized by a nonhydrothermal method, using sodium silicate as a source of silica and cetyltrimethylammonium bromide as a template agent. Catalysts were characterized using thermogravimetric analysis, N2 physisorption, X-ray diffraction, FTIR spectroscopy, pyridine adsorption, potentiometric titration with n-butylamine, scanning electronic microscopy, and transmission electronic microscopy. The surface area of the materials synthesized was greater than 800 m2/g. The introduction of zirconium atoms within the porous silicates increased their acid strength from −42 to 115 mV, while the addition of sulfate ions raised this value to 470 mV. The catalytic activity for the dehydration of alcohols yields conversions of up to 70% for ethanol and 30% for methanol.

  11. Revisiting curcumin chemistry part I: A new strategy for the synthesis of curcuminoids

    Directory of Open Access Journals (Sweden)

    E Venkata Rao

    2011-01-01

    Full Text Available A new strategy for the synthesis of curcuminoids is described involving the reaction of acetylacetone difluroboronite with an aromatic aldehyde in the presence of n-butylamine as catalyst. The new intermediate products, curcuminoid difluroboronites, of symmetrically substituted curcuminoids like curcumin and bisdemethoxycurcumin are stable, can be isolated and hydrolysed with aq. methanol at pH 5.8 to get the curcuminoids of high purity. The method is applicable for unsymmetrical curcuminoids like demethoxycurcumin also with some modification involving column chromatography. The intermediate curcuminoid difluroboronites, as also the natural β-diketone pongamol difluroboronite, prepared for the first time were characterized on the basis of physical and chemical properties and spectroscopic data. The advantage of using borontrifluoride to protect the enol group in acetylacetone over the generally used boric oxide is brought out. The importance of conducting biological activity studies using pure curcuminoids is explained.

  12. Base effects on fabrication of silver nanoparticles embedded silica nanocomposite for surface-enhanced Raman scattering (SERS).

    Science.gov (United States)

    Kang, Homan; Kang, Taegyu; Kim, Seongyong; Kim, Jong-Ho; Jun, Bong-Hyun; Chae, Jinjoo; Park, Juyoung; Jeong, Dae-Hong; Lee, Yoon-Sik

    2011-01-01

    In this paper, we studied on the effect of organic bases in the case of ethylene glycol based fabrication of silver nanoparticles embedded silica nanocomposite (Ag SNC) without heating. Considering their chemical structures, butylamine (BA), ethanolamine (EA), triethanolamine (TEA), tributylamine (TBA), octylamine (OA) and Jeffamine 500 (JA) were used as an organic base. In addition, the effect of the concentrations of AgNO3 and organic bases on the formation of Ag SNC was also examined. In conformity with the characteristics of Ag SNC, SERS signal intensity of benzenethiol on Ag SNC was measured. As a result, the SERS signal intensity of Ag SNCs was strongly dependent on the reaction conditions. Furthermore, when reacted under the best reaction condition with concentrations of AgNO3 and OA, 3 mM and 5 mM, respectively, a large-scale production of Ag SNC was possible under the mild conditions. PMID:21446501

  13. Synthesis of tritiated clenbuterol

    Energy Technology Data Exchange (ETDEWEB)

    Pri-Bar, Ilan; Buchman, Ouri (Israel Atomic Energy Commission, Beersheba (Israel). Nuclear Research Center-Negev)

    1990-12-01

    Tritiated clenbuterol was prepared starting from 4-aminoacetophenone (I) which was selectively brominated to 4-amino-3,5-dibromoacetophenone (II), then to 4-amino-{alpha},3,5-tribromoacetophenone (III) and reacted with tert. butylamine to 4-amino-3,5-dibromo-{alpha}-tert.butylaminoacetophenone (IV). (IV) was dehalogenated and reduced with tritium gas to give 2-(tert.butylamino)-1-(4-amino-(3,5-{sup 3}H)-phenyl)-(1-{sup 3}H)-ethanol (V). This tritiated compound underwent selective aromatic chlorination to give the desired 2-(tert.butylamino)-1-(4-amino-3,5-dichlorophenyl)-(1-{sup 3}H)-ethanol, (ethanol-1-{sup 3}H)clenbuterol, with specific activity of 13.4 Ci/mmol (496 GBq/mmol). (author).

  14. Nuclear spin dipolar relaxation in paramagnetic systems undergoing multiple internal motions

    International Nuclear Information System (INIS)

    A theoretical treatment is proposed for the relaxation induced by the dipolar interaction between two spins separated by several bonds. The influence of the internal and overall molecular motions upon the carbon 13 longitudinal relaxation is discussed on the model of n-butylamine coordinated to a paramagnetic ion having a comparatively long electron spin relaxation time like Mn2+. A computer program has been made to analyze in terms of internal motions and transient conformations the 13C longitudinal dipolar relaxation in flexible and partially rigid molecules. The calculations of 13C relaxation rates have been also applied to the conformational study of less simple molecules undergoind several internal motions as leucine and norleucine coordinated to Gd3+ in aqueous solution. Numerical values are given on electron spin relaxation time and reorientation correlation time for these molecules: Mn, Ni, La, Gd, Dy amino-complexes and leucine and norleucine complexes

  15. Research into aroma changes in irradiated foodstuffs. I.- Studies on Fish; Investigacion de Alteraciones de Aroma en alimentos irradiados. I Estudio sobre Pescado

    Energy Technology Data Exchange (ETDEWEB)

    Barreiro Pinero, R.; Gasco Sanchez, L.; Valverde Garcia, F.

    1972-07-01

    Radiolytic formation of volatile compounds have been investigated in fillets of hake, codfish and bonito gamma-irradiated at a dose range of 0.1-5 Mrads. Analytical methods have been developed by gas chromatography of functional group derivatives: carbonyls as 2,4,-dinitrophenyl hydrazones, primary and secondary amines as N-alkyl benzamides, and thiols as 2,4-dinitrophenyl alkyl thioethers. The main results are as follows: increasing with the integral dose of the whole carbonyls, the most significant components being acetaldehyde, propional dehyde and formaldehyde; no significant variations with the integral dose od the traces of ammonia, methylamine, trimethylamine, ethylamine, diethylamine, propylamine, butylamine and pentylamine found in unirradiated samples; and radiolytic formation of methanethiol and dimethyl disulfide. (Author) 98 refs.

  16. Electrokinetic investigations of solid/organic liquid dispersions: Effects of temperature treatment of the solid and alkyl chain length of adsorbed amines

    Energy Technology Data Exchange (ETDEWEB)

    Jada, A.; Siffert, B.; Eleli-Letsango, J. [Centre de Recherches sur la Physico-Chimie des Surfaces Solides 24, avenue du President Kenedy 68200 MULHOUSE (France)

    1996-01-01

    Zeta potential of two oxides TiO{sub 2} and Al{sub 2}O{sub 3}, dispersed in various organic solvents were measured at room temperature. The inorganic particles were dried at temperatures ranging from 100 to 500{degree}C for several days and were allowed to cool under vacuum just before use. Electrokinetic investigations of TiO{sub 2} particles in n-alkylamine-hexane solutions with various amine chain lengths (C{sub n}H{sub 2n+1}NH{sub 2}, n=1{endash}10) were also done and allowed the determination of the shear plane position in the eventual electric double layer surrounding the solid surface. Furthermore, in order to estimate the thickness {delta} of the electrical double layer surrounding the solid surface, DLVO theory was applied to TiO{sub 2} particles dispersed in n-hexane, in the presence of butylamine. {copyright} {ital 1996 American Institute of Physics.}

  17. Use of modified clay materials in toluene conversion

    International Nuclear Information System (INIS)

    Clay materials, montmorillonite from Maghniya deposits (Algeria), were used as an acidic catalyst in toluene conversion. Toluene disproportionation reaction in gaseous phase was used. These clays were modified by ion exchange with uranyl ions UO22+. The surface acidity of catalysts was determined by the stepwise desorption technique (STD) of probe molecules using butylamine and ammonia. Thus, total acidity and distribution of the acidity strength were determined. The results show that materials presented an appreciable total acidity and catalytic activity in studied reaction. The acidity strength of catalysts due to UO22+ ions was kept at a temperature of 550 C. A relationship was found between the catalytic activity and acidity strength generated by the introduction of uranyl ions in the clay structure. (authors)

  18. Use of modified clay materials in toluene conversion; Utilisation de materiaux a base d'argiles modifiees dans la conversion du toluene

    Energy Technology Data Exchange (ETDEWEB)

    Amokrane, S. [Universite des sciences et de la technologie Houari Boumediene, Departement genie chimique et cryogenie, Alger (Algeria); Nibou, D. [Universite des sciences et de la technologie Houari Boumediene, Departement sciences des materiaux, Alger (Algeria)

    2010-05-15

    Clay materials, montmorillonite from Maghniya deposits (Algeria), were used as an acidic catalyst in toluene conversion. Toluene disproportionation reaction in gaseous phase was used. These clays were modified by ion exchange with uranyl ions UO{sub 2}{sup 2+}. The surface acidity of catalysts was determined by the stepwise desorption technique (STD) of probe molecules using butylamine and ammonia. Thus, total acidity and distribution of the acidity strength were determined. The results show that materials presented an appreciable total acidity and catalytic activity in studied reaction. The acidity strength of catalysts due to UO{sub 2}{sup 2+} ions was kept at a temperature of 550 C. A relationship was found between the catalytic activity and acidity strength generated by the introduction of uranyl ions in the clay structure. (authors)

  19. Research into aroma changes in irradiated foodstuffs. I.- Studies on Fish

    International Nuclear Information System (INIS)

    Radiolytic formation of volatile compounds have been investigated in fillets of hake, codfish and bonito gamma-irradiated at a dose range of 0.1-5 Mrads. Analytical methods have been developed by gas chromatography of functional group derivatives: carbonyls as 2,4,-dinitrophenyl hydrazones, primary and secondary amines as N-alkyl benzamides, and thiols as 2,4-dinitrophenyl alkyl thioethers. The main results are as follows: increasing with the integral dose of the whole carbonyls, the most significant components being acetaldehyde, propional dehyde and formaldehyde; no significant variations with the integral dose od the traces of ammonia, methylamine, trimethylamine, ethylamine, diethylamine, propylamine, butylamine and pentylamine found in unirradiated samples; and radiolytic formation of methanethiol and dimethyl disulfide. (Author) 98 refs

  20. Determination of regioselectivity in ring opening of tert-butylaziridinones by a combination of (15)N labeling and electrospray ionization-ion trap mass spectrometry.

    Science.gov (United States)

    Talaty, E R; Van Stipdonk, M J; Hague, M J; Provenzano, F A; Boese, C A

    2002-01-01

    The ring opening of 1,3-di-tert-butylaziridinone by tert-butylamine and aniline was investigated by using electrospray ionization and collision-induced dissociation in an ion trap mass spectrometer in conjunction with (15)N labeling of the two amine nucleophiles. Using the MS(n) capabilities of the ion trap instrument, we were able to monitor the retention of the (15)N label through successive fragmentation steps. Both amines exhibited a remarkable degree of selectivity in that they both cleaved exclusively the 1,3-bond (the alkyl-nitrogen bond). This result is in contrast to that obtained previously with methylamine, which cleaved just the opposite bond, namely, the 1,2-bond (the acyl-nitrogen bond). These contrasting results could not have been predicted by previously published guidelines. PMID:11813308

  1. Analysis of dibutylphosphoric acid (DBP) in degraded solvent by utilizing gas chromatograph-mass spectrometry

    International Nuclear Information System (INIS)

    In JAEA, a washing process of tributylphosphate (TBP) in the Purex reprocessing have been investigated by means of n-butylamine oxalate as a washing reagent, which is decomposable by incineration or electrolysis. The concentration of the dibutylphosphoric acid (DBP) in organic and aqueous phase has been determined by an ion-chromatography. In this analytical method, however; we found out that the quantitative analysis for DBP exhibited poor reproducibility because of low sensitivity for DBP. Here we report a new analytical method for DBP by means of a gas chromatograph-mass spectrometry (GC-MS). From our investigation, silylation of DBP was efficient to improve the sensitivity and the reproducibility of the quantitative analysis for DBP. Moreover, we found out that the silylation was effective for the analysis of monobutylphosphoric (MBP). (author)

  2. OPTIMIZATION OF THE AMINOREDUCTONE FORMATION IN THE MAILLARD REACTION

    Directory of Open Access Journals (Sweden)

    Vu Thu TRANG

    2015-03-01

    Full Text Available The optimization of process parameters for the production of aminoreductone (AR, a bioactive product formed in the initial stage of Maillard reaction was investigated using response surface methodology (RSM and Box-Behnken design technique. The optimum process conditions were determined by analyzing the response surface of three-dimensional surface plot and solving the regression model equation with the Design Expert software. The optimum conditions include: heating time of 15 min, temperature of 112.85°C, pH of 8.33 and buffer concentration of 0.53 which were used to obtain the maximum AR yield (76.6 mM in the model solution of lactose (0.3 M and butylamine (0.3 M.

  3. Synthesis of symmetrical 2,2',4,4'-tetrasubstituted [4,4'-bithiazole]-5,5'(4H,4'H)-diones and their reactions with some nucleophiles

    DEFF Research Database (Denmark)

    Andersen, Kenneth K.; Bray, Diana D.; Kjær, Anders;

    1997-01-01

    ,4'-dibenzyl-[4,4'-bithiazole]-5,5'(4H,4'H)-dione were treated with nocleophiles. The former gave imide derivatives of alfa,alfa-dehydrodimeric amino acids when the nucleophile was L-alanine ethyl ester or 1-butylamine. The structure of one of the reaction products, (4R*,5R*)-2,5-diphenyl-2-thiazoline-4......-carboxylic acid and piperidylamide, was established by X-ray crystallography. Treatment of stereoisomeric mixtures of 2,2'-diethoxy-4,4'-bithiazolones with HCl in benzene gave the corresponding racemic and meso bis-(N-carboxythioanhydride)s. A stereoisomeric mixture of the bis(N-carboxythioanhydride)s of...... leucine treated with glycine ethyl ester gave a bicyclic derivative of the alfa,alfa-dehydrodimeric amino acid....

  4. Oxygen gas permeability in water and mechanical properties of poly(n-butylamino) (di-allylamino) phosphazene membranes cured with the irradiation

    International Nuclear Information System (INIS)

    Poly(n-butylamino) (di-allylamino)phosphazenes were prepared by the reaction of (NPCl2)n with n-butylamine and di-allylamine. After the membranes were prepared by the casting method, they were irradiated by ultraviolet electron beam, 60Co γ-rays. It was found from Fourier transform-infrared data that the CH=CH2/N-H ratios of the irradiated membranes decreased with increasing dose. Also, the membrane did not dissolve in tetrahydrofuran or other organic solvents. This supported the idea that the CH=CH2 bond was cleaved by the irradiation and the cross-linking occurred intermolecularly. Oxygen gas permeability values, Dk, of the irradiated membrane were determined from oxygen permeability and mechanical properties were determined with a Tensilon instrument. Dk values decreased with increasing Young's modulus in the case of low concentrations of di-allylamine. (author)

  5. Equilibria and kinetics for pH-dependent axial ligation of bromomethyl(aquo)cobaloxime by aliphatic amine ligands

    Indian Academy of Sciences (India)

    M Bhoopal; N Ravi Kumar Reddy; S Satyanarayana

    2003-04-01

    Kinetics and equilibria of axial ligation of bromomethyl(aquo) cobaloxime by a series of straight chain primary amines (methylamine, ethylamine, propylamine, butylamine, pentylamine, hexylamine), cycloamines (cyclopentylamine, cyclohexylamine, cycloheptylamine) and secondary amines (N,N-dimethylamine, N,N-diethylamine) have been measured as functions of pH by spectrophotometric technique in aqueous solution, ionic strength 1 M (KCl) at 25°C. The rate of substitution of H2O varies with the Ka of incoming ligand, thus establishing nucleophilic participation of the ligand in the transition state. Binding and kinetic data are interpreted based on the basicity and steric influence of the entering ligand. To compare the rate constants of the entering ligands, pH independent second-order rate constants (on) are calculated.

  6. Synthesis and characterization of nano/micro structured crystalline germanium dioxide with novel morphology

    Institute of Scientific and Technical Information of China (English)

    WANG XiaoYan; DUAN Lian; DONG GuiFang; WEI Peng; WANG Wei; WANG LiDuo; QIU Yong

    2009-01-01

    Nano/micro-structured germanium oxide (GeO2) was prepared using GeCl4 and KOH by a simple solution method in alkalic alcoholic solution.Different morphologies of GeO2 were obtained by changing the reaction conditions.The effects of the reaction time,the concentration of the reactants,the reaction temperature and the dispersant upon the morphology of the deposited GeO2 have been investigated.The products were detected by X-ray diffraction (XRD),atomic force microscope (AFM),scanning electron microscope (SEM) and transmission electron microscope (TEM).Novel cross-like structures were obtained by using n-butylamine as the dispersant.The formation of the cross-like structures has been discussed and a solution-liquid-solid (SLS) mechanism was proposed.

  7. Amine effect on lanthanum and scandium extraction with caproic and α-bromocaproic acids

    International Nuclear Information System (INIS)

    Lanthanum and scandium extraction with 1 mol. chloroform solutions of n-caproic and α-bromocaproic acids in the presence of benzyl amine and n-butyl-amine, pyridine and 2-aminopyridine is investigated. Composition of carboxylates in organic phase is determined. It is established that introduction of strong organic nitrogen-containing bases-n-butylamine, benzyl amine-extends considerably pH range at which the mentioned metals are extracted into chloroform quantitatively. The effect of citrate- and tartrate- ions upon the extraction of capronates and aminocapronates of scandium and lanthanum is investigated. To separate lanthanum and scandium from interfering elements investigated is extraction of magnesium, calcium, strontium and barium by the mixtures of the above carboxylic acids and amines. Developed are methods of extraction separation of scandium and lanthanum from alkaline-earth elements taking solutions of artificial mixtures as examples

  8. Isopropylation of benzene with 2-propanol over substituted large pore aluminophosphate-based molecular sieves

    Indian Academy of Sciences (India)

    K Joseph Antony Raj; V R Vijayaraghavan

    2004-03-01

    Large pore aluminophosphate-based molecular sieves like AlPO4-5, MAPO-5, MnAPO-5 and ZAPO-5 were synthesised hydrothermally using triethylamine as a structure directing agent. These materials were characterised by X-ray diffraction (XRD), 27Al and 31P MAS-NMR, ICP-MS, -butylamine- TPD, BET and SEM. The catalytic performance of these materials was tested for isopropylation of benzene with 2-propanol at 250, 300, 350 and 400°C. The products were cumene, -DIPB (-diisopropylbenzene) and -DIPB (-diisopropylbenzene). MnAPO-5 was found to be more active than the other catalysts. Maximum conversion (20%) was noted at 350°C over MnAPO-5. The selectivity to DIPB was found to decrease with time on stream but the selectivity to cumene showed an increase after 3 h of time on stream.

  9. Electroless Deposition and Surface-Enhanced Raman Scattering Application of Palladium Thin Films on Glass Substrates

    International Nuclear Information System (INIS)

    In this work, we describe a very simple electroless deposition method to prepare moderate-SERS-active nanostructured Pd films deposited on the glass substrates. To the best of our knowledge, this is the first report on the one-pot electroless method to deposit Pd nanostructures on the glass substrates. This method only requires the incubation of negatively charged glass substrates in ethanol-water mixture solutions of Pd(NO3)2 and butylamine at elevated temperatures. Pd films are then formed exclusively and evenly on glass substrates. Due to the aggregated structures of Pd, the SERS spectra of benzenethiol and organic isonitrile could be clearly identified using the Pd-coated glass as a SERS substrate. This one-step fabrication method of Pd thin film on glass is cost-effective and suitable for the mass production

  10. Electroless Deposition and Surface-Enhanced Raman Scattering Application of Palladium Thin Films on Glass Substrates

    Energy Technology Data Exchange (ETDEWEB)

    Shin, Kuan Soo; Cho, Young Kwan [Soongsil Univ., Seoul (Korea, Republic of); Kim, Kyung Lock; Kim, Kwan [Seoul National Univ., Seoul (Korea, Republic of)

    2014-03-15

    In this work, we describe a very simple electroless deposition method to prepare moderate-SERS-active nanostructured Pd films deposited on the glass substrates. To the best of our knowledge, this is the first report on the one-pot electroless method to deposit Pd nanostructures on the glass substrates. This method only requires the incubation of negatively charged glass substrates in ethanol-water mixture solutions of Pd(NO{sub 3}){sub 2} and butylamine at elevated temperatures. Pd films are then formed exclusively and evenly on glass substrates. Due to the aggregated structures of Pd, the SERS spectra of benzenethiol and organic isonitrile could be clearly identified using the Pd-coated glass as a SERS substrate. This one-step fabrication method of Pd thin film on glass is cost-effective and suitable for the mass production.

  11. Preparation of selective magnetic dispersive solid-phase sorbent and its application for recognition clenbuterol from bovine urine.

    Science.gov (United States)

    Qiao, Fengxia; Wang, Mengge

    2016-04-01

    A new kind of selective magnetic dispersive solid-phase sorbent based on multiple Fe3O4 nanospheres as the core structure and molecular imprinted material as the shell structure was synthesized with tert-butylamine and 2-chloroaniline as the templates. The obtained multicore-shell-structured sorbent was spherical (diameter distribution 25-90μm) with porous morphologies, thus incorporating strong magnetic properties and specific molecular recognition coupled with rapid adsorption and dynamic equilibrium. The sorbent was applied for rapid and selective screening of clenbuterol (CLB) in bovine urine samples. Good linearity was obtained in the range 1.25-200ngmL(-1) with the average recovery at three spiked levels ranging from 91.4% to 105.3%. The proposed method significantly improved the purification and extraction efficiency of CLB in urine samples and eliminated the effect of template leakage during quantitative analysis. PMID:26937590

  12. Synthesis of tritiated clenbuterol

    International Nuclear Information System (INIS)

    Tritiated clenbuterol was prepared starting from 4-aminoacetophenone (I) which was selectively brominated to 4-amino-3,5-dibromoacetophenone (II), then to 4-amino-α,3,5-tribromoacetophenone (III) and reacted with tert. butylamine to 4-amino-3,5-dibromo-α-tert.butylaminoacetophenone (IV). (IV) was dehalogenated and reduced with tritium gas to give 2-(tert.butylamino)-1-(4-amino-[3,5-3H]-phenyl)-[1-3H]-ethanol (V). This tritiated compound underwent selective aromatic chlorination to give the desired 2-(tert.butylamino)-1-(4-amino-3,5-dichlorophenyl)-[1-3H]-ethanol, [ethanol-1-3H]clenbuterol, with specific activity of 13.4 Ci/mmol (496 GBq/mmol). (author)

  13. Solution-phase synthesis of nanomaterials at low temperature

    Institute of Scientific and Technical Information of China (English)

    2009-01-01

    This paper reviews the solution-phase synthesis of nanoparticles via some routes at low temperatures, such as room temperature route, wave-assisted synthesis (γ-irradiation route and sonochemical route), directly heating at low temperatures, and hydrothermal/solvothermal methods. A number of strategies were developed to control the shape, the size, as well as the dispersion of nanostructures. Using diethylamine or n-butylamine as solvent, semiconductor nanorods were yielded. By the hydrothermal treatment of amorphous colloids, Bi2S3 nanorods and Se nanowires were obtained. CdS nanowires were prepared in the presence of polyacrylamide. ZnS nanowires were obtained using liquid crystal. The polymer poly (vinyl acetate) tubule acted as both nanoreactor and template for the CdSe nanowire growth. Assisted by the surfactant of sodium dodecyl benzenesulfonate (SDBS), nickel nanobelts were synthesized. In addition, Ag nanowires, Te nanotubes and ZnO nanorod arrays could be prepared without adding any additives or templates.

  14. Layered metal uranyl phosphates

    International Nuclear Information System (INIS)

    HUO2PO4·4H2O (HUP) forms a laminar intercalate with butylamine, c = 29.30(5) angstrom, which accepts cationic metals in exchange for the n-butylammonium ions. Hydrated uranyl metal phosphates M(UO2PO4)2·nH2O (M=Mn,Co,Ni,Cu,Zn,Cd) are obtained by ionic exchange and were studied by thermal analysis and X-ray diffraction. The tetragonal structures of all these product compounds are derived from HUP. The diffuse electronic reflectance spectra of every sample show characteristic UO22+ absorption bands. In the spectra of the Co, Ni and Cu phosphates there are other bands in the 500-800 nm zone compatible with their observed aquocation transitions

  15. [Synthesis of particle-free silver conductive ink and investigation of fabrication of conductive film by printing].

    Science.gov (United States)

    Nie, Xiao-Lei; Wang, Hong; Zou, Jing

    2012-11-01

    Particle-free conductive ink was prepared, taking silver citrate as conductive metal precursor, sec-butylamine as complexing agent and ethanol as media adjusting the viscosity and wettability. The ink could be printed on PET substrate by gravure printing, and silver conductive film with high electrical conductivity was obtained after thermal treated at low temperature. Silver citrate, silver citrate based conductive ink and silver conductive film were characterized with EDS, STA, IR, XRD, SEM and four point probe method. The results of STA showed that the mass of the conductive ink came to constant at 132 degrees C which is much lower than that of silver citrate (210 degrees C); the results of SEM and XRD showed that the silver conductive film cured at 150 C was constituted by compact silver nano particles with high purity; the result of four point probe method showed that its sheet resistance was 1.83 omega x square(-1). PMID:23387185

  16. Thermodynamic and spectroscopic investigations of aluminas and thermodynamic studies of other solid systems

    Energy Technology Data Exchange (ETDEWEB)

    Healy, M.H.

    1987-01-01

    This dissertation describes thermodynamic studies of the adsorption of a variety of liquid and gaseous bases on to a variety of solid acids, such as transition aluminas, a sulfonic acid resin (Dowex), graphite and anthracite coal. Fourier transform infrared spectroscopy studies were also conducted to identify the type, strength, and quantity of acid sites present on two transition aluminas, delta-theta and kappa. Heats of immersion of delta-theta and kappa aluminas into a variety of adsorbates of differing base strengths and geometries were obtained to quantify heterogeneous Lewis acid-base behavior. An in situ infrared spectroscopy investigation was conducted using four basic adsorbates to identify the acidic sites present on delta-theta and kappa aluminas. For two adsorbates, pyridine and 2,6-lutidine, adsorption studies were conducted between 298 and 983 K and at adsorbate pressures spanning from 1.33 Pascal (Pa) to 1.33 kPa. The adsorption of acetonitrile and n-butylamine was conducted at 298K using adsorbate pressures ranging from 0.66 Pa to 8.65 kPa. With all of the adsorbates a Lewis acid coordination site, designated as an outer or weaker site, and hydrogen-bonded complexes are identified. Broensted acid coordination is detected only when a strongly basic adsorbate, n-butylamine, is employed as the probe molecule. The strength of the sites, as quantified with pyridine is similar on both aluminas; however, with acetonitrile, a stronger coordination complex is formed on kappa alumina than on delta-theta alumina. The environment surrounding the acid site affects the adsorption of 2,6-lutidine; although it is a stronger base towards protonic acids than pyridine and might be expected to interact more strongly with alumina, only a weakly bound species is formed.

  17. In situ growth BaTiO3 nanocubes and their superlattice from an aqueous process

    Science.gov (United States)

    Dang, Feng; Mimura, Kenichi; Kato, Kazumi; Imai, Hiroaki; Wada, Satoshi; Haneda, Hajime; Kuwabara, Makoto

    2012-02-01

    Ordered aggregated BaTiO3 nanocubes with a narrow size distribution were obtained in an aqueous process by using bis(ammonium lactate) titanium dihydroxide (TALH) as Ti source in the presence of oleic acid and tert-butylamine. Kinetics of the formation of BaTiO3 nanocubes indicated that an in situ growth mechanism was dominant and the superlattice of nanocubes formed in situ through the growth of BaTiO3 nanoparticles in Ti-based hydrous gel. The size and morphology of nanocubes were controlled by tuning the concentration and molar ratio of surfactants. A novel growth model dependant on the structure of Ti precursor for the formation and morphology control of BaTiO3 nanocubes and their superlattice was demonstrated.Ordered aggregated BaTiO3 nanocubes with a narrow size distribution were obtained in an aqueous process by using bis(ammonium lactate) titanium dihydroxide (TALH) as Ti source in the presence of oleic acid and tert-butylamine. Kinetics of the formation of BaTiO3 nanocubes indicated that an in situ growth mechanism was dominant and the superlattice of nanocubes formed in situ through the growth of BaTiO3 nanoparticles in Ti-based hydrous gel. The size and morphology of nanocubes were controlled by tuning the concentration and molar ratio of surfactants. A novel growth model dependant on the structure of Ti precursor for the formation and morphology control of BaTiO3 nanocubes and their superlattice was demonstrated. Electronic supplementary information (ESI) available. See DOI: 10.1039/c2nr11594h

  18. Aliphatic amines in Antarctic CR2, CM2, and CM1/2 carbonaceous chondrites

    Science.gov (United States)

    Aponte, José C.; McLain, Hannah L.; Dworkin, Jason P.; Elsila, Jamie E.

    2016-09-01

    Meteoritic water-soluble organic compounds provide a unique record of the processes that occurred during the formation of the solar system and the chemistry preceding the origins of life on Earth. We have investigated the molecular distribution, compound-specific δ13C isotopic ratios and enantiomeric compositions of aliphatic monoamines present in the hot acid-water extracts of the carbonaceous chondrites LAP 02342 (CR2), GRA 95229 (CR2), LON 94101 (CM2), LEW 90500 (CM2), and ALH 83100 (CM1/2). Analyses of the concentration of monoamines in these meteorites revealed: (a) the CR2 chondrites studied here contain higher concentrations of monoamines relative to the analyzed CM2 chondrites; (b) the concentration of monoamines decreases with increasing carbon number; and (c) isopropylamine is the most abundant monoamine in these CR2 chondrites, while methylamine is the most abundant amine species in these CM2 and CM1/2 chondrites. The δ13C values of monoamines in CR2 chondrite do not correlate with the number of carbon atoms; however, in CM2 and CM1/2 chondrites, the 13C enrichment decreases with increasing monoamine carbon number. The δ13C values of methylamine in CR2 chondrites ranged from -1 to +10‰, while in CM2 and CM1/2 chondrites the δ13C values of methylamine ranged from +41 to +59‰. We also observed racemic compositions of sec-butylamine, 3-methyl-2-butylamine, and sec-pentylamine in the studied carbonaceous chondrites. Additionally, we compared the abundance and δ13C isotopic composition of monoamines to those of their structurally related amino acids. We found that monoamines are less abundant than amino acids in CR2 chondrites, with the opposite being true in CM2 and CM1/2 chondrites. We used these collective data to evaluate different primordial synthetic pathways for monoamines in carbonaceous chondrites and to understand the potential common origins these molecules may share with meteoritic amino acids.

  19. CCN activity of aliphatic amine secondary aerosol

    Directory of Open Access Journals (Sweden)

    X. Tang

    2014-01-01

    Full Text Available Aliphatic amines can form secondary aerosol via oxidation with atmospheric radicals (e.g. hydroxyl radical and nitrate radical. The particle composition can contain both secondary organic aerosol (SOA and inorganic salts. The fraction of organic to inorganic materials in the particulate phase influences aerosol hygroscopicity and cloud condensation nuclei (CCN activity. SOA formed from trimethylamine (TMA and butylamine (BA reactions with hydroxyl radical (OH is composed of organic material of low hygroscopicity (single hygroscopicity parameter, κ ≤ 0.25. Secondary aerosol formed from the tertiary aliphatic amine (TMA with N2O5 (source of nitrate radical, NO3, contains less volatile compounds than the primary aliphatic amine (BA aerosol. TMA + N2O5 form semi-volatile organics in low RH conditions that have κ ~ 0.20, indicative of slightly soluble organic material. As RH increases, several inorganic amine salts are formed as a result of acid-base reactions. The CCN activity of the humid TMA-N2O5 aerosol obeys Zdanovskii, Stokes, and Robinson (ZSR ideal mixing rules. Higher CCN activity (κ > 0.3 was also observed for humid BA+N2O5 aerosols compared with dry aerosol (κ ~ 0.2, as a result of the formation of inorganic salts such as NH4NO3 and butylamine nitrate (C4H11N · HNO3. Compared with TMA, BA+N2O5 reactions produce more volatile aerosols. The BA+N2O5 aerosol products under humid experiments were found to be very sensitive to the temperature within the stream-wise continuous flow thermal gradient CCN counter. The CCN counter, when set above a 21 °C temperature difference, evaporates BA+N2O5 aerosol formed at RH ≥ 30%; κ ranges from 0.4 to 0.7 and is dependent on the instrument supersaturation (ss settings. The aerosol behaves non-ideally, hence simple ZSR rules cannot be applied to the CCN results from the primary aliphatic amine system. Overall, aliphatic amine aerosol systems κ ranges from 0.2 < κ < 0.7. This work indicates that

  20. Nitrosamine occurrence at Korean surface water using an analytical method based on GC/LRMS.

    Science.gov (United States)

    Kim, Gyung-A; Son, Hee-Jong; Kim, Chang-Won; Kim, Seung-Hyun

    2013-02-01

    The survey of nitrosamine occurrence at Korean surface water of Nakdong river is conducted in this study. For this purpose, the nitrosamine analytical method based on more affordable GC/LRMS (low resolution mass spectrometry) has been developed. According to the study results, six nitrosamine compounds (NDEA as N-nitrosomethylethylamine, NDPA as N-nitrosodi-n-propylamine, NDMA as N-nitrosodimethylamine, NMEA as N-nitrosomethylethylamine, NDBA as N-nitrosodi-n-butylamine, and NDPHA as N-nitrosodiphenylamine) were detected at the Nakdong river. Among these, NDEA and NDPA are the most important compounds in terms of the nitrosamine contamination of the Nakdong river. The detected concentration of NDEA exceeded the CDHCS (California Department of Health Care Services) response level of 100 ng/L at several sites. The detected concentration of NDPA approached the response level (500 ng/L) at a few sites. When all nitrosamine concentrations were summed up, the maximum concentration of 735.7 ng/L was detected at the Nakdong river. An equation describing a decrease in total nitrosamine concentration along downstream sampling sites was proposed in this study. The equation can be used to predict the downstream nitrosamine contamination at the Nakdong river. Among various water quality parameters, T-N showed a good correlation with total nitrosamine concentration. PMID:22569988

  1. Ag-deposited silica-coated Fe3O4 magnetic nanoparticles catalyzed reduction of p-nitrophenol

    International Nuclear Information System (INIS)

    In this paper, a novel approach was successfully developed for advanced catalyst Ag-deposited silica-coated Fe3O4 magnetic nanoparticles, which possess a silica coated magnetic core and growth active silver nanoparticles on the outer shell using n-butylamine as the reductant of AgNO3 in ethanol. The as-synthesized nanoparticles have been characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM), energy dispersive X-ray analysis (EDX), Fourier transform infrared spectra (FT-IR), vibration sample magnetometer (VSM), and have been exploited as a solid phase catalyst for the reduction of p-nitrophenol in the presence of NaBH4 by UV-vis spectrophotometry. The obtained products exhibited monodisperse and bifunctional with high magnetization and excellent catalytic activity towards p-nitrophenol reduction. As a result, the as-obtained nanoparticles showed high performance in catalytic reduction of p-nitrophenol to p-aminophenol with conversion of 95% within 14 min in the presence of an excess amount of NaBH4, convenient magnetic separability, as well as remained activity after recycled more than 6 times. The Fe3O4-SiO2-Ag functional nanostructure could hold great promise for various catalytic reactions.

  2. Variations in product in reactions of naphthoquinone with primary amines

    Directory of Open Access Journals (Sweden)

    Barooah Nilotpal

    2007-03-01

    Full Text Available Abstract Reaction of 1,2-naphthoquinone with primary amines gives a 2-amino-1,4-naphthoquinone derivative which is equivalent to 1,2 to 1,4 carbonyl transposition. For example the reaction of 1,2-naphthoquinone with 4-methoxyaniline gives 2-(4-methoxyanilino-naphthoquinone-1,4-(4-methoxyanil (1 and with n-butylamine gives 2-(butylamino-naphthoquinone-1,4-butylimine (2 respectively. The compounds 1 and 2 are characterized by X-ray crystallography; they have hydrogen-bonded dimeric structures. Similar reaction of 1,4-naphthoquinone with 3-picolylamine and 4-picolylamine gives the corresponding 2-amino 1,4-naphthoquinones; two products are characterized by X-ray crystallography. The reaction of 1,4-naphthoquinone with 4-aminothiophenol and 1,4-naphthoquinone with 4-aminophenol are compared. The former leads to C-S and the latter to C-N bond formation. The reaction of 1,4-naphthoquinone with 4-aminothiophenol in an NMR tube is studied to explain that 2-(4-anilinothiolato 1,4-naphthoquinone derivative to be the sole product in the reaction.

  3. X-ray crystallographic, FT-IR and NMR studies as well as anticancer and antibacterial activity of the salt formed between ionophore antibiotic Lasalocid acid and amines

    Science.gov (United States)

    Huczyński, Adam; Rutkowski, Jacek; Wietrzyk, Joanna; Stefańska, Joanna; Maj, Ewa; Ratajczak-Sitarz, Małgorzata; Katrusiak, Andrzej; Brzezinski, Bogumil; Bartl, Franz

    2013-01-01

    Two new complexes of the ionophore antibiotic Lasalocid acid (LAS) with phenylamine (PhA) and butylamine (BuA) were synthesized and their molecular structures were studied using single crystal X-ray diffraction and spectroscopic methods. In the solid state both amines are protonated and all NH3+ protons are hydrogen bonded to etheric, hydroxyl and carboxylic oxygen atoms of the LAS anion. In chloroform solutions the structure observed in the crystal of LAS-BuA complex is preserved and an equilibrium between the LAS-PhA complex and dissociated Lasalocid acid and phenylamine is observed. In vitro antimicrobial tests of the complexes showed a significant activity towards some strains of Gram-positive bacteria. For the first time Lasalocid acid and its complexes with amines were tested in vitro for cytotoxic activity against human cancer cell lines: A-549 (lung), MCF-7 (breast), HT-29 (colon) and mouse cancer cell line P-388 (leukemia). We found that LAS and its complexes are strong cytotoxic agents towards all tested cell lines. The cytostatic activity of the compounds studied is greater than that of cisplatin, indicating that Lasalocid and its complexes are promising candidates for new anticancer drugs.

  4. MOCVD of hexagonal boron nitride thin films on Si(100) using new single source precursors

    CERN Document Server

    Boo, J H; Yu, K S; Kim, Y S; Kim, Y S; Park, J T

    1999-01-01

    We have been carried out the growth of hexagonal boron nitride (h-BN) thin films on Si(100) substrates by low pressure metal-organic chemical vapor deposition (LPMOCVD) method using triethylborane tert-butylamine complex (TEBTBA), Et sub 3 BNH sub 2 ( sup t Bu), and triethylborane isopropylamine complex (TEBIPA), Et sub 3 BNH sub 2 ( sup t Pr) as a new single molecular precursors in the temperature range of 850 approx 1000 .deg. C. polycrystalline, crack-free h-BN film was successfully grown on Si(100) substrate at 850 .deg. C using TEBTBA. This growth temperature is very lower than those in previous reports. Carbon-rich polycrystalline BN was also obtained at 900 .deg. C from TEBIPA. With increasing substrate temperature to 1000 .deg. C, however, BC sub 4 N-like species are strongly formed along with h-BN and the BN films obtained from both TEBTBA and TEBIPA but almost polycrystalline. To our best knowledge, this is the first report of the growth of h-BN films formed with the new single source precursors of ...

  5. Synthesis and Antimicrobial Activities of Some Novel Quinoxalinone Derivatives

    Directory of Open Access Journals (Sweden)

    Y. A. Ammar

    2000-06-01

    Full Text Available Condensation of 4-benzoyl-1,2-phenylenediamine with sodium pyruvate in acetic acid furnished two products which were identified as 6-benzoyl and 7-benzoyl-3-methyl-2(1Hquinoxalinones (1a,b. Fusion of 1a with aromatic aldehydes furnished the styryl derivatives 2a-c. Alkylation of 1a,b with dimethyl sulphate or ethyl chloroacetate produced the N-alkyl derivatives 3a,b and 4a,b. Hydrazinolysis of the ester derivative 4a with hydrazine hydrate afforded the hydrazide derivative 5 which underwent condensation with aldehydes to give the corresponding hydrazone derivatives 6a,b. In addition, chlorination of 1a with thionyl chloride afforded the 2-chloro derivative 7 which was subjected to reaction with sodium azide and n-butylamine to yield the corresponding tetrazolo (8 and n-butylamino (9 derivatives, respectively. The structures of the compounds prepared were confirmed by analytical and spectral data. Also, some of the synthesized compounds were screened for antimicrobial activity.

  6. Electrochemical characterization of platinum nanoparticles stabilized by amines

    Energy Technology Data Exchange (ETDEWEB)

    Ramirez-Meneses, E., E-mail: esthervincent@yahoo.co [Centro de Investigacion en Ciencia Aplicada y Tecnologia Avanzada, CICATA-IPN Unidad Altamira, Km 14.5 Carretera Tampico-Puerto Industrial, C.P. 89600 Altamira, Tamaulipas (Mexico); Dominguez-Crespo, M.A. [Centro de Investigacion en Ciencia Aplicada y Tecnologia Avanzada, CICATA-IPN Unidad Altamira, Km 14.5 Carretera Tampico-Puerto Industrial, C.P. 89600 Altamira, Tamaulipas (Mexico); Montiel-Palma, V. [Centro de Investigaciones Quimicas, Universidad Autonoma del Estado de Morelos, Av. Universidad 1001, Colonia Chamilpa, C.P. 62201 Cuernavaca, Morelos (Mexico); Chavez-Herrera, V.H. [Centro de Investigacion en Ciencia Aplicada y Tecnologia Avanzada, CICATA-IPN Unidad Altamira, Km 14.5 Carretera Tampico-Puerto Industrial, C.P. 89600 Altamira, Tamaulipas (Mexico); Gomez, E. [Instituto de Quimica-Universidad Nacional Autonoma de Mexico, Ciudad Universitaria, C.P. 04510 Mexico, D.F. (Mexico); Hernandez-Tapia, G. [Gerencia de Catalizadores y Proceso, Instituto Mexicano del Petroleo, Eje Central Lazaro Cardenas norte 152, 07730 Mexico, D.F. (Mexico)

    2009-08-26

    In this work we present the synthesis by Chaudret approach of Pt nanoparticles stabilized by primary amine (-NH{sub 2}) compounds. Their electrochemical performance as cathodes in low temperature polymer electrolite fuel cells on the oxygen reduction reaction (ORR) is also presented. Transmission electron microscopy (TEM) images of the samples show Pt nanostructures with particle size varying from 10 to 100 nm depending on the kind of the stabilizer used during the catalyst preparation. In some cases well-dispersed isolated platinum nanoparticles were observed. The activity of the dispersed catalysts (Pt/C) with respect to the ORR was investigated using steady state polarization measurements. The kinetic parameters showed that although no significant differences between the Tafel slopes of the Pt catalysts exist, transfer coefficients and exchange current densities show higher activities when the Pt nanoparticles were stabilized by tert-butylamine (TBA). The performance with respect to the ORR of the Pt/C catalyst on vulcan carbon substrate is active and comparable to that reported in the literature for state-of-art electrocatalysts.

  7. Electrochemical characterization of platinum nanoparticles stabilized by amines

    International Nuclear Information System (INIS)

    In this work we present the synthesis by Chaudret approach of Pt nanoparticles stabilized by primary amine (-NH2) compounds. Their electrochemical performance as cathodes in low temperature polymer electrolite fuel cells on the oxygen reduction reaction (ORR) is also presented. Transmission electron microscopy (TEM) images of the samples show Pt nanostructures with particle size varying from 10 to 100 nm depending on the kind of the stabilizer used during the catalyst preparation. In some cases well-dispersed isolated platinum nanoparticles were observed. The activity of the dispersed catalysts (Pt/C) with respect to the ORR was investigated using steady state polarization measurements. The kinetic parameters showed that although no significant differences between the Tafel slopes of the Pt catalysts exist, transfer coefficients and exchange current densities show higher activities when the Pt nanoparticles were stabilized by tert-butylamine (TBA). The performance with respect to the ORR of the Pt/C catalyst on vulcan carbon substrate is active and comparable to that reported in the literature for state-of-art electrocatalysts.

  8. Facile synthesis of monodisperse of hollow mesoporous SiO2 nanoparticles and in-situ growth of Ag nanoparticles for antibacterial.

    Science.gov (United States)

    Xu, Peng; Liang, Juan; Cao, Xiaoyong; Tang, Jingen; Gao, Juan; Wang, Liying; Shao, Wei; Gao, Qinwei; Teng, Zhaogang

    2016-07-15

    Monodispersed hollow mesoporous silica nanoparticles (HMSNs) are successfully synthesized via a facile dual template method, in which poly(styrene-co-methyl methacrylate-co-methacrylic acid) (PS-PMMA-PMAA) particles are used as hard template for producing the hollow structure and cetyltrimethylammonium bromide (CTAB) used for introducing the mesopores in the silica shells. The obtained HMSNs possess uniform diameter and morphology, and the shell of which could be adjusted by changing the addition of silicon precursor. The synthesized HMSNs have been characterized by transmission electron microscopy (TEM) and nitrogen physisorption. Furthermore, the HMSNs are used as support for in-situ deposition of silver nanoparticles (Ag NPs) using n-butylamine as reducing agent for AgNO3 in ethanol. Significantly, Ag NPs were successfully supported in the HMSNs without any aggregation. The Ag-deposited HMSNs showed excellent dispersibility in ethanol and water, and their antibacterial activity against Escherichia coli (E. coli) ATCC 25922 and Staphylococcus aureus (S. aureus) ATCC 6538 have been demonstrated. Therefore, the unique nanostructure based on the HMSNs provided a useful platform for the fabrication of antibacterial agent with superior activity and accessibility. And also, it is expected to be a significant template for the synthesis of other novel nanostructures. PMID:27115332

  9. Volumetric Behavior of Binary Mixtures of Alkoxyethanols and Some Selected Amines at 298.15 K

    Directory of Open Access Journals (Sweden)

    Ayasen Jermaine Kemeakegha

    2015-01-01

    Full Text Available Densities of binary mixtures of 2-methoxyethanol (2-MeO-EtOH and 2-ethoxyethanol (2-EtO-EtOH with hexylamine (HLA, diethylamine (DEA, triethylamine (TEA, tert-butylamine (TBA, aniline (ANL, and benzylamine (BLA have been determined at varying compositions of the alkoxyalkanols at 298.15 K. The excess molar volumes, VE, of the binary mixtures were calculated from the experimental density data of the mixtures and the component single solvents. The calculated excess molar volumes were fitted into the Redlich-Kister polynomial to obtain the fitting coefficients and standard deviations. The excess molar volumes of the binary mixtures of all the solvent systems investigated were negative over the entire range of the solvents composition. The negative values were attributed to stronger hydrogen bond formations between the unlike molecules of mixtures than those between the like molecules of the pure components. The magnitude of the excess molar volumes of the binary mixtures of 2-methoxyethanol and the aliphatic amines were in the order TBA > TEA > DEA > HEA. For the two aromatic amines, the magnitudes were in the order BLA > ANL. For binary mixtures of the amines and 2-ethoxyethanol, the magnitudes were in the order DEA > TEA > TBA > HEA at compositions where the mole fraction of 2-EtO-EtOH was ≤0.5 and TBA > TEA > DEA > HEA above 0.5 mole fraction of 2-EtO-EtOH.

  10. Computational Study and Kinetic Analysis of the Aminolysis of Thiolactones.

    Science.gov (United States)

    Desmet, Gilles B; D'hooge, Dagmar R; Sabbe, Maarten K; Marin, Guy B; Du Prez, Filip E; Espeel, Pieter; Reyniers, Marie-Françoise

    2015-09-01

    The aminolysis of three differently α-substituted γ-thiolactones (C4H5OSX, X = H, NH2, and NH(CO)CH3) is modeled based on CBS-QB3 calculated free energies corrected for solvation using COSMO-RS. For the first time, quantitative kinetic and thermodynamic data are provided for the concerted path and the stepwise path over a neutral tetrahedral intermediate. These paths can take place via an unassisted, an amine-assisted, or a thiol-assisted mechanism. Amine assistance lowers the free energy barriers along both paths, while thiol assistance only lowers the formation of the neutral tetrahedral intermediate. Based on the ab initio calculated rate coefficients, a kinetic model is constructed that is able to reliably describe experimental observations for the aminolysis of N-acetyl-dl-homocysteine thiolactone with n-butylamine in THF and CHCl3. Reaction path analysis shows that for all conditions relevant for applications in polymer synthesis and postpolymer modification, an assisted stepwise mechanism is operative in which the formation of the neutral tetrahedral intermediate is rate-determining and which is mainly amine-assisted at low conversions and thiol-assisted at high conversions. PMID:26280542

  11. Synthesis and characterization of Fe3O4@Ag core-shell: structural, morphological, and magnetic properties

    Directory of Open Access Journals (Sweden)

    Mahdi Ghazanfari

    2014-12-01

    Full Text Available This paper is a report on the synthesis of the Fe3O4@Ag core-shell with high saturation magnetization of magnetite nanoparticles as the core, by using polyol route and silver shell by chemical reduction. X-ray diffraction (XRD and Fourier transform infrared spectroscopy analyses confirmed that the particles so produced were monophase. The magnetic properties of the product were investigated by using a vibrating sample magnetometer. Magnetic saturation of magnetite was 91 emu/g that around about bulk magnetization. This high saturation magnetization can be attributed to the thin dead layer. By using polyethylene glycol as a surfactant to separate and restrict the growth of the particles, magnetostatic interactions are in good agreement with the remanence ratio analysis. Morphology and the average size of the particles were determined with field emission scanning electron microscope (FESEM. Spherical aggregates of Fe3O4 (size around 73 nm are composed of a small primary particle size of about 16 nm. Silver deposition was done using butylamine as the reductant of AgNO3 in ethanol with different ratio. The silver layers were estimated using statistical histogram images of FESEM. Silver-coated iron oxide nanohybrids have been used in a broad range of applications, including chemical and biological sensing, due to the broad absorption in the optical region associated with localized surface plasmon resonance.

  12. Survivability and reactivity of glycine and alanine in early oceans: effects of meteorite impacts.

    Science.gov (United States)

    Umeda, Yuhei; Fukunaga, Nao; Sekine, Toshimori; Furukawa, Yoshihiro; Kakegawa, Takeshi; Kobayashi, Takamichi; Nakazawa, Hiromoto

    2016-01-01

    Prebiotic oceans might have contained abundant amino acids, and were subjected to meteorite impacts, especially during the late heavy bombardment. It is so far unknown how meteorite impacts affected amino acids in the early oceans. Impact experiments were performed under the conditions where glycine was synthesized from carbon, ammonia, and water, using aqueous solutions containing (13)C-labeled glycine and alanine. Selected amino acids and amines in samples were analyzed with liquid chromatography-mass spectrometry (LC/MS). In particular, the (13)C-labeled reaction products were analyzed to distinguish between run products and contaminants. The results revealed that both amino acids survived partially in the early ocean through meteorite impacts, that part of glycine changed into alanine, and that large amounts of methylamine and ethylamine were formed. Fast decarboxylation was confirmed to occur during such impact processes. Furthermore, the formation of n-butylamine, detected only in the samples recovered from the solutions with additional nitrogen and carbon sources of ammonia and benzene, suggests that chemical reactions to form new biomolecules can proceed through marine impacts. Methylamine and ethylamine from glycine and alanine increased considerably in the presence of hematite rather than olivine under similar impact conditions. These results also suggest that amino acids present in early oceans can contribute further to impact-induced reactions, implying that impact energy plays a potential role in the prebiotic formation of various biomolecules, although the reactions are complicated and depend upon the chemical environments as well. PMID:26369758

  13. Separation and conductimetric detection of C1-C7 aliphatic monocarboxylic acids and C1-C7 aliphatic monoamines on unfunctionized polymethacrylate resin columns.

    Science.gov (United States)

    Ohta, Kazutoku; Towata, Atsuya; Ohashi, Masayoshi; Takeuchi, Toyohide

    2004-06-11

    The application of unfunctionized polymethacrylate resin (TSKgel G3000PWXL) as a stationary phase in liquid chromatography with conductimetric detection for C1-C7 aliphatic monocarboxylic acids (formic acid, acetic acid, propionic acid, butyric acid, isovaleric acid, valeric acid, 3,3-dimethylbutyric acid, 4-methylvaleric acid, hexanoic acid, 2-methylhexanoic acid, 5-methylhexanoic acid and heptanoic acid) and C1-C7 aliphatic monoamines (methylamine, ethylamine, propylamine, isobutylamine, butylamine, isoamylamine, amylamine, 1,3-dimethylbutylamine, hexylamine, 2-heptylamine and heptylamine) was attempted with C8 aliphatic monocarboxylic acids (2-propylvaleric acid, 2-ethylhexanoic acid, 2-methylheptanoic acid and octanoic acid) and C8 aliphatic monoamines (1,5-dimethylhexylamine, 2-ethylhexylamine, 1-methylheptylamine and octylamine) as eluents, respectively. Using 1 mM 2-methylheptanoic acid at pH 4.0 as the eluent, excellent separation and relatively high sensitive detection for these C1-C7 carboxylic acids were achieved on a TSKgel G3000PWXL column (150 mm x 6 mm i.d.) in 60 min. Using 2 mM octylamine at pH 11.0 as the eluent, excellent separation and relatively high sensitive detection for these C1-C7 amines were also achieved on the TSKgel G3000PWXL column in 60 min. PMID:15250420

  14. Retention behavior of C1-C6 aliphatic monoamines on anion-exchange and polymethacrylate resins with heptylamine as eluent.

    Science.gov (United States)

    Ohta, Kazutoku; Ohashi, Masayoshi; Jin, Ji-Ye; Takeuchi, Toyohide; Fujimoto, Chuzo; Choi, Seong-Ho; Ryoo, Jae Jeong; Lee, Kwang-Pill

    2004-06-11

    Retention behavior of C1-C6, aliphatic monoamines (methylamine, ethylamine, propylamine, butylamine, amylamine and hexylamine) on columns (150 mm x 6 mm i.d.) packed with various anion-exchange resins (styrene-divinylbenzene (PS-DVB) copolymer-based strongly basic anion-exchange resin: TSKgel SAX, polymethacrylate-based strongly basic anion-exchange resin: TSKgel SuperQ-5PW and polymethacrylate-based weakly basic anion-exchange resin: TSKgel DEAE-5PW) and unfunctionized polymethacrylate resins (TSKgel G5000PW and TSKgel G3000PWXL) was investigated with basic solutions (sodium hydroxide and heptylamine) as the eluents. Due to strongly electrostatic repulsion (ion-exclusion effect) between these anion-exchange resins and these amines, peak resolution between these amines on these anion-exchange resin columns was unsatisfactory with both sodium hydroxide and heptylamine as the eluents. In contrast, these polymethacrylate resins were successfully applied as the stationary phases for the separation of these C1-C6 amines with heptylamine as eluent, because of both small hydrophobicity and small cation-exchange ability of these resins. Excellent simultaneous separation, highly sensitive conductimetric detection and symmetrical peaks for these C1-C6 amines were achieved on the TSKgel G3000PWXL column in 35 min with 5 mM heptylamine at pH 11.1 as the eluent. PMID:15250421

  15. FUNCTIONALIZING PS MICROSPHERES BY SUPERCRITICAL DEPOSITION OF P(S-b-tBA) FOR DIVERSE INTERFACIAL PROPERTIES EXEMPLIFIED WITH BIOCIDAL ABILITY

    Institute of Scientific and Technical Information of China (English)

    Yong Chen; Hong-ni Teng

    2012-01-01

    Polystyrene (PS) microspheres were functionalized with poly(styrene-b-tert-butyl acrylate) (P(S-b-tBA)) by adsorption from supercritical mixture of CO2 and hexane.Supercritical deposition formed a shell-core structure that contained a shell of poly(tert-butyl acrylate) (PtBA) blocks and a core of the PS blocks entangling with the PS microspheres.The thickness of the PtBA layer and thereby the areal density oftert-butyl ester groups increased with the deposition pressure until plateau values attained at 20 MPa and higher.The tert-butyl ester groups were hydrolyzed to carboxyl groups for conjugation with tert-butylamine molecules via amide bonds that were further chlorinated into biocidal N-halamine moieties.The functionalization layer and its bonded N-halamine moieties were stable in flowing water and the chlorine could be regenerated upon eventual loss.This functionalization concept is applicable to polymers of any external and internal surfaces to achieve diverse surface properties by varying block copolymer and conjugated moieties.

  16. Synthesis, Spectroscopic, and Antimicrobial Studies of Binuclear Metallocene (M = Ti, Zr, or Hf Derivatives of Bis(mercaptoazoles

    Directory of Open Access Journals (Sweden)

    Akhilesh Kumar Srivastava

    2007-05-01

    Full Text Available The reactions of (η5−C5H52MCl2 (M = Ti, Zr, or Hf with mercaptoazoles (LH2, namely, bis(mercaptotriazoles, bis(mercap-tooxadiazoles, and bis(mercaptothiadiazoles in 2 : 1 molar ratio, respectively, have been studied in dry tetrahydrofuran in the presence of n-butylamine and the binuclear complexes of the type [{(η−C5H52M}2(L] (M = Ti/Zr/Hf are obtained. Tentative structural conclusions are drawn for the reaction products based upon elemental analysis, electrical conductance, magnetic moment, and spectral data (UV-Vis, IR, H1 NMR, and C13 NMR. FAB-mass spectra of few complexes of each series were also carried out to confirm the binuclear structures. Studies were conducted to assess the growth-inhibiting potential of the complexes synthesized, and the ligands against various fungal and bacterial strains.

  17. Biosynthesis of amorphous mesoporous aluminophosphates using yeast cells as templates

    International Nuclear Information System (INIS)

    Graphical abstract: Display Omitted Highlights: ► Amorphous aluminophosphates can take place using yeast as template. ► A mesoporous material was obtained. ► The specific surface area after calcinations ranged between 176 and 214 m2 g−1. -- Abstract: In this study aluminophosphates have been synthesized from aluminum isopropoxide and phosphoric acid solutions using yeast cells as template. The physicochemical characterization was carried out by thermogravimetric analysis; X-ray diffraction; Fourier transform infrared; N2 adsorption–desorption isotherms; scanning electron microscopy; transmission electron microscopy and potentiometric titration with N-butylamine for determination of: thermal stability; crystalline structure; textural properties; morphology and surface acidity, respectively. The calcined powders consisted of an intimate mixture of amorphous and crystallized AlPO particles with sizes between 23 and 30 nm. The average pore size observed is 13–16 nm and the specific surface area after calcinations (at 650 °C) ranged between 176 and 214 m2 g−1.

  18. Molecular Dynamics Simulations of Aldol Condensation Catalyzed by Alkylamine-Functionalized Crystalline Silica Surfaces.

    Science.gov (United States)

    Kim, Ki Chul; Moschetta, Eric G; Jones, Christopher W; Jang, Seung Soon

    2016-06-22

    Molecular dynamics simulations are performed to investigate the cooperatively catalyzed aldol condensation between acetone and 4-nitrobenzaldehyde on alkylamine (or alkylenamine)-grafted silica surfaces, focusing on the mechanism of the catalytic activation of the acetone and 4-nitrobenzaldehyde by the acidic surface silanols followed by the nucleophilic attack of the basic amine functional group toward the activated reactant. From the analysis of the correlations between the catalytically active acid-base sites and reactants, it is concluded that the catalytic cooperativity of the acid-base pair can be affected by two factors: (1) the competition between the silanol and the amine (or enamine) to form a hydrogen bond with a reactant and (2) the flexibility of the alkylamine (or alkylenamine) backbone. Increasing the flexibility of the alkylamine facilitates the nucleophilic attack of the amine on the reactants. From the molecular dynamics simulations, it is found that C3 propylamine and C4 butylamine linkers exhibit the highest probability of reaction, which is consistent with the experimental observation that the activity of the aldol reaction on mesoporous silica depends on the length of alkylamine grafted on the silica surface. This simulation work serves as a pioneering study demonstrating how the molecular simulation approach can be successfully employed to investigate the cooperative catalytic activity of such bifunctional acid-base catalysts. PMID:27238580

  19. Solution-phase synthesis of nanomaterials at low temperature

    Institute of Scientific and Technical Information of China (English)

    ZHU YongChun; QIAN YiTai

    2009-01-01

    This paper reviews the solution-phase synthesis of nanoparticles via some routes at low temperatures, such as room temperature route, wave-assisted synthesis (γ-irradiation route and sonochemical route), directly heating at low temperatures, and hydrothermal/solvothermal methods. A number of strategies were developed to control the shape, the size, as well as the dispersion of nanostructures. Using di-ethylamine or n-butylamine as solvent, semiconductor nanorods were yielded. By the hydrothermal treatment of amorphous colloids, Bi2S3 nanorods and Se nanowires were obtained. CdS nanowires were prepared in the presence of polyacrylamide. ZnS nanowires were obtained using liquid crystal. The polymer poly (vinyl acetate) tubule acted as both nanoreactor and template for the CdSe nanowire growth. Assisted by the surfactant of sodium dodecyl benzenesulfonate (SDBS), nickel nanobelts were synthesized. In addition, Ag nanowires, Te nanotubes and ZnO nanorod arrays could be prepared without adding any additives or templates.

  20. Novel 2,7-Substituted (S)-1,2,3,4-Tetrahydroisoquinoline-3-carboxylic Acids: Peroxisome Proliferator-Activated Receptor γ Partial Agonists with Protein-Tyrosine Phosphatase 1B Inhibition.

    Science.gov (United States)

    Otake, Kazuya; Azukizawa, Satoru; Takeda, Shigemitsu; Fukui, Masaki; Kawahara, Arisa; Kitao, Tatsuya; Shirahase, Hiroaki

    2015-01-01

    A novel series of 2,7-substituted 1,2,3,4-tetrahydroisoquinoline-3-carboxylic acid derivatives were synthesized and biologically evaluated. (S)-2-(2-Furylacryloyl)-7-[2-(2-methylindane-2-yl)-5-methyloxazol-4-yl]methoxy-1,2,3,4-tetrahydroisoquinoline-3-carboxylic acid tert-butylamine salt (13jE) was identified as a potent human peroxisome proliferator-activated receptor γ (PPARγ)-selective agonist (EC50=85 nM) and human protein-tyrosine phosphatase 1B (PTP-1B) inhibitor (IC50=1.0 µM). Compound 13jE partially activated PPARγ, but not PPARα or PPARδ, and antagonized farglitazar, a full PPARγ agonist. Cmax after the oral administration of 13jE at 10 mg/kg was 28.6 µg/mL (53 µM) in male Sprague-Dawley (SD) rats. Repeated administration of 13jE and rosiglitazone for 14 d at 10 mg/kg/d decreased plasma glucose and triglyceride levels significantly in male KK-A(y) mice. Rosiglitazone, but not 13jE, significantly increased the plasma volume and liver weight. In conclusion, 13jE showed stronger hypoglycemic and hypolipidemic effects and weaker hemodilution and hepatotoxic effects than rosiglitazone, suggesting that its safer efficacy may be due to its partial PPARγ agonism and PTP-1B inhibition. PMID:26633022

  1. Characterization of 12-molybdophosphoric acid supported on mesoporous silica MCM-41 and its catalytic performance in the synthesis of hydroquinone diacetate

    International Nuclear Information System (INIS)

    12-molybdophosphoric acid (PMA) was supported on mesoporous molecular sieves MCM-41 by impregnation of 12-molybdophosphoric acid followed by calcination. The nanochannels of MCM-41 provide a large surface area for the solid state dispersion of 12-molybdophosphoric acid. The samples have been characterized by N2 adsorption–desorption at −196 °C, transmission electron microscopy (TEM), powder X-ray diffraction (PXRD), and FT-IR measurements. The acidity and catalytic activity have been, respectively, examined by nonaqueous titration of n-butylamine in acetonitrile and synthesis of hydroquinone diacetate. The results showed that ordered hexagonal pore structure was observed in the synthesized MCM-41. Also the results indicate that PMA are highly dispersed on mesoporous silica MCM-41 spherical nanoparticles while PMA retains its Keggin structure. On the other hand, with increasing the introduced PMA amount, the specific surface area decreases, and the mesoporous ordering of the samples become poor. Both the surface acidity and the catalytic activity sharply increase with the modification of MCM-41 by PMA but decrease by increasing the calcination temperature. The sample with 55 wt% PMA/MCM-41 calcined at 350 °C shows the highest acidity and catalytic activity.

  2. Characterization of 12-molybdophosphoric acid supported on mesoporous silica MCM-41 and its catalytic performance in the synthesis of hydroquinone diacetate

    Energy Technology Data Exchange (ETDEWEB)

    Ahmed, Awad I., E-mail: awahmed@mans.edu.eg [Chemistry Department, Faculty of Science, Mansoura University, Mansoura (Egypt); Samra, S.E.; El-Hakam, S.A. [Chemistry Department, Faculty of Science, Mansoura University, Mansoura (Egypt); Khder, A.S. [Faculty of Applied Science, Umm Al Qura University, Makkah (Saudi Arabia); El-Shenawy, H.Z.; El-Yazeed, W.S. Abo [Chemistry Department, Faculty of Science, Mansoura University, Mansoura (Egypt)

    2013-10-01

    12-molybdophosphoric acid (PMA) was supported on mesoporous molecular sieves MCM-41 by impregnation of 12-molybdophosphoric acid followed by calcination. The nanochannels of MCM-41 provide a large surface area for the solid state dispersion of 12-molybdophosphoric acid. The samples have been characterized by N{sub 2} adsorption–desorption at −196 °C, transmission electron microscopy (TEM), powder X-ray diffraction (PXRD), and FT-IR measurements. The acidity and catalytic activity have been, respectively, examined by nonaqueous titration of n-butylamine in acetonitrile and synthesis of hydroquinone diacetate. The results showed that ordered hexagonal pore structure was observed in the synthesized MCM-41. Also the results indicate that PMA are highly dispersed on mesoporous silica MCM-41 spherical nanoparticles while PMA retains its Keggin structure. On the other hand, with increasing the introduced PMA amount, the specific surface area decreases, and the mesoporous ordering of the samples become poor. Both the surface acidity and the catalytic activity sharply increase with the modification of MCM-41 by PMA but decrease by increasing the calcination temperature. The sample with 55 wt% PMA/MCM-41 calcined at 350 °C shows the highest acidity and catalytic activity.

  3. Characterization of 12-molybdophosphoric acid supported on mesoporous silica MCM-41 and its catalytic performance in the synthesis of hydroquinone diacetate

    Science.gov (United States)

    Ahmed, Awad I.; Samra, S. E.; El-Hakam, S. A.; Khder, A. S.; El-Shenawy, H. Z.; El-Yazeed, W. S. Abo

    2013-10-01

    12-molybdophosphoric acid (PMA) was supported on mesoporous molecular sieves MCM-41 by impregnation of 12-molybdophosphoric acid followed by calcination. The nanochannels of MCM-41 provide a large surface area for the solid state dispersion of 12-molybdophosphoric acid. The samples have been characterized by N2 adsorption-desorption at -196 °C, transmission electron microscopy (TEM), powder X-ray diffraction (PXRD), and FT-IR measurements. The acidity and catalytic activity have been, respectively, examined by nonaqueous titration of n-butylamine in acetonitrile and synthesis of hydroquinone diacetate. The results showed that ordered hexagonal pore structure was observed in the synthesized MCM-41. Also the results indicate that PMA are highly dispersed on mesoporous silica MCM-41 spherical nanoparticles while PMA retains its Keggin structure. On the other hand, with increasing the introduced PMA amount, the specific surface area decreases, and the mesoporous ordering of the samples become poor. Both the surface acidity and the catalytic activity sharply increase with the modification of MCM-41 by PMA but decrease by increasing the calcination temperature. The sample with 55 wt% PMA/MCM-41 calcined at 350 °C shows the highest acidity and catalytic activity.

  4. Hydrogen-transfer and charge-transfer in photochemical and radiation induced reactions. Progress report, November 1, 1975--October 31, 1976

    International Nuclear Information System (INIS)

    The relative importance of light absorption, quenching of triplet, and hydrogen transfer repair has been examined in retardation by mercaptans of photoreduction of aromatic ketones by alcohols. In the reduction of benzophenone by 2-propanol, retardation is efficient and, after correction for the first two effects, is due entirely to hydrogen-transfer repair, as indicated by deuterium labeling. In reduction of acetophenone by α-methylbenzyl alcohol, repair by hydrogen transfer is also operative. In reduction of benzophenone by benzhydrol, retardation is less efficient and is due to quenching, as the ketyl radical does not abstract hydrogen from mercaptan rapidly in competition with coupling. Deuterium isotope effects are discussed in terms of competitive reactions. Photoreduction of benzophenone by 2-butylamine and by triethylamine is retarded by aromatic mercaptans and disulfides. Of the retardation not due to light absorption and triplet quenching by the sulfur compounds, half is due to hydrogen-transfer repair, as indicated by racemization and deuterium labeling. The remainder is attributed to quenching by the sulfur compound of the charge-transfer-complex intermediate. Photoreduction by primary and secondary amines, but not by tertiary amines, is accelerated by aliphatic mercaptans. The acceleration is attributed to catalysis of hydrogen transfer by the mercaptan in the charge-transfer complex. The effect is large in hydrocarbon solvent, less in polar organic solvents and absent in water

  5. Adsorption of iodine by silver-impregnated hydrophobic adsorbent

    International Nuclear Information System (INIS)

    Hydrophobic adsorbents, which consist of porous styrene-divinylbenzene copolymer (SDB) impregnated with silver, were developed for the removal of iodine from the dissolver off-gas (DOG). The adsorption of iodine in a simulated off-gas including iodine, NOx and water vapor was examined by use of an adsorption column packed with the hydrophobic adsorbents. Silver impregnation methods using organic solutions were proposed. By use of dioxan and butylamine, which can swell the SDB easily, silver nitrate and metallic silver were uniformly distributed in the SDB particles. The breakthrough of iodine was not influenced by the presence of NOx and water vapor. For a macroporous SDB with the pore volume of 1.59 ml/g-SDB and the average pore diameter of 500A, impregnated with metallic silver at silver content of 28 wt%, a high adsorption capacity of 0.14g-I2/cm3-adsorbent was obtained, compared to that of a commercial adsorbent. AgNO3-impregnated silica gel. The impregnated silver was utilized about 91% for the iodine adsorption. (author)

  6. Dopamine agonist activity of EMD 23,448

    Energy Technology Data Exchange (ETDEWEB)

    Martin, G.E.; Pettibone, D.J. (Merck Sharp and Dohme Research Laboratories, West Point, Pennsylvania (USA). Dept. of Pharmacology)

    1985-01-01

    EMD 23,448 was examined in tests of dopaminergic function and was found to be an atypical dopamine (DA) agonist. EMD 23,448 was a weak or inactive DA agonist when examined in tests of normal postsynaptic DA receptor function: production of stereotypy in the rat (ED/sub 50/ greater than sign 5.0 mg/kg.i.p.); production of emesis in beagles (minimum effective dose = 81..mu..g/kg i.v.); and, enhanced locomotor activity of the mouse (no excitation in doses <=50 mg/i.p.). Moreover, EMD 23,448 was relatively weak in competing for (/sup 3/H)-apomorphine binding to rat striatal membranes (Ki, 205 nM). On the other hand, this indolyl-3-butylamine did activate supersensitive postsynaptic DA receptors. Specifically, it elicited contralateral turning in rats with a unilateral 6-hydroxydopamine lesion of the substantia nigra (ED/sub 50/ value = 0.9 mg/kg) and did elicit stereotypy in rats given chronic daily haloperidol treatments. EMD 23,448 also exerted pharmacological effects in tests designed to measure activation of dopamine autoreceptors. It inhibited the ..gamma..-butyrolactone-induced increase in striatal dopa levels (ED/sub 50/ = 1 mg/kg i.p.) and produced a dose-related fall in the locomotor activity of the mouse. The results are discussed and contrasted with data derived for apomorphine and the putatively selective autoreceptor agonist (+-)-3-PPP.

  7. Plasma Functionalized Multiwalled Carbon Nanotubes for Immobilization of Candida antarctica Lipase B: Production of Biodiesel from Methanolysis of Rapeseed Oil.

    Science.gov (United States)

    Rastian, Zahra; Khodadadi, Abbas Ali; Guo, Zheng; Vahabzadeh, Farzaneh; Mortazavi, Yadollah

    2016-03-01

    Surface modification of multiwalled carbon nanotubes (MWCNTs) through functionalization could improve the characteristics of these nanomaterials as support for enzymes. Carboxylation of MWCNTs (MWCNT-COOH) has been carried out in this study using the dielectric barrier discharge (DBD) plasma reactor through humidified air. The chemical method was also used for further functionalization of the MWCNT-COOH through which the amidation of the surfaces with either butylamine (MWCNT-BA) or octadecylamine (MWCNT-OA) was performed. By immobilization of Candida antarctica B lipase (CALB) on these nanoparticles, performance of the immobilized enzyme in catalyzing methanolysis of rapeseed oil was evaluated. The CALB loading on the MWCNT-BA and MWCNT-COOH was 20 mg protein/g, while the value for MWCNT-OA was 11 mg protein/g. The yield of biodiesel was determined as percentage of mass of fatty acid methyl ester (FAME) produced per initial mass of the oil, and the yield value for the two of these three supports namely, MWCNT-COOH and MWCNT-BA used for the CALB immobilization was similar at about 92 %, while 86 % was the yield for the reaction catalyzed by the lipase immobilized on MWCNT-OA. Thermal stability of the immobilized CALB and the catalytic ability of the enzyme in the repeated batch experiments have also been determined. PMID:26588921

  8. The Effect of Solvent on Isocyanate Group Content Determination in Polyurethane Prepolymer%溶剂对聚氨酯预聚体中异氰酸根含量测定的影响

    Institute of Scientific and Technical Information of China (English)

    郭焕; 谭舸

    2014-01-01

    采用丙酮溶解预聚体,甲苯-二正丁胺为反应体系,考察不同溶剂及反应时间对聚氨酯预聚体中异氰酸酯含量测定的影响,同时考察了溶剂用量对测定结果的影响。结果表明,丙酮为溶剂,甲苯-二正丁胺与异氰酸根反应,结果准确度在国家标准允许范围内,测定异氰酸根含量结果与理论值基本一致。%The effects of different solvents and reaction times on determination of isocyanate group content in polyurethane prepolymer were studied, reaction system was toluene-butylamine using acetone dissolving prepoly-mer. Meanwhile the influence of the solvent dosage on the test results was investigated. The tests showed that the result accuracy was in the extent permitted of national standard when solvent was acetone, isocyanate reacted with toluene-dibutylamine. The test result of isocyanate group content was consistent with theoretical values.

  9. Physicochemical studies of the carbamate-CO2-solvent system

    International Nuclear Information System (INIS)

    The formation of carbamate from CO2 and the various amine solutions has been investigated for the purpose of elucidating the structure of the species generated in the reaction. The amine solutions used were 1 and 2 molar solutions of di-n-butylamine (DNBA) in triethylamine (TEA), pure DNBA and pure TEA. It has been found that the nonaqueous solvent participates in the formation of carbamate in 1 and 2M-DNBA/TEA solutions as a proton acceptor in DNBA-carbamate formation. However, due to the high concentration of the solutions and the basicities of the amines, a significant amount of DNBA which does not form the DNBA-carbamate anion is also found to be participating as a proton acceptor. Pure TEA absorbs only 1/60 of the absorption by pure DNBA. The extent of TEA participation in the CO2-absorption process other than as a proton acceptor in DNBA-carbamate is negligible. The formation of carbamic acid and zwitterion have been found unlikely. 7 tables, 15 figs

  10. The Indian drawings of the poet Cesare Pascarella: non-destructive analyses and conservation treatments.

    Science.gov (United States)

    Bicchieri, Marina; Monti, Michela; Piantanida, Giovanna; Pinzari, Flavia; Iannuccelli, Simonetta; Sotgiu, Silvia; Tireni, Lorena

    2012-02-01

    The Italian dialect poet Cesare Pascarella travelled all around the world, noting down in notebooks his keen and caustic observations, and drawing sketches that are a visual reportage of his journeys. The sketches were mounted as a random collage over acidic cardboards that were exposed to direct sunlight in his studio. Their poor state of conservation is related to the use of modern paper: chemical instability of raw materials caused acidification and strong oxidation of the support, with intense yellowing of the surfaces and brittleness of the paper. To ensure future preservation of the drawings, chemical stabilisation with simultaneous alcoholic treatment by deacidification (calcium propionate) and reduction (borane tert-butylamine complex) appeared necessary. To verify its applicability, it was indispensible to characterise the support and identify the nature of all the graphic media. The use of Raman, Infrared, X-ray fluorescence spectroscopies and scanning electron microscopy coupled with X-ray microanalysis allowed us to clear the problems related to the different penetration depth of each analytical technique and the different responses of pigments/dyes to each spectroscopy. The palette, how it varied along the journeys, the different supports used and preparations were completely identified showing a choice of colours compatible with the reduction treatment. PMID:21750878

  11. Oxidative Dehydrogenation of Methanol on Chromium Oxide/Montmorillonite K10 Catalysts

    International Nuclear Information System (INIS)

    Methanol conversion was carried out on one of meso porous materials, Chromia I Montmorillonite K10 (MK10) in a pulse micro catalytic system. Methanol was converted to formaldehyde and ethylene by two different mechanisms. Methanol dehydrogenation increases by reaction temperature (300-400 degree C) and as chromia loading decrease. In contradiction, the dehydration of methanol takes place at higher temperature (400-500 degree C) and as chromia loading increase, 3-18% Cr. Redox and exposed non-redox Cr3+ are responsible for HCHO formation. There is relationship between increasing of C2H4 production and the increase of Cr+6 phase (from TPR and UV-Vis) according to the acidity of chromia catalysts 34 and 76 μL tert-Butylamine /gram catalyst for 3% Cr and 18% Cr, respectively. Formaldehyde formation is diffusional controlled at high temperature (400-500 degree C) and kinetically controlled at lower reaction temperature (300-400 degree C) while methanol dehydration to ethylene is surface reaction controlled at 400-500 degree C

  12. Biosynthesis of amorphous mesoporous aluminophosphates using yeast cells as templates

    Energy Technology Data Exchange (ETDEWEB)

    Sifontes, Ángela B., E-mail: asifonte@ivic.gob.ve [Centro de Química, Instituto Venezolano de Investigaciones Científicas, Apartado 20632, Caracas 1020-A (Venezuela, Bolivarian Republic of); González, Gema [Centro de Ingeniería de Materiales y Nanotecnología, Instituto Venezolano de Investigaciones Científicas, Apartado 20632, Caracas 1020-A (Venezuela, Bolivarian Republic of); Tovar, Leidy M.; Méndez, Franklin J. [Centro de Química, Instituto Venezolano de Investigaciones Científicas, Apartado 20632, Caracas 1020-A (Venezuela, Bolivarian Republic of); Gomes, Maria E. [Centro de Ingeniería de Materiales y Nanotecnología, Instituto Venezolano de Investigaciones Científicas, Apartado 20632, Caracas 1020-A (Venezuela, Bolivarian Republic of); Cañizales, Edgar [Área de Análisis Químico Inorgánico, PDVSA, INTEVEP, Los Teques 1070-A (Venezuela, Bolivarian Republic of); Niño-Vega, Gustavo; Villalobos, Hector [Centro de Microbiología y Biología Celular, Instituto Venezolano de Investigaciones Científicas, Apartado 20632, Caracas 1020-A (Venezuela, Bolivarian Republic of); Brito, Joaquin L. [Centro de Química, Instituto Venezolano de Investigaciones Científicas, Apartado 20632, Caracas 1020-A (Venezuela, Bolivarian Republic of)

    2013-02-15

    Graphical abstract: Display Omitted Highlights: ► Amorphous aluminophosphates can take place using yeast as template. ► A mesoporous material was obtained. ► The specific surface area after calcinations ranged between 176 and 214 m{sup 2} g{sup −1}. -- Abstract: In this study aluminophosphates have been synthesized from aluminum isopropoxide and phosphoric acid solutions using yeast cells as template. The physicochemical characterization was carried out by thermogravimetric analysis; X-ray diffraction; Fourier transform infrared; N{sub 2} adsorption–desorption isotherms; scanning electron microscopy; transmission electron microscopy and potentiometric titration with N-butylamine for determination of: thermal stability; crystalline structure; textural properties; morphology and surface acidity, respectively. The calcined powders consisted of an intimate mixture of amorphous and crystallized AlPO particles with sizes between 23 and 30 nm. The average pore size observed is 13–16 nm and the specific surface area after calcinations (at 650 °C) ranged between 176 and 214 m{sup 2} g{sup −1}.

  13. Sub-10 nm Platinum Nanocrystals with Size and Shape Control: Catalytic Study for Ethylene and Pyrrole Hydrogenation

    Energy Technology Data Exchange (ETDEWEB)

    Tsung, Chia-Kuang; Kuhn, John N.; Huang, Wenyu; Aliaga, Cesar; Hung, Ling-I; Somorjai, Gabor A.; Yang, Peidong

    2009-03-02

    Platinum nanocubes and nanopolyhedra with tunable size from 5 to 9 nm were synthesized by controlling the reducing rate of metal precursor ions in a one-pot polyol synthesis. A two-stage process is proposed for the simultaneous control of size and shape. In the first stage, the oxidation state of the metal ion precursors determined the nucleation rate and consequently the number of nuclei. The reaction temperature controlled the shape in the second stage by regulation of the growth kinetics. These well-defined nanocrystals were loaded into MCF-17 mesoporous silica for examination of catalytic properties. Pt loadings and dispersions of the supported catalysts were determined by elemental analysis (ICP-MS) and H2 chemisorption isotherms, respectively. Ethylene hydrogenation rates over the Pt nanocrystals were independent of both size and shape and comparable to Pt single crystals. For pyrrole hydrogenation, the nanocubes enhanced ring-opening ability and thus showed a higher selectivity to n-butylamine as compared to nanopolyhedra.

  14. Synergistic effects of amine and protein modified epoxy-support on immobilized lipase activity.

    Science.gov (United States)

    Cui, Caixia; Tao, Yifeng; Ge, Chunling; Zhen, Yueju; Chen, Biqiang; Tan, Tianwei

    2015-09-01

    We have developed an improved and effective method to immobilize Yarrowia lipolytica lipase Lip2 (YLIP2) on an epoxy poly-(glycidylmethacrylate-triallyisocyanurate-ethyleneglycoldimethacrylate) (PGMA-TAIC-EGDMA) support structure with or without amine or/and protein modifications. Our results show that there is an increase in the activity of the immobilized lipase on n-butylamine (BA) modified support (420U/g support) and the biocompatible gelatin modified support (600U/g support) when compared to the support without modification (240U/g support). To further study the influences of BA and gelatin modification on the activity of the immobilized lipase, gelatin and BA were concurrently used to decorate the support structure. Lipase immobilized on 2% BA/gelatin (1:1) modified support obtained the highest activity (1180U/g support), which was five-fold higher than that on a native support structure. These results suggest that the activity of a support-immobilized lipase depends on the support surface properties and a moderate support surface micro-environment was crucial for elevated activity. Collectively, these data show that a combined gelatin and BA modification regulates the support surface more suitable for immobilizing YLIP2. PMID:26073154

  15. Synthesis of ZnS hollow nanospheres with holes using different amine templates

    Institute of Scientific and Technical Information of China (English)

    Eingang LI; Yu TANG; Yuanming ZHANG; Jun YANG; Biying DU

    2008-01-01

    ZnS hollow nanospheres with holes were prepared by reacting ZnSO4 with H2S, the sulfide source formed in the reaction of CS2 with ethylenediamine, 1,3-propylenediamine, butylamine or 2-(2-aminoethylamino) ethanol, which also acted as a template agent, at 50℃ under agitation. The shape, particle size of about 100-850 nm and hole size of about 150-600 nm of ZnS hollow nanospheres with holes were shown by SEM and TEM images. These ZnS nanospheres with β cubic ZnS phase and composed of 2-5 nm nanocrystals were characterized by XRD and HRTEM. The blue shift of maximum absorption in UV-vis displayed the effect of quantum size. The two amino groups of amine templates reacted favorably with Zn2+ to form uniform and relatively smooth ZnS nanospheres with holes, while hydroxyethyl played a disadvantageous role. A reason-able mechanism of hole formation by H2S rushing out is suggested.

  16. Complex formation reactions of uranyl(VI) with neutral N-donors in dimethyl sulfoxide. Influence of small amounts of water

    International Nuclear Information System (INIS)

    Quantitative information about the existence and thermodynamic stability of uranyl(VI) ion complexes based solely upon nitrogen coordination has been obtained in the solvent dimethyl sulfoxide. Calorimetric, potentiometric, and FT-IR investigations, under controlled anhydrous conditions, show that the uranyl(VI) ion can form both mono and bis chelates with the ethylenediamine ligand and only a mono chelate of rather low stability with propylenediamine. With the monodentate ligand n-butylamine only a very weak metal-ligand interaction has been detected. The stability constants and the enthalpy and entropy changes have been calculated for the identified coordinated species. All data refer to 25.0 degree C and a tetraethylammonium perchlorate medium of ionic strength 0.1 M. All the complexes are enthalpy stabilized whereas the entropy contributions oppose the complex formation. Calorimetric and FT-IR measurements carried out to investigate the effects of small amounts of water present show that a very low water concentration, comparable to that of the coordinating metal ion, can give rise to hydrolysis reactions that may compete with complex formation. This is due to the combined action of different factors that are discussed. 39 refs., 6 figs., 1 tab

  17. Determination of coumarin anticoagulant rodenticide residues in animal tissue by high-performance liquid chromatography. I. Fluorescence detection using post-column techniques.

    Science.gov (United States)

    Hunter, K

    1983-11-18

    A multi-residue method was developed for the determination of the rodenticides warfarin, coumatetralyl, bromadiolone, difenacoum and brodifacoum in animal tissues by high-performance liquid chromatography with fluorescence detection. Extracts were cleaned-up by gel permeation chromatography on Bio-Beads SX-3 and residues determined by normal and reversed-phase high-performance liquid chromatography using post-column pH-switching, with chloroform -sec.-butylamine and borate buffer (pH 10.4) respectively, to maximise the native fluorimetric responses. Confirmation of identification was possible by re-chromatographing extracts in the absence of the post-column reagent. Chloroform-acetone (1:1) was significantly better than chloroform for the extraction of residues of these rodenticides from liver tissues. Recoveries from spiked liver tissue were generally greater than 90% at levels of 0.05-1 mg kg-1. Detection limits in animal tissues of 0.002 mg kg-1 for coumatetratyl, difenacoum and brodifacoum, 0.01 mg kg-1 for bromadiolone and 0.02 mg kg-1 for warfarin and could be routinely achieved. PMID:6655019

  18. Novel fabrication of Ag thin film on glass for efficient surface-enhanced Raman scattering.

    Science.gov (United States)

    Park, Hyoung Kun; Yoon, Jae Keun; Kim, Kwan

    2006-02-14

    This paper describes a very simple electroless-plating method used to prepare optically tunable nanostructured Ag films. Very stable Ag films can be reproducibly fabricated simply by soaking glass substrates in ethanolic solutions of AgNO3 and butylamine. The grain size of silver can be readily controlled to range from 20 to 150 nm, and these nanostructural features correlated well with their UV/vis absorption characteristics, as well as with their surface-enhanced Raman scattering (SERS) activities. It is also very advantageous that the Ag films prepared exhibit very even SERS activity over an area up to hundreds thousand square-micrometers, and the enhancement factor estimated using benzenethiol as a prototype adsorbate reaches approximately 2 x 10(5). Since the proposed method is cost-effective and is suitable for the mass production of diverse Ag films irrespective of the shapes of the underlying substrates, it is expected to play a significant role in the development of surface plasmon-based analytical devices. PMID:16460083

  19. Temperature-dependent photoluminescence of cadmium-free Cu-Zn-In-S quantum dot thin films as temperature probes.

    Science.gov (United States)

    Wang, Lan; Kang, Xiaojiao; Huang, Lijian; Pan, Daocheng

    2015-12-21

    We reported temperature-dependent photoluminescence (PL) studies on Cu-Zn-In-S quantum dot (QD) thin films. In this paper, cadmium-free and luminescent Cu-Zn-In-S quantum dot thin films were in situ formed by thermal decomposition of molecular-based precursors in the open air, without need of the complicated quantum dot synthesis. Molecular-based precursor solutions were prepared by dissolving Cu2O, ZnO, and In(OH)3 in the ethanol solution of butylamine and carbon disulfide. The effects of sintering temperature, sintering time, and the concentration of capping agents on the photoluminescence properties of Cu-Zn-In-S QD thin films have been systematically investigated. It was found that alkali metal ions play an important role in enhancing the PL quantum yield of quantum dot thin films. The as-prepared QD thin films show composition-tunable emission in the range of 535 nm to 677 nm, and the absolute PL quantum yields can reach as high as 22.1%. All of the as-deposited QD thin films show a single-exponential decay to temperature, indicating that these cadmium-free QD thin films have high potential as temperature probes. PMID:26567537

  20. NIOSH Manual of Analytical Methods (third edition). Fourth supplement

    Energy Technology Data Exchange (ETDEWEB)

    1990-08-15

    The NIOSH Manual of Analytical Methods, 3rd edition, was updated for the following chemicals: allyl-glycidyl-ether, 2-aminopyridine, aspartame, bromine, chlorine, n-butylamine, n-butyl-glycidyl-ether, carbon-dioxide, carbon-monoxide, chlorinated-camphene, chloroacetaldehyde, p-chlorophenol, crotonaldehyde, 1,1-dimethylhydrazine, dinitro-o-cresol, ethyl-acetate, ethyl-formate, ethylenimine, sodium-fluoride, hydrogen-fluoride, cryolite, sodium-hexafluoroaluminate, formic-acid, hexachlorobutadiene, hydrogen-cyanide, hydrogen-sulfide, isopropyl-acetate, isopropyl-ether, isopropyl-glycidyl-ether, lead, lead-oxide, maleic-anhydride, methyl-acetate, methyl-acrylate, methyl-tert-butyl ether, methyl-cellosolve-acetate, methylcyclohexanol, 4,4'-methylenedianiline, monomethylaniline, monomethylhydrazine, nitric-oxide, p-nitroaniline, phenyl-ether, phenyl-ether-biphenyl mixture, phenyl-glycidyl-ether, phenylhydrazine, phosphine, ronnel, sulfuryl-fluoride, talc, tributyl-phosphate, 1,1,2-trichloro-1,2,2-trifluoroethane, trimellitic-anhydride, triorthocresyl-phosphate, triphenyl-phosphate, and vinyl-acetate.

  1. Ionic liquid matrix-based dispersive liquid-liquid microextraction for enhanced MALDI-MS analysis of phospholipids in soybean.

    Science.gov (United States)

    Shrivas, Kamlesh; Tapadia, Kavita

    2015-09-15

    Ionic liquid matrix (ILM) is found to be a very versatile substance for analysis of broad range of organic molecules in matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) due to good solubility for a variety of analytes, formation of homogenous crystals and high vacuum stability of the matrix. In the present work, an ILM, cyno-4-hydroxycinnamic acid-butylamine (CHCAB) was employed in dispersive liquid-liquid microextraction (DLLME) as sample probe and matrix for extraction and ionization of phospholipids from food samples (soybean) prior to MALDI-MS analysis. With the employed technique, 8-125 fold improvement in signal intensity and limit of detection were achieved for the analysis of phospholipids. The best extraction efficiency of phospholipids in ILM-DLLME was obtained with 5min extraction time in presence 30mg/mL CHCAB and 1.2% NaCl using chloroform as an extracting solvent and methanol as a dispersing solvent. Further, the developed ILM-DLLME procedure has been successfully applied for the analysis of phospholipids in soybean samples in MALDI-MS. PMID:26276066

  2. In situ crosslinked smart polypeptide nanoparticles for multistage responsive tumor-targeted drug delivery

    Science.gov (United States)

    Yi, Huqiang; Liu, Peng; Sheng, Nan; Gong, Ping; Ma, Yifan; Cai, Lintao

    2016-03-01

    Smart tumor-targeted drug delivery is crucial for improving the effect of chemotherapy and reducing the adverse effects. Here, we synthesized a smart polypeptide copolymer based on n-butylamine-poly(l-lysine)-b-poly(l-cysteine) (PLL-PLC) with functionalization of folic acid (FA) and 1,2-dicarboxylic-cyclohexene anhydride (DCA) for multistage responsive tumor-targeted drug delivery. The copolymers (FA-PLL(DCA)-PLC) spontaneously crosslinked in situ to form redox and pH dual responsive FA-PLL(DCA)-PLC nanoparticles (FD-NPs), which had a reversible zeta potential around -30 mV at pH 7.4, but switched to +15 mV at pH 5.0. Moreover, FD-NPs effectively loaded DOX with a loading capacity at 15.7 wt%. At pH 7.4, only 24.5% DOX was released within 60 h. However, at pH 5.0, the presence of 10 mM DTT dramatically accelerated DOX release with over 90% of DOX released within 10 h. Although the FD-NPs only enhanced DOX uptake in FA receptor positive (FR+) cancer cells at pH 7.4, a weak acidic condition promoted FD-NP-facilitated DOX uptake in both FR+ HeLa and FR- A549 cells, as well as significantly improving cellular binding and end/lysosomal escape. In vivo studies in a HeLa cancer model demonstrated that the charge-reversible FD-NPs delivered DOX into tumors more effectively than charge-irreversible nanoparticles. Hence, these multistage responsive FD-NPs would serve as highly efficient drug vectors for targeted cancer chemotherapy.Smart tumor-targeted drug delivery is crucial for improving the effect of chemotherapy and reducing the adverse effects. Here, we synthesized a smart polypeptide copolymer based on n-butylamine-poly(l-lysine)-b-poly(l-cysteine) (PLL-PLC) with functionalization of folic acid (FA) and 1,2-dicarboxylic-cyclohexene anhydride (DCA) for multistage responsive tumor-targeted drug delivery. The copolymers (FA-PLL(DCA)-PLC) spontaneously crosslinked in situ to form redox and pH dual responsive FA-PLL(DCA)-PLC nanoparticles (FD-NPs), which had a reversible

  3. 高纯氢氧化镁非均相合成与表征%Synthesis and Characterization of High-purity Magnesium Hydroxide by Heterogenous Precipitation Method

    Institute of Scientific and Technical Information of China (English)

    王景峰; 周莹莹; 胡宏; 张勇

    2013-01-01

      报道了二正丁胺沉淀镁离子制备高纯度氢氧化镁粉体的方法,使用红外、热分析、X射线衍射表征了产物的纯度,使用扫描电镜观测了产物的表面形貌,对反应体系的热力学和动力学过程进行了研究。研究结果表明,所合成的氢氧化镁为片状结晶,具有结晶程度高、纯度高和粒度小的优点。该方法可控程度高,镁离子沉淀效率高,胺用量小,与氨法相比具有明显的优势,为氢氧化镁的合成提供了一种可行性高、工艺简单、条件温和的绿色化学方法。%  A method for preparing high pure Mg(OH)2 powders was reported by di-n-butylamine precipitating Mg2+. The purity was measured by FT-IR, TG and XRD, the surface topography was analyzed by SEM. The thermodynamic and kinetic process of reaction system was also discussed. The results showed that the magnesium hydroxide powders were flaky crystal with high purity, high crys-tallinity and smaller size. This method could be well controlled which provided a high feasibility, simple technology, green chemistry and mild conditions for the synthesis of magnesium hydroxide. Compared with ammonia method, this method had obvious advan-tages of high precipitation efficiency and little amine consumption.

  4. 利用高岭土合成ZSM-5沸石%Synthesis of ZSM-5 zeolite with kaoline

    Institute of Scientific and Technical Information of China (English)

    戴泳; 罗一斌; 王殿中

    2011-01-01

    The properties of Suzhou kaoline and the structure change of the kaoline calcined at different temperature were investigated. The contents of active SiO2 and Al2O3 of kaoline were determined by extraction test with alkali. ZSM-5 zeolites with higher relative crystallinity were synthesized by the methods with and without n-butylamine (NBA) and characterized by XRD, SEM and MAS NMR, etc. The results showed that the optimal calcination temperature of the kaoline was 950 ℃ ;the relative crystallinity of the kaoline synthesized with and without NBA reached 54.6% and 53.3% ,respectively;a lot of (3 ~7) nm mesopores in the products appeared, due to the formation of the cavities leaved by solution of active SiO2 and Al2O3 from kaoline surface.%对苏州高岭土的特性以及不同温度焙烧的高岭土结构变化进行了考察,以碱抽法确定其中的活性SiO2和活性Al2O3的含量,分别以有胺法(正丁胺)和无胺法合成得到较高相对结晶度的ZSM-5沸石,并对产物进行表征.结果表明,高岭土最佳焙烧温度为950℃,有胺法和无胺法合成的ZSM-5沸石相对结晶度分别达54.6%和53.3%,产物中出现大量的(3~7)nm中孔孔道,是由高岭土表面活性SiO2和AL2O3解聚留下的空穴形成.

  5. Study on Progress in Synthesis of Natural Product Curcumin%天然产物姜黄素合成工艺研究

    Institute of Scientific and Technical Information of China (English)

    邹春阳; 王凤秋; 田家明

    2011-01-01

    Curcumin was prepared by a modified method in this paper. Meanwhile, the optimum condition was also established. The mixture of acetylacetone and boric anhydride in ethyl acetate was stirred under reflux temperature for 30 minutes and gived a boron complex of acetylacetone. N - Butylamine was added dropwise to a solution of vanillin, tributyl borate and boron complex of acetylacetone in DMF (N, N -dimethylformamide) at 80X1. After stirred for 3 hours, crude curcumin was obtained by use 5% acetic acid to destroy the boron complex of curcumin. It was furtherly purified by re-crystallization from chloroform methanol. The overyield reaches 70% under the condition of inventory rating reaching one hundred grams - level. This method provides a reference for the large scale preparation of curcumin.%采用了一种改良的合成方法制备姜黄素,并确定了最优工艺条件.即:先将乙酰丙酮与硼酸酐于乙酸乙酯内回流反应30min,制得乙酰丙酮的硼络合物;然后在DMF(N,N-二甲基甲酰胺)中,将香兰素、三丁基硼酸酯及新制的乙酰丙酮的硼络合物于80℃,以正丁胺为催化剂反应3h;最后向其中加入5%的醋酸破坏络合物得到姜黄素粗品,以氯仿-甲醇重结晶得到姜黄素纯品.在投料量为百克级情况下,总收率达到了70%.这也为大量制备提供参考.

  6. Two-dimensional tin selenide nanostructures for flexible all-solid-state supercapacitors.

    Science.gov (United States)

    Zhang, Chunli; Yin, Huanhuan; Han, Min; Dai, Zhihui; Pang, Huan; Zheng, Yulin; Lan, Ya-Qian; Bao, Jianchun; Zhu, Jianmin

    2014-04-22

    Due to their unique electronic and optoelectronic properties, tin selenide nanostructures show great promise for applications in energy storage and photovoltaic devices. Despite the great progress that has been achieved, the phase-controlled synthesis of two-dimensional (2D) tin selenide nanostructures remains a challenge, and their use in supercapacitors has not been explored. In this paper, 2D tin selenide nanostructures, including pure SnSe2 nanodisks (NDs), mixed-phase SnSe-SnSe2 NDs, and pure SnSe nanosheets (NSs), have been synthesized by reacting SnCl2 and trioctylphosphine (TOP)-Se with borane-tert-butylamine complex (BTBC) and 1,3-dimethyl-3,4,5,6-tetrahydro-2(1H)-pyrimidinone. Utilizing the interplay of TOP and BTBC and changing only the amount of BTBC, the phase-controlled synthesis of 2D tin selenide nanostructures is realized for the first time. Phase-dependent pseudocapacitive behavior is observed for the resulting 2D nanostructures. The specific capacitances of pure SnSe2 NDs (168 F g(-1)) and SnSe NSs (228 F g(-1)) are much higher than those of other reported materials (e.g., graphene-Mn3O4 nanorods and TiN mesoporous spheres); thus, these tin selenide materials were used to fabricate flexible, all-solid-state supercapacitors. Devices fabricated with these two tin selenide materials exhibited high areal capacitances, good cycling stabilities, excellent flexibilities, and desirable mechanical stabilities, which were comparable to or better than those reported recently for other solid-state devices based on graphene and 3D GeSe2 nanostructures. Additionally, the rate capability of the SnSe2 NDs device was much better than that of the SnSe NS device, indicating that SnSe2 NDs are promising active materials for use in high-performance, flexible, all-solid-state supercapacitors. PMID:24601530

  7. ATR-FTIR characterization of transport properties of benzoic acid ion-pairs in silicone membranes.

    Science.gov (United States)

    Tantishaiyakul, Vimon; Phadoongsombut, Narubodee; Wongpuwarak, Wibul; Thungtiwachgul, Jatupit; Faroongsarng, Damrongsak; Wiwattanawongsa, Kamonthip; Rojanasakul, Yon

    2004-09-28

    A novel technique based on Attenuated Total Reflectance Fourier Transform Infrared (ATR-FTIR) spectroscopy was used to study the transport of benzoic acid ion-pairs/salts in silicone membranes. The benzoic acid ion-pairs were prepared using various counter-ions with different degrees of lipophilicity, e.g. triethylamine (TA), diethylamine (DE), tert-butylamine (t-BA), 2-amino-2-methyl-propanol (AMP), and 2-amino-2-methyl-propanediol (AMPD). Silicone membrane, treated or untreated with propylene glycol (PG), was placed on the surface of a ZnSe crystal and the transport solution was applied to the upper surface of the membrane. A mathematical model, based on Fick's second law describing the build up of permeant concentration at the membrane/crystal interface with time was applied to determine diffusion coefficients. Absorption due to the acid (1700 cm(-1)) or benzoate anion (1555 cm(-1)) was observed at different regions without the interference from PG or silicone membrane. Benzoate anion, a charged species, was observed to permeate the membrane. The permeation of benzoate anion from sodium benzoate and polar ion-pairs of AMP and AMPD was very low in contrast to their high-saturated concentrations in PG as compared to the t-BA ion-pair. This indicated that benzoate anion preferentially permeates the membrane as an ion-pair rather than a single anion; otherwise its permeation should correspond to its concentration in PG instead of the lipophilicity of the ion-pairs. Additionally, the diffusion coefficient values of benzoic acid and benzoate anions through the treated and untreated membranes were not statistically different. PMID:15363507

  8. Crystal engineered acid–base complexes with 2D and 3D hydrogen bonding systems using p-hydroxybenzoic acid as the building block

    Directory of Open Access Journals (Sweden)

    PU SU ZHAO

    2010-04-01

    Full Text Available p-Hydroxybenzoic acid (p-HOBA was selected as the building block for self-assembly with five bases, i.e., diethylamine, tert-butylamine, cyclohexylamine, imidazole and piperazine, and generation of the corresponding acid–base complexes 1–5. Crystal structure analyses suggest that proton-transfer from the carboxyl hydrogen to the nitrogen atom of the bases can be observed in 1–4, while only in 5 does a solvent water molecule co-exist with p--HOBA and piperazine. With the presence of O–H···O hydrogen bonds in 1–4, the deprotonated p-hydroxybenzoate anions (p-HOBAA– are simply connected each other in a head-to-tail motif to form one-dimensional (1D arrays, which are further extended to distinct two-dimensional (2D (for 1 and 4 and three-dimensional (3D (for 2 and 3 networks via N–H···O interactions. While in 5, neutral acid and base are combined pair-wise by O–H···N and N–H···O bonds to form a 1D tape and then the 1D tapes are sequentially combined by water molecules to create a 3D network. Some interlayer or intralayer C–H···O, C–H···p and p×××p interactions help to stabilize the supramolecular buildings. Melting point determination analyses indicate that the five acid–base complexes are not the ordinary superposition of the reactants and they are more stable than the original reactants.

  9. Synthesis of highly effective adsorbents from natural raw materials (zeolites)

    International Nuclear Information System (INIS)

    Natural raw materials bentonite, silica tuff and diatomaceous earth from Macedonia were used in synthesis of zeolites type A, ZSM-5 and multilayer silicate magadiite-adsorbents. The bentonite was subject to pretreatment with acids (HCl and H2SO4 - 5, 10, 15 and W%) or NaOH, and used in synthesis of zeolite type A having molar ratio of: 2Na2O : Al2O3 : 2SiO2 : 100H2O. Silicate tuff was applied (without any pretreatment, in a two stage reaction) in a high temperature synthesis, using butylamine as an organic 'template' component in order to get high silica zeolite type ZSM-5 having molar ratio of: 59.37SiO2 : Al2O3 : 3.84Na2O : 1.90R2O : 2025.10H2O. Multilayer silicate magadiite MS-H was synthesized from natural raw material diatomaceous earth. The product with a molar ratio of: 8SiO2 : Na2O : 75H2O showed the best characteristics. The proposed method of alkaline pretreatment is a new one and it is acceptable from the economy point of view due to low energy consumption. The conclusion shows that the final result of the synthesis was not perfect, i.e. it has 70% of zeolite ZSM-5 and the rest were some amorphous phases. This product is suitable for industrial application in catalytic processes due to the fact that commercial catalyst contain typically 20 to 50% of zeolite type ZSM-5. On the other hand, the magadiite being multilayer silicate with no aluminium inside, is well suited as a carrier due to its ability of intercalation. The experimental results indicate that natural raw materials from Macedonia could be used for synthesis of synthetical silicates with high qualities and acceptable overall costs, specially when alkaline pretreatment is used. 14 refs., 4 tabs., 11 figs

  10. Synthesis and reactivity of cyclic-carbamate derivatives%环状氨基甲酸酯衍生物的合成及反应研究

    Institute of Scientific and Technical Information of China (English)

    王静; 郭爽; 王家喜

    2011-01-01

    Cyclic carbamate has been prepared by the reaction of ethanolamine with dimethyl carbonate as raw material and zinc acetate as catalyst. The cyclic carbamate reacted with methyl acrylate producing methyl 3- (2-oxo-oxazolidin-3-yl) propanoate, which reacted with n-butylamine and 1,6-hexanediamine to give mono and bis cyclic carbamate derivatives. The attack of amine to carbonyl of heterocyclic ring of carbamate produced the hydroxylethyl substituted urea, while the attack to carbon-oxygen bond generated carbamic acid, which further underwent dehydration forming cyclic urea and/or de-carbon dioxide forming polyamine. The products were characterized by NMR and FT-IR. The reaction mechanism is finally proposed.%以乙醇胺和碳酸二甲酯为原料,在醋酸锌的催化下合成环状氨基甲酸酯,与丙烯酸甲酯反应制备3-(2-噁唑烷酮)丙酸甲酯,在K2CO3催化下进一步与正丁胺、1,6-己二胺发生酰胺化反应,得到了单、双环状氨基甲酸酯衍生物.有机胺与环状氨基甲酸酯的羰基反应形成羟乙基取代脲,与烷氧基反应形成开环的胺基甲酸,该化合物进一步脱水形成环状脲,脱二氧化碳形成多胺化合物.用NMR和红外谱图对开环产物进行表征,并初步探讨了其反应历程.

  11. Occurrence and profiling of multiple nitrosamines in source water and drinking water of China.

    Science.gov (United States)

    Wang, Wanfeng; Yu, Jianwei; An, Wei; Yang, Min

    2016-05-01

    The occurrence of multiple nitrosamines was investigated in 54 drinking water treatment plants (DWTPs) from 30 cities across major watersheds of China, and the formation potential (FP) and cancer risk of the dominant nitrosamines were studied for profiling purposes. The results showed that N-nitrosodimethylamine (NDMA), N-nitrosodiethylamine (NDEA) and N-nitrosodi-n-butylamine (NDBA) were the most abundant in DWTPs, and the concentrations in source water and finished water samples were not detected (ND) -53.6ng/L (NDMA), ND -68.5ng/L (NDEA), ND -48.2ng/L (NDBA). The frequencies of detection in source waters were 64.8%, 61.1% and 51.8%, and 57.4%, 53.7%, and 37% for finished waters, respectively. Further study indicated that the FPs of the three main nitrosamines during chloramination were higher than those during chlorination and in drinking water. The results of Principal Components Analysis (PCA) showed that ammonia was the most closely associated factor in nitrosamine formation in the investigated source water; however, there was no significant correlation between nitrosamine-FPs and the values of dominant water-quality parameters. The advanced treatment units (i.e., ozonation and biological activated carbon) used in DWTPs were able to control the nitrosamine-FPs effectively after disinfection. The target pollutants posed median and maximum cancer risks of 2.99×10(-5) and 35.5×10(-5) to the local populations due to their occurrence in drinking water. PMID:26896577

  12. Effect of different fat sources on in vitro degradation of nutrients and certain blood parameters in sheep.

    Science.gov (United States)

    Fébel, Hedvig; Husvéth, F; Veresegyházy, T; Andrásofszky, Emese; Várhegyi, Ildikó; Huszár, Szilvia

    2002-01-01

    This study was designed to determine the effects of calcium salt of palm oil fatty acids (CS), hydroxyethylsoyamide (HESA), butylsoyamide (BSA) and soybean oil (SO) on degradation of crude protein and fibre in vitro, and on the blood plasma lipid parameters in vivo. Five mature wethers (body weight 75 kg) were fed five diets in a 5 x 5 Latin square experiment. The control diet consisted of 50% meadow hay and 50% concentrate with no added fat. The control diet was supplemented with CS, HESA, BSA, or SO. Fat was added at 3.5% of dietary dry matter (DM). The final ether extract content of the ration was near 6%. Each period lasted 20 days. Fat supplements, except HESA, consistently decreased the in vitro DM disappearance of soybean meal as compared to control. In contrast to the effect of other treatments, crude protein degradation was greatest in the test tubes with inocula obtained from sheep fed diet with HESA. Fat supplements equally inhibited the DM and fibre breakdown of alfalfa pellet. CS and HESA seemed to be less detrimental to in vitro fermentation of neutral detergent fibre (NDF) than BSA and SO. All fat supplements increased blood plasma triglyceride, cholesterol and total lipid content. Plasma concentration of cholesterol and total lipid was highest with SO. The inclusion of CS in the diet increased 16:0, while all fat supplements increased plasma 18:0 and decreased 16:1 and 18:1 fatty acid content. Plasma 18:2n-6 was not changed by feeding CS and SO. However, compared to the control diet, 18:2n-6 increased with 12 and 41% in plasma fatty acids when sheep were fed HESA and BSA, respectively. The results showed that plasma concentration of linoleic acid was enhanced more when the amide was synthesised from butylamine than when from ethanolamine. PMID:12113177

  13. Labelling of endogenous target protein via N-S acyl transfer-mediated activation of N-sulfanylethylanilide.

    Science.gov (United States)

    Denda, Masaya; Morisaki, Takuya; Kohiki, Taiki; Yamamoto, Jun; Sato, Kohei; Sagawa, Ikuko; Inokuma, Tsubasa; Sato, Youichi; Yamauchi, Aiko; Shigenaga, Akira; Otaka, Akira

    2016-07-14

    The ligand-dependent incorporation of a reporter molecule (e.g., fluorescence dye or biotin) onto a endogenous target protein has emerged as an important strategy for elucidating protein function using various affinity-based labelling reagents consisting of reporter, ligand and reactive units. Conventional labelling reagents generally use a weakly activated reactive unit, which can result in the non-specific labelling of proteins in a ligand-independent manner. In this context, the activation of a labelling reagent through a targeted protein-ligand interaction could potentially overcome the problems associated with conventional affinity-based labelling reagents. We hypothesized that this type of protein-ligand-interaction-mediated activation could be accomplished using N-sulfanylethylanilide (SEAlide) as the reactive unit in the labelling reagent. Electrophilically unreactive amide-type SEAlide can be activated by its conversion to the corresponding active thioester in the presence of a phosphate salt, which can act as an acid-base catalyst. It has been suggested that protein surfaces consisting of hydrophilic residues such as amino, carboxyl and imidazole groups could function as acid-base catalysts. We therefore envisioned that a SEAlide-based labelling reagent (SEAL) bearing SEAlide as a reactive unit could be activated through the binding of the SEAL with a target protein. Several SEALs were readily prepared in this study using standard 9-fluorenylmethyloxycarbonyl (Fmoc)-based solid-phase protocols. These SEAL systems were subsequently applied to the ligand-dependent labelling of human carbonic anhydrase (hCA) and cyclooxyganese 1. Although we have not yet obtained any direct evidence for the target protein-mediated activation of the SEAlide unit, our results for the reaction of these SEALs with hCA1 or butylamine indirectly support our hypothesis. The SEALs reported in this study represent valuable new entries to the field of affinity-based labelling reagents

  14. Synthesis and profiling of [3H]trantinterol excretion following oral administration of rats

    Institute of Scientific and Technical Information of China (English)

    ZHANG Tian-hong; ZHANG Cheng; YANG Cui-ping; WANG Xiao-ying; LIAO Sha; SUN Mu-zhen; LI Jing-lai; ZHANG Zhen-qing

    2015-01-01

    OBJECTIVE To synthesize[3H]labelled trantinterol and determine the mass balance in rats and the profile of trantinterol and its metabolites in excreta. METHODS [3H]Trantinterol was synthesised from the intermediate1-(4-amino-3-chloro-5-trifluoromethyl-phenyl)-2-bromo-ethanone through reduction by sodium borotritide and aminolysis by t-butylamine. Following an oral dose of[3H] trantinterol(45.5 MBq·kg-1)to bile duct cannulated(BDC)rats and normal rats. Bile,urine and faeces were collected individually before and after dosing at different times. Liquid scintillation counter(LSC) was used to detect total radioactivity recovery and HPLC/radio-detector for metabolite profiling in urine and bile. RESULTS The majority(73.6%)of the administered radioactivity was recovered in the first 24 h postdose with 48.3%in urine and 25.4%in faeces. It was cumulated to(84.7±6.8)%till 168 h. In BDC rats,29.3%of the dose was recovered in the bile 3 d post-dose. According to the peak area ratio determined by HPLC/radio-detector,only 4.7%and 9.5%of the radioactive dose were excreted as the parent drug in urine and bile,respectively,while the majority of the remaining radioactivity was excreted in the form of various metabolites. CONCLUSION Following oral administration in rats,trantinterol is completely absorbed,extensively metabolized and rapidly excreted mainly in urine as various metabolites.

  15. Airborne thermal degradation products of polyurethene coatings in car repair shops.

    Science.gov (United States)

    Karlsson, D; Spanne, M; Dalene, M; Skarping, G

    2000-10-01

    A methodology for workplace air monitoring of aromatic and aliphatic, mono- and polyisocyanates by derivatisation with di-n-butylamine (DBA) is presented. Air sampling was performed using midget impinger flasks containing 10 ml of 0.01 mol l(-1) DBA in toluene and a glass-fibre filter in series after the impinger flask, thereby providing the possibility of collecting and derivatising isocyanates in both the gas and particle phases. Quantification was made by LC-MS, monitoring the molecular ions [MH]+. Air samples taken with this method in car repair shops showed that many different isocyanates are formed during thermal decomposition of polyurethane (PUR) coatings. In addition to isocyanates such as hexamethylene (HDI), isophorone (IPDI), toluene (TDI) and methylenediphenyl diisocyanate (MDI), monoisocyanates such as methyl (MIC), ethyl (EIC), propyl (PIC), butyl (BIC) and phenyl isocyanate (PhI) were found. In many air samples the aliphatic monoisocyanates dominated. During cutting and welding operations, the highest levels of isocyanates were observed. In a single air sample from a welding operation in a car repair shop, the highest concentrations found were: MIC, 290; EIC, 60; PIC, 20; BIC, 9; PhI, 27; HDI, 105; IPDI, 39; MDI, 4; and 2,4-TDI and 2,6-TDI 140 microg m(-3). Monitoring the particle size distribution and concentration during grinding, welding and cutting operations showed that ultrafine particles (volatility were mainly found in the particle phase, but isocyanates with a relatively high volatility such as TDI, were found in both the particle and gas phases. PMID:11254051

  16. The genotoxicities of N-nitrosamines in Drosophila melanogaster in vivo: the correlation of mutagenicity in the wing spot test with the DNA damages detected by the DNA-repair test.

    Science.gov (United States)

    Negishi, T; Shiotani, T; Fujikawa, K; Hayatsu, H

    1991-04-01

    The genotoxicities of a series of N-nitrosamines were assayed in the wing spot test and a new short-term test of Drosophila melanogaster. In the spot test, larval flies trans-heterozygous for the somatic cell markers mwh and flr3 were fed the test reagents and the wing hairs in adults were inspected for clones expressing the phenotypes of the markers. In the other test, larval stock consisting of meiotic recombination-deficient (Rec-) double mutant mei-9a and mei-41D5 males and repair-proficient Rec+ females were grown on feed containing the reagents and the DNA damages were detected with the preferential killing of the Rec- larvae as an endpoint. The carcinogenic nitrosamines tested, N-nitrosodimethylamine (NDMA), N-nitrosodiethylamine (NDEA), N-nitrosodi-n-butylamine (NDBA), N-nitrosomorpholine (NMOR), N-nitro-sopiperidine (NPIP) and N-nitrosopyrrolidine (NPYR), all showed clearly positive activities in both tests. The activities in the wing spot test were ranked in a sequence of NDMA much greater than NMOR greater than NPIP greater than NDEA greater than NPYR greater than NDBA. A similar ranking was obtained in the repair assay. The genotoxicity of N-nitrosodiphenylamine (NDPhA), carcinogenicity studies of which are inconclusive, was marginal in the spot test. The non-carcinogenic N-nitrosoproline (NPRO) and the non-mutagenic N-nitrosothioproline (NTPRO) were negative in the spot test. NDPhA and NPRO were negative in the repair test as well. The DNA-repair test is thus a convenient technique for estimating the mutagenicity of compounds because of its simplicity compared with the wing spot test. These Drosophila tests may be useful in predicting carcinogenic potentials of compounds. PMID:1901957

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-07-01

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

  18. 15th International Sunflower Conference Synthesis of new derivatives from vegetable sunflower oil methyl esters via epoxydation and oxirane opening

    Directory of Open Access Journals (Sweden)

    Pages Xavier

    2001-03-01

    Full Text Available Recently, epoxides have received increased attention because they are of interest both as end-products and as chemical intermediates; epoxidized oils, mainly High Oleic Sunflower Oil, and their ester derivatives have thus found important applications as plasticizers and additives for polyvinyl chloride (PVC. Epoxidized esters have been produced classically from High Oleic Sunflower Methyl Esters (HOSME using H2O2 and formic acid. The epoxidation reaches 90% on pilot scale (5kg. Epoxidized esters produced from HOSME have respectively hydroxyl values of 0, oxirane values of 5.2/4.5 and iodine values of 1.7/1.5. Cleavage trials of the oxirane group of the epoxidized esters with different reactants have been undertaken in order to produce on pilot scale new derivatives to be characterized and tested in different fields of application (lubrication, detergency and as chemical intermediates. Reaction of Epoxy-HOSME with an excess of oleic acid was conducted under atmospheric pressure without any catalyst and solvent. The oxirane opening leads to complete estolide formation: after neutralization, analytical controls (chemical values, GC and HPLC analysis indicate that the estolides are composed of a mixture of C36 (oleate of methyl hydroxystearate and C54 (di-oleate of methyl dihydroxystearate. Oxirane opening with alcohols (ethanol and octanol was preferentially performed by acid catalysis at 100°C under atmospheric pressure. Analytical controls show the formation of different etheralcohols and secondary products resulting from dehydration, transesterification and dimerization side-reactions. Cleavage reaction of Epoxy-HOSME with a primary amine (butylamine was conducted under pressure, at high temperature (180/200°C. Both transesterification and opening of the oxirane group occur under these conditions. Reaction products are composed of amides formed by transesterification and a mixture of fatty amines/imines obtained by ring opening as established

  19. TUNGSTOPHOSPHORIC ACID HETEROGENIZED ONTO NH4ZSM5 AS AN EFFICIENT AND RECYCLABLE CATALYST FOR THE PHOTOCATALYTIC DEGRADATION OF DYES

    Directory of Open Access Journals (Sweden)

    Candelaria Leal Marchena

    2015-05-01

    Full Text Available Materials based on tungstophosphoric acid (TPA immobilized on NH4ZSM5 zeolite were prepared by wet impregnation of the zeolite matrix with TPA aqueous solutions. Their concentration was varied in order to obtain TPA contents of 5%, 10%, 20%, and 30% w/w in the solid. The materials were characterized by N2 adsorption-desorption isotherms, XRD, FT-IR, 31P MAS-NMR, TGA-DSC, DRS-UV-Vis, and the acidic behavior was studied by potentiometric titration with n-butylamine. The BET surface area (SBET decreased when the TPA content was raised as a result of zeolite pore blocking. The X-ray diffraction patterns of the solids modified with TPA only presented the characteristic peaks of NH4ZSM5 zeolites, and an additional set of peaks assigned to the presence of (NH43PW12O40. According to the Fourier transform infrared and 31P magic angle spinning-nuclear magnetic resonance spectra, the main species present in the samples was the [PW12O40]3- anion, which was partially transformed into the [P2W21O71]6- anion during the synthesis and drying steps. The thermal stability of the NH4ZSM5TPA materials was similar to that of their parent zeolites. Moreover, the samples with the highest TPA content exhibited band gap energy values similar to those reported for TiO2. The immobilization of TPA on NH4ZSM5 zeolite allowed the obtention of catalysts with high photocatalytic activity in the degradation of methyl orange dye (MO in water, at 25 ºC. These can be reused at least three times without any significant decrease in degree of degradation.

  20. Investigating the Synthesis of Ligated Metal Clusters in Solution Using a Flow Reactor and Electrospray Ionization Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Olivares, Astrid M.; Laskin, Julia; Johnson, Grant E.

    2014-09-18

    The scalable synthesis of subnanometer metal clusters containing an exact number of atoms is of interest due to the highly size-dependent catalytic, electronic and optical properties of these species. While significant research has been conducted on the batch preparation of clusters through reduction synthesis in solution, the processes of metal complex reduction as well as cluster nucleation, growth and post-reduction etching are still not well understood. Herein, we demonstrate a temperature-controlled flow reactor for studying cluster formation in solution at well-defined conditions. Employing this technique methanol solutions of a chloro(triphenylphosphine)gold precursor, 1,4-bis(diphenylphosphino)butane capping ligand and borane-tert-butylamine reducing agent were combined in a mixing tee and introduced into a heated capillary with an adjustable length. In this manner, the temperature dependence of the relative abundance of different ionic reactants, intermediates and products synthesized in real time was characterized using online mass spectrometry. A wide distribution of doubly and triply charged cationic gold clusters was observed as well as smaller singly charged metal-ligand complexes. The results demonstrate that temperature plays a crucial role in determining the relative population of cationic gold clusters and, in general, that higher temperature promotes the formation of doubly charged clusters and singly charged metal-ligand complexes while hindering the growth of triply charged clusters. Moreover, the distribution of clusters observed at elevated temperatures is found to be consistent with that obtained at longer reaction times at room temperature, thereby demonstrating that heating may be used to access cluster distributions characteristic of different stages of reduction synthesis in solution.

  1. Isotope separation by chemical exchange

    International Nuclear Information System (INIS)

    Nitrogen-15 and oxygen-18 enrichment by chemical exchange in the (NO/NO2) - (H2O/HNO3) system, using a laboratory-scale experimental plant and a cascade for production of two isotopes, is presented. The results obtained from the laboratory-scale plant indicate that optimal flow rate for 15N separation is 1.55 - 1.86 ml/cm2 · min at 8 - 10 M/l nitric acid and 63.4 mg at. oxygen/cm2 · min for 18O separation at 5.8 M/l nitric acid. The height equivalent to a theoretical plate (HETP) of 4.11 - 4.56 cm is in good agreement with other published data for 15N separation using exchange column with Helipak packing. The HETP of 7.74 - 10.58 cm for 18O separation is greater by 20 - 30 % than those presented by Saxena and Taylor for 'Helipak' column packing, but in good agreement with the HRTP published by Borisov et al. on 'Levina' column packing. The HETP obtained for 15N separation by the production plant is in the range 11.5 - 13.8 cm at a flow rate of 2.2 ml HNO3(10M/l)/cm2 · min for the first column and 4.4 - 4.7 cm at a flow rate of 1.66 ml HNO3(10M/l)/cm2 · min for the second column. The optimal flow rate for 18O separation by the production plant is about 63 mg at. oxygen/cm2 · min (1.01 ml HNO3/cm2 · min). Enrichment of 13C and 18O by chemical exchange of carbon dioxide with its monoethanolamine carbamate in methanol and di-n-butylamine carbamate in triethylamine has also been studied, and optimum operating conditions for the separation of 13C in a packed column was determined. The HETP obtained for the 13C in a packed column was determined. The HETP obtained for the 13C separation column is 3.62 - 8.26 cm at a flow rate of 1.1 - 4.0 mmol carbamate/cm2 · min using the same column packing as for 15N and 18O separation, that is, stainless steel triangular wire springs (2.3 x 2.3 x 0.2 mm). (author)

  2. High-Performance Supercapacitor of Functionalized Carbon Fiber Paper with High Surface Ionic and Bulk Electronic Conductivity: Effect of Organic Functional Groups

    International Nuclear Information System (INIS)

    Highlights: • A supercapacitor of organic functionalized carbon fiber paper (f-CFP) exhibits high areal and volumetric capacitances. • The performance of the supercapacitor depends on the organic functional group on the surface of the f-CFP. • Hydroxyl and carboxylic groups modified on the surface of f-CFP have higher pseudocapacitive property than amide and amine functional groups. • The f-CFP exhibits high surface ionic and bulk electrical conductivities. - Abstract: Although carbon fiber paper (CFP) or nonwovens are widely used as a non-corrosive and conductive substrate or current collector in batteries and supercapacitors as well as a gas diffusion layer in proton exchange membrane fuel cells, the CFP cannot store charges due to its poor ionic conductivity and its hydrophobic surface. In this work, the chemically functionalized CFP (f-CFP) consisting of hydroxyl and carboxylic groups on its surface was produced by an oxidation reaction of CFP in a mixed concentrated acid solution of H2SO4:HNO3 (3:1 v/v) at 60 °C for 1 h. Other amide and amine groups modified CFP were also synthesized for comparison using a dehydration reaction of carboxylic modified CFP with ethylenediamine and n-butylamine. Interestingly, it was found that hydroxyl and carboxylic groups modified CFP behave as a pseudocapacitor electrode, which can store charges via the surface redox reaction in addition to electrochemical double layer capacitance. The aqueous-based supercapacitor of f-CFP has high areal, volumetric, and specific energy (49.0 μW.h/cm2, 1960 mW.h/L, and 5.2 W.h/Kg) and power (3.0 mW/cm2, 120 W/L, and 326.2 W/Kg) based on the total geometrical surface area and volume as well as the total weight of positive and negative electrodes. High charge capacity of the f-CFP stems from high ionic charge and pseudocapacitive behavior due to hydroxyl and carboxylic groups on its surface and high bulk electronic conductivity (2.03 mS/cm) due to 1D carbon fiber paper. The acid

  3. Determination of eight nitrosamines in water at the ng L{sup -1} levels by liquid chromatography coupled to atmospheric pressure chemical ionization tandem mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Ripolles, Cristina; Pitarch, Elena; Sancho, Juan V.; Lopez, Francisco J. [Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat, E-12071 Castellon (Spain); Hernandez, Felix, E-mail: felix.hernandez@qfa.uji.es [Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat, E-12071 Castellon (Spain)

    2011-09-19

    Highlights: {center_dot} Eight N-nitrosamines in water by LC(APCI)MS/MS QqQ analysis. {center_dot} Validation at two levels: 10 ng L{sup -1} (LOQ) and 100 ng L{sup -1} in drinking water. {center_dot} Developed method applied to different types of water samples. {center_dot} NDMA was the analyte more frequently detected and at the highest concentration levels. - Abstract: In this work, we have developed a sensitive method for detection and quantification of eight N-nitrosamines, N-nitrosodimethylamine (NDMA), N-nitrosomorpholine (NMor), N-nitrosomethylethylamine (NMEA), N-nitrosopirrolidine (NPyr), N-nitrosodiethylamine (NDEA), N-nitrosopiperidine (NPip), N-nitroso-n-dipropylamine (NDPA) and N-nitrosodi-n-butylamine (NDBA) in drinking water. The method is based on liquid chromatography coupled to tandem mass spectrometry, using atmospheric pressure chemical ionization (APCI) in positive mode with a triple quadrupole analyzer (QqQ). The simultaneous acquisition of two MS/MS transitions in selected reaction monitoring mode (SRM) for each compound, together with the evaluation of their relative intensity, allowed the simultaneous quantification and reliable identification in water at ppt levels. Empirical formula of the product ions selected was confirmed by UHPLC-(Q)TOF MS accurate mass measurements from reference standards. Prior to LC-MS/MS QqQ analysis, a preconcentration step by off-line SPE using coconut charcoal EPA 521 cartridges (by passing 500 mL of water sample) was necessary to improve the sensitivity and to meet regulation requirements. For accurate quantification, two isotope labelled nitrosamines (NDMA-d{sub 6} and NDPA-d{sub 14}) were added as surrogate internal standards to the samples. The optimized method was validated at two concentration levels (10 and 100 ng L{sup -1}) in drinking water samples, obtaining satisfactory recoveries (between 90 and 120%) and precision (RSD < 20%). Limits of detection were found to be in the range of 1-8 ng L{sup -1

  4. In-situ Studies of the Reactions of Bifunctional and Heterocyclic Molecules over Noble Metal Single Crystal and Nanoparticle Catalysts Studied with Kinetics and Sum-Frequency Generation Vibrational Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Kliewer, Christopher J. [Univ. of California, Berkeley, CA (United States)

    2009-06-30

    Sum frequency generation surface vibrational spectroscopy (SFG-VS) in combination with gas chromatography (GC) was used in-situ to monitor surface bound reaction intermediates and reaction selectivities for the hydrogenation reactions of pyrrole, furan, pyridine, acrolein, crotonaldehyde, and prenal over Pt(111), Pt(100), Rh(111), and platinum nanoparticles under Torr reactant pressures and temperatures of 300K to 450K. The focus of this work is the correlation between the SFG-VS observed surface bound reaction intermediates and adsorption modes with the reaction selectivity, and how this is affected by catalyst structure and temperature. Pyrrole hydrogenation was investigated over Pt(111) and Rh(111) single crystals at Torr pressures. It was found that pyrrole adsorbs to Pt(111) perpendicularly by cleaving the N-H bond and binding through the nitrogen. However, over Rh(111) pyrrole adsorbs in a tilted geometry binding through the {pi}-aromatic orbitals. A surface-bound pyrroline reaction intermediate was detected over both surfaces with SFG-VS. It was found that the ring-cracking product butylamine is a reaction poison over both surfaces studied. Furan hydrogenation was studied over Pt(111), Pt(100), 10 nm cubic platinum nanoparticles and 1 nm platinum nanoparticles. The product distribution was observed to be highly structure sensitive and the acquired SFG-VS spectra reflected this sensitivity. Pt(100) exhibited more ring-cracking to form butanol than Pt(111), while the nanoparticles yielded higher selectivities for the partially saturated ring dihydrofuran. Pyridine hydrogenation was investigated over Pt(111) and Pt(100). The α-pyridyl surface adsorption mode was observed with SFG-VS over both surfaces. 1,4-dihydropyridine was seen as a surface intermediate over Pt(100) but not Pt(111). Upon heating the surfaces to 350K, the adsorbed pyridine changes to a flat-lying adsorption mode. No evidence was found for the pyridinium cation. The hydrogenation of the

  5. The Influences of Surface Passivation on Luminescence Properties of Porous Silicon%多孔硅表面钝化对其发光性能的影响

    Institute of Scientific and Technical Information of China (English)

    李宏建; 瞿述; 剪之渐; 彭景翠; 向建南

    2000-01-01

    By using n-butylamine as carbon resource,a layer of carbon film is covered on the parous silicon(PS)surface by means of radio frequency glow discharge.Raman spectra and IR spectra of the carbon film indicate that there are amino-groups and hydrogen atoms in the carbon film.IR spectra exhibits that the surface of the treated sample is mainly covered with Si-C,Si-N and Si-O.The influences of surface passivation of photoluminescence and electroluminescence properties of porous silicon have been presented.PL and EL spectra indicate that PL and EL intensity of the treated samples increase greatly and the blueshift of PL and EL peak compared with the samples without treatment and stable while storing in atmosphere.I~V characteristics reveal that the treated devices have a lower onset voltage.We present that the enhancement of the PL and EL intensity、stability and lower onset voltage of the treated sample is due to the existence of Si-C,Si-N and Si-O on the PS surface simultaneously,and blueshift of the PL and El peak are attributed to amino-groups and hydrogen atmos in the carbon film,As a result,carbon film passivation is a good way to enhance PS luminescent intensity and stability and improve the properties of PS devices.%报道多孔硅(PS)的表面钝化对其光致发光(PL)和电致发光(EL)的影响。PL和EL谱表明,经钝化处理的PS的PL和EL强度明显增强,且发光峰位较大蓝移;存放实验表明,经钝化处理的PS的PL和EL发光强度和发光峰位具有较好的稳定性;I~V曲线显示,经钝化处理的PS发光器件具有较低的启动电压。这些结果表明:用钝化处理的方法是提高PS的PL和EL强度和稳定性及改善其器件性能的有效途径。

  6. Determination of 10 Volatile Nitrosamines in Cosmetics by Gas Chromatography-Tandem Mass Spectrometry%气相色谱-串联质谱法同时测定化妆品中的10种挥发性亚硝胺

    Institute of Scientific and Technical Information of China (English)

    马强; 席海为; 王超; 白桦; 席广成; 苏宁; 徐丽艳; 王军兵

    2011-01-01

    建立了同时测定化妆品中10种挥发性亚硝胺(N-亚硝基二甲基胺,N-亚硝基二乙基胺、N-亚硝基二正丙基胺、N-亚硝基吗啉、N-亚硝基毗咯烷、N-亚硝基哌啶,N-亚硝基二正丁基胺、N-亚硝基二苯基胺、N-亚硝基二环己基胺及N-亚硝基二苄基胺)的气相色谱-串联质谱分析方法.膏霜、水剂、散粉、香波、唇膏等不同类型的化妆品样品分别采用适宜的提取溶剂经超声提取后,样品提取液高速离心处理,上清液以Oasis HLB固相萃取柱净化,收集甲醇洗脱液,DB-624(30 m × 0.25 mm,1.40 μm)石英毛细管色谱柱分离后经El-GC-MS/MS多反应监测技术进行定性及定量分析.10种挥发性亚硝胺的方法定量限为2.5-10 mg/kg;在低、中、高的3个添加水平的平均回收率为85.2%-102.3%;相对标准偏差为3.0%-9.2%.本方法准确、快速、灵敏度高,可用于化妆品的实际检验.%A comprehensive analytical method based on gas chromatography tandem mass spectrome-try has been developed for the determination of 10 volatile nitrosamines (N-nitrosodimethylamine, N-nitrosodiethylamine, N-nitrosodi-n-propylamine, N-nitrosomorpholine, N-nitrosopyrrolidine, N-nitrosopiperidine, N-nitrosodi-n-butylamine, N-nitrosodiphenylamine, N-nitrosodicyclohexylamine and N-nitrosodibenzylamine) in cosmetics. Various cosmetic samples, including cream, lotion, powder, shampoo and lipstick, were extracted with appropriate solvents under ultrasonication. The extract was centrifuged, and the upper solution was then cleaned up by an Oasis HLB solid phase extraction cartridge. Qualitative and quantitative analysis was carried out for the analytes under the MRM mode after the chromatographic separation on a DB-624 (30 m×0. 25 mm, 1. 40 μm) capillary column. The limits of quantitation (LOQs) for 10 volatile nitrosamines were 2. 5 -10 mg/kg. The mean recoveries at the three spiked levels were 85. 2% -102. 3%, with the relative standard devia

  7. Coverage Dependent Charge Reduction of Cationic Gold Clusters on Surfaces Prepared Using Soft Landing of Mass-selected Ions

    Energy Technology Data Exchange (ETDEWEB)

    Johnson, Grant E.; Priest, Thomas A.; Laskin, Julia

    2012-11-29

    The ionic charge state of monodisperse cationic gold clusters on surfaces may be controlled by selecting the coverage of mass-selected ions soft landed onto a substrate. Polydisperse diphosphine-capped gold clusters were synthesized in solution by reduction of chloro(triphenylphosphine)gold(I) with borane tert-butylamine in the presence of 1,3-bis(diphenylphosphino)propane. The polydisperse gold clusters were introduced into the gas phase by electrospray ionization and mass selection was employed to select a multiply charged cationic cluster species (Au11L53+, m/z = 1409, L = 1,3-bis(diphenylphosphino)propane) which was delivered to the surfaces of four different self-assembled monolayers on gold (SAMs) at coverages of 1011 and 1012 clusters/mm2. Employing the spatial profiling capabilities of in-situ time-of-flight secondary ion mass spectrometry (TOF-SIMS) it is shown that, in addition to the chemical functionality of the monolayer (as demonstrated previously: ACS Nano, 2012, 6, 573) the coverage of cationic gold clusters on the surface may be used to control the distribution of ionic charge states of the soft-landed multiply charged clusters. In the case of a 1H,1H,2H,2H-perfluorodecanethiol SAM (FSAM) almost complete retention of charge by the deposited Au11L53+ clusters was observed at a lower coverage of 1011 clusters/mm2. In contrast, at a higher coverage of 1012 clusters/mm2, pronounced reduction of charge to Au11L52+ and Au11L5+ was observed on the FSAM. When soft landed onto 16- and 11-mercaptohexadecanoic acid surfaces on gold (16,11-COOH-SAMs), the mass-selected Au11L53+ clusters exhibited partial reduction of charge to Au11L52+ at lower coverage and additional reduction of charge to both Au11L52+ and Au11L5+ at higher coverage. The reduction of charge was found to be more pronounced on the surface of the shorter (thinner) C11 than the longer (thicker) C16-COOH-SAM. On the surface of the 1-dodecanethiol (HSAM) monolayer, the most abundant charge state

  8. Determination of PASHs by various analytical techniques based on gas chromatography-mass spectrometry: application to a biodesulfurization process.

    Science.gov (United States)

    Mezcua, Milagros; Fernández-Alba, Amadeo R; Boltes, Karina; Alonso Del Aguila, Raul; Leton, Pedro; Rodríguez, Antonio; García-Calvo, Eloy

    2008-06-15

    . Recoveries of the selected compound in both media were studied. They were in the range of 80-100% for the watery and in the range of 40-60% for the organic phase, respectively. Gas chromatography coupled to mass spectrometry (GC-MS) has been employed for the identification of these selected compounds. Three different ionization modes were applied: conventional electron impact (EI); positive chemical ionization (PCI), using methane as the reagent gas; and a recently developed ionization mode known as hybrid chemical ionization (HCI), using perfluorotri-n-butylamine as the reagent gas. Limits of detection and identification capabilities have been compared between the three analytical techniques. The sensitivity of the three analytical techniques was studied and LOD between 0.05 and 1, between 0.09 and 2 and between 0.001 and 0.043 were achieved for PCI, EI and HCI, respectively. The developed method was applied in samples from a biodesulfurization process. The biodesulfurization reactions were conducted in resting cell operation mode, using Erlenmeyer flasks or an agitated tank bioreactor. The microorganism employed was Pseudomonas putida CECT 5279. The reaction was performed under controlled air flow, stirring and temperature conditions. PMID:18585197