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Sample records for butylamine

  1. Fiber-optic sensor for butylamine

    Energy Technology Data Exchange (ETDEWEB)

    Boldov, I A; Kuchyanov, A S; Plekhanov, A I [Institute of Automation and Electrometry SB RAS, Novosibirsk (Russian Federation); Orlova, N A; Kargapolova, I Yu; Shelkovnikov, V V, E-mail: boldov.ivan@gmail.com [Novosibirsk Institute of Organic Chemistry SB RAS, Novosibirsk (Russian Federation)

    2011-04-01

    Fiber-optic chemical sensor for butylamine was realized. The sensor includes a thin layer nanostructure on the end of optical fiber with a diameter of 600 {mu}m. It consists of luminescent silica nanoparticles modified with pyrylocyanine dye, silver nanoparticles and photonic-crystal film. The sensitivity of the sensor is increased tenfold due to an additional covering of the film with photonic crystal as a porous mirror and the injection of silver nanoparticles with a diameter of 5-7 nm.

  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. 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.

  4. 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.

  5. 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.

  6. 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.

  7. 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.

  8. 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

  9. 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

  10. 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)

  11. 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)

  12. 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.

  13. Construction of 1D SnO2-coated ZnO nanowire heterojunction for their improved n-butylamine sensing performances

    Science.gov (United States)

    Wang, Liwei; Li, Jintao; Wang, Yinghui; Yu, Kefu; Tang, Xingying; Zhang, Yuanyuan; Wang, Shaopeng; Wei, Chaoshuai

    2016-10-01

    One-dimensional (1D) SnO2-coated ZnO nanowire (SnO2/ZnO NW) N-N heterojunctions were successfully constructed by an effective solvothermal treatment followed with calcination at 400 °C. The obtained samples were characterized by means of XRD, SEM, TEM, Scanning TEM coupled with EDS and XPS analysis, which confirmed that the outer layers of N-type SnO2 nanoparticles (avg. 4 nm) were uniformly distributed onto our pre-synthesized n-type ZnO nanowire supports (diameter 80~100 nm, length 12~16 μm). Comparisons of the gas sensing performances among pure SnO2, pure ZnO NW and the as-fabricated SnO2/ZnO NW heterojunctions revealed that after modification, SnO2/ZnO NW based sensor exhibited remarkably improved response, fast response and recovery speeds, good selectivity and excellent reproducibility to n-butylamine gas, indicating it can be used as promising candidates for high-performance organic amine sensors. The enhanced gas-sensing behavior should be attributed to the unique 1D wire-like morphology of ZnO support, the small size effect of SnO2 nanoparticles, and the semiconductor depletion layer model induced by the strong interfacial interaction between SnO2 and ZnO of the heterojunctions. The as-prepared SnO2/ZnO NW heterojunctions may also supply other novel applications in the fields like photocatalysis, lithium-ion batteries, waste water purification, and so on.

  14. 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.

  15. 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

  16. 气相色谱法测定果蔬中防腐剂仲丁胺残留量%GC Determination of Residual Amount of the Preservative Butylamine in Fruits and Vegetables

    Institute of Scientific and Technical Information of China (English)

    郝蔚霞

    2012-01-01

    提出了气相色谱法测定果蔬中防腐剂仲丁胺残留量的方法。果蔬样品经匀浆处理后置于顶空瓶中,在碱性条件下于55℃恒温平衡40min。吸取100μL液上气体注入气相色谱仪,用氮磷检测器测定,外标法定量。仲丁胺的质量浓度在0.000 5~0.040 0mg.L-1范围内与其峰面积呈线性关系,检出限(3S/N)为0.5μg.L-1。在两个浓度水平上对方法进行回收试验,测得回收率在87.4%~102.8%之间,测定值的相对标准偏差(n=10)在2.6%~9.6%之间。%A method of GC for determination of residual amount of the preservative butylamine in fruits and vegetables was proposed.After pounding and homogenization,the sample of fruit or vegetable was weighed into a head-space bottle,and equilibrated for 40 min in an alkaline solution at 55 ℃.A portion of 100 μL of the gas over the liquid solution was taken and injected into the instrument for GC analysis,with NPD and external standard calibration.Linear relationship between values of peak area and mass concentration of butylamine was obtained in the range of 0.000 5-0.040 0 mg·L-1,with detection limit(3S/N) of 0.5 μg·L-1.Recovery was tested at 2 concentration levels,the results found were in the range of 87.4%-102.8%,with values of RSD(n=10) ranged form 2.6%-9.6%.

  17. Effect of protonation on the isomerization properties of n-butylamine Schiff base of isomeric retinal as revealed by direct HPLC analyses: selection of isomerization pathways by retinal proteins.

    Science.gov (United States)

    Koyama, Y; Kubo, K; Komori, M; Yasuda, H; Mukai, Y

    1991-09-01

    Alumina adsorption chromatography and ion-pair reversed-phase chromatography were developed to analyze the isomers of unprotonated and protonated n-butylamine Schiff base of retinal (RSB and PRSB), respectively. Photoisomerization starting from the all-trans, 11-cis and 13-cis isomers was traced for RSB in n-hexane, acetonitrile, methanol and 1-butanol, and for PRSB in methanol, acetonitrile and 1-butanol. The quantum yields of photoisomerization for the all-trans, 9-cis, 11-cis and 13-cis isomers were determined for RSB and PRSB in the above solvents except 1-butanol. On the other hand, photoisomerization of isomeric retinal bound (through Schiff base linkage) to bovine serum albumin (RBSA) in aqueous solution (pH 3, 7 and 12) as well as thermal isomerization of RSB (in n-hexane), PRSB (in methanol) and RBSA (in aqueous solution, pH 7) were traced starting from the all-trans, 11-cis, and 13-cis isomers. Protonation of RSB drastically changes the pathway of photoisomerization and increases the quantum yields of isomeric RSB. The solvent polarity increases the quantum yields of RSB differently depending on the configuration. Protonation enhances thermal isomerization also. The results of the above model systems are compared with those of retinal proteins to rationalize their selection of the particular isomerization pathways.

  18. 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.

  19. Synthesis of 4- (5-Quinolin-3-yl-tetrazol-2-yl) butylamine%4-(5-喹啉-3-基-四氮唑-2-基)丁胺的合成

    Institute of Scientific and Technical Information of China (English)

    郭葆秦; 陈卫民

    2011-01-01

    Quinoline-3-carbonitrile(l) was synthesized by cyanogenation of 3-bromoquinoline with Zn (CN)2 using Pd(PPh3)4 as the catalyst. 3-(2H-tetrazol-5-yl)quinoline(2) was prepared by [2 +3] cycloaddition of 1 with sodium azide. 2 reacted with N-(4-bromobutyl)phthalimide to obtain 2-[4-(5-quinolin-3-yl-tetrazol-2-yl) butyl] isoindole-1,3-dione (3). 4-( 5-Quinolin-3-yl-tetrazol-2-yl) bu-tylamine(4) was synthesized by hydrazinolysis of 3. The structures of 1 ~4 were characterized by NMR and MS. 2 ~ 4 of them were new compounds.%三苯基膦钯催化3-溴喹啉完成氰化取代制得3-氰喹啉(1);1与叠氮化钠经[2+3]环加成合成了3-(2H-四氮唑-5-基)喹啉(2);2与N-(4-溴丁基)邻苯二甲酰亚胺反应制得2-[4-(5-喹啉-3-基-四氮唑-2-基)丁基]异吲哚-1,3-二酮(3);3经肼解合成了4-(5-喹啉-3-基-四氮唑-2-基)丁胺(4),1~4的结构经NMR和MS表征,其中2~4未见文献报道.

  20. 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

  1. Unprecedented Catalytic Wet Oxidation of Glucose to Succinic Acid Induced by the Addition of n-Butylamine to a Ru(III) Catalyst.

    Science.gov (United States)

    Podolean, Iunia; Rizescu, Cristina; Bala, Camelia; Rotariu, Lucian; Parvulescu, Vasile I; Coman, Simona M; Garcia, Hermenegildo

    2016-09-01

    A new pathway for the catalytic wet oxidation (CWO) of glucose is described. Employing a cationic Ru@MNP catalyst, succinic acid is obtained in unprecedently high yield (87.5 %) for a >99.9 % conversion of glucose, most probably through a free radical mechanism combined with catalytic didehydroxylation of vicinal diols and hydrogenation of the resulted unsaturated intermediate. PMID:27511900

  2. 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.

  3. 沙丁胺醇、布地耐德联合吸入治疗小儿毛细支气管炎疗效观察%The sand butylamine mellow,the cloth bears the German union inspiration to treat the young child capillarity bronchitis curative effect observation

    Institute of Scientific and Technical Information of China (English)

    叶红玲

    2010-01-01

    目的:观察沙丁胺醇雾化液与布地奈德混悬液联合雾化吸入治疗毛细支气管炎的疗效.方法:将60例毛细支气管炎患儿随机分为两组,治疗组30例,对照组30例.两组均予常规抗炎、吸氧、止咳、平喘、静脉补液等治疗.治疗组在此基础上加用沙丁胺醇0.03ml/kg+盐水至2ml氧气雾化吸入,间隔4-6小时后布地耐德1ml+盐水1ml氧气雾化吸入,每日二次.结果:治疗组的总有效率为93%,对照组为67%.两组比较差异有显著性(P < 0.05).结论:沙丁胺醇雾化液与布地奈德混悬液联合雾化吸入可尽快缓解喘憋症状,缩短毛细支气管炎的病程及住院时间.

  4. 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.

  5. Preintercalation of Layered γ-Zirconium Phosphate for Preparation of Immobilized Hemoglobin

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    Layeredγ-Zirconium phosphate (γ-ZrP) preintercalated with butylamine, tetra (n-butylammonium)hydroxide, dimethylamine respectively, or only ultrasonificated, for preparation of immobilized hemoglobin were investigated in this report.

  6. 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.

  7. 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)

  8. 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.

  9. 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.

  10. 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.

  11. 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.

  12. 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...

  13. 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 ...

  14. 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...

  15. 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...

  16. 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.

  17. 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.

  18. 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

  19. Preparation of porous lanthanum phosphate with templates

    Energy Technology Data Exchange (ETDEWEB)

    Onoda, Hiroaki, E-mail: onoda@kpu.ac.jp [Department of Informatics and Environmental Sciences, Faculty of Life and Environmental Sciences, Kyoto Prefectural University, 1-5, Shimogamo Nakaragi-cyo, Sakyo-ku, Kyoto 606-8522 (Japan); Ishima, Yuya [Department of Applied Chemistry, Faculty of Life Sciences, Ritsumeikan University, 1-1-1, Nojihigashi, Kusatsu, Shiga 525-8577 (Japan); Takenaka, Atsushi [Department of Materials Science, Yonago National College of Technology, 4448, Hikona-cho, Yonago, Tottori 683-8502 (Japan); Tanaka, Isao [Department of Materials Science and Engineering, Faculty of Engineering, Kyoto University, Yoshida-Honmachi, Sakyo-ku, Kyoto 606-8501 (Japan)

    2009-08-05

    Malonic acid, propionic acid, glycine, n-butylamine, and urea were added to the preparation of lanthanum phosphate from lanthanum nitrate and phosphoric acid solutions. All additives were taken into lanthanum phosphate particles. The additives that have a basic site were easy to contain in precipitates. The addition of templates improved the specific surface area of lanthanum phosphate. The amount of pore, with radius smaller than 4 nm, increased with the addition of templates. The remained additives had influence on the acidic properties of lanthanum phosphate.

  20. 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...

  1. 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).

  2. 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.

  3. 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.

  4. 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.

  5. 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

  6. 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.

  7. 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.

  8. 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

  9. 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

  10. 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.

  11. 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

  12. Pyrrole Hydrogenation over Rh(111) and Pt(111) Single-Crystal Surfaces and Hydrogenation Promotion Mediated by 1-Methylpyrrole: A Kinetic and Sum-Frequency Generation Vibrational Spectroscopy Study

    Energy Technology Data Exchange (ETDEWEB)

    Kliewer, Christopher J.; Bieri, Marco; Somorjai, Gabor A.

    2008-03-04

    Sum-frequency generation (SFG) surface vibrational spectroscopy and kinetic measurements using gas chromatography have been used to study the adsorption and hydrogenation of pyrrole over both Pt(111) and Rh(111) single-crystal surfaces at Torr pressures (3 Torr pyrrole, 30 Torr H{sub 2}) to form pyrrolidine and the minor product butylamine. Over Pt(111) at 298 K it was found that pyrrole adsorbs in an upright geometry cleaving the N-H bond to bind through the nitrogen evidenced by SFG data. Over Rh(111) at 298 K pyrrole adsorbs in a tilted geometry relative to the surface through the p-aromatic system. A pyrroline surface reaction intermediate, which was not detected in the gas phase, was seen by SFG during the hydrogenation over both surfaces. Significant enhancement of the reaction rate was achieved over both metal surfaces by adsorbing 1-methylpyrrole before reaction. SFG vibrational spectroscopic results indicate that reaction promotion is achieved by weakening the bonding between the N-containing products and the metal surface because of lateral interactions on the surface between 1-methylpyrrole and the reaction species, reducing the desorption energy of the products. It was found that the ring-opening product butylamine was a reaction poison over both surfaces, but this effect can be minimized by treating the catalyst surfaces with 1-methylpyrrole before reaction. The reaction rate was not enhanced with elevated temperatures, and SFG suggests desorption of pyrrole at elevated temperatures.

  13. 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.

  14. A fiber-optic sensor to detect volatile organic compounds based on a porous silica xerogel film.

    Science.gov (United States)

    Echeverría, Jesús C; de Vicente, Pablo; Estella, Juncal; Garrido, Julián J

    2012-09-15

    Fiber-optic sensors are increasingly used for the determination of volatile organic compounds (VOCs) in air matrices. This paper provides experimental results on the sensitivity of a fiber-optic sensor that uses a film of a porous silica xerogel as the sensing element. This film was synthesized by the sol-gel process and affixed to the end of the optical fiber by the dip-coating technique. This intrinsic sensor works in reflection mode, and the transduction takes place in the light that travels through the core of the fiber. The VOCs included in this research cover a wide range of compounds with different functional groups and polarities. The highest sensitivity was for 2-propanol (13.1±1.4 M(-1) nm(-1)), followed by toluene (11.4±1.4 M(-1) nm(-1)), and 1-butylamine (9.5±0.4 M(-1) nm(-1)). Acetone and cyclohexane had the lowest sensitivity of all studied VOCs. Limits of detection varied between 9.1×10(-5) M for 1-butylamine and 1.6×10(-3) M for ethanol. Silanol groups on the xerogel surface act as weak acids and interact strongly with molecules that contain OH groups like alcohols, π-electrons like toluene, or a lone pair of electrons like toluene. Stronger interaction of methanol and ethanol with the silanol groups on the film led to some irreversible adsorption of these analytes at room temperature.

  15. 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.

  16. 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

  17. Photo-promoted carbonylation of chloroalkanes with carbon monoxide by non-precious metal catalysts

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    The photo-promoted carbonylation of chloroalkanes with carbon monoxide was carried out under ambient conditions with copper and cadmium salts catalysts. The results indicated that the corresponding esters were produced with three salt catalysts, i.e.CuBr2, CuCl2 and CdI2. Among these catalysts, CdI2 was the most efficient in terms of ester yield and selectivity, particularly, 60% yield and 75% selectivity in the carbonylation of chlorocyclohexane were achieved. Furthermore, the yield and selectivity of the ester can be improved greatly by adding tri-n-butylamine in the CuBr2 and CuCl2 catalyst systems. On the other hand, the additive. As a result, we suggest that iodide ion plays an important role in the catalyst system of the cadmium salts.(C) 2007 Ying Ping Jia. Published by Elsevier B.V. on behalf of Chinese Chemical Society. All rights reserved.

  18. 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).

  19. 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.

  20. 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.

  1. Self-Assembled PbSe Nanowire:Perovskite Hybrids.

    Science.gov (United States)

    Yang, Zhenyu; Yassitepe, Emre; Voznyy, Oleksandr; Janmohamed, Alyf; Lan, Xinzheng; Levina, Larissa; Comin, Riccardo; Sargent, Edward H

    2015-12-01

    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.

  2. 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.

  3. 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.

  4. 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.

  5. 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.}

  6. Dehydration of lactic acid to acrylic acid over lanthanum phosphate catalysts: the role of Lewis acid sites.

    Science.gov (United States)

    Guo, Zhen; Theng, De Sheng; Tang, Karen Yuanting; Zhang, Lili; Huang, Lin; Borgna, Armando; Wang, Chuan

    2016-09-14

    Lanthanum phosphate (LaP) nano-rods were synthesized using n-butylamine as a shape-directing agent (SDA). The resulting catalysts were applied in the dehydration of lactic acid to acrylic acid. Aiming to understand the nature of the active sites, the chemical and physical properties of LaP materials were studied using a variety of characterization techniques. This study showed that the SDA not only affected the porosity of the LaP materials but also modified the acid-base properties. Clearly, the modification of the acid-base properties played a more critical role in determining the catalytic performance than porosity. An optimized catalytic performance was obtained on the LaP catalyst with a higher concentration of Lewis acid sites. Basic sites showed negative effects on the stability of the catalysts. Good stability was achieved when the catalyst was prepared using the appropriate SDA/La ratio.

  7. Autoinduced catalysis and inverse equilibrium isotope effect in the frustrated Lewis pair catalyzed hydrogenation of imines.

    Science.gov (United States)

    Tussing, Sebastian; Greb, Lutz; Tamke, Sergej; Schirmer, Birgitta; Muhle-Goll, Claudia; Luy, Burkhard; Paradies, Jan

    2015-05-26

    The frustrated Lewis pair (FLP)-catalyzed hydrogenation and deuteration of N-benzylidene-tert-butylamine (2) was kinetically investigated by using the three boranes B(C6F5)3 (1), B(2,4,6-F3-C6H2)3 (4), and B(2,6-F2-C6H3)3 (5) and the free activation energies for the H2 activation by FLP were determined. Reactions catalyzed by the weaker Lewis acids 4 and 5 displayed autoinductive catalysis arising from a higher free activation energy (2 kcal mol(-1)) for the H2 activation by the imine compared to the amine. Surprisingly, the imine reduction using D2 proceeded with higher rates. This phenomenon is unprecedented for FLP and resulted from a primary inverse equilibrium isotope effect.

  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. 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.

  10. 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

  11. 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

  12. Purification and characterization of methylamine oxidase induced in Aspergillus niger AKU 3302.

    Science.gov (United States)

    Frébort, I; Matsushita, K; Toyama, H; Lemr, K; Yamada, M; Adachi, O

    1999-01-01

    Crude extract of Aspergillus niger AKU 3302 mycelia incubated with methylamine showed a single amine oxidase activity band in a developed polyacrylamide gel that weakly cross-reacted with the antibody against a copper/topa quinone-containing amine oxidase (AO-II) from the same strain induced by n-butylamine. Since the organism cannot grow on methylamine and the already known quinoprotein amine oxidases of the organism cannot catalyze oxidation of methylamine, the organism was forced to produce another enzyme that could oxidize methylamine when the mycelia were incubated with methylamine. The enzyme was separated and purified from the already known two quinoprotein amine oxidases formed in the same mycelia. The purified enzyme showed a sharp symmetric sedimentation peak in analytical ultracentrifugation showing S20,w0 of 6.5s. The molecular mass of 133 kDa estimated by gel chromatography and 66.6 kDa found by SDS-PAGE confirmed the dimeric structure of the enzyme. The purified enzyme was pink in color with an absorption maximum at 494 nm. The enzyme readily oxidized methylamine, n-hexylamine, and n-butylamine, but not benzylamine, histamine, or tyramine, favorite substrates for the already known two quinoprotein amine oxidases. Inactivation by carbonyl reagents and copper chelators suggested the presence of a copper/topa quinone cofactor. Spectrophotometric titration by p-nitrophenylhydrazine showed one reactive carbonyl group per subunit and redox-cyclic quinone staining confirmed the presence of a quinone cofactor. pH-dependent shift of the absorption spectrum of the enzyme-p-nitrophenylhydrazone (469 nm at neutral to 577 nm at alkaline pH) supported the identity of the cofactor with topaquinone. Nothern blot analysis indicated that the methylamine oxidase encoding gene is largely different from the already known amine oxidase in the organism.

  13. Preparation of Magnesium Hydroxide Flame Retardant with Additives%添加剂辅助制备氢氧化镁阻燃剂

    Institute of Scientific and Technical Information of China (English)

    张红进

    2012-01-01

    Magnesium hydroxide is a kind of flame retardant with high anti -flame effect, which is widely used in high polymer, such as plastic, rubber. In the experiment, synthesis reaction - hydrothermal treatment the flame - retardant magnesium hydroxide is prepared by the two -stpe way( ammonia synthesis reaction - hydrothermal treatment) with the help of additives and the products are detected by XRD, SEM and TEM methods. The results show that; ethylenediamine, n - butylamine and sodium stearate have enhancing effect on the preparation of Magnesium hydroxide , flame retardant, especially for the combination of n - butylamine and sodium stearate, and ethanol has no effect in this aspect.%氢氧化镁因具有良好的阻燃效果而被广泛应用于塑料、橡胶等高聚物中.实验使用两步法(氨水合成—水热处理法)在几种添加剂辅助条件下制备氢氧化镁阻燃剂粉体,对制备出的粉体进行了XRD、SEM和TEM表征.结果表明,加入有机添加剂对水热制备氢氧化镁阻燃剂影响较大,乙二胺、正丁胺、硬脂酸钠对制备阻燃型氢氧化镁具有促进作用,正丁胺和硬脂酸钠复合使用效果更佳,而无水乙醇未表现出促进作用.

  14. cine-Substitution reactions of metallabenzenes: an experimental and computational study.

    Science.gov (United States)

    Wang, Tongdao; Zhang, Hong; Han, Feifei; Long, Lipeng; Lin, Zhenyang; Xia, Haiping

    2013-08-12

    Alkali-resistant osmabenzene [(SCN)2(PPh3)2Os{CHC(PPh3)CHCICH}] (2) can undergo nucleophilic aromatic substitution with MeOH or EtOH to give cine-substitution products [(SCN)2(PPh3)2Os{CHC(PPh3)CHCHCR}] (R=OMe (3), OEt(4)) in the presence of strong alkali. However, the reactions of compound 2 with various amines, such as n-butylamine and aniline, afford five-membered ring species, [(SCN)2(PPh3)2Os{CH=C(PPh3)CH=C(CH=NHR')}] (R'=nBu(8), Ph(9)), in addition to the desired cine-substitution products, [(SCN)2(PPh3)2Os{CHC(PPh3)CHCHC(NHR')}] (R'=nBu(6), Ph(7)), under similar reaction conditions. The mechanisms of these reactions have been investigated in detail with the aid of isotopic labeling experiments and density functional theory (DFT) calculations. The results reveal that the cine-substitution reactions occur through nucleophilic addition, dissociation of the leaving group, protonation, and deprotonation steps, which resemble the classical "addition-of-nucleophile, ring-opening, ring-closure" (ANRORC) mechanism. DFT calculations suggest that, in the reaction with MeOH, the formation of a five-membered metallacycle species is both kinetically and thermodynamically less favorable, which is consistent with the experimental results that only the cine-substitution product is observed. For the analogous reaction with n-butylamine, the pathway for the formation of the cine-substitution product is kinetically less favorable than the pathway for the formation of a five-membered ring species, but is much more thermodynamically favorable, again consistent with the experimental conversion of compound 8 into compound 6, which is observed in an in situ NMR experiment with an isolated pure sample of 8. PMID:23843260

  15. cine-Substitution reactions of metallabenzenes: an experimental and computational study.

    Science.gov (United States)

    Wang, Tongdao; Zhang, Hong; Han, Feifei; Long, Lipeng; Lin, Zhenyang; Xia, Haiping

    2013-08-12

    Alkali-resistant osmabenzene [(SCN)2(PPh3)2Os{CHC(PPh3)CHCICH}] (2) can undergo nucleophilic aromatic substitution with MeOH or EtOH to give cine-substitution products [(SCN)2(PPh3)2Os{CHC(PPh3)CHCHCR}] (R=OMe (3), OEt(4)) in the presence of strong alkali. However, the reactions of compound 2 with various amines, such as n-butylamine and aniline, afford five-membered ring species, [(SCN)2(PPh3)2Os{CH=C(PPh3)CH=C(CH=NHR')}] (R'=nBu(8), Ph(9)), in addition to the desired cine-substitution products, [(SCN)2(PPh3)2Os{CHC(PPh3)CHCHC(NHR')}] (R'=nBu(6), Ph(7)), under similar reaction conditions. The mechanisms of these reactions have been investigated in detail with the aid of isotopic labeling experiments and density functional theory (DFT) calculations. The results reveal that the cine-substitution reactions occur through nucleophilic addition, dissociation of the leaving group, protonation, and deprotonation steps, which resemble the classical "addition-of-nucleophile, ring-opening, ring-closure" (ANRORC) mechanism. DFT calculations suggest that, in the reaction with MeOH, the formation of a five-membered metallacycle species is both kinetically and thermodynamically less favorable, which is consistent with the experimental results that only the cine-substitution product is observed. For the analogous reaction with n-butylamine, the pathway for the formation of the cine-substitution product is kinetically less favorable than the pathway for the formation of a five-membered ring species, but is much more thermodynamically favorable, again consistent with the experimental conversion of compound 8 into compound 6, which is observed in an in situ NMR experiment with an isolated pure sample of 8.

  16. Formation of simple biomolecules from alanine in ocean by impacts

    Science.gov (United States)

    Umeda, Y.; Sekine, T.; Furukawa, Y.; Kakegawa, T.; Kobayashi, T.

    2013-12-01

    phenylalanine) and four amines (methylamine, ethylamine, propylamine, and butylamine). The results in the presence of olivine have indicated the formation glycine, methylamine, ethylamine, propylamine, and butylamine. However, the results in the presence of Fe2O3 detect little glycine, methylamine, and ethylamine but no formation of propylamine and butylamine. Valine, and phenylalanine were not detected. The survival alanine as a function of pressure has been affected significantly by the oxygen fugacity, and there seems to be a threshold pressure of around 5.2 GPa. On the other hand, the glycine in alanine solution was below 5% being little variation. We have checked the solid run products by XRD. Peaks for olivine did not change, but past of Fe2O3 changed to Fe3O4. Thermodynamic calculation gives oxygen fugacities for these assemblies. These experimental results on alanine suggest that simple amino acid may be affected by pressure, oxygen fugacity, and chemical environments during impact.

  17. 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.

  18. CCN activity of aliphatic amine secondary aerosol

    Science.gov (United States)

    Tang, X.; Price, D.; Praske, E.; Vu, D.; Purvis-Roberts, K.; Silva, P. J.; Cocker, D. R., III; Asa-Awuku, A.

    2014-01-01

    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 CCN activity. Thermal gradient CCN

  19. 胺型离子液体催化合成乙酸己酯%Synthesis of hexyl acetate catalyzed by ammonium ionic liquid

    Institute of Scientific and Technical Information of China (English)

    叶庆华; 侯梦吟; 张文霞; 占晓友; 许映杰

    2011-01-01

    合成了硝酸正丁胺(N_4NO_3)、醋酸正丁胺(N_4AC)、醋酸正丙胺(N_3AC)和醋酸乙胺(N_2AC)4种胺型离子液体,采用~1HNMR对其结构进行了表征。以上述胺型离子液体为催化剂,冰醋酸和正己醇为原料,环己烷为带水剂,通过酯化反应制备了乙酸己酯。考察了催化剂种类、反应温度和反应时间等因素对乙酸己酯酯化率的影响,优化了反应工艺。最佳反应条件为:15mL环己烷为带水剂,n(冰醋酸):n(正己醇):n(N_4NO_3)=1:1.2:0.1,反应温度为95℃,反应时间为4.5h,乙酸己酯的酯化率可达90.52%。%Four ammonium ionic liquids,n-butylamine nitrate(N_4NO_3),n-butylamine acetate(N_4AC), n-propylamine acetate(N_3AC) and ethylamine acetate(N_2AC) were synthesized.Their structures were identified by ~1HNMR.The hexyl acetate was synthesized from n-hexanol and acetic acid using the ammonium ionic liquids as the catalyst by direct esterification.The influences of catalyst,reaction temperature and reaction time were investigated. The proper reactions condition was as follow:using 15mL cyclohexane as water carrier agent,n(acetic acid):n(n-hexanol):n(N_4NO_3)=1:1.2:0.1,the reaction temperature was 95℃and reaction time was 4.5h.The yield of the product was 90.5%.

  20. 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

  1. Pure Cubic-Phase Hybrid Iodobismuthates AgBi2 I7 for Thin-Film Photovoltaics.

    Science.gov (United States)

    Kim, Younghoon; Yang, Zhenyu; Jain, Ankit; Voznyy, Oleksandr; Kim, Gi-Hwan; Liu, Min; Quan, Li Na; García de Arquer, F Pelayo; Comin, Riccardo; Fan, James Z; Sargent, Edward H

    2016-08-01

    Bismuth-based hybrid perovskites are candidates for lead-free and air-stable photovoltaics, but poor surface morphologies and a high band-gap energy have previously limited these hybrid perovskites. A new materials processing strategy to produce enhanced bismuth-based thin-film photovoltaic absorbers by incorporation of monovalent silver cations into iodobismuthates is presented. Solution-processed AgBi2 I7 thin films are prepared by spin-coating silver and bismuth precursors dissolved in n-butylamine and annealing under an N2 atmosphere. X-ray diffraction analysis reveals the pure cubic structure (Fd3m) with lattice parameters of a=b=c=12.223 Å. The resultant AgBi2 I7 thin films exhibit dense and pinhole-free surface morphologies with grains ranging in size from 200-800 nm and a low band gap of 1.87 eV suitable for photovoltaic applications. Initial studies produce solar power conversion efficiencies of 1.22 % and excellent stability over at least 10 days under ambient conditions.

  2. Mechanism of retinal schiff base formation and hydrolysis in relation to visual pigment photolysis and regeneration: resonance raman spectroscopy of a tetrahedral carbinolamine intermediate and oxygen-18 labeling of retinal at the metarhodopsin stage in photoreceptor membranes

    Energy Technology Data Exchange (ETDEWEB)

    Cooper, A.; Dixon, S.F.; Nutley, M.A.; Robb, J.L.

    1987-11-25

    The mechanism of formation and hydrolysis of N-retinylidene-n-butylamine, as a model of the rhodopsin chromophore, has been investigated by a study of the kinetic and equilibrium properties in aqueous anionic, cationic, and neutral detergent micelle systems. The pH dependence of steady-state formation and hydrolysis rate constants is consistent with the classical imine reaction mechanism involving tetrahedral carbinolamine intermediates. Kinetic transients consistent with such intermediates can be seen using rapid stopped-flow techniques. Hydrolysis rates in neutral detergent micelles exhibit general base catalysis, and there are pronounced detergent-specific effects which can be qualitatively interpreted in terms of ionic effects on Schiff base pK/sub a/ and micellar hydrogen ion activities. This suggests a rational explanation for the anomalous pK/sub a/ and thermodynamic stability of visual pigment chromophores under physiological conditions. The tetrahedral intermediate has been observed directly at room temperature by continuous-flow, pH-jump resonance Raman spectroscopy, and the spectrum of this transient species shows remarkable similarity with the previously reported Raman spectrum of the metarhodopsin II intermediate of bovine rhodopsin photolysis. Isotope-labeling experiments on bovine photoreceptor membranes exposed to oxygen-18 enriched water during bleaching show incorporation of /sup 18/O at the retinal aldehyde site during the metarhodopsin I ..-->.. II transition.

  3. 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.

  4. 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.

  5. STUDIES ON REVERSE OSMOSIS SEPARATION OF AQUEOUS ORGANIC SOLUTIONS BY PAA/PSF COMPOSITE MEMBRANE

    Institute of Scientific and Technical Information of China (English)

    Jun Fang; De-min Jia; Ji-cai Huang; Qun-hui Guo; Feng-lian Wu

    2000-01-01

    The reverse osmosis (RO) separation of aqueous organic solutions, such as alcohols, amines, aldehydes, acids,ketones, and esters etc., by PAA (polyacrylic acid)/PSF (polysulfone) composite membrane has been studied. It was found that the separation results for aliphatic alcohols, amines and aldehydes are satisfactory, the solute rejection (Ra) and the volume fluxes of solutions (Jr) for 1000 ppm ethanol, ethylamine and ethyl aldehyde are 66.2%, 61.0%, 84.0% and 0.90×alcohols, amines and aldehydes, and the Ra for n-amyl alcohol, n-butylamine and n-butyl aldehyde reached 94.3%, 88.6%and 96.0%, respectively. Satisfactory separation results (Ra>70%) for ketones, esters, phenols and polyols have been obtained with the PAA/PSF composite membrane. The effect of operating pressure on the properties of reverse osmosis has also been investigated. Analysis of experimental data with Spiegler-Kedem's transport model has been carried out and the membrane constants such as reflection coefficient σ, solute and hydraulic permeabilities ω and Lp for several organic solutes have been obtained.

  6. Linear energy relationships in ground state proton transfer and excited state proton-coupled electron transfer.

    Science.gov (United States)

    Gamiz-Hernandez, Ana P; Magomedov, Artiom; Hummer, Gerhard; Kaila, Ville R I

    2015-02-12

    Proton-coupled electron transfer (PCET) processes are elementary chemical reactions involved in a broad range of radical and redox reactions. Elucidating fundamental PCET reaction mechanisms are thus of central importance for chemical and biochemical research. Here we use quantum chemical density functional theory (DFT), time-dependent density functional theory (TDDFT), and the algebraic diagrammatic-construction through second-order (ADC(2)) to study the mechanism, thermodynamic driving force effects, and reaction barriers of both ground state proton transfer (pT) and photoinduced proton-coupled electron transfer (PCET) between nitrosylated phenyl-phenol compounds and hydrogen-bonded t-butylamine as an external base. We show that the obtained reaction barriers for the ground state pT reactions depend linearly on the thermodynamic driving force, with a Brønsted slope of 1 or 0. Photoexcitation leads to a PCET reaction, for which we find that the excited state reaction barrier depends on the thermodynamic driving force with a Brønsted slope of 1/2. To support the mechanistic picture arising from the static potential energy surfaces, we perform additional molecular dynamics simulations on the excited state energy surface, in which we observe a spontaneous PCET between the donor and the acceptor groups. Our findings suggest that a Brønsted analysis may distinguish the ground state pT and excited state PCET processes.

  7. 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

  8. Determination of isocyanic acid in air.

    Science.gov (United States)

    Karlsson, D; Dalene, M; Skarping, G; Marand, A

    2001-08-01

    A method is presented for the determination of isocyanic acid (ICA), HNCO, in air samples as a di-n-butylamine (DBA) derivative. The method is based on sampling in midget impinger flasks containing 10 ml of 0.01 mol l-1 DBA in toluene. Quantification was made using liquid chromatography (LC) and electrospray mass spectrometry (MS) monitoring positive ions. The instrumental detection limit for the LC-MS was 10 fmol of ICA-DBA. ICA was generated by thermal decomposition of urea. A standard solution containing the DBA derivatives of ICA was prepared by collecting the emitted ICA in an impinger flask containing DBA. ICA in the reference solution was characterised by LC and time-of-flight (TOF) MS and quantified by LC chemiluminescent nitrogen detection (LC-CLND). The instrumental detection limit for the LC-CLND was 1 ng of nitrogen. ICA was emitted during thermal degradation of PFU resins and polyurethane (PUR) lacquers, from car metal sheets. ICA was the most dominant isocyanate and in PUR coating up to 8% of the total weight was emitted as ICA and for PFU resins up to 14% was emitted as ICA. When air samples were collected in an iron foundry during casting in sand moulds with furan resins, concentrations of ICA in the range 50-700 micrograms m-3 were found in the working atmosphere. PMID:11523446

  9. Development of a Validated LC Method for Separation of Process-Related Impurities Including the R-Enantiomer of S-Pramipexole on Polysaccharide Chiral Stationary Phases.

    Science.gov (United States)

    Ramisetti, Nageswara Rao; Kuntamukkala, Ramakrishna; Arnipalli, Manikanta Swamy

    2015-07-01

    Despite the availability of a few methods for individual separation of S-pramipexole from its process-related impurities, no common liquid chromatography (LC) method is reported so far in the literature. The present article describes the development of a single-run LC method for simultaneous determination of S-pramipexole and its enantiomeric and process-related impurities on a Chiralpak AD-H (150 x 4.6 mm, 5μm) column using n-hexane/ethanol/n-butylamine (75:25:0.1 v/v/v) as a mobile phase in an isocratic mode of elution at a flow rate of 1.2 ml/min at 30°C. The chromatographic eluents were monitored at a wavelength of 260 nm using a photodiode array detector. Excellent enantioseparation with good resolutions (Rs ≥ 2.88) and peak shapes (As ≤ 1.21) for all analytes was achieved. The proposed method was validated according to International Conference Harmonization (ICH) guidelines in terms of accuracy, precision, sensitivity, and linearity. Limits of quantification of impurities (0.25-0.55 μg/ml) indicate the highest sensitivity achievable by the proposed method. The method has an advantage of selectivity and suitability for routine determination of not only chiral impurity but also all possible related substances in active pharmaceutical ingredients of S-pramipexole.

  10. Synthesis and physicochemical characterization of titanium oxide and sulfated titanium oxide obtained by thermal hydrolysis of titanium tetrachloride

    Directory of Open Access Journals (Sweden)

    H. Esteban Benito

    2014-09-01

    Full Text Available This work reports the synthesis of titanium oxide (TiO2 and sulfated titanium oxide (TiO2-SO4(2- obtained by thermal hydrolysis of titanium tetrachloride. Titanium hydroxide synthesized by this method was impregnated with a 1 N H2SO4 solution, to give amounts of sulfate ions (SO4(2- of 3 and 7 wt%. The synthesized samples were dried at 120 °C during 24 h and then calcined for 3 h at 400 °C. Thermal analyses, X-ray diffraction, nitrogen physisorption, infrared spectroscopy, potentiometric titration with n-butylamine, U.V.-visible diffuse reflectance spectroscopy and scanning electron microscopy were used to characterize the materials. The results of physicochemical characterization revealed that a mixture of crystalline structures, anatase, brookite and rutile developed in the titanium oxide, stabilizing the anatase structure in the sulfated titanium oxides, and coexisting with a small amount of brookite structure. The synthesized mesoporous materials developed specific surface areas between 62 and 70 m² g-1, without detecting an important influence of sulfation on this parameter. The presence of sulfate ions improved the acidity of titanium oxide and modified the characteristics of light absorption in the 425-600 nm region, which suggests the possibility of using these materials in reactions assisted by visible light.

  11. 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.

  12. 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.

  13. 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

  14. MALDI Matrix Research for Biopolymers

    Science.gov (United States)

    Fukuyama, Yuko

    2015-01-01

    Matrices are necessary materials for ionizing analytes in matrix-assisted laser desorption/ionization-mass spectrometry (MALDI-MS). The choice of a matrix appropriate for each analyte controls the analyses. Thus, in some cases, development or improvement of matrices can become a tool for solving problems. This paper reviews MALDI matrix research that the author has conducted in the recent decade. It describes glycopeptide, carbohydrate, or phosphopeptide analyses using 2,5-dihydroxybenzoic acid (2,5-DHB), 1,1,3,3-tetramethylguanidinium (TMG) salts of p-coumaric acid (CA) (G3CA), 3-aminoquinoline (3-AQ)/α-cyano-4-hydroxycinnamic acid (CHCA) (3-AQ/CHCA) or 3-AQ/CA and gengeral peptide, peptide containing disulfide bonds or hydrophobic peptide analyses using butylamine salt of CHCA (CHCAB), 1,5-diaminonaphthalene (1,5-DAN), octyl 2,5-dihydroxybenzoate (alkylated dihydroxybenzoate, ADHB), or 1-(2,4,6-trihydroxyphenyl)octan-1-one (alkylated trihydroxyacetophenone, ATHAP). PMID:26819908

  15. 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.

  16. 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.

  17. 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.

  18. 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

  19. 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)

  20. 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.

  1. Characterization of the microbial community structure and nitrosamine-reducing isolates in drinking water biofilters.

    Science.gov (United States)

    Wang, Wanfeng; Guo, Yanling; Yang, Qingxiang; Huang, Yao; Zhu, Chunyou; Fan, Jing; Pan, Feng

    2015-07-15

    Two biofilters were constructed using biological activated carbon (BAC) and nitrosamine-containing water from two drinking water treatment plants. The microbiome of each biofilter was characterized by 454 high-throughput pyrosequencing, and one nitrosamine-reducing bacterium was isolated. The results showed that nitrosamines changed the relative abundance at both the phylum and class levels, and the new genera were observed in the microbial communities of the two BAC filters after cultivation. As such, the genus Rhodococcus, which includes many nitrosamine-reducing strains reported in previous studies, was only detected in the BAC2 filter after cultivation. These findings indicate that nitrosamines can significantly affect the genus level in the microbial communities. Furthermore, the isolated bacterial culture Rhodococcus cercidiphylli A41 AS-1 exhibited the ability to reduce five nitrosamines (N-nitrosodimethylamine, N-nitrosodiethylamine, N-nitrosodi-n-propylamine, N-nitrosopyrrolidine, and N-nitrosodi-n-butylamine) with removal ratios that ranged from 38.1% to 85.4%. The isolate exhibited a better biodegradation ability with nitrosamine as the carbon source when compared with nitrosamine as the nitrogen source. This study increases our understanding of the microbial community in drinking water biofilters with trace quantities of nitrosamines, and provides information on the metabolism of nitrosamine-reducing bacteria.

  2. Detection technology research progress on preservative and antistaling agent for fruits and vegetables in China%中国果蔬防腐保鲜剂检测技术研究进展

    Institute of Scientific and Technical Information of China (English)

    綦艳; 李聪; 王力清; 黄秋研

    2013-01-01

    在介绍中国果蔬市场现状以及果蔬保鲜防腐技术的基础上,阐述噻苯咪唑、邻苯基苯酚、联苯、抑霉唑、仲丁胺、多菌灵、桂醛、乙萘酚、2,4-二氯苯氧乙酸等采后果蔬保鲜防腐剂的作用,综述各类果蔬保鲜防腐剂残留量检测方法的研究进展.%Fresh fruit and vegetables play an important role in people's everyday life.The current status of China's fruit and vegetable market and the effects of different fruit preservatives are summarized,including thiabendazole,o-phenylphenate,biphenyl,2-Naphthol,imazalil,sec-butylamine,carbendazim,Cinnamal and (2,4-Dichlorophenyloxy)acetic acid.The paper emphasized on the detection methods of preservatives and antistaling agent residues.

  3. 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.

  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. 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

  6. 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.

  7. Acetaldehyde behavior over platinum based catalyst in hydrogen stream generated by ethanol reforming

    Energy Technology Data Exchange (ETDEWEB)

    de Lima, Adriana F.F. [Laboratorio de Catalise, Instituto Nacional de Tecnologia, Av. Venezuela 82/507, 20081-310 Rio de Janeiro, RJ (Brazil); Instituto de Quimica e INOG (Instituto Nacional de Oleo Gas), UERJ-CNPq, FAPERJ, Universidade do Estado do Rio de Janeiro, Rua Sao Francisco Xavier, 524, 20550-900 Rio de Janeiro, RJ (Brazil); Colman, Rita C. [Departamento de Engenharia Quimica e de Petroleo, Universidade Federal Fluminense, Av. Passos da Patria, 156/bl E/240, 24210-240 Niteroi, RJ (Brazil); Zotin, Fatima M.Z. [Instituto de Quimica e INOG (Instituto Nacional de Oleo Gas), UERJ-CNPq, FAPERJ, Universidade do Estado do Rio de Janeiro, Rua Sao Francisco Xavier, 524, 20550-900 Rio de Janeiro, RJ (Brazil); CETEM-MCT, Av. Pedro Calmon, 900, Cidade Universitaria, 21941-908 Rio de Janeiro, RJ (Brazil); Appel, Lucia G. [Laboratorio de Catalise, Instituto Nacional de Tecnologia, Av. Venezuela 82/507, 20081-310 Rio de Janeiro, RJ (Brazil)

    2010-12-15

    Due to the greenhouse effect, hydrogen production from bioethanol reforming is a very important subject in heterogeneous catalysis research. Pt based catalysts are employed in H{sub 2} purification processes and also as electrocatalysts of PEM (''Proton Exchange Membrane'') fuel cells. Hydrogen obtained from ethanol reforming may contain, as contaminants, acetaldehyde and small amounts of CO. This aldehyde can be decarbonylated on Pt based catalysts generating carbon monoxide and methane, rendering the hydrogen purification more challenging. Moreover, acetaldehyde might also change the electrocatalyst behavior. Therefore, this contribution aims at studying the acetaldehyde behavior in the presence of platinum based catalysts in hydrogen atmosphere. The Pt/SiO{sub 2}, Pt/USY catalysts and an electrocatalyst were characterized by n-butylamine, H{sub 2} and CO{sub 2} adsorption, ATG/DTG measurements and cyclohexane dehydrogenation reaction. It was observed that the acid-basic properties of the supports promote condensation reactions. When in contact with Pt based catalysts, acetaldehyde undergoes C-C and C=O bond scissions. The former occurs at a wide range of temperatures, whereas the latter only at low temperatures (<200 C). The C-C bond scission (decarbonylation) produces methane and CO. The C=O bond scission generates carbon residues on the catalyst as well as oxygen species, which in turn is able to eliminate CO from the catalytic surface. The data also show that decarbonylation is not a structure-sensitive reaction. (author)

  8. 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

  9. 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.

  10. 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

  11. 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.

  12. Electrodialytic membrane suppressors for ion chromatography make programmable buffer generators.

    Science.gov (United States)

    Chen, Yongjing; Srinivasan, Kannan; Dasgupta, Purnendu K

    2012-01-01

    The use of buffer solutions is immensely important in a great variety of disciplines. The generation of continuous pH gradients in flow systems plays an important role in the chromatographic separation of proteins, high-throughput pK(a) determinations, etc. We demonstrate here that electrodialytic membrane suppressors used in ion chromatography can be used to generate buffers. The generated pH, computed from first principles, agrees well with measured values. We demonstrate the generation of phosphate and citrate buffers using a cation-exchange membrane (CEM) -based anion suppressor and Tris and ethylenediamine buffers using an anion-exchange membrane (AEM) -based cation suppressor. Using a mixture of phosphate, citrate, and borate as the buffering ions and using a CEM suppressor, we demonstrate the generation of a highly reproducible (avg RSD 0.20%, n = 3), temporally linear (pH 3.0-11.9, r(2) > 0.9996), electrically controlled pH gradient. With butylamine and a large concentration (0.5 M) of added NaCl, we demonstrate a similar linear pH gradient of large range with a near-constant ionic strength. We believe that this approach will be of value for the generation of eluents in the separation of proteins and other biomolecules and in online process titrations.

  13. 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

  14. 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}.

  15. 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

  16. 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.

  17. Effect of acids on the infrared spectra of the Schiff base of trans-retinal

    Energy Technology Data Exchange (ETDEWEB)

    Lussier, L.S.; Sandorfy, C.; Le-Thanh, H.; Vocelle, D.

    1987-04-23

    trans-Retinylidene-tert-butylamine was put into contact with a series of acids (HCl, HBr, and HI and six carboxylic acids, trichloro-, dichloro-, monochloro-, and monobromoacetic acids, and 3-chloropropionic and propionic acids) whose pK/sub a/ values vary from 0.66 to 4.87. It can be inferred from the Fourier-transform infrared spectra that in order to obtain complete protonation of the Schiff base in chloroform solution an acid having a pK/sub a/ value of at least 2 is needed. With a pK/sub a/ value of about 4, similar to that of aspartic or glutamic acid, the estimated degree of protonation is about 65%. This shows that a mechanism is required to bring about 100% or nearly 100% protonation in rhodopsins. The intensification of the C double bond C bands upon protonation shows that the positive charge is delocalized along the conjugated chain. The N/sup +/H stretching region of the spectrum could be studied to advantage but the N/sup +/H in-plane bending bands could not be identified.

  18. 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.

  19. 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.

  20. 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.

  1. Silver-coated magnetite-carbon core-shell microspheres as substrate-enhanced SERS probes for detection of trace persistent organic pollutants.

    Science.gov (United States)

    An, Qiao; Zhang, Peng; Li, Jun-Mei; Ma, Wan-Fu; Guo, Jia; Hu, Jun; Wang, Chang-Chun

    2012-08-21

    Highly active surface-enhanced Raman scattering (SERS) substrates of Ag nanoparticle (Ag-NP) modified Fe(3)O(4)@carbon core-shell microspheres were synthesized and characterized. The carbon coated Fe(3)O(4) microspheres were prepared via a one-pot solvothermal method and were served as the magnetic supporting substrates. The Ag-NPs were deposited by in situ reduction of AgNO(3) with butylamine and the thickness of the Ag-NP layer was variable by controlling the AgNO(3) concentrations. The structure and integrity of the Fe(3)O(4)@C@Ag composite microspheres were confirmed by TEM, XRD, VSM and UV-visible spectroscopy. In particular, the Ag-NP coated Fe(3)O(4)@carbon core-shell microspheres were shown to be highly active for SERS detections of pentachlorophenol (PCP), diethylhexyl phthalate (DEHP) and trinitrotoluene (TNT). These analytes are representatives of environmentally persistent organic pollutants with typically low SERS activities. The results suggested that the interactions between the carbon on the microsphere substrates and the aromatic cores of the target molecules contributed to the facile pre-concentration of the analytes near the Ag-NP surfaces.

  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. PREPARATION AND ADSORPTION PROPERTIES OF BILIRUBIN ADSORBENTS WITH DIFFERENT LIGANDS BASED ON SEPHAROSE CL-4B%胆红素吸附剂功能基组成及其吸附特性研究

    Institute of Scientific and Technical Information of China (English)

    王智; 陈书博; 徐丽; 谢健; 贾凌云

    2011-01-01

    为了获得性能较佳的胆红素吸附剂,本研究考察了功能基种类、链长、偶联密度等因素对吸附剂吸附性能的影响.结果表明,当功能基具有足够的链长,与胆红素相似的疏水性及较高的偶联密度时,能够提高吸附剂的胆红素吸附能力.实验表明,链长21个原子、偶联73μmol/mL正丁胺的吸附剂对胆红素的吸附能力最强,在30℃、300mg/L的白蛋白结合胆红素溶液中,吸附1h即达到平衡,胆红素吸附量达到3.01 mg/mL (90.3mg/g干重);较高的温度有利于其对胆红素的吸附.50mL材料对500mL实际病人血浆动态吸附2.5h,总胆红素(277.4mg/L)去除率达到55.2%,同时对血浆蛋白的吸附较低.所有结果显示该吸附剂具有很强的实际应用的潜力.%A series of bilirubin adsorbents with different ligand type, length and density were prepared by activation of Sepharose CL-4B and their adsorption capacities to bilirubin were measured in static adsorption experiments. The results showed that the structure and properties of ligands, such as sufficient spacer-length, higher grafting density on the adsorbent and the similar hydrophobicity with bilirubin, were helpful to improve adsorption capacity of bilirubin. These experiments provided some ideas for designing new adsorbents. Among these adsorbents, the adsorbent with 73μmol/mL butylamine and 23-atom spacer showed the strongest adsorption ability to bilirubin in BSA-bilirubin solution, which could reach the adsorption balance at 30°C in lh, and got binding capacity of 3.01mg/mL gel. Moreover, higher temperature was more favorable to the adsorption of bilirubin. The in vitro hemoperfusion experiments were carried out by adding 50mL adsorbent into 500mL patient's plasma and 55.2% of bilirubin (277.4mg/L) was removed after 2.5h, and at the same time, adsorption for plasma proteins was low. These results indicated that the Butylamine-Sepharose adsorbents could be a potential choice for specific

  4. 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.

  5. 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

  6. Effect of foamability index of short chain alkyl amines on flotation of quartz

    Directory of Open Access Journals (Sweden)

    Szczerkowska Sabina

    2016-01-01

    Full Text Available Amines can be used for flotation of various minerals, especially quartz. The flotation efficiency of quartz depends on the amine type and dose. It was proved that the shorter alkyl amine, higher amine concentration has to be used to recover quartz at the same level. In flotation amines play a role of both collectors and frothers. The ability of a amine to collect particles can be expressed in the form of contact angle, while the foaming properties by different parameters including dynamic foamability index (DFI and critical coalescence concentration (CCC. Determination of DFI and CCC requires advanced techniques and methods. Therefore, in this paper a rapid and facile method for determination of foaming properties of amines and also other surfactants was used. It was based on measuring the initial foam and froth heights in a conventional flotation machine at different concentrations of surfactants. The foam height-concentration curve was described by utilizing an empirical equation which was based on one-adjustable parameter called the foamability index (FI. In this work the foamability index was determined for butylamine (ButNH2, hexylamine (HexNH2 and octylamine (OctNH2 as examples of short chain alkyl amines. The determined foamability indices were 92, 12 and 4 mg/dm3 for ButNH2, HexNH2 and OctNH2, respectively. It was shown that when the flotation results of quartz were presented in the form of recovery versus normalized amine concentration in relation to the foamability index (c/FI, all the experimental data points converged to one curve. It indicates that amines act similarly but at different concentrations expressed as FI. The foamability index seems to be a useful parameter for characterizing any flotation frother.

  7. Ambient temperature nanoelectrospray ion mobility detector for high performance liquid chromatography in determining amines.

    Science.gov (United States)

    Chen, Chuang; Hou, Keyong; Wang, Weiguo; Li, Jinghua; Li, Haiyang

    2014-09-01

    A nanoelectrospray ionization ion mobility spectrometer (nanoESI-IMS) working at ambient pressure and ambient temperature was developed as a detector of high performance liquid chromatography (HPLC) to achieve sensitive detection of amines with no derivatization and meanwhile provide another dimension of separation. The easier desolvation property of the charged droplets formed in nanoESI source enabled complete desolvation of the product ions of sixteen amines and drugs using the nanoESI-IMS at ambient temperature. Working at ambient temperature was good for suppressing the dissociation of thermal volatile ions, such as only the proton adducted molecular ions were observed for morphine in the nanoESI-IMS. Besides, the resolving power of the nanoESI-IMS also showed an increasing tendency as lowering the working temperature, an increment of 19 percent and 10 percent was observed for diethylamine and triethylamine as the temperature dropped from 92°C to 32°C. The resolving power of the nanoESI-IMS at 32°C for the 16 tested compounds was amid 33-44. With the nanoESI-IMS coupled to HPLC, a six-compound mixture including isomers was successfully separated and detected without any derivatization. And linear response ranges of 1 to 20, 0.5 to 20, and 0.8 to 20μgml(-1) and limits of detection of 0.25, 0.15, and 0.17μgml(-1) for triethylamine, diethylamine, and butylamine, respectively, were obtained with the hyphenated system. These results showed the excellent performance of the two-dimensional separation and detection method in direct qualitative and quantitative analyses of amines.

  8. 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.

  9. 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.

  10. 曲克芦丁钯配合物的制备及其对Heck反应的催化性能%Synthesis of troxerutin-Pd complex and its catalytic properties for Heck reaction

    Institute of Scientific and Technical Information of China (English)

    徐启杰; 时文中; 刘雷英; 王文豪; 崔元臣

    2011-01-01

    The complex of troxerutin-Pd was synthesized. The structure of the complex was characterized by means of infrared spectrometry and ultraviolet spectrometry. Besides, the catalytic performance of the complex for the Heck arylation reaction of bromobenzene and acrylic acid was examined. Results showed that the complex had good catalytic performance for the Heck arylation reaction of bromobenzene and acrylic acid under optimized reaction conditions.Namely, a yield of above 70% was reached at bromobenzene to acrylic acid molar ratio of 1∶ 2,reaction time of 8 h, and reaction temperature of 120 ℃ in the presence of tri-n-butylamine as the alkali and tetrabutylammonium bromide as the solvent.%制备了曲克芦丁钯配合物,利用红外光谱和紫外光谱表征了配合物的结构;同时考察了其对溴苯和丙烯酸的Heck芳基化反应的催化性能.结果表明:在反应物的物质的量之比(溴苯与丙烯酸)为1:2、反应温度120℃、反应时间8 h、三正丁胺为碱、四丁基溴化铵为溶剂的条件下,曲克芦丁钯配合物对溴苯和丙烯酸的Heck芳基化反应有较好的催化作用,产率可达70%以上.

  11. 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

  12. Determination of eight nitrosamines in water at the ng L(-1) levels by liquid chromatography coupled to atmospheric pressure chemical ionization tandem mass spectrometry.

    Science.gov (United States)

    Ripollés, Cristina; Pitarch, Elena; Sancho, Juan V; López, Francisco J; Hernández, Félix

    2011-09-19

    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(6) and NDPA-d(14)) were added as surrogate internal standards to the samples. The optimized method was validated at two concentration levels (10 and 100 ng L(-1)) in drinking water samples, obtaining satisfactory recoveries (between 90 and 120%) and precision (RSDwater samples: chlorinated from drinking water and wastewater treatment plants (DWTP and WWTP, respectively), wastewaters subjected to ozonation and tap waters.

  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. H3PW12O40 Encapsulation by Nanoporous Metal Organic Framework HKUST-1: Synthesis, Characterization, Activity and Stability.

    Science.gov (United States)

    Rafiee, Ezzat; Nobakht, Narges

    2016-01-01

    Hybrid composite material was obtained through encapsulation of H3PW12O40 (PW) into HKUST-1 (Cu3(BTC)2, BTC = 1,3,5-benzenetricarboxylic acid), in molar composition of 5 Cu(NO3)2 · 3H2O/2.8 BTC/0.3 PW/0.6 CTAB by adding solutions of PW and copper salts to mixture of BTC and surfactant. The catalyst was characterized by various techniques including powder X-ray diffraction (XRD), Fourier transform infrared (FT-IR), scanning electron microscopy (SEM), energy dispersive X-ray (EDX), laser particle size analyzer, Brunauer Emmett-Teller (BET). The acidity of the catalyst was measured by a potentiometric titration with n-butylamine and PW/HKUST-1 presented very strong acidic sites with Ei > 100 mV. This nano catalyst was successfully used for the synthesis of various β-keto enol ethers at 45 °C with 51-98% yield after 5-75 min. The catalyst was easily recycled and reused at least four times without significant loss of its activity (94% yield after forth run). The presence of the PW in PW/HKUST-1 and reused PW/HKUST-1 structure, eliminating any doubt about collapse of the HKUST-1 after catalytic reaction and can be followed by FT-IR, XRD and SEM techniques. Brönsted and Lewis acidity of the PW/HKUST-1 catalyst was distinguished by studying the FT-IR and determined by chemisorption of pyridine. The strength and dispersion of the protons on PW/HKUST-1 was considerably high and active surface protons became more available for reactant. PMID:27333553

  16. Determination of isocyanates, aminoisocyanates and amines in air formed during the thermal degradation of polyurethane.

    Science.gov (United States)

    Karlsson, Daniel; Dahlin, Jakob; Skarping, Gunnar; Dalene, Marianne

    2002-04-01

    An air sampling method for the determination of isocyanates, aminoisocyanates and amines formed during the thermal degradation of polyurethane (PUR) is presented. The method is based on the collection of air samples using impinger flasks containing di-n-butylamine (DBA) in toluene with a glass fibre filter in series. Isocyanates are derivatized with DBA to urea derivatives, and amines are derivatized in a subsequent work-up procedure with ethyl chloroformate (ET) to carbamate esters. Amine, aminoisocyanate and isocyanate derivatives were characterized using liquid chromatography-time of flight mass spectrometry (LC-TOFMS) and liquid chromatography-chemiluminescent nitrogen detection (LC-CLND). Quantification was performed by LC-MS, monitoring molecular ions [MH]+ in the electrospray mode. The instrumental detection limits for amines, aminoisocyanates and isocyanates were in the ranges 30-40, 2-3 and 3-70 fmol, respectively. Thermal degradation products of PUR were observed in high concentrations during welding in district heating pipes and PUR-coated metal sheets. Eleven isocyanates, three amines and five aminoisocyanates were identified. The concentrations of isocyanates, aminoisocyanates and amines in samples collected in the smoke close to the welding spot were in the ranges 150-650, 4-290 and 1-70 ppb, respectively. In samples collected in the breathing zone, isocyanates and aminoisocyanates were observed in the ranges 9-120 and 4-19 ppb, respectively. The compounds were present in both gas and particle phases. Volatile compounds dominated in the gas phase, whereas less volatile compounds dominated in the particle phase. The method presented makes it possible to sample and determine amines and aminoisocyanates, in addition to isocyanates. The need to monitor these compounds is clearly illustrated by the high concentrations found during the thermal degradation of PUR.

  17. 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.

  18. 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.

  19. 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.

  20. 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)

  1. Preparation of Zeolite X Membranes on Porous Ceramic Substrates with Zeolite Seeds

    Institute of Scientific and Technical Information of China (English)

    Zhongqiang Xu; Qingling Chen; Guanzhong Lu

    2002-01-01

    Zeolite X membranes were investigated by in-situ hydrothermal synthesis on porous ceramic tubes precoated with zeolite X seeds or precursor amorphous aluminosilicate, and porous α-Al2O3 ceramic tubes with a pore size of 50 200 nm were employed as supports. Zeolite X crystals were synthesized by the classic method and mixed into deionized water as a slurry with a concentration of 0.2 0.5wt%, having a range of crystal sizes from 0.2 to 2μm. Crystal seeds were pressed into the pores near the inner surface of the ceramic tubes, and crystallization took place at 95℃ for 24-96 h. It was also investigated that Boehmite sol added with zeolite X seeds was precoated on ceramic supports to form a layer of γ-Al2O3 by heating, and hydrothermal crystallization could then take place to prepare the zeolite membranes on the composite ceramic tubes. The crystal species were characterized by XRD, and the morphology of the supports subjected to crystallization was characterized by SEM. The composite zeolite membranes have zeolitic top-layers with a thickness of 10-25 μm, and zeolite crystals can be intruded into pores of the supports as deeply as 100μm. The experimental results indicate that the precoating of zeolitic seeds on supports is beneficial to crystallization by shortening the synthesis time and improving the membrane strength. The resulting zeolite X membrane shows permselectivity to tri-n-butylamine((C4H9)3N) over perfluro-tributyl-amine ((C4Fg)3N), and a permeance ratio of 57 for ((C4Hg)3N to (C4F9)3N could be reached at 350℃. Permeances of BZ, EB and TIPB through the zeolite membrane were also measured and were found to slightly increase with temperature.

  2. 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

  3. N-nitrosamine formation by monochloramine, free chlorine, and peracetic acid disinfection with presence of amine precursors in drinking water system.

    Science.gov (United States)

    West, Danielle M; Wu, Qihua; Donovan, Ariel; Shi, Honglan; Ma, Yinfa; Jiang, Hua; Wang, Jianmin

    2016-06-01

    In this study, the formation of eight N-nitrosamines, N-nitrosodimethylamine (NDMA), N-nitrosodiethylamine, N-nitrosomethylamine, N-nitrosodi-n-propylamine, N-nitrosodi-n-butylamine, N-Nitrosopiperidine, N-Nitrosopyrrolidine, N-Nitrosomorpholine, were systematically evaluated with respect to seven N-nitrosamine precursors (dimethylamine, trimethylamine, 3-(dimethylaminomethyl)indole, 4-dimethylaminoantipyrine, ethylmethylamine, diethylamine, dipropylamine) and three disinfectants (monochloramine, free chlorine, peracetic acid) under variable dosages, exposure times, and pH in a drinking water system. Without the presence of the seven selected N-nitrosamine precursors N-nitrosamine formation was not observed under any tested condition except very low levels of N-Nitrosopyrrolidine under some conditions. With selected N-nitrosamine precursors present N-nitrosamines formed at different levels under different conditions. The highest N-nitrosamine formation was NDMA with a maximum concentration of 1180 ng/L by monochloramine disinfection with precursors present; much lower levels of N-nitrosamines were formed by free chlorine disinfection; and no detectable level of N-nitrosamines were observed by peracetic acid disinfection except low level of N-Nitrosodi-n-propylamine under some conditions. NDMA formation was not affected by pH while four other N-nitrosamine formations were slightly affected by sample pH tested between 7 and 9, with formation decreasing with increasing pH. Monochloramine exposure time study displayed fast formation of N-nitrosamines, largely formed in four hours of exposure and maximized after seven days. This was a systematic study on the N-nitrosamine formation with the seven major N-nitrosamine precursors presence and absence under different conditions, including peracetic acid disinfection which has not been studied elsewhere.

  4. Palladium nanoparticles decorated on reduced graphene oxide rotating disk electrodes toward ultrasensitive hydrazine detection: effects of particle size and hydrodynamic diffusion.

    Science.gov (United States)

    Krittayavathananon, Atiweena; Srimuk, Pattarachai; Luanwuthi, Santamon; Sawangphruk, Montree

    2014-12-16

    Although metal nanoparticle/graphene composites have been widely used as the electrode in electrochemical sensors, two effects, consisting of the particle size of the nanoparticles and the hydrodynamic diffusion of analytes to the electrodes, are not yet fully understood. In this work, palladium nanoparticles/reduced graphene oxide (PdNPs/rGO) composites were synthesized using an in situ polyol method. Palladium(II) ions and graphene oxide were reduced together with a reducing agent, ethylene glycol. By varying the concentration of palladium(II) nitrate, PdNPs with different sizes were decorated on the surface of rGO sheets. The as-fabricated PdNPs/rGO rotating disk electrodes (RDEs) were investigated toward hydrazine detection. Overall, a 3.7 ± 1.4 nm diameter PdNPs/rGO RDE exhibits high performance with a rather low limit of detection of about 7 nM at a rotation speed of 6000 rpm and provides a wide linear range of 0.1-1000 μM with R(2) = 0.995 at 2000 rpm. This electrode is highly selective to hydrazine without interference from uric acid, glucose, ammonia, caffeine, methylamine, ethylenediamine, hydroxylamine, n-butylamine, adenosine, cytosine, guanine, thymine, and l-arginine. The PdNPs/rGO RDEs with larger sizes show lower detection performance. Interestingly, the detection performance of the electrodes is sensitive to the hydrodynamic diffusion of hydrazine. The as-fabricated electrode can detect trace hydrazine in wastewater with high stability, demonstrating its practical use as an electrochemical sensor. These findings may lead to an awareness of the effect of the hydrodynamic diffusion of analyte that has been previously ignored, and the 3.7 ± 1.4 nm PdNPs/rGO RDE may be useful toward trace hydrazine detection, especially in wastewater from related chemical industries.

  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. The stability and generation pattern of thermally formed isocyanic acid (ICA) in air - potential and limitations of proton transfer reaction-mass spectrometry (PTR-MS) for real-time workroom atmosphere measurements.

    Science.gov (United States)

    Jankowski, Mikolaj Jan; Olsen, Raymond; Thomassen, Yngvar; Molander, Paal

    2016-07-13

    Isocyanic acid (ICA) in vapour phase has been reported to be of unstable nature, making the occupational hygienic relevance of ICA questionable. The stability of pure ICA in clean air at different humidity conditions was investigated by Fourier transform-infrared spectrometric (FT-IR) measurements. Furthermore, the stability of ICA in a complex atmosphere representative thermal degradation hot-work procedures were examined by performing parallel measurements by proton transfer reaction-mass spectrometric (PTR-MS) instrumentation and off-line denuder air sampling using di-n-butylamine (as a derivatization agent prior to liquid chromatography mass spectrometric (LC-MS) determination). The apparent half-life of ICA in pure ICA atmospheres was 16 to 4 hours at absolute humidity (AH) in the range 4.2 to 14.6 g m(-3), respectively. In a complex atmosphere at an initial AH of 9.6 g m(-3) the apparent half-life of ICA was 8 hours, as measured with the denuder method. Thus, thermally formed ICA is to be considered as a potential occupational hazard with regard to inhalation. The generation pattern of ICA formed during controlled gradient (100-540 °C) thermal decomposition of different polymers in the presence of air was examined by parallel PTR-MS and denuder air sampling. According to measurement by denuder sampling ICA was the dominant aliphatic isocyanate formed during the thermal decomposition of all polymers. The real-time measurements of the decomposed polymers revealed different ICA generation patterns, with initial appearance of thermally released ICA in the temperature range 200-260 °C. The PTR-MS ICA measurements was however affected by mass overlap from other decomposition products at m/z 44, illustrated by a [ICA]Denuder/[ICA]PTR-MS ratio ranging from 0.04 to 0.90. These findings limits the potential use of PTR-MS for real time measurements of thermally released ICA in field, suggesting parallel sampling with short-term sequential off-line methodology. PMID

  7. Ⅱ型二元氢气水合物相边界条件测定及分解焓计算%Measurement of Phase Boundary Conditions and Calculation of Dissociation Enthalpy of sⅡ Binary Hydrogen Hydrate

    Institute of Scientific and Technical Information of China (English)

    杜建伟; 李栋梁; 陈玉凤; 梁德青; 李新军

    2011-01-01

    Experiments on Sii binary hydrogen hydrate phase boundary conditions of the cyclo-pentane/tetrahydrofuran/tert-butylamine/acetone-hydrogen-water system were conducted in a high pressure visual sapphire reactor to obtain the phase equilibrium data for hydrogen hydrate. On the basis of the experimental data, the dissociation enthalpy of Sii binary hydrogen hydrate was calculated with the Clausius-Clapeyron equation. The results show that the phase equilibrium pressure of Sii binary hydrogen hydrate is one-tenth or even more lower that of hydrogen hydrate without additives. The dissociation enthalpy of Sii binary hydrogen hydrate is related to the additives and the phase equilibrium temperature, and with the same kind of additives the dissociation enthalpy of the binary hydrogen hydrate increases with the phase equilibrium temperature. The results of this study may lead to the development of hydrogen storage by hydrate technique.%针对水合物法储氢存在相平衡数据较少及其分解焓直接实验测定非常困难的问题,在已有的高压可视蓝宝石反应釜中测定了环戊烷/丙酮/叔丁胺/四氢呋喃-水-氢气三组分体系中的水合物相边界条件,并结合Clausius-Clapeyron方程计算确定了4种Ⅱ型二元氢气水合物的分解焓.结果表明:含环戊烷/丙酮/叔丁胺/四氢呋喃的Ⅱ型二元氢气水合物的相平衡压力可降低至纯氢气水合物同温度下相平衡压力的1/10甚至更多.二元氢气水合物的分解焓与添加剂和相平衡温度有关,对于同一种添加剂,随着相平衡温度的升高,所得到的二元氢气水合物分解焓增加.二元氢气水合物相平衡边界和分解焓的测定对进一步研究和开发水合物法储氢技术具有重要价值.

  8. HPLC法测定馥感啉口服液中盐酸麻黄碱和盐酸伪麻黄碱的含量%Determination of Ephedrine Hydrochloride and Pseudoephedrine Hydrochloride in Fuganlin Oral Liquid by HPLC

    Institute of Scientific and Technical Information of China (English)

    曾永长; 张莉; 曾晓燕; 陈艺文

    2015-01-01

    目的:采用高效液相色谱法建立同时测定馥感啉口服液中盐酸麻黄碱和盐酸伪麻黄碱含量的检测方法。方法使用Phenomenex Synergi Polar-RP柱(250 mm×4.6 mm,4μm),以甲醇-0.092%磷酸溶液(含0.04%三乙胺和0.02%二正丁胺)(1.5∶98.5)为流动相,流速:1.0 mL·min-1,检测波长为210 nm。结果盐酸麻黄碱和盐酸伪麻黄碱在进样1~100μg·mL-1范围内线性关系良好,平均回收率(n=6)分别为97.43%(RSD=0.80%)、98.59%(RSD=1.77%)。结论该方法操作简便、分离度好、稳定可靠,可同时快速测定盐酸麻黄碱和盐酸伪麻黄碱,为馥感啉口服液的质量评价提供科学依据。%Objective To establish a HPLC method to determine the content of ephedrine hydrochloride and pseudoephedrine hydrochloride in Fuganlin oral liquid. Methods The chromatographic conditions was as follows:Phenomenex Synergi Polar-RP column(250 mm ×4.6 mm, 4 μm), methanol-0.092 % phosphoric acid solution (containing 0.04 % triethylamine and 0.02 % di-n-butylamine)(1.5∶98.5)as the mobile phase, flow rate being 1.0 mL ·min-1, detection wavelength set as 210 nm. Results The linear range of ephedrine hydrochloride and pseudoephedrine hydrochloride was 1~100 μg·mL-1,and the average recovery(n=6)was 97.43 % (RSD=0.80 %) and 98.59 %(RSD=1.77 %)respectively. Conclusion The method is simple,accurate and reliable,and can be used for the simultaneous determination of ephedrine hydrochloride and pseudoephedrine hydrochloride,which will provide a scientific basis for quality evaluation of Fuganlin oral liquid.

  9. HPLC测定克咳片中生物碱成分的含量%Content Determination of Alkaloids in Keke Tablets by HPLC

    Institute of Scientific and Technical Information of China (English)

    郑英昊; 鲁寅生

    2013-01-01

    Objective To establish the method for determining ephedrine hydochloride and pseudoephedrine hydrochloride in Keke Tablets by HPLC. Methods The samples were analyzed by a phemomenex Synergi Polar-RP column (4.6 mm×250 mm, 4 µm), with mobile phase methanol∶0.092%phosphoric acid (0.04%triethylamine and 0.02%second butylamine)=1.5∶98.5 at flow rate of 1.0 mL/min and detection at UV wavelength of 210 nm. The column temperature was 30 ℃. Results The linear ranges of ephedrine hydrochloride and pseudoephedrine hydrochloride were 6.51×10-3-0.651 µg (r=0.999 9) and 6.27×10-3-0.627 µg (r=1), respectively. The average recoveries (n=6) of ephedrine hydrochloride and pseudoephedrine hydrochloride were 102.26%and 103.71%, with RSD of 0.34%and 0.22%, respectively. Conclusion This method is simple, accurate, reproducible, highly specific and reliable results, and has the ability to effectively control the quality of alkaloids in Keke Tablets.%目的建立高效液相色谱法同时测定克咳片中盐酸麻黄碱、盐酸伪麻黄碱含量的方法。方法色谱柱:phenomenex Synergi Polar-RP柱(4.6 mm×250 mm,4µm);流动相:甲醇∶0.092%磷酸溶液(含0.04%三乙胺和0.02%二正丁胺)=1.5∶98.5;检测波长:210 nm;流速:1.0 mL/min;柱温:30℃。结果盐酸麻黄碱和盐酸伪麻黄碱的线性范围分别为6.51×10-3~0.651µg(r=0.9999)、6.27×10-3~0.627µg(r=1),平均加样回收率(n=6)分别为102.26%、103.71%,RSD 分别为0.34%、0.22%。结论该方法简便、准确,重复性好,专属性高,结果可靠,可有效控制克咳片中生物碱成分的质量。

  10. 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

  11. 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.

    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 {alpha}-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

  12. 有机胺法制备氢氧化镁及其阻燃性能%Preparation and Its Antiflaming Properties of Magnesium Hydroxide by Organic-Amine Method

    Institute of Scientific and Technical Information of China (English)

    汪苏平; 海吉忠; 杨小波; 张志君; 吴江渝; 陈喆; 张勇

    2016-01-01

    Magnesium hydroxide was prepared by using di-n-butylamine as a precipitating agent instead of the traditional inorganic basic precursor. The reaction conditions were optimized by employing the single variable method. The morphology and particle size of the obtained magnesium hydroxide were characterized, and its anti⁃flaming mechanism was investigated. The results show that the optimal experimental conditions for the prepara⁃tion of magnesium hydroxide are as follows:reaction temperature of 70℃, reaction time of 50 minutes, and stir⁃ring rate of 400 r/min. The magnesium hydroxide has a form of lamellar crystal with an average diameter of 1.8μm, and its performances meet the industrial requirements. The precipitant can be recovered and recycled, thus this method is expected to improve the traditional technology for magnesium hydroxide preparation. The results of thermal gravimetric analysis and simulated combustion test suggest that the antiflaming mechanism of magne⁃sium hydroxide can be ascribed to:it improves the thermal decomposition temperature of the used materials, and the magnesium oxide produced by the decomposition of magnesium hydroxide with the carbon forms a layer to achieve thermal insulation and oxygen exclusion.%以二正丁胺代替传统无机碱性前驱物作为沉淀剂的方法制备氢氧化镁.通过控制单一变量法,得到了最佳的实验条件,对氢氧化镁产品进行了形貌表征和粒径分析,并对氢氧化镁的阻燃机理进行了探索.研究表明,通过该方法制备氢氧化镁的最佳实验条件为:反应温度70℃左右,反应时间50 min左右,搅拌速率400 r/min;制得的氢氧化镁为片状结晶,尺寸在1.8μm左右,产品各项性能符合当前工业要求,且沉淀剂可回收二次利用,有望改善氢氧化镁的传统制备工艺.通过热重分析与模拟燃烧实验,推测氢氧化镁的阻燃机理为:一方面提高了材料的热分解温度,另一方

  13. CdS-K2Ti4-xPbxO9复合物的制备及其光催化制氢%Preparation of CdS-pillared K2Ti4-xPbxO9 Composite Photocatalysts and Its Photocatalytic Property for Hydrogen Evolution

    Institute of Scientific and Technical Information of China (English)

    梁英华; 崔文权; 刘利; 李立业; 齐跃丽

    2013-01-01

    采用高温固相法合成铅掺杂的K2Ti4-xPbxO9,微波辅助通过酸交换、胺柱撑、离子交换等步骤制备了硫化镉(CdS)插层的K2Ti4-xPbxO9(CdS-K2Ti4-xPbxO9)复合光催化剂.催化剂的结构利用X射线粉末衍射、紫外-可见漫反射吸收光谱和X射线光电子能谱等进行表征.考察了CdS-K2Ti4-xPbxO9在紫外光及可见光下催化制氢活性.催化剂的可见光吸收范围在Pb掺杂和CdS插层共同作用下得到了扩展,光催化活性也随之提高.催化剂在紫外光和可见光下3h产氢量分别为150.43 mmol/(g cat)和2.43 mmol/(g eat).最后对光催化机理进行了分析.%The K2Ti4-χPbχO9 powder was prepared by a host compound method. CdS-intercalated K2Ti4-χPbχO9 composite photocatalysts (designated as CdS-K2Ti4-χPbχO9) were synthesized via the ion-exchange reaction, butylamine pillaring and sulfuration processes with the irradiation of microwave. The photocatalysts were determined by X-ray diffraction, ultraviolet-visible diffuse reflection spectra and X-ray photoelectron spectroscopy, respectively. The photocatalytic activities of CdS-K2Ti4-χPbχO9 for hydrogen evolution were also investigated under Ultraviolet (UV) and visible light irradiation. The results reveal that the Pb irons doping and CdS-intercalated K2Ti4-χPbχO9 photocatalysts can increase the range of absorb visible light and enhance the photocatalytic activity. The photocatalytic activities for hydrogen production of the CdS-intercalated K2Ti4-χPbχO9 were 150.43 mmol/(g cat) and 2.43 mmol/(g cat) under UV light and visible light irradiation after 3-h irradiation, respectively. In addition, the mechanism of photocataly-sis was discussed.

  14. 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

  15. Inhibition Evaluation of Common Small Molecule Inhibitors of CCR5 for HIV%HIV辅助受体CCR5常见小分子抑制剂抑制效果的综合评价

    Institute of Scientific and Technical Information of China (English)

    焦诗卉; 何淼

    2012-01-01

    The study endeavors to find the optimal inhibitor and the best poses of CCR5 for HIV by comparing the inhibition of common small molecule inhibitors systematically. The results will be helpful to design new drugs of inhibitors. The 3D structures of 29 kinds of small molecule inhibitors from 7 classes were built by using Material Studio software The docking results that each inhibitor docks with CCR5 protein were obtained. Several parameters had been used to evaluate the inhibition effects of these molecules , which include absolute free energy, relative free energy, docking attitude percentage and LibDock composite score et al. And finally the study also revealed the optimal site of CCR5 which located in the second cell outer ring and the N-terminal. The inhibitions from strong to weak are sorted as following; Inhibitor 27 (pyrrolidine) , inhibitors ( benzo cycloheptane vinyl) , inhibitor 12 (piperidine) , inhibitor 14 ( spiro diketone piperidine), inhibitor 21 (4-piperazine pyridine-1-the butylamine class), 5 inhibitors (natural small molecule class), inhibitor 17 (tropicamide alkanes). Among which, inhibitor 27 (pyrrolidine) may be the candidate of optimal inhibitor of CCR5 protein.%通过系统比较CCR5常见小分子抑制剂的抑制效果,寻找CCR5的优化对接靶点,筛选最优抑制剂,为新型抑制剂的研发提供理论依据.基于Material Studio软件,我们构建了7类29种小分子抑制剂的三维结构,全面模拟了各种抑制剂与CCR5对接的效果;利用分子对接绝对自由能、相对自由能、对接姿态百分比和LibDock综合得分等参数评估小分子抑制剂的抑制效果.研究初步发现,CCR5小分子抑制剂的最优对接位点是第二个胞外环与N末端之间的site4.小分子抑制剂的抑制效果由强到弱排序依次为:抑制剂27(吡咯烷类)、抑制剂8(苯并环庚烯类)、抑制剂12(哌啶类)、抑制剂14(螺环二酮哌啶类)、抑制剂21(4-哌啶-1-丁胺类)、抑制剂5(