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Sample records for 2-propanol

  1. Partial oxidation of 2-propanol on perovskites

    Energy Technology Data Exchange (ETDEWEB)

    Sumathi, R.; Viswanathan, B.; Varadarajan, T.K. [Indian Inst. of Tech., Madras (India). Dept. of Chemistry

    1998-12-31

    Partial oxidation of 2-propanol was carried out on AB{sub 1-x}B`{sub x}O{sub 3} (A=Ba, B=Pb, Ce, Ti; B`=Bi, Sb and Cu) type perovskite oxides. Acetone was the major product observed on all the catalysts. All the catalysts underwent partial reduction during the reaction depending on the composition of the reactant, nature of the B site cation and the extent of substitution at B site. The catalytic activity has been correlated with the reducibility of the perovskite oxides determined from Temperature Programmed Reduction (TPR) studies. (orig.)

  2. Sex differences in the toxicokinetics of inhaled solvent vapors in humans 2. 2-propanol

    International Nuclear Information System (INIS)

    The aim of this study was to evaluate possible sex differences in the inhalation toxicokinetics of 2-propanol vapor. Nine women and eight men were exposed on different occasions for 2 h during light physical exercise (50 W) to 2-propanol (350 mg/m3) and to clean air (control exposure). The level corresponds to the Swedish occupational exposure limit. 2-Propanol and its metabolite acetone were monitored up to 24 h after exposure in exhaled air, blood, saliva, and urine by headspace gas chromatography. Body fat and lean body mass were estimated from sex-specific equations using bioelectrical impedance, body weight, height, and age. Genotypes were determined by PCR-based assays for alcohol dehydrogenase and cytochrome P450 2E1 (CYP2E1). The CYP2E1 phenotype was assessed by the 2-h plasma 6-hydroxychlorzoxazone/chlorzoxazone metabolic ratio in vivo. The toxicokinetic profile in blood was analyzed using a one-compartment population model. The following sex differences were significant at the p 0.05 level (Student's t test). The respiratory uptake was lower and the volume of distribution smaller in females. The women had a slightly shorter half-time of 2-propanol in blood and a higher apparent total clearance when corrected for body composition. However, women reached approximately four times higher 2-propanol levels in exhaled air at 10-min postexposure and onward. Acetone in blood was markedly higher in females than in males in the control experiment and slightly higher following exposure to 2-propanol. A marked sex difference was that of a 10-fold higher in vivo blood:breath ratio in men, suggesting sex differences in the lung metabolism of 2-propanol. The most marked sex difference was that of salivary acetone, for which an approximately 100-fold increase was seen in women, but no increase in men, after exposure to 2-propanol compared to clean air. The toxicokinetic analysis revealed no significant differences in toxicokinetics between subjects of different metabolic

  3. Structure and dynamics of aqueous 2-propanol: a THz-TDS, NMR and neutron diffraction study.

    Science.gov (United States)

    McGregor, James; Li, Ruoyu; Zeitler, J Axel; D'Agostino, Carmine; Collins, James H P; Mantle, Mick D; Manyar, Haresh; Holbrey, John D; Falkowska, Marta; Youngs, Tristan G A; Hardacre, Christopher; Stitt, E Hugh; Gladden, Lynn F

    2015-11-11

    Aqueous liquid mixtures, in particular, those involving amphiphilic species, play an important role in many physical, chemical and biological processes. Of particular interest are alcohol/water mixtures; however, the structural dynamics of such systems are still not fully understood. Herein, a combination of terahertz time-domain spectroscopy (THz-TDS) and NMR relaxation time analysis has been applied to investigate 2-propanol/water mixtures across the entire composition range; while neutron diffraction studies have been carried out at two specific concentrations. Excellent agreement is seen between the techniques with a maximum in both the relative absorption coefficient and the activation energy to molecular motion occurring at ∼90 mol% H2O. Furthermore, this is the same value at which well-established excess thermodynamic functions exhibit a maximum/minimum. Additionally, both neutron diffraction and THz-TDS have been used to provide estimates of the size of the hydration shell around 2-propanol in solution. Both methods determine that between 4 and 5 H2O molecules per 2-propanol are found in the 2-propanol/water clusters at 90 mol% H2O. Based on the acquired data, a description of the structure of 2-propanol/water across the composition range is presented.

  4. Molecular conformation and liquid structure of 2-propanol through neutron diffraction

    Indian Academy of Sciences (India)

    A Sahoo; S Sarkar; P S R Krishna; R N Joarder

    2010-05-01

    The neutron diffraction data analysis of deuterated liquid 2-propanol at room temperature to define its molecular conformation is presented. 2-Propanol being a large molecule with twelve atomic sites, the conformation analysis is tricky and an improved method of data analysis is given. The intermolecular structural correlations, i.e., hydrogen-bonded liquid structure, can be modelled accurately to extract the nature of the average hydrogen-bonded molecular association in liquid state at room temperature. Like other alcohols these are mostly hexamer ring chain (HRC) clusters. The cluster analysis of recent X-ray data available in the literature also support the same liquid structure.

  5. Photodissociation dynamics of 1-propanol and 2-propanol at 193.3 nm

    International Nuclear Information System (INIS)

    193.3-nm photodissociation dynamics of jet-cooled 1-propanol and 2-propanol and their partially deuterated variants are examined by using the high-n Rydberg-atom time-of-flight technique. Isotope labeling studies show that O-H bond fission is the primary H-atom production channel in the ultraviolet photodissociation of both 1-propanol and 2-propanol. Center-of-mass (c.m.) product translational energy release of the RO-H dissociation channel is large, with T>=0.78 for H+1-propoxy (n-propoxy) and 0.79 for H+2-propoxy (isoproxy). Maximum c.m. translational energy release yields an upper limit of the O-H bond dissociation energy: 433±2 kJ/mol in 1-propanol and 435±2 kJ/mol in 2-propanol. H-atom product angular distribution is anisotropic (with β≅-0.79 for 1-propanol and -0.77 for 2-propanol), suggesting an electronic transition moment perpendicular to the H-O-C plane and a short excited-state dissociation lifetime (less than a rotational period). Information about photodissociation dynamics and bond energies of the partially deuterated propanols are also obtained. The 193.3-nm photodissociation dynamics of 1-propanol and 2-propanol are nearly identical to each other and are similar to those of methanol and ethanol. This indicates a common RO-H dissociation mechanism: after the nO→σ*(O-H)/3s excitation localized on the H-O-C moiety, the H atom is ejected promptly in the H-O-C plane in a time scale shorter than a rotational period of the parent molecule, and it dissociates along the O-H coordinate on the repulsive excited-state potential-energy surface with a large translational energy release

  6. Measurement and Correlation of Solubility for Propylene in 2-Propanol-Water Solutions

    Institute of Scientific and Technical Information of China (English)

    刘国柱; 任永利; 米镇涛; 吴玉龙

    2003-01-01

    In order to obtain the solubility data of propylene in 2-propanol-water solutions, gas-liquid equilibrium (GLE) experiments were carried out at 303.15-333.15 K, 0.27-0.98 MPa in a static equilibrium still. The original mass ratio of 2-propanol to water was 9∶1,8∶2,7∶3,1∶0, respectively. The equilibrium data were correlated with an empirical model and the regression of model parameters was completed by Gauss-Newton nonlinear least square (NLS). The average relative deviation (ARD) between the experimental and calculated value is 1.5700, and the maximum relative deviation (MRD) is 4.8200. In addition, a simple approach that correlated the model parameters with the system composition was also provided.

  7. Gas Chromatography Method of Cleaning Validation Process for 2-Propanol Residue Determination in Pharmaceutical Manufacturing Equipment

    Directory of Open Access Journals (Sweden)

    Łukasz Czubak

    2014-07-01

    Full Text Available Cleaning validation is an integral operation of good manufacturing practice in pharmaceutical industry. The aim of this study was to validate simple analytical method for detection of 2-propanol residue in equipment, which is likely contaminated with 2-propanol, usually used in the production area. The gas chromatography with flame ionization detection (GC-FID method was validated on a GC system using DB-FFAP capillary column at the flow rate of 4.9 mL/min. The calibration curve was linear over concentration range from 2.8µg/mL to 110.7µg/mL with a correlation coefficient equal to 0.99981. The detection limit (LOD and quantitation limit (LOQ were 1.1µg/mL and 2.8µg/mL, respectively. The simplicity of gas chromatography method makes it useful for routine analysis of 2-propanol residue and is an alternative to corresponding methods.

  8. An investigation into the electro-oxidation of ethanol and 2-propanol for application in direct alcohol fuel cells (DAFCs)

    Indian Academy of Sciences (India)

    Sagar Sen Gupta; Jayati Datta

    2005-07-01

    A comparative study of the electro-oxidation of ethanol and 2-propanol was carried out on carbon-supported platinum particles. Cyclic voltammetry, steady state polarisation, and electrochemical impedance spectroscopy were used to investigate the oxidation reactions. A difference in the mechanistic behaviour of the oxidation of ethanol and 2-propanol on Pt was observed, thereby highlighting the fact that the molecular structure of the alcohol has great influence on its electroreactivity. The study emphasizes the fact that 2-propanol is a promising fuel candidate for a direct alcohol fuel cell.

  9. Ultrasonic study on molecular interactions in binary mixtures of formamide with 1-propanol or 2-propanol

    Institute of Scientific and Technical Information of China (English)

    Manju Rani; Suman Gahlyan; Ankur Gaur; Sanjeev Maken

    2015-01-01

    Ultrasonic speeds have been measured at 298.15 K and 308.15 K for mixtures of formamide+1-propanol or 2-propanol. For an equimolar mixture, excess molar compressibility follows the sequence of 1-propanol N 2-propanol. The ultrasonic speed data are correlated by various correlations such as Nomoto's relation, van Dael's mixing relation and impedance dependence relation, and analyzed in terms of Jacobson's free length theory and Schaaff's collision factor theory. Excess isentropic compressibility is calculated from ex-perimental ultrasonic speed data and previously reported excess volume data. The excess molar ultrasonic speed and isentropic compressibility values are fitted to Redlich–Kister polynomial equation. Other proper-ties such as molecular association, avallable volume, free volume, and intermolecular free length are also calculated. The excess isentropic compressibility data are also interpreted in terms of graph theoretical ap-proach. The calculated isentropic compressibility values are well consistent with the experimental data. It is found that the interaction between formamide and propanol increases when hydroxyl group attached to a carbon atom has more–CH3 groups.

  10. Formation of 2-propanol in condensed molecular films of acetaldehyde following electron impact ionisation-induced proton transfer*

    Science.gov (United States)

    Borrmann, Tobias; Swiderek, Petra

    2016-06-01

    Experimental studies on thin condensed layers of acetaldehyde have previously revealed that electron exposure at an energy above the ionisation threshold leads to formation of 2-propanol. However, the mechanism of this reaction remained unclear. Therefore, a computational approach is used to explore the electron-induced reactions of acetaldehyde yielding 2-propanol. Starting from hydrogen-bonded dimers of acetaldehyde we show that the initial ionisation event triggers proton transfer between the two acetaldehyde moieties resulting in a hydrogen-bonded complex of a [OCCH3] radical and a protonated acetaldehyde cation. Given an excess energy of up to 0.75 eV and a favourable arrangement, a methyl radical released upon dissociation of the CC bond within the [OCCH3] radical can migrate to the carbonyl carbon of the protonated acetaldehyde cation. This produces a 2-propanol radical cation and CO. Neutral 2-propanol is then obtained by recombination with a second electron. A mechanism involving ionisation-driven proton transfer is thus proposed as pathway to the formation of 2-propanol during electron exposure of condensed layers of acetaldehyde.

  11. Correlation and Prediction of Salt Effect on Vapor Liquid Equilibrium for the System of 2-Propanol/Water

    Institute of Scientific and Technical Information of China (English)

    Fu Jiquan

    2008-01-01

    Binary vapor liquid equilibrium (VLE) data were measured for the systems of 2-propanol/ethanediol and ethanediol/potassium acetate (KAc). VLE data for the system of propanol/ethanediol was tested using thermodynamic consistency test. The average values of Δy1 and ΔP were 0.0776 and 0.1542 kPa, respectively. The above two sets of VLE data were correlated with the NRTL model. Ternary VLE data for the system of 2-propanol/water/KAc was used to obtain the more suitable parameters of NRTL model for binary systems of 2-propanol/KAc and water/KAC (called TDCM). For multicomponent systems, ternary and quaternary, the VLE values predicted by the NRTL model agreed well with the literature data. Influence of KAc, ethanediol, and the mixture of KAc and ethanediol on volatility between 2propanol and water was investigated respectively. The results showed that the above-mentioned materials and mixture had different influence on volatility between 2-propanol and water. The method for correlation and prediction of salt-containing VLE is simple and effective for the said system.

  12. 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.

  13. PHOTOREDUCTION OF ALKYL VIOLOGENS AND POLYVIOLOGENS IN 2-PROPANOL AQUEOUS SOLUTION

    Institute of Scientific and Technical Information of China (English)

    LIANG Zhaoxi; LI Wen; LI Manfu

    1987-01-01

    In order to study the effect of alkyl chain length and the polymer effect on the photoreduction behavior of some viologens, a series of alkyl viologen, polyviologen and bisviologen compounds have been synthesized. In the presence of excess 2-propanol, the initial photoreduction of alkyl viologens and polyviologens follow the peudo-second-order reaction, the calculated rate constants are related to the alkyl chain length. In addition, the intramolecular association of radical cations of polyviologens has been found even in dilute solution. However the extent of association is varied with the alkyl chain length. The observed polymer effect of polyviologens in the photoreduction is significant which can be explained in terms of the nature of second order reaction.

  14. Study on Salt-Containing Extractive Distillation for the 2-Propanol/Water System

    Institute of Scientific and Technical Information of China (English)

    Fu Jiquan

    2008-01-01

    The salt-containing extractive distillation column and the salt-containing agent recovery column for the 2-propanol/water/ethanediol/KAc system were simulated by the NRTL model and the modified Rose Relaxation method. The simulation results showed that prediction of the salt effect in vapor-liquid equilib-rium and the correlation method (TDCM) of NRTL parameters were suitable for the said system. Four different distillation technology processes were investigated; the results showed that the salt-containing extractive distillation process was the best one. The simulating design of the extractive distillation column was performed under the conditions of different total stage number, feeding location, reflux ratio, amount of mixed agent and concentration of KAc. The results showed that such factors as 17 stages, a feeding location at the 9th stage, a reflux ratio of 1.2, and a mixed agent feeding rate of 1.141 kmol/h, might be the best suited operating conditions. The simulating design was also done for the column for recovering the salt-containing agent. The simulation method of the salt-containing extractive distillation is simple and effective in this work.

  15. Effect of (+)-limonene and 1-methoxy-2-propanol on Ips typographus response to pheromone blends

    Institute of Scientific and Technical Information of China (English)

    Miroslav Bla(z)enec; Rastislav Jaku(s)

    2009-01-01

    We compared two different strategies to increase the catches of Ips typographus (L.), particularly males, in pheromone-baited traps. The first of these strategies, the barrier approach, used alternating pheromone blends, targeting males and females respectively, in closely-spaced traps forming a barrier around forest stands. The second strategy, the single trap approach, used widely-spaced traps that were all baited with the same lure and intended to trap the highest possible numbers of males without compromising trapping of females. In the blend used for the barrier traps targeting primarily males, with a lower percentage of (4S)-cis-verbenol (cV), the (-)-α-pinene was replaced step wise with (+)-limonene at rates of 0%, 1%, 10%, 35%, 60% and 90%. This replacement had no significant effect on the numbers of responding I. Typographus males, but there was a slight effect on the percentage of males caught. In the attractant blend for the barrier traps targeting females, with a higher percentage of cV, the 2-methyl-3-buten-2-ol (MB) was replaced with 1-methoxy-2-propanol (MP) in a similar fashion as for the male-specific blends. The replacement did not significantly affect the catch of females. Thus, it is possible to use the MP in the blend with cV and ipsdienol without significant change in catch efficacy. In the blends for single traps, the (-)-α-pinene was replaced with (+)-limonene and MB with MP. The replacement of (-)-α-pinene had only a slight effect on the percentage of males, but the results suggest that replacing MB with MP in the blend will not significantly reduce trapping efficacy.

  16. Measurement and Modeling of Vapor-Liquid Equilibrium for Ternary System Water+2-Propanol+1-Butyl-3-methylimidazolium Chloride

    Institute of Scientific and Technical Information of China (English)

    邓东顺; 乔玉珍; 姬登祥; 葛筠; 章连众

    2014-01-01

    Vapor-liquid equilibrium (VLE) data for water+2-propanol+1-butyl-3-methylimidazolium chloride ([bmim]Cl) were measured. Six sets of complete T, x, y data are reported, in which the 2-propanol mole fraction on IL-free basis is fixed separately at 0.1, 0.2, 0.4, 0.6, 0.8, and approximate 0.98, while the IL mass fraction is varied from 0.1 to 0.8, in an interval of 0.1. The non-random-two-liquid (NRTL) and electrolyte non-random-two-liquid (eNRTL) equations are used to correlate the experimental data with satisfactory results. The ternary VLE behavior is also modeled with the parameters obtained by correlating two data sets, in which the mole fraction of 2-propanol on IL-free basis is approximately 0.1 and 0.98. In this way, the six sets of data are reproduced satisfactorily. With the eNRTL model, the root-mean-square deviation for temperature is 0.82 K and that for vapor-phase mole fraction is 0.0078. The influences of IL on activity coefficients and relative volatility of the volatile components are also graphically illustrated.

  17. Studies on Dechlorination of DDT with Alkaline 2-propanol and Iron-Nickel (Fe-Ni) Catalyst.

    Science.gov (United States)

    Shareef, A.; Zaman, S. U.

    2009-05-01

    The Persistent Organic Pollutants (POPs) pesticides were previously extensively used in the cotton production and other agricultural activities in Pakistan and at least three thousand metric tons of obsolete pesticides have been stored under extreme hazardous conditions in more than thousand sites. Locally banned or severely restricted pesticides are easily available and DDT is continuously illegally imported and use in our country. Elimination of organochlorine pesticides (OCPs) waste has received considerable attention over the past two decades. Existing catalytic hydrodechlorinated techniques for disposing of OCPs are very costly due to the use of noble metals as catalysts. The aim of our study is to develop the cost effective and efficient method for the safe disposal of OCPs. This study is in continuation work on dechlorination of organochlorine pesticides with Fe-Ni catalyst in alkaline 2-propanol media. We turned our attention to the development of DDT disposal method for the third world countries. Herein, we report our first finding that in alkaline 2-propanol with Fe-Ni catalyst is an effective method for dechlorination of DDT. Catalytic dechlorination of DDT was carried out in an alkaline solution of NaOH and 2-propanol in the presence of catalyst at the temperature below 82 oC and end products were analyzed by using Gas Chromatography (GC-ECD) and Ion Chromatography (IC) techniques. Results obtained with initial concentration of DDT ranging between 10-100 μg/ml showed conversion of DDT to chlorine free product within 4 hrs.

  18. Inhibition of alcohol dehydrogenase after 2-propanol exposure in different geographic races of Drosophila mojavensis: lack of evidence for selection at the Adh-2 locus.

    Science.gov (United States)

    Pfeiler, Edward; Reed, Laura K; Markow, Therese A

    2005-03-15

    High frequencies of the fast allele of alcohol dehydrogenase-2 (Adh-2F) are found in populations of Drosophila mojavensis that inhabit the Baja California peninsula (race BII) whereas the slow allele (Adh-2S) predominates at most other localities within the species' geographic range. Race BII flies utilize necrotic tissue of pitaya agria cactus (Stenocereus gummosus) which contains high levels of 2-propanol, whereas flies from most other localities utilize different cactus hosts in which 2-propanol levels are low. To test if 2-propanol acts as a selective force on Adh-2 genotype, or whether some other yet undetermined genetic factor is responsible, mature males of D. mojavensis lines derived from the Grand Canyon (race A) and Santa Catalina Island (race C), each with individuals homozygous for Adh-2F and Adh-2S, were exposed to 2-propanol for 24 h and ADH-2 specific activity was then determined on each genotype. Flies from five other localities homozygous for either the fast or slow allele also were examined. Results for all reported races of D. mojavensis were obtained. 2-propanol exposure inhibited ADH-2 specific activity in both genotypes from all localities, but inhibition was significantly less in two populations of race BII flies homozygous for Adh-2F. When F/F and S/S genotypes in flies from the same locality were compared, both genotypes showed high 2-propanol inhibition that was not statistically different, indicating that the F/F genotype alone does not provide a benefit against the inhibitory effects of 2-propanol. ADH-1 activity in female ovaries was inhibited less by 2-propanol than ADH-2. These results do not support the hypothesis that 2-propanol acts as a selective factor favoring the Adh-2F allele. PMID:15726639

  19. The electro-oxidation of the mixture of formaldehyde and 2-propanol on gold (100) and (111) single crystal planes in alkaline medium

    OpenAIRE

    BRANISLAV Z. NIKOLIC; MILKA L. AVRAMOV-IVIC; TANJA R. VIDAKOVIC

    2000-01-01

    The effect of formaldehyde on the oxidation of 2-propanol and vice versa on gold single crystal planes (100 and 111) was studied. An activating effect in the reaction of the simultaneous oxidation of 2-propanol and formaldehyde was obtained on a gold (100) plane. In the case of a gold (111) electrode, the activation effect was not obtained. It was concluded that the adsorption of formaldehyde on the electrode surface prevents the adsorption of poisoning species formed during the electro-oxida...

  20. Quaternary liquid/liquid equilibria of sodium sulfate, sodium sulfite and water with two solvents: Acetone and 2-propanol

    Energy Technology Data Exchange (ETDEWEB)

    Schiozer, A.L.

    1994-03-01

    Aqueous solutions of sodium sulfate and sodium sulfite are produced from sodium carbonate in flue-gas scrubbers; recovery of these salts often requires multi-effect evaporators; however, a new energy-efficient unit operation called extractive crystallization has been shown to have reduced energy costs. In this process, an organic solvent is added to the aqueous salt solution to precipitate salt. Acetone is a suitable solvent for this process, better than 2-propanol. Liquid/liquid/solid equilibria for ternary systems containing a salt, water, and an organic solvent were measured. Systems investigated were sodium sulfite/water/acetone and sodium sulfite/water/2-propanol. Experiments were conducted at salt saturation covering a temperature range between the lower consolute temperature and 48.6{degrees}C. In the attempt to improve the extractive crystallization process for recovery of sodium sulfate from flue-gas scrubbers, attention was given to a feed containing a mixture of sodium sulfite and sodium sulfate. Liquid-liquid equilibria for quaternary systems containing two salts, water, and an organic solvent were experimentally determined at 35{degrees}C. The systems investigated were sodium sulfate/sodium sulfite/water/acetone and sodium sulfate/sodium sulfite/water/2propanol. The systems were studied at three salt ratios. For each salt ratio, experiments were conducted starting at saturation, water was then added until the one-phase region was reached. Mixtures of the two salts proved to have a small disadvantage relative to the 100 % sulfate feed process. Therefore, a sulfate-based extractive crystallization process is recommended.

  1. Catalytic properties of pure and K{sup +}-doped Cu O/Mg O system towards 2-propanol conversion

    Energy Technology Data Exchange (ETDEWEB)

    El-Molla, S. A.; Amin, N. H.; Hammed, M. N.; Sultan, S. N. [Ain Shams University, Faculty of Education, Chemistry Department, Roxy, Heliopolis, Cairo 11757 (Egypt); El-Shobaky, G. A., E-mail: saharelmolla@yahoo.com [National Research Center, Dokki, Cairo (Egypt)

    2013-08-01

    Cu O/Mg O system having different compositions was prepared by impregnation method followed by calcination at 400-900 C. The effect of Cu O content, calcination temperature and doping with small amounts of K{sup +} species (1-3 mol %) on physicochemical, surface and catalytic properties of the system were investigated using X-ray diffraction, adsorption of N{sub 2} at - 196 C, and conversion of isopropyl alcohol at 150-400 C using a flow technique. The results revealed that the solids having the formulae 0.2 and 0.3 Cu O/Mg O calcined at 400 C consisted of nano sized Mg O and Cu O as major phases together with Cu{sub 2}O as minor phase. The Bet-surface areas of different absorbents are decreased by increasing Cu O content, calcination temperature and K{sup +}-doping. Mg O-support material showed very small catalytic activity in 2-propanol conversion. The investigated system behaved as selective catalyst for dehydrogenation of 2-propanol with selectivity >80%. The catalytic activity increased by increasing Cu O content and decreased by increasing the calcination temperature within 400-900 C. K{sup +}-doping increased the catalytic activity and catalytic durability. (Author)

  2. Catalytic properties of pure and K+-doped Cu O/Mg O system towards 2-propanol conversion

    International Nuclear Information System (INIS)

    Cu O/Mg O system having different compositions was prepared by impregnation method followed by calcination at 400-900 C. The effect of Cu O content, calcination temperature and doping with small amounts of K+ species (1-3 mol %) on physicochemical, surface and catalytic properties of the system were investigated using X-ray diffraction, adsorption of N2 at - 196 C, and conversion of isopropyl alcohol at 150-400 C using a flow technique. The results revealed that the solids having the formulae 0.2 and 0.3 Cu O/Mg O calcined at 400 C consisted of nano sized Mg O and Cu O as major phases together with Cu2O as minor phase. The Bet-surface areas of different absorbents are decreased by increasing Cu O content, calcination temperature and K+-doping. Mg O-support material showed very small catalytic activity in 2-propanol conversion. The investigated system behaved as selective catalyst for dehydrogenation of 2-propanol with selectivity >80%. The catalytic activity increased by increasing Cu O content and decreased by increasing the calcination temperature within 400-900 C. K+-doping increased the catalytic activity and catalytic durability. (Author)

  3. Isotopic labeling as a tool to establish intramolecular vibrational coupling: The reaction of 2-propanol on Mo(110)

    Energy Technology Data Exchange (ETDEWEB)

    Uvdal, P.; Wiegand, B.C.; Serafin, J.G.; Friend, C.M. (Department of Chemistry, Harvard University, Cambridge, Massachusetts 02138 (United States))

    1992-12-01

    The reactions of 2-propanol on Mo(110) were investigated using temperature programmed reaction, high resolution electron energy loss, and x-ray photoelectron spectroscopies. 2-Propanol forms 2-propoxide upon adsorption at 120 K on Mo(110). The 2-propoxide intermediate deoxygenates via selective {gamma} C--H bond scission to eliminate propene as well as C--O bond hydrogenolysis to form trace amounts of propane. The C--O bond of 2-propoxide is estimated to be nearly perpendicular to the surface. Selective isotopic labeling was used to establish the coupling between the C--O stretch and modes associated with the hydrocarbon framework. The degree of coupling was strongly affected by bonding to the surface, primarily due to weakening of the C--O bond when 2-propoxide is bound to Mo(110). Selective isotopic labeling was, therefore, essential in making vibrational assignments and in identifying key reaction steps. Only a small kinetic isotope effect was observed during reaction of (CD{sub 3})(CH{sub 3})CHOH, consistent with a substantial component of C--O bond breaking in the transition state for propene elimination. Coupling of the C--O stretch to motion of the methyl group is also suggested to be important in the transition state for propene elimination.

  4. Equilibrium solubility of CO2 in aqueous solutions of 1-amino-2-propanol as function of concentration, temperature, and pressure

    International Nuclear Information System (INIS)

    Research highlights: → Gas solubility of CO2 in aqueous solutions of 1-amino-2-propanol was measured. → Solubility increases as pressure and concentration of 1-amino-2-propanol increase. → The Kent-Eisenberg model was used to correlate all the experimental results. → Aqueous solutions of MIPA are an excellent alternative to use in gas purification. - Abstract: Using a dynamic method with recirculation of the vapour phase, experimental values for the gas solubility of carbon dioxide in aqueous solutions of 1-amino-2-propanol (MIPA) were measured at T = (313.15 and 393.15) K, over the pressure range of (0.2 to 2436.4) kPa. The concentrations of the studied aqueous MIPA solutions were (0.20, 0.30, 0.40, and 0.50) mass fraction. The results of gas solubility are given as the partial pressure of CO2, pCO2, against its mole ratio, αCO2 (mol CO2 · mol-1 MIPA), and its mole fraction, xCO2. It is observed that the solubility of CO2 increases as the concentration of MIPA in solution increases, at a given temperature throughout the pressure range considered; also the solubility values increase, under constant temperature, as the pressure increases in the studied concentration range of MIPA. The physicochemical model of Kent and Eisenberg was used to correlate simultaneously all the experimental results of the solubility of CO2 in the studied aqueous solutions of MIPA. The model correlates satisfactorily the experimental results. The deviation for pressure was 96.9 kPa using 62 experimental solubility points. The solubility results of carbon dioxide presented in this work are compared with those reported in the literature for aqueous solutions of monoethanolamine (MEA), diethanolamine (DEA), diisopropanolamine (DIPA), and N-methyldiethanolamine (MDEA) and it is possible to conclude that the aqueous solutions of MIPA are an excellent alternative to use in gas purification processes, since the magnitude of the solubility results of MIPA solutions was found to be

  5. (Liquid + liquid) equilibrium of (water + 2-propanol + 1-butanol + salt) systems at T = 313.15 K and T = 353.15 K: Experimental data and correlation

    Energy Technology Data Exchange (ETDEWEB)

    Pereira, Milton A.P. [School of Chemical Engineering, State University of Campinas, P.O. Box 6066, 13081-970 Campinas-SP (Brazil); Aznar, Martin [School of Chemical Engineering, State University of Campinas, P.O. Box 6066, 13081-970 Campinas-SP (Brazil)]. E-mail: maznar@feq.unicamp.br

    2006-06-15

    (Liquid + liquid) equilibrium data for the quaternary systems (water + 2-propanol + 1-butanol + potassium bromide) and (water + 2-propanol + 1-butanol + magnesium chloride) were measured at T = 313.15 K and T = 353.15 K. The overall salt concentrations were 5 and 10 mass percent. Ternary (liquid + liquid) equilibrium data for the salt-free system (water + 2-propanol + 1-butanol) were also determined and found to be in good agreement with data from the literature. The NRTL model for the activity coefficient was used to correlate the data. New interaction parameters were estimated, using the Simplex minimization method and a concentration-based objective function. The results are very satisfactory, with root mean square deviations between experimental and calculated compositions of both phases being less than 0.5%.

  6. The electro-oxidation of the mixture of formaldehyde and 2-propanol on gold (100 and (111 single crystal planes in alkaline medium

    Directory of Open Access Journals (Sweden)

    BRANISLAV Z. NIKOLIC

    2000-12-01

    Full Text Available The effect of formaldehyde on the oxidation of 2-propanol and vice versa on gold single crystal planes (100 and 111 was studied. An activating effect in the reaction of the simultaneous oxidation of 2-propanol and formaldehyde was obtained on a gold (100 plane. In the case of a gold (111 electrode, the activation effect was not obtained. It was concluded that the adsorption of formaldehyde on the electrode surface prevents the adsorption of poisoning species formed during the electro-oxidation of 2-propanol on the Au(100 plane, while this is not the case on the Au(111 plane. The different behaviour is caused by the difference in the symmetry of the surface atoms of these two Au single-crystal planes.

  7. ELECTROCHEMICAL DETERMINATION OF ETHANOL, 2- PROPANOL AND 1-BUTANOL ON GLASSY CARBON ELECTRODE MODIFIED WITH NICKEL OXIDE FILM

    Directory of Open Access Journals (Sweden)

    A. Benchettara

    2014-12-01

    Full Text Available In this work, we present the modification of a glassy carbon electrode with nickel oxide film which is performed in two successive steps. In the first one, the electrochemical deposition of metallic nickel on the glassy carbon electrode (GCE is achieved in 0.1M boric acid; in the second step, the metallic deposit is anodically oxidized in 0.1M NaOH. These two operations were carried out in a three electrode cell with a filiform platinum auxiliary electrode, a SCE as potential reference and a working microelectrode of modified glassy carbon with nickel oxides. This electrode is characterized by several electrochemical techniques and is used for the catalytic determination of ethanol, 2-propanol and 1-butanol in 0.1 M NaOH. The proposed chemical mechanism shows that NiO2 acts as a mediator.

  8. ELECTROCHEMICAL DETERMINATION OF ETHANOL, 2- PROPANOL AND 1-BUTANOL ON GLASSY CARBON ELECTRODE MODIFIED WITH NICKEL OXIDE FILM

    Directory of Open Access Journals (Sweden)

    A. Benchettara

    2015-07-01

    Full Text Available In this work, we present the modification of a glassy carbon electrode with nickel oxide film which is performed in two successive steps. In the first one, the electrochemical deposition of metallic nickel on the glassy carbon electrode (GCE is achieved in 0.1M boric acid; in the second step, the metallic deposit is anodically oxidized in 0.1M NaOH. These two operations were carried out in a three electrode cell with a filiform platinum auxiliary electrode, a SCE as potential reference and a working microelectrode of modified glassy carbon with nickel oxides. This electrode is characterized by several electrochemical techniques and is used for the catalytic determination of ethanol, 2-propanol and 1-butanol in 0.1 M NaOH. The proposed chemical mechanism shows that NiO2 acts as a mediator.

  9. Photocatalytic Oxidation of Low-Level Airborne 2-Propanol and Trichloroethylene over Titania Irradiated with Bulb-Type Light-Emitting Diodes

    Directory of Open Access Journals (Sweden)

    Wan-Kuen Jo

    2013-01-01

    Full Text Available This study examined the photocatalytic oxidation of gas-phase trichloroethylene (TCE and 2-propanol, at indoor levels, over titanium dioxide (TiO2 irradiated with light-emitting diodes (LED under different operational conditions. TiO2 powder baked at 450 °C exhibited the highest photocatalytic decomposition efficiency (PDE for TCE, while all photocatalysts baked at different temperatures showed similar PDEs for 2-propanol. The average PDEs of TCE over a three hour period were four, four, five, and 51% for TiO2 powders baked at 150, 250, 350, and 450 °C, respectively. The average PDEs of 2-propanol were 95, 97, 98, and 96% for TiO2 powders baked at 150, 250, 350, and 450 °C, respectively. The ratio of anatase at 2θ = 25.2° to rutile at 2θ = 27.4° was lowest for the TiO2 powder baked at 450 °C. Although the LED-irradiated TiO2 system revealed lower PDEs of TCE and 2-propanol when compared to those of the eight watt, black-light lamp-irradiated TiO2 system, the results for the PDEs normalized to the energy consumption were reversed. Other operational parameters, such as relative humidity, input concentrations, flow rate, and feeding type were also found to influence the photocatalytic performance of the UV LED-irradiated TiO2 system when applied to the cleaning of TCE and 2-propanol at indoor air levels.

  10. Densities, viscosities, refractive indices, and surface tensions for binary and ternary mixtures of 2-propanol, tetrahydropyran, and 2,2,4-trimethylpentane

    Energy Technology Data Exchange (ETDEWEB)

    Kao, Y.-C. [Department of Applied Chemistry, Providence University, Shalu 43301, Taiwan (China); Tu, C.-H., E-mail: chtu@pu.edu.t [Department of Applied Chemistry, Providence University, Shalu 43301, Taiwan (China)

    2011-02-15

    Densities, viscosities, refractive indices, and surface tensions of the ternary system (2-propanol + tetrahydropyran + 2,2,4-trimethylpentane) at T = 303.15 K and its constituent binary systems (2-propanol + tetrahydropyran, 2-propanol + 2,2,4-trimethylpentane, and tetrahydropyran + 2,2,4-trimethylpentane) at T = (293.15, 303.15, 313.15, and 323.15) K were measured at atmospheric pressure. Densities were determined using a vibrating-tube densimeter. Viscosities were measured with an automatic microviscometer based on the rolling-ball principle. Refractive indexes were measured using a digital Abbe-type refractometer. Surface tensions were determined by the Wilhelmy-plate method. From these data, excess molar volumes, deviations in viscosity, deviations in refractive index, and deviations in surface tension were calculated. The results for the binary and ternary systems were fitted to the Redlich-Kister equation and the variable-degree polynomials in terms of compositions, respectively. The experimental and calculated quantities are used to study the nature of mixing behaviour between mixture components.

  11. Excess isentropic compressibility and speed of sound of the ternary mixture 2-propanol + diethyl ether + n-hexane and the constituent binary mixtures at 298.15 K

    Indian Academy of Sciences (India)

    Gokhan Sovaroglu; Ertunc Aral

    2006-02-01

    Speed of sound and densities of the ternary mixture 2-propanol + diethyl ether + n-hexane and also the binary mixtures 2-propanol + diethyl ether and 2-propanol + n-hexane have been measured at the entire composition range at 298.15 K. The excess isentropic compressibilities and the excess speed of the sound have been calculated from experimental densities and speed of sound. These excess properties of the binary mixtures were fitted to Redlich-Kister equation, while the Cibulka's equation was used to fit the values related to the values to the ternary system. These excess properties have been used to discuss the presence of significant interactions between the component molecules in the binary mixtures and also the ternary mixtures. Speed of sound of the binary mixtures and the ternary mixture have been compared with calculated values from free length theory (FLT), collision factor theory (CFT), Nomoto's relation (NR), Van Deal's ideal mixing relation (IMR) and Junjie's relation (JR). The results are used to compare the relative merits of these theories and relations in terms of the root mean square deviation relative (RMSDr).

  12. LIQUID-LIQUID EQUILIBRIA FOR MIXTURES OF WATER,DECANE and 1-ETHOXY-2-PROPANOL%1-乙氧基-2-丙醇/水/癸烷的液液平衡

    Institute of Scientific and Technical Information of China (English)

    陈瑶; 李任强; 田村和弘

    2003-01-01

    Experimental data of ternary liquid-liquid equilibria for mixtures of 1-ethoxy-2-propanol, water and decane were measured at 298.15K.Extended UNIQUAC model was empolyed to correlate those data. The extended UNIQUAC model successfully represented the thermodynamic properties for the ternary system of 1-ethoxy-2-propanol, water and decane. These experimental results are useful for designing the separation and extraction process.

  13. A Computational Study on the Mechanism for the K_2CO_3-catalyzed Reaction of Carbon Dioxide and 1-Chlo-2-propanol

    Institute of Scientific and Technical Information of China (English)

    张福兰; 万邦江; 黄辉胜

    2012-01-01

    The microcosmic reaction mechanism of K2CO3-catalyzed 1-chlo-2-propanol and carbon dioxide has been investigated by density functional theory(DFT) at the GGA/PW91/DNP level.We optimize the geometric configurations of reactants,intermediates,transition states,and products.The energy analysis calculation approves the authenticity of intermediates and transition states.According to our calculations,four feasible reaction pathways are found.The main pathway of the reaction is ReA → IMA1 → TSA1 → IMA2 → IMA5 → TSA5 → P.Besides,we also in-vestigate the reaction mechanism of 1-chlo-2-propanol and carbon dioxide without K2CO3-catalyzation by the same theory and level.The computational results indicate that the activation barrier with K2CO3-catalyzed is smaller than the activation barrier without K2CO3-catalyzed.That is to say,K2CO3 can promote the reaction to give the product in a high yield,which is in agreement with the experimental results.

  14. Equilibrium solubility of CO{sub 2} in aqueous solutions of 1-amino-2-propanol as function of concentration, temperature, and pressure

    Energy Technology Data Exchange (ETDEWEB)

    Rebolledo-Morales, Miguel Angel; Rebolledo-Libreros, Maria Esther [Instituto Mexicano del Petroleo, Direccion de Investigacion y Posgrado, Programa de Ingenieria Molecular, Area de Investigacion de Termofisica, Eje Central Lazaro Cardenas Norte 152, 07730 Mexico, D.F. (Mexico); Trejo, Arturo, E-mail: atrejo@imp.m [Instituto Mexicano del Petroleo, Direccion de Investigacion y Posgrado, Programa de Ingenieria Molecular, Area de Investigacion de Termofisica, Eje Central Lazaro Cardenas Norte 152, 07730 Mexico, D.F. (Mexico)

    2011-05-15

    Research highlights: Gas solubility of CO{sub 2} in aqueous solutions of 1-amino-2-propanol was measured. Solubility increases as pressure and concentration of 1-amino-2-propanol increase. The Kent-Eisenberg model was used to correlate all the experimental results. Aqueous solutions of MIPA are an excellent alternative to use in gas purification. - Abstract: Using a dynamic method with recirculation of the vapour phase, experimental values for the gas solubility of carbon dioxide in aqueous solutions of 1-amino-2-propanol (MIPA) were measured at T = (313.15 and 393.15) K, over the pressure range of (0.2 to 2436.4) kPa. The concentrations of the studied aqueous MIPA solutions were (0.20, 0.30, 0.40, and 0.50) mass fraction. The results of gas solubility are given as the partial pressure of CO{sub 2}, p{sub CO{sub 2}}, against its mole ratio, {alpha}{sub CO{sub 2}} (mol CO{sub 2} {center_dot} mol{sup -1} MIPA), and its mole fraction, x{sub CO{sub 2}}. It is observed that the solubility of CO{sub 2} increases as the concentration of MIPA in solution increases, at a given temperature throughout the pressure range considered; also the solubility values increase, under constant temperature, as the pressure increases in the studied concentration range of MIPA. The physicochemical model of Kent and Eisenberg was used to correlate simultaneously all the experimental results of the solubility of CO{sub 2} in the studied aqueous solutions of MIPA. The model correlates satisfactorily the experimental results. The deviation for pressure was 96.9 kPa using 62 experimental solubility points. The solubility results of carbon dioxide presented in this work are compared with those reported in the literature for aqueous solutions of monoethanolamine (MEA), diethanolamine (DEA), diisopropanolamine (DIPA), and N-methyldiethanolamine (MDEA) and it is possible to conclude that the aqueous solutions of MIPA are an excellent alternative to use in gas purification processes, since the

  15. Ternary liquid-liquid equilibria of dimethyl carbonate + 2-propanol + water system at 303.15 and 313.15 K

    Science.gov (United States)

    Ginting, Rizqy Romadhona; Mustain, Asalil; Tetrisyanda, Rizki; Gunardi, Ignatius; Wibawa, Gede

    2015-12-01

    In this work, liquid-liquid equilibria data of dimethyl carbonate (DMC) + 2-propanol + water system were accurately determined at 303.15 and 313.15 K using stirred and jacketed equilibrium cell under atmospheric pressure. The reliabilities of the experimental data were confirmed using Bachman-Brown correlation giving r-squared value of 0.9993 and 0.9983 at 303.15 and 313.15 K, respectively. Experimental data obtained in this work exhibit Treybal's Type I ternary phase behavior. The selectivity and distribution coefficient of DMC increases with addition of DMC concentration in the organic phase. On the other hand, the effect of temperature to phase boundary was found to be not significant. The data were correlated well using the Non-Random Two Liquid (NRTL) and Universal Quasi-Chemical (UNIQUAC) activity coefficient models with root-mean-square deviation of 1.5% and 1.3%, respectively.

  16. Catalytic Oxidative Conversion from Naphthol to 2-Hydroxy-1, 4-naphthoquinone over Iron Porphyrin Catalysts by Molecular Oxygen in an Alkaline 2-Propanol Solution

    Institute of Scientific and Technical Information of China (English)

    YANG Ke-er; TONG Shan-ling; YAN Yan; KANG En-hua; XIAO Feng-shou; LI Qing; CHANG Xin; FANG Chi-guang

    2005-01-01

    In an alkaline 2-propanol solution with 5,10,15,20-tetra(4-methoxyl phenyl) porphyrin iron chloride(TOMPPFeCl) as a catalyst and oxygen as a cheap green oxidant, 2-naphthol was conversed to 2-hydroxy-1,4-naphthoquinone(HNQ) with a yield of 62.17% and a selectivity of 100%, and the conversion number of TMOPPFeCl catalyst was 8.32/min. The catalytic oxidation products were characterized by means of UV-Vis, IR, GC-MS, 1H NMR and melting point determination. In this catalytic oxidation, the catalytic activity of TMOPPFeCl was researched in detail and the reacting conditions were optimized. A possible reaction mechanism is summarized based on in situ EPR determination.

  17. Synthesis, radiolabeling and in vivo evaluation of [11C](R)-1-[4-[2-(4-methoxyphenyl)phenyl]piperazin-1-yl]-3-(2-pyrazinyloxy)-2-propanol, a potential PET radioligand for the 5-HT7 receptor

    DEFF Research Database (Denmark)

    Hansen, Hanne Demant; Lacivita, Enza; Di Pilato, Pantaleo;

    2014-01-01

    In the search for a novel serotonin 7 (5-HT7) receptor PET radioligand we synthesized and evaluated a new series of biphenylpiperazine derivatives in vitro. Among the studied compounds, (R)-1-[4-[2-(4-methoxyphenyl)phenyl]piperazin-1-yl]-3-(2-pyrazinyloxy)-2-propanol ((R)-16), showed the best...

  18. Decomposition mechanism of 2-propanol and 1,1,1-trifluoro-2-propanol on Ni(100) surface%2-丙醇和1,1,1-三氟-2-丙醇在Ni(100)表面的裂解机理

    Institute of Scientific and Technical Information of China (English)

    张福兰

    2016-01-01

    本文研究了2-丙醇和1,1,1-三氟-2-丙醇在Ni(100)表面解离的可能微观反应机理,使用完全线性同步和二次同步变换( complete LST/QST)方法确定解离反应的过渡态.采用基于第一性原理的密度泛函理论与周期平板模型相结合的方法,优化了2-丙醇和1,1,1-三氟-2-丙醇裂解反应过程各物种在Ni(100)表面的top,hollow和bridge位的吸附模型,计算了能量,并对布局电荷进行了分析,得到了各物种的有利吸附位.结果表明:2-丙醇和1,1,1-三氟-2-丙醇在Ni(100)表面都存在β-H和γ-H两个平行竞争的解离过程,其中2-丙醇在Ni(100)表面β-H解离的速控步骤活化能为64.7 kJ· mol -1猯,而γ-H 解离速控步骤活化能为233.1 kJ · mol-1猯,故β-H 解离过程占优势,主要产物是CH3COCH3;相反,1,1,1-三氟-2-丙醇在Ni(100)表面β-H解离的速控步骤活化能为257.1 kJ· mol-1猯,而γ-H解离速控步骤活化能为148.1 kJ · mol -1猯,故γ-H解离过程占优势,主要产物是CF3 CH=CH2.由此说明,电负性更大的氟原子取代2-丙醇中的氢原子之后,2-丙醇在Ni表面的解离机理发生了改变.理论预测结果与实验结论一致.%The possible decomposition mechanism of 2 -propanol and 1,1,1 -trifluoro -2 -propanol on Ni (100) surface was investigated utilizing the first -principles density functional theory (DFT) and self-consist-ent periodic calculation.The transition states were testified by using the complete Linear Synchronous Transit and the Quadratic Synchronous Transit ( LST/QST) methods.All the species involved in this process on three possi-ble adsorption sites (top, hollow, and bridge) on Ni(100) surface were fully optimized to obtain their equilibri-um geometries.The corresponding adsorption energies and Mullikan charge analysis of these species were predic -ted and

  19. Studies of mixing properties of binary systems of 2-propanol with hexadecane and squalane at T = (298.15, 303.15, and 308.15) K

    Energy Technology Data Exchange (ETDEWEB)

    Dubey, Gyan P. [Department of Chemistry, Kurukshetra University, Kurukshetra 136 119 (India)], E-mail: gyan.dubey@rediffmail.com; Sharma, Monika [Department of Chemistry, Kurukshetra University, Kurukshetra 136 119 (India)], E-mail: sharmamonika20@rediffmail.com

    2009-01-15

    The present paper reports the experimental data for density, {rho}, viscosity, {eta}, and speeds of sound, u for the binary mixtures of 2-propanol, (CH{sub 3}){sub 2}CHOH with hexadecane, C{sub 16}H{sub 34} over the miscibility region (0 < x{sub 1} < 1) and with squalane (2,4,6,10,15,19,23-hexametyltetracosane), C{sub 30}H{sub 62} over the miscibility region (0 < x{sub 1} < 0.6) at T = (298.15, 303.15, and 308.15) K. The experimental data have been used to calculate various parameters like excess molar volumes, V{sub m}{sup E}, viscosity deviations, {delta}{eta}, excess molar isentropic compressibility, K{sub S,m}{sup E}, and deviations in speed of sound, u{sup D}, from their ideal values u{sup id}. These excess parameters and deviations are used to interpret the molecular interactions in these binary mixtures.

  20. Preparation of promoted platinum catalysts of designed geometry and the role of promoters in the liquid-phase oxidation of 1-methoxy-2-propanol

    Energy Technology Data Exchange (ETDEWEB)

    Mallat, T.; Bodnar, Z.; Baiker, A. (Swiss Federal Institute of Technology, Zuerich (Switzerland)); Greis, O.; Struebig, H. (Technical Univ., Hamburg (Germany)); Reller, A. (Univ. of Hamburg (Germany))

    1993-07-01

    Alumina-supported or unsupported M/Pt-type catalysts were prepared by consecutive reduction of Bi, Pb, Sn, Ru, Au, or Ag modifiers (M) onto Pt particles. Structural and chemical properties of the bimetallics were studied by electron microscopy combined with energy dispersive X-ray analysis and an electrochemical (cyclic voltammetric) polarization method. Preferential deposition of promoter metal submonolayers on Pt was observed at moderate surface coverages ([theta][sub M]<0.5-0.8). Some bulk metal crystallite formation as [open quotes]bridges[close quotes] between small Pt particles covered partially with promoter was also observed on alumina-supported Bi/Pt and Pb/Pt catalysts. Measurement of the electrochemical potential of the catalyst slurry during the oxidation of 1-methoxy-2-propanol to methoxyacetone and the cyclic voltammetric polarization of the bimetallic catalysts revealed that the catalysts are in an oxidized state during reaction. The following order of promoting influence was observed: Bi > Pb [approximately] Sn > Au [approximately] Ru. Two major effects of promoters are suggested: (i) they suppress the initial irreversible adsorption of the reactant alcohol on Pt which results in self-poisoning, and (ii) they form new active centers that adsorb the oxidizing species (OH) better than Pt. A formal rate equation is suggested (r = f [center dot] [theta][sub org] [center dot] [theta][sub OH]) which explains the optimum in promoter/platinum ratio. The different influences of the promoters are explained by their hydrogen and oxygen sorption characteristics and by the surface geometry of the bimetallic catalysts. 51 refs., 12 figs., 1 tab.

  1. Structure–acidity correlation of supported tungsten(VI)-oxo-species: FT-IR and TPD studies of adsorbed pyridine and catalytic decomposition of 2-propanol

    Energy Technology Data Exchange (ETDEWEB)

    Zaki, M.I., E-mail: mizaki@mu.edu.eg; Mekhemer, G.A.H.; Fouad, N.E.; Rabee, A.I.M.

    2014-07-01

    The amount of 10 wt%-WO{sub 3} was supported on alumina, titania or silica by impregnation with aqueous solution of ammonium paratungstate and subsequent calcination at 500 °C for 10 h. Tungstate-related chemical and physical changes in the calcination products were resolved by ex-situ infrared (IR) spectroscopy. Nature of exposed surface acid sites were probed by in-situ IR spectroscopy of adsorbed pyridine (Py) molecules at room temperature (RT). The relative strength of the acid sites thus probed was gauged by combining results of temperature-programmed desorption (TPD) measurements of the RT-adsorbed Py with those communicated by in-situ IR spectra of residual Py on the surface after a brief thermoevacuation at high temperatures (100–300 °C). Reactivity of the surface acid sites was tested toward 2-propanal catalytic decomposition, and observed by in-situ IR gas phase spectra. Results obtained were correlated with predominant structures assumed by the supported tungstate species. Accordingly, polymerization of the supported tungstate into 2-/3-dimensional structures, was found to be relatively most advanced on favorable locations of titania surfaces as compared to the case on alumina or silica surfaces. Consequently, the Lewis acidity was strengthened, and strong Bronsted acidity was evolved, leading to a 2-propanol dehydration catalyst (tungstate/titania) of optimal activity and selectivity. Strong tungstate/support interfacial interactions were found to hamper the formation of the strongly acidic and catalytically active polymeric structures of the supported tungstate (i.e., the case on alumina or silica).

  2. 正丙醇和异丙醇的紫外光解动力学%Ultraviolet Photodissociation Dynamics of 1-Propanol and 2-Propanol by High-n Rydberg-Atom Time-of-flight(HRTOF) Technique

    Institute of Scientific and Technical Information of China (English)

    周卫东; 张劲松

    2002-01-01

    利用高里德堡态氢原子飞行时间(HRTOF)探测技术,研究了正丙醇和异丙醇的紫外光解动力学过程.在193.3 nm光辐射下,O-H键快速断裂过程构成主要的氢原子生成通道.伴随O-H键的碎裂,相当大的一部分能量转换成氢原子及其相应碎片的平动能(正丙醇〈fv〉=0.76; 异丙醇〈fv〉=0.78).氢原子碎片具有各向异性的角度分布;其角分布异向因子β分别为-0.79(正丙醇)和-0.77(异丙醇).研究结果表明,吸收1个193.3 nm光子后,丙醇分子跃迁到一个寿命很短的电子激发态;沿着O-H反应坐标,该激发态势能面是排斥的,因而O-H键快速断裂.此外,还得到了丙醇的O-H键离解能: (432±2)kJ/mol(正丙醇)和(433±2)kJ/mol(异丙醇).%193.3 nm photodissociation dynamics of jet-cooled 1-propanol and 2-propanol has been examined by using high-n Rydberg-atom time-of-flight (HRTOF) technique. Isotope labeling study indicates that O-H bond fission is the primary H-atom production channel. Center-of-mass (CM) product translational energy release of this channel is large, with 〈fT〉= 0.76 for H+1-propoxy and 0.78 for H+2-propoxy. Maximum CM translational energy release yields an upper limit of the O-H bond dissociation energy: (432±2)kJ/mol in 1-propanol and (433±2)kJ/mol in 2-propanol. H-atom product angular distribution is anisotropic (with β≈-0.79 for 1-propanol and -0.77 for 2-propanol), indicating a short excited-state lifetime. The 193.3 nm H-atom dissociation of both 1-propanol and 2-propanol is prompt and occurs on a repulsive excited-state potential energy surface.

  3. Determination of Acetophenone and 2-Phenyl-2-propanol Release in EVA Material%EVA材料中苯乙酮和2-苯基-2-丙醇释放量的测定

    Institute of Scientific and Technical Information of China (English)

    陈皖芳; 穆江华; 钱明伟

    2011-01-01

    本方法采用顶空GC-MS测定EVA材料中的苯乙酮和2-苯基-2-丙醇的释放量。方法检测限为5 mg/kg,EVA材料中的平均加标回收率为90.0%~105%。方法简捷、快速、准确,适用于EVA材料中苯乙酮和2-苯基-2-丙醇释放量的测定。%An analytical method based on using headspace extraction EVA material,the capillary vessel column gas phase mass spectrography carried on qualitative and quota to acetophenone and 2-Phenyl-2-propanol release.The method examination limit was 5 mg/kg,the mean recoveries for packaging material samples were 90.0 %~105 %.The method was accurate,simple,rapid and feasible for the inspection of acetophenone and 2-Phenyl-2-propanol release in EVA materials.

  4. Application of the margin of exposure (MoE) approach to substances in food that are genotoxic and carcinogenic: example: (CAS No. 96-23-1) 1,3-dichloro-2-propanol (DCP).

    Science.gov (United States)

    Williams, Gary; Leblanc, Jean-Charles; Setzer, R Woodrow

    2010-01-01

    1,3-Dichloro-2-propanol (DCP) is formed in foods under a variety of conditions. It was positive in a variety of in vitro genotoxicity tests, but was negative in two in vivo studies. DCP produced neoplasms at several sites in rats. Kidney tumours in male rats were selected as the critical tumour type. Dose-response modelling of the data for DCP gave a BMDL(10) for combined kidney carcinomas and adenomas in male rats of 9.62 mg/kg-body weight (bw)/day. The exposure of humans was estimated at an average of 0.00009 mg/kg-bw/day and a high exposure of 0.000136 mg/kg-bw/day. The MOEs for these exposures were 100,000 and 70,000, respectively. PMID:20113855

  5. Application of the margin of exposure (MoE) approach to substances in food that are genotoxic and carcinogenic: example: (CAS No. 96-23-1) 1,3-dichloro-2-propanol (DCP).

    Science.gov (United States)

    Williams, Gary; Leblanc, Jean-Charles; Setzer, R Woodrow

    2010-01-01

    1,3-Dichloro-2-propanol (DCP) is formed in foods under a variety of conditions. It was positive in a variety of in vitro genotoxicity tests, but was negative in two in vivo studies. DCP produced neoplasms at several sites in rats. Kidney tumours in male rats were selected as the critical tumour type. Dose-response modelling of the data for DCP gave a BMDL(10) for combined kidney carcinomas and adenomas in male rats of 9.62 mg/kg-body weight (bw)/day. The exposure of humans was estimated at an average of 0.00009 mg/kg-bw/day and a high exposure of 0.000136 mg/kg-bw/day. The MOEs for these exposures were 100,000 and 70,000, respectively.

  6. Synthesis and preliminary evaluation of (R,S)-1-[2-((carbamoyl-4-hydroxy)phenoxy)-ethylamino]-3-[4-(1-[11C]-met hyl-4-trifluoromethyl-2-imidazolyl)phenoxy]-2-propanol ([11C]CGP 20712A) as a selective beta 1-adrenoceptor ligand for PET

    NARCIS (Netherlands)

    Elsinga, P H; Van Waarde, A; Visser, Gerben; Vaalburg, W

    1994-01-01

    The most selective beta 1-adrenoceptor ligand known at this moment is (S)-1-[2-((carbamoyl-4-hydroxy) phenoxy)ethylamino]-3-[4-(1-methyl-4-trifluoromethyl-2-imidazolyl) phenoxy]-2-propanol (CGP 26505), the S-isomer of CGP 20712A. We prepared the racemic 11C analogue by methylation with [11C]CH3I of

  7. 1-丙醇和2-丙醇真空紫外光电离质谱研究%A Vacu um Ultraviolet Photoionization Mass Spectrometric Study of 1-Propanol and 2-Propanol

    Institute of Scientific and Technical Information of China (English)

    卫立夏; 杨斌; 王晶; 黄超群; 盛六四; 齐飞

    2006-01-01

    The photoionization and dissociative photoionization of 1-propanol and 2-propanols have been studied at the photon energy range of 9.84~11.80 eV. Photoionization efficiency spectra for ions CH3CH2CH2OH+, CH3CH2CHOH+,CH2CH2OH+, CH3CH2CH2+, CH3CH=CH+2, CH2OH+ from 1-propanol, and CH3CH(OH)CH3+, CH3C(OH)CH3+, CH3CHOH+,CH2=CHOH+, CH3CHCH3+, CH3CH=CH2+ from 2-propanol have been measured. In addition, the energetics of the dissociative photoionization has been examined by ab initio Gaussion-3(G3) calculations. The computational results are useful in establishing the dissociation channels near the ionization thresholds. With the help of G3 results, the dissociation channels for formation of the fragment ions CH3CH2CHOH+, CH2CH2OH+, CH3CH2CH2+, CH3CH=CH2+,CH2OH+ from 1-propanol, and CH3C(OH)CH3+, CH3CHOH+, CH2=CHOH+, CH3CHCH3+, CH3CH=CH2+ from 2-propanol have been established. The G3 results are in excellent agreement with the experimental data.%研究了9.84~11.80 eV光子能量范围内1-丙醇和2-丙醇的光电离和离解光电离现象,测量了1-丙醇离解光电离产生的碎片离子CH3CH2CH2OH+、CH3CH2CHOH+、CH2CH2OH+、CH3CH2CH2+、CH3CH=CH2+和CH2OH+及2-丙醇离解光电离产生的碎片离子CH3CH(OH)CH3+、CH3C(OH)CH3+、CH3CHOH+、CH2=CHOH+、CH3CHCH3+和CH3CH=CH2+的光电离效率谱,得到了这些离子的出现势.结合从头算理论计算,给出了1-丙醇的碎片离子CH3CH2CHOH+、CH2CH2OH+、CH3CH2CH2+、CH3CH=CH2+、CH2OH+和2-丙醇的碎片离子CH3C(OH)CH3+、CH3CHOH+、CH2=CHOH+、CH3CHCH+3、CH3CH=CH2+等的解离通道和解离能.理论计算结果与实验结果符合得很好.

  8. 正丙醇和异丙醇对水溶液中牛血清白蛋白的构象及其荧光光谱的影响%Effects of 1-Propanol and 2-Propanol on the Conformation and Fluorescence Spectra of Bovine Serum Albumin in Aqueous Solutions

    Institute of Scientific and Technical Information of China (English)

    马林; 刘东群; 杨华; 童张法

    2008-01-01

      A combination of emission fluorescence spectroscopy (λex=280 nm,295 nm) and synchronous fluorescence spectroscopy (Δλ=15 nm、60 nm) with static light scattering measurement was used to investigate the effects of 1-propanol and 2-propanol on the conformation and fluorescence spectroscopy of Bovine Serum Albumin (BSA) in BSA-1-propanol-water and BSA-2-propanol-water systems. The results showed that 1-propanol and 2-propanol generally decreased, however at dilute solutions slightly increased, the stability of the structure of protein. And it was found that 1-propanol and 2-propanol were week protein denaturants, so that the fluorescence intensity of BSA was controlled by the mixing state of the mixtures at high 1-propanol and 2-propanol concentration.%  通过测定BSA-正丙醇-水和BSA-异丙醇-水体系中BSA的发射荧光(λex=280 nm、295 nm)和同步荧光(△λ=15 nm、60 nm),结合静态光散射技术,探索正丙醇和异丙醇对水溶液中蛋白质的构象和荧光光谱的影响。结果表明,正丙醇和异丙醇使蛋白质发生部分解折叠现象,但是,低浓度的正丙醇和异丙醇水溶液能轻微增强蛋白质的结构稳定性。总体上,正丙醇和异丙醇是弱的蛋白质变性剂,在浓度较高的体系中,体系的混合状态的变化对 BSA 的荧光强度的变化起主导作用。

  9. Chemical-physical properties of spinel CoMn2O4 nano-powders and catalytic activity in the 2-propanol and toluene combustion: Effect of the preparation method.

    Science.gov (United States)

    Hosseini, Seyed Ali; Salari, Dariush; Niaei, Aligholi; Deganello, Francesca; Pantaleo, Giuseppe; Hojati, Pejman

    2011-01-01

    Spinel-type CoMn(2)O(4)nano-powders are prepared using sol-gel auto combustion (SGC) and co-precipitation (CP) methods and their catalytic activities are evaluated in combustion of 2-propanol and toluene. The chemical-physical properties of the oxides are characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), N(2)-adsorption-desorption, temperature programmed reduction (TPR) and scanning electron microscopy (SEM). After calcination at 700°C, CoMn(2)O(4)-SGC shows higher amounts of the normal-type spinel phase and is more crystalline than CoMn(2)O(4)-CP. Higher calcination temperatures (850°C) do not affect very much the weight percentage of the normal-type spinel phase; although the crystal size slightly increased. The TPR analysis evidences a large number of Mn(3+) cations in CoMn(2)O(4)-SGC compared to CoMn(2)O(4)-CP. This difference, together with the higher surface area, could justify the higher activity of CoMn(2)O(4)-SGC in both the investigated reactions.

  10. 双回流动态累积间歇精馏分离正丙醇-异丙醇物系过渡馏分的研究%Slop Cut in Separation of 1-Propanol from 2-Propanol by Dynamic-Accumulation Batch Distillation with Double-Reflux

    Institute of Scientific and Technical Information of China (English)

    陈立峰; 张兵; 李文秀; 于巍; 白鹏

    2011-01-01

    在双回流动态累积间歇精馏实验装置中,以正丙醇-异丙醇为物系进行了间歇精馏实验,考察了操作时间对过渡馏分采出段塔顶馏出液中正丙醇和异丙醇的含量及塔顶温度、塔釜液正丙醇含量及塔釜温度的影响.实验结果表明,原料中异丙醇质量分数别为30%,50%,70%时,对应的过渡馏分采出段操作时间分别为38,46,57 min;原料中异丙醇的含量越低,正丙醇回收率越高.在原料加入量为1L、加热功率为150 W、原料中异丙醇质量分数为30%的条件下,回收得到的正丙醇质量分数可达到86.66%,此时正丙醇的回收率为67.57%,过渡馏分的量最少,操作时间最短.%Batch distillation of 1 -propanol-2-propanol binary system was carried out in a set of dynamic-accumulation batch distillation apparatus with double- reflux. The effects of operation time on mass fractions of 1 -propanol and 2-propanol in the column top distillate, the column top temperature, mass fraction of 1 -propanol in the column bottoms and the column bottom temperature in the slop cut stage were investigated. The experimental results indicated that, when mass fraction of 2-propanol in the feed was 30% , 50% and 70% , the operation time of the corresponding slop cut stage was 38, 46 and 57 min. The 1-propanol yield increased while the mass fraction of 2-propanol in the feed decreased. Under the conditions of feed 1000 mL, heating power 150W and mass fraction of 2-propanol in the feed 30% , mass fraction of 1-propanol in the products was 86.66% and its yield was 67.57% , and the slop cut mass reached the minimum and the operation time of the slop cut stage was the shortest.

  11. Effects of Additives on Catalytic Oxidation of 1-Methoxy-2-Propanol to Methoxyacetone%添加物对1-甲氧基-2-丙醇催化氧化制甲氧基丙酮反应的影响

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

    The system WⅥ-H2O2 has good selectivity for methoxyacetone in oxidation of 1-methoxy-2-propanol. The effects of acid and base additives on selectivit y for methoxyacetone were studied. The results showed that the acid additive, i.e. NaHSO4, was favorable to Na2WO4-H2O2 system, while the base ad ditive NEt3 was favorable to other tungsten compounds. A 71.2% of yield of me thoxyacetone with 98.9% of selectivity for methoxyacetone was obtained in Na2 WO4-H2O2-NaHSO4-MeCOMe oxidation system.

  12. Henry's law constants and infinite dilution activity coefficients of cis-2-butene, dimethylether, chloroethane, and 1,1-difluoroethane in methanol, 1-propanol, 2-propanol, 1-butanol, 2-butanol, isobutanol, tert-butanol, 1-pentanol, 2-pentanol, 3-pentanol, 2-methyl-1-butanol, 3-methyl-1-butanol, and 2-methyl-2-butanol

    International Nuclear Information System (INIS)

    Henry's law constants and infinite dilution activity coefficients of cis-2-butene, dimethylether, chloroethane, and 1,1-difluoroethane in methanol, 1-propanol, 2-propanol, 1-butanol, 2-butanol, isobutanol, tert-butanol, 1-pentanol, 2-pentanol, 3-pentanol, 2-methyl-1-butanol, 3-methyl-1-butanol, and 2-methyl-2-butanol in the temperature range of 250 K to 330 K were measured by a gas stripping method and partial molar excess enthalpies were calculated from the activity coefficients. A rigorous formula for evaluating the Henry's law constants from the gas stripping measurements was used for the data reduction of these highly volatile mixtures. The uncertainty is about 2% for the Henry's law constants and 3% for the estimated infinite dilution activity coefficients. In the evaluation of the infinite dilution activity coefficients, the nonideality of the solute such as the fugacity coefficient and Poynting correction factor cannot be neglected, especially at higher temperatures. The estimated uncertainty of the infinite dilution activity coefficients includes 1% for nonideality

  13. Kraftig eksplosion efter sammenblanding af salpetersyre og 2-propanol

    DEFF Research Database (Denmark)

    Hedlund, Frank Huess

    2015-01-01

    Det er velkendt, at koncentreret salpetersyre reagerer med mange stoffer, ofte voldsomt, med varmeudvikling og frigivelse af giftige brune nitrøse gasser. Kun få er klar over, at det under særlige omstændigheder ved blanding med isopropylalkohol, eller andre alkoholer, kan udvikle raketbrændstof....

  14. Support vector classification for structure-activity-relationship of 1-(1H-1,2,4-triazole-1-yl)-2-(2,4-difluorophenyl)-3-substituted-2-propanols%支持向量分类算法用于1-(1H-1,2,4-三唑-1-基)-2-(2,4-二氟苯基)-3-取代-2-丙醇化合物的构效关系研究

    Institute of Scientific and Technical Information of China (English)

    纪晓波; 陆文聪; 蔡煜东; 陈念贻

    2007-01-01

    The support vector classification (SVC) was employed to make a model for classification of antifungal activities of 1-(1H-1,2,4-triazole-1-yl)-2-(2,4-difluorophenyl)-3-substituted-2-propanols triazole derivatives. The compounds with high antifungal activities and those with low antifungal activities were compared on the basis of the following molecular descriptors: net atomic charge on the atom N connecting with R, dipole moment and heat of formation. By using the SVC, a mathematical model was constructed, which can predict the antifungal activities of the triazole derivatives, with an accuracy of 91% on the basis of the leave-one-out cross-validation (LOOCV) test. The results indicate that the performance of the SVC model can exceed that of the principal component analysis (PCA) and K-Nearest Neighbor (KNN) models for this real world data set.

  15. Catalytic Hydrotreatment of Humins in Mixtures of Formic Acid/2-Propanol with Supported Ruthenium Catalysts.

    Science.gov (United States)

    Wang, Yuehu; Agarwal, Shilpa; Kloekhorst, Arjan; Heeres, Hero Jan

    2016-05-10

    The catalytic hydrotreatment of humins, which are the solid byproducts from the conversion of C6 sugars (glucose, fructose) into 5-hydroxymethylfurfural (HMF) and levulinic acid (LA), by using supported ruthenium catalysts has been investigated. Reactions were carried out in a batch setup at elevated temperatures (400 °C) by using a hydrogen donor (formic acid (FA) in isopropanol (IPA) or hydrogen gas), with humins obtained from d-glucose. Humin conversions of up to 69 % were achieved with Ru/C and FA, whereas the performance for Ru on alumina was slightly poorer (59 % humin conversion). Humin oils were characterized by using a range of analytical techniques (GC, GC-MS, GCxGC, gel permeation chromatography) and were shown to consist of monomers, mainly alkyl phenolics (>45 % based on compounds detectable by GC) and higher oligomers. A reaction network for the reaction is proposed based on structural proposals for humins and the main reaction products. PMID:26836970

  16. Cholesteryl ester transfer protein inhibitors in coronary heart disease: Validated comparative QSAR modeling of N, N-disubstituted trifluoro-3-amino-2-propanols.

    Science.gov (United States)

    Mondal, Chanchal; Halder, Amit Kumar; Adhikari, Nilanjan; Jha, Tarun

    2013-10-01

    Cholesteryl ester transfer protein (CETP) converts high density lipoprotein cholesterol to low density lipoproteins. It is a promising target for treatment of coronary heart disease. Two dimensional quantitative structure activity relationship (2D-QSAR), hologram QSAR (HQSAR) studies and comparative molecular field analysis (CoMFA) as well as comparative molecular similarity analysis (CoMSIA) were performed on 104 CETP inhibitors. The statistical qualities of generated models were justified by internal and external validation, i.e., q(2) and R(2)pred respectively. The best 2D-QSAR model was obtained with q(2) and R(2)pred values of 0.794 and 0.796 respectively. The 2D-QSAR study suggests that unsaturation, branching and van der Waals volumes may play important roles. The HQSAR model showed q(2) and R(2)pred values of 0.628 and 0.550 respectively. Similarly, CoMFA model showed q(2) and R(2)pred values of 0.707 and 0.755 respectively whereas CoMSIA model was obtained with q(2) and R(2)pred values of 0.696 and 0.703 respectively. CoMFA and CoMSIA studies indicate that steric factors are important at substituted phenoxy and tetrafluoroethoxy groups whereas electropositive factors play important role at difluoromethyl group. The results of 3D-QSAR studies validate those of 2D-QSAR and HQSAR studies as well as the earlier observed SAR data. Current work may help to develop better CETP inhibitors.

  17. 75 FR 43076 - 2-Propanol, 1,1′,1′′-nitrilotris-; Exemption from the Requirement of a Tolerance

    Science.gov (United States)

    2010-07-23

    ...-5805. II. Petition for Exemption In the Federal Register of April 8, 2009 (74 FR 15971) (FRL-8407- 4...-occupational, non-dietary exposure (e.g., textiles (clothing and diapers), carpets, swimming pools, and hard... exposures are safe by comparing aggregate exposure estimates to the acute PAD (aPAD) and chronic PAD...

  18. Hydrogen transfer reaction of cyclohexanone with 2-propanol catalysed by CeO2-ZnO materials: Promoting effect of ceria

    Indian Academy of Sciences (India)

    Braja Gopal Mishra; G Ranga Rao; B Poongodi

    2003-10-01

    Ce-Zn-O mixed oxides were prepared by amorphous citrate process and decomposition of the corresponding acetate precursors. The resulting materials were characterised by TGA, XRD, UV-Vis-DRS, EPR, SEM and surface area measurements. XRD and DRS results indicated fine dispersion of the ceria component in the ZnO matrix. EPR results clearly indicate the presence of oxygen vacancy and defect centres in the composite oxide. Addition of CeO2 to ZnO produced mixed oxides of high surface area compared to the pure ZnO. Hydrogen transfer reaction was carried out on these catalytic materials to investigate the effect of rare earth oxide on the activity of ZnO. Addition of ceria into zinc oxide was found to increase the catalytic activity for hydrogen transfer reaction. The catalytic activity also depended on the method of preparation. Citrate process results in uniformly dispersed mixed oxide with higher catalytic activity.

  19. Preparation of(S)-1-Phenylsulfonyl-2-Propanol through Asymmetric Reduction by Baker's Yeast%面包酵母不对称还原制备(S)-1-苯砜基-2-丙醇

    Institute of Scientific and Technical Information of China (English)

    石月丹; 周子彦; 谢玉忠

    2006-01-01

    用自制的溴代丙酮与苯亚磺酸钠反应合成1-苯砜基-2-丙酮,然后利用面包酵母在有机溶剂中不对称催化还原1-苯砜基-2-丙酮,制备了光学活性的手性化合物(S)-1-苯砜基-2-丙醇,此反应具有操作简便、光学产率高等优点,其化学产率可达94%以上,对映体过量值为100%.

  20. Synthesis and antifungal activity of 1- ( 1 H-1, 2,4-triazol-1-yl) -2- (2,4-difluorophenyl)-3-(4-substituted acyl piperazin-1-yl)-2-propanols

    Institute of Scientific and Technical Information of China (English)

    LIANG Shuang; LIU Chao-mei; ZHU Jie; HE Qiu-qin; JIANG Yuan-ying; CAO Yong-bin

    2004-01-01

    Objective: To study the effect of fluconzole derivatives from a side chain containing 4-substituted acyl piperazin-1-yl on antifungal activity. Methods: Fourteen title compounds were synthesized and confirmed by the elementary analysis, 1HNMR and IR spectra. Five deep fungal strains and 3 shallow fungal strains were chosen as the experimental strains. Minimum inhibitory concentrations(MICs) of all title compounds were determined by the method recommended by the National Committee for Clinical Laboratory Standards (NCCLS) using RPMI 1640 test medium. Results: Among the 14title compounds, 12 were first reported. The results of preliminary antifungal test showed that all the title compounds exhibited potent antifungal activities to a certain extent. The activity of 4 compounds were more than 4 times as high as that of fluconazole and equal to that of ketoconazole against Candida albicans in vitro(MIC80 value≤0. 125 μg/ml). Conclusion:Introduction of a side chain containing 4-substituted acyl piperazin-l-yl into the main part of fluconazole has important influence on antifungal activities of title compounds.

  1. Synthesis of Isochroman Derivatives from 1-Alkoxy (phenoxy)-3-(3,4- methylenedioxy) phenyl-2-propanol by Oxa-Pictet-Spengler Reaction%通过氧杂Pictet-Spengler反应从1-烷(苯)氧基-3-(3,4-亚甲基二氧)苯基-2-丙醇合成异色满衍生物

    Institute of Scientific and Technical Information of China (English)

    赵宝祥; 沙磊; 谭伟; 左华; 王大威

    2004-01-01

    通过氧杂Pictet-Spengler反应从1-烷氧基-3-(3,4-亚甲基二氧)苯基-2-丙醇及1-苯氧基-3-(3,4-亚甲基二氧)苯基-2-丙醇合成一系列异色满衍生物,即3-烷(苯)氧基-1-苯基-6,7-亚甲基二氧异色满和3-烷(苯)氧基-1,1-二甲基-6,7-亚甲基二氧异色满,收率为50%~90%.

  2. Kinetics of the asymmetrie synthesis of 1-phenylsulfonyl-2-propanol by baker's yeast in microaqueous organic solvent%微水有机溶剂中面包酵母催化不对称还原(S)-1-苯砜-2-丙酮的动力学研究

    Institute of Scientific and Technical Information of China (English)

    谢玉忠; 李向霞; 周子彦

    2005-01-01

    探讨在微水有机溶剂中面包酵母催化不对称还原(S)-1-苯砜-2-丙酮的动力学,分别求出30 ℃和35 ℃下的反应速率常数和米氏常数.实验结果表明面包酵母在35℃时的催化活性比30 ℃时要高.

  3. Excess Molar Volumes and Viscosities for Binary Mixtures of 1-Alkoxypropan-2-ols with 1-Butanol,and 2-Butanol at 298.15 K and Atmospheric Pressure

    Institute of Scientific and Technical Information of China (English)

    PAL Amalendu; GABA Rekha

    2007-01-01

    Excess molar volumes VEm and kinematic viscosities v have been measured as a function of composition for binary mixtures of propylene glycol monomethyl ether (1-methoxy-2-propanol),MeOCH2CH(OH)Me,propylene glycol monoethyl ether (1-ethoxy-2-propanol), EtOCH2CH(OH)Me,propylene glycol monopropyl ether (1-propoxy-2-propanol), PrOCH2CH(OH)Me, propylene glycol monobutyl ether (1-butoxy-2-propanol),BuOCH2CH(OH)Me,and propylene glycol tert-butyl ether (1-tert-butoxy-2-propanol),t-BuOCH2CH(OH)Me with 1-butanol,and 2-butanol,at 298.15 K and atmospheric pressure.The excess molar volumes are negative across the entire range of composition for all the systems with 1-butanol,and positive for the systems 2-butanol+1-methoxy-2-propanol,and +1-propoxy-2-propanol,negative for the systems 2-butanol+1-butoxy-2-propanol,and change sign for the systems 2-butanol+1-ethoxy-2-propanol,and +1-tert-butoxy-2-propanol.From the experimental data,the deviation in dynamic viscosity η from Σxiηi has been calculated.Both excess molar volumes and viscosity deviations have been correlated using a Redlich-Kister type polynomial equation by the method of least-squares for the estimation of the binary coefficients and the standard errors.

  4. Determination of p-Acetaminobenzoic Acid and N,N-Dimethylamino-2-propanol in Human Urine by LC-MS and Study on Their Urinary Excretion Profiles%人尿中对乙酰氨基苯甲酸和N,N-甲氨基-2-丙醇的液质联用法测定及尿药排泄特征研究

    Institute of Scientific and Technical Information of China (English)

    于勇; 孙鲁宁; 杜晓琅; 饶雅琨; 丁雯; 丁黎; 肖慧凤; 陈益智

    2011-01-01

    目的:建立分别测定人尿中对乙酰氨基苯甲酸和N,N-二甲氨基-2-丙醇的液质联用法,考察二者在中国健康受试者尿液中的排泄特征.方法:以LC-MS法测定尿样中对乙酰氨基苯甲酸,色谱采用Amethyst C18柱(150 mm×2.1 mm,5 μm),流动相为甲醇-0.1%甲酸水溶液(25:75),流速为0.4 mL·min-1;质谱采用气动辅助电喷雾离子化和正离子选择性离子检测.以LC-MS/MS法测定尿样中N,N-二甲氨基-2-丙醇,色谱采用Hedera CN柱(150 mm×2.1 mm,5 μm),流动相为乙腈-5 mmol·L-1醋酸铵水溶液(含0.03%甲酸)(55:45),流速为0.35 mL·min-1;质谱采用气动辅助电喷雾离子化和正离子多反应检测.10名受试者单次口服异丙肌苷片(1.0 g),测定对乙酰氨基苯甲酸和N,N-二甲氨基-2-丙醇的尿药排泄参数.结果:对乙酰氨基苯甲酸的尿药浓度在0.202 0-202.0 mg·L-1范围内线性关系良好,平均回收率大于97.7%;N,N-二甲氨基-2-丙醇尿药浓度在0.797 8-398.9 mg·L-1范围内线性关系良好,平均回收率大于99.1%.受试者服药后,对乙酰氨基苯甲酸和N,N-二甲氨基-2-丙醇分别在6和12 h后基本随尿排泄完全,36 h内其平均尿药累积排泄百分率分别为(30.7±5.7)%和(49.0±8.6)%.结论:本法适用于人尿中对乙酰氨基苯甲酸和N,N-二甲氨基-2-丙醇的测定及其尿药排泄特征研究.

  5. The methods of synthesis of glycerin derivatives

    International Nuclear Information System (INIS)

    In this chapter of book authors present some methods of synthesis of glycerin derivatives, in particular, synthesis of 3-met oxi-1.2-propandiol, 1.3-di-benzil-oxi-2-propanol, 1-ge xi-lox-3-chlorine-2-propanol and other

  6. Dissociation Constants and Thermodynamic Properties of Amines and Alkanolamines from (293 to 353) K

    NARCIS (Netherlands)

    Hamborg, Espen S.; Versteeg, Geert F.

    2009-01-01

    The dissociation constants of protonated 2-amino-2-ethyl-1,3-propanediol, 2-amino-2-methyl-1-propanol, diethylmonoethanolamine, diisopropanolamine, dimethylmonoethanolamine, monoethanolamine, 1-amino-2-propanol, methylmonoethanolamine, triethanolamine, and the first and the second dissociation const

  7. Research of component adsorption from the binary mixture of organic solvents

    OpenAIRE

    Карван, Світлана Анатоліївна; Сарібєков, Георгій Савич

    2010-01-01

    Results of superficial tension determinaition of solutions of mixed solvents on the basis of perchloroethylene and 2-propanol are resulted, characteristics of absorption monolayer of their molecules are calculated. Regularities of solvents adsorption by textile materials are investigated.

  8. Reconstitution baking tests with defatted wheat flour are suitable for determining the functional effects of lipase-treated wheat lipids.

    Science.gov (United States)

    Schaffarczyk, Monika; Østdal, Henrik; Matheis, Olivia; Jekle, Mario; Koehler, Peter

    2016-06-01

    A microscale reconstitution baking test, using wheat flour defatted with 2-propanol at 20 °C, was established to determine the functional effects of lipids isolated from lipase-treated wheat dough. Proper selection of solvent and extraction temperature was of major importance to maintain the functionality of defatted flour. Dough and gluten from flour defatted with water-saturated 1-butanol (WSB; extracted at 20 °C) and 2-propanol (extracted at 75 °C) had inferior extensibility and loaf volume compared to control flour extracted with 2-propanol at 20 °C. Quantitation of gluten proteins showed that defatting with WSB (20 °C) or 2-propanol (75 °C) decreased the gliadin and increased the glutenin content. Possible reasons were thiol-disulfide interchange reactions, caused either by heat (2-propanol, 75 °C) or by the solvent WSB, which affected gluten proteins. Confocal laser scanning microscopy showed that regular, interconnected gluten structures were only present in dough from flour defatted with 2-propanol at 20 °C. PMID:26830576

  9. Catalytic activity of poly[(methacrylato)aluminum(III)] obtained at different gamma-radiation doses

    Energy Technology Data Exchange (ETDEWEB)

    Vilchis-Nestor, A.R. [Facultad de Quimica, Universidad Autonoma del Estado de Mexico, Paseo Tollocan and Paseo Colon, A.P. A-20, Toluca, C.P. 50120 (Mexico); Urena-Nunez, F., E-mail: fernando.urena@inin.gob.mx [Instituto Nacional de Investigaciones Nucleares, km 36.5, Carretera Mexico-Toluca, Ocoyoacac, Estado de Mexico, C.P. 52750 (Mexico); Sanchez-Mendieta, V. [Facultad de Quimica, Universidad Autonoma del Estado de Mexico, Paseo Tollocan and Paseo Colon, A.P. A-20, Toluca, C.P. 50120 (Mexico); Perez-Hernandez, R. [Instituto Nacional de Investigaciones Nucleares, km 36.5, Carretera Mexico-Toluca, Ocoyoacac, Estado de Mexico, C.P. 52750 (Mexico)

    2011-11-15

    A novel coordination polymer was obtained throughout the polymerization of aluminum(III) methacrylate at different doses (10, 20, 30, 40, 50 and 80 kGy) using gamma-radiation as initiator. The materials were characterized by electronic paramagnetic resonance (EPR), thermogravimetric analyses (TGA) and scanning electron microscopy/electron dispersive X-ray analyses (SEM/EDAX) techniques; particle size distribution and surface areas were also determined. The samples of poly[(methacrylato)aluminum(III)] obtained at different {gamma}-doses were found to catalyze 2-propanol dehydrogenation and dehydration to acetone and propene. A noticeable activity was observed with Poly[(methacrylato)aluminum(III)] obtained at 50 kGy, which has higher conversion of 2-propanol and the highest selectivity to acetone ({approx}90%). Results suggest that the decomposition of 2-propanol is correlated with the effect of gamma-radiation on the structure and surface area of the catalysts. - Highlights: > We report the synthesis of micro-crystalline novel poly[(methacrylato)aluminum(III)]. > Polymer was obtained throughout the polymerization of Al(III) methacrylate at different doses. > PMALs were found to catalyze 2-propanol dehydrogenation and dehydration to acetone and propene. > PMAL obtained at 50 kGy has the higher conversion of 2-propanol and selectivity to acetone ({approx}90%).

  10. Polymer Production by Plasma Polymerization of Oxygenated Organic Compounds

    Directory of Open Access Journals (Sweden)

    Antonio P. Nascimento Filho

    2002-10-01

    Full Text Available This work was aimed at producing new polymeric materials using oxygenated organic compounds as main reactants and plasma enhanced chemical vapor deposition (PECVD as a production technique. The films obtained were analyzed by profilometry, in order to determine the deposition rate, by Infrared Spectroscopy (FTIR to identify the species deposited and by contact angle measurements to determine the polarity of the surface. For the reactants used, namely ethanol, acetone and 2-propanol, the plasma deposition process was least efficient with ethanol followed by acetone and 2-propanol. With the latter, reproducible thin films were obtained with a high deposition rate (up to 400 Å/min. These films had a high amount of OH and could be wetted by common organic solvents, such as 2-propanol or acetone. The contact angle formed by drops of 2-propanol or acetone aqueous solution on the film produced from 2-propanol varied significantly with the concentration, from 0.9% to 50% by vol., indicating that the film is sensitive to polar solutions.

  11. Preconcentration in gas or liquid phases using adsorbent thin films

    Directory of Open Access Journals (Sweden)

    Antonio Pereira Nascimento Filho

    2006-03-01

    Full Text Available The possibility of preconcentration on microchannels for organic compounds in gas or liquid phases was evaluated. Microstructures with different geometries were mechanically machined using poly(methyl methacrylate - PMMA as substrates and some cavities were covered with cellulose. The surfaces of the microchannels were modified by plasma deposition of hydrophilic or hydrophobic films using 2-propanol and hexamethyldisilazane (HMDS, respectively. Double layers of HMDS + 2-propanol were also used. Adsorption characterization was made by Quartz Crystal Measurements (QCM technique using reactants in a large polarity range that showed the adsorption ability of the structures depends more on the films used than on the capillary phenomena. Cellulose modified by double layer film showed a high retention capacity for all gaseous compounds tested. However, structures without plasma deposition showed low retention capacity. Microchannels modified with double layers or 2-propanol plasma films showed higher retention than non-modified ones on gas or liquid phase.

  12. Investigation of the solubility and the potentials for purification of serum amyloid A (SAA) from equine acute phase serum

    DEFF Research Database (Denmark)

    Christensen, Michelle Brønniche; Sørensen, Jens Christian; Jacobsen, Stine;

    2013-01-01

    for purification of equine SAA based on biochemical properties.Freeze dried equine acute phase serum was dissolved in 70% 2-propanol, 8 M urea, and milli-Q water, respectively. Supercritical fluid extraction (SFE), size-exclusive chromatography (FPLC-SEC), and preparative isoelectric focusing (IEF) were performed...... in the attempt to purify. Immunostaining of IEF blots were used for isoform-specific detection of SAA in the preparations and purity was assessed by silverstained SDS-PAGE. FINDINGS: SAA was soluble in 70% 2-propanol, 8 M urea and Milli-Q water. SAA was not separated in the lipophilic or ampipathic fractions...

  13. KBPh4由水到系列水 -醇混合溶剂的迁移自由能%Systematic Study of the Standard Transfer Gibbs Energy of Potassium Tetrophenylborate from Water to Water and Alcohol Mixtures

    Institute of Scientific and Technical Information of China (English)

    曹立新; 周保学; 史鹏飞; 邹立壮

    2001-01-01

    The standard transfer Gibbs energies (Δ trG° )of KBPh4 from reference solvent of water to water/ethanol, water/propanol, water/2-propanol,water/ethylene glycol, water/glycerol mixtures in different proportional ratio have been studied. The interactions of KBPh4 with the above mixed solvents were analyzed. The standard transfer Gibbs energy of cavity(Δ trG° cav) and the standard transfer Gibbs energy of interaction(Δ trG° int) from water to water/2-propanol mixtures at 298.15 K were calculated by the Scaled Particle Theory (SPT).

  14. REMEDIATING PESTICIDE CONTAMINATED SOILS USING SOLVENT EXTRACTION

    Science.gov (United States)

    Bench-scale solvent extraction studies were performed on soil samples obtained from a Superfund site contaminated with high levels of p,p'-DDT, p,p'-DDD,, p,p'-DDE and toxaphene. The effectiveness of the solvent extraction process was assessed using methanol and 2-propanol as sol...

  15. An Inexpensive, Relatively Green, and Rapid Method to Purify Genomic DNA from "Escherichia Coli": An Experiment for the Undergraduate Biochemistry Laboratory

    Science.gov (United States)

    Sims, Paul A.; Branscum, Katie M.; Kao, Lydia; Keaveny, Virginia R.

    2010-01-01

    A method to purify genomic DNA from "Escherichia coli" is presented. The method is an amalgam of published methods but has been modified and optimized for use in the undergraduate biochemistry laboratory. Specifically, the method uses Tide Free 2x Ultra laundry detergent, which contains unspecified proteases and lipases, "n"-butanol, 2-propanol,…

  16. Design,Synthesis and Antifungal Activity of Novel Triazole Derivatives

    Institute of Scientific and Technical Information of China (English)

    Chun Quan SHENG; Wan Nian ZHANG; Hai Tao JI; Yun Long SONG; Min ZHANG; You Jun ZHOU; Jia Guo LU; Jü ZHU

    2004-01-01

    Twenty-one 1-(1H-1,2,4-triazolyl)-2-(2,4-diflurophenyl)-3-(4-substituted-1- piperazinyl)-2-propanol derivatives were designed and synthesized,on the basis of the active site of lanosterol 14(-demethylase.In vitro antifungal activities showed that some of the target compounds had higher antifungal activity and broader antifungal spectrum than fluconazole.

  17. AROMATIC AMINES IN AND NEAR THE BUFFALO RIVER

    Science.gov (United States)

    Three sediment samples taken from the Buffalo River and two soil samples taken near its bank have been analyzed for 2-propanol-extractable, basic organic compounds by using GC/MS. Eleven aromatic amines related to the commercial production of malachite green and crystal violet we...

  18. Bepaling van theofylline (1,3-dimethylxanthine) in hondeplasma met behulp van reversed-phase vloeistofchromatografie

    NARCIS (Netherlands)

    Olling; M; Besamusca; P.; Rauws; A.G.

    1985-01-01

    In dit rapport wordt een snelle en nauwkeurige methode beschreven voor de bepaling van theofylline in plasma. Theofylline wordt uit plasma geextraheerd met chloroform/2-propanol en met behulp van reversed-phase hogedruk vloeistofchromatografie gescheiden en met spectrofotometrische detectie bepa

  19. The Optical Resolution of Chiral Tetrahedrone-type Clusters Contai- ning SCoFeM (M=Mo or W) Using High Performance Liquid Chromatography Chiral Stationary Phase

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    Amylose tris (phenylcarbamate) chiral stationary phase (ATPC-CSP) was prepared and used for optical resolution of clusters 1 and 2. n-Hexane/2-propanol ( 99/1; v/v) were found to be the most suitable mobile phase on ATPC-CSP.

  20. DIFFUSION MEASUREMENTS DURING PERVAPORATION THROUGH A ZEOLITE MEMBRANE

    Science.gov (United States)

    An isotopic-transient technique was used to directly measure diffusion times of H2O, methanol, ethanol, 2-propanol, and acetone in pure and binary mixture feeds transporting through a zeolite membrane under steady-state pervaporation conditions. Diffusivities can be determ...

  1. Solid–liquid equilibria for binary and ternary systems with the Cubic-Plus-Association (CPA) equation of state

    DEFF Research Database (Denmark)

    Fettouhi, André; Thomsen, Kaj

    2010-01-01

    A systematic investigation of the CPA model's performance within solid-liquid equilibria (SLE) in binary mixtures (methane + ethane, methane + heptane, methane + benzene, methane + CO2, ethane + heptane, ethane + CO2, 1-propanol + 1,4-dioxane, ethanol + water, 2-propanol + water) is presented...

  2. Microwave Assisted Synthesis of N-Arylheterocyclic Substituted-4-aminoquinazoline Derivatives

    Directory of Open Access Journals (Sweden)

    Ping Lu

    2006-04-01

    Full Text Available A simple, efficient, and general method has been developed for the synthesis of various N-aryl heterocylic substituted-4-aminoquinazoline compounds from 4-chloro- quinazoline and aryl heterocyclic amines under microwave irradiation using 2-propanol as solvent. The advantages of the use of microwave irradiation in relation to the classical method were demonstrated.

  3. The plasma membrane proteome of germinating barley embryos

    DEFF Research Database (Denmark)

    Hynek, Radovan; Svensson, Birte; Jensen, O.N.;

    2009-01-01

    with amphiphilicity and low abundance of membrane proteins. A fraction enriched in plasma membranes was prepared from embryos dissected from 18 h germinated barley seeds using aqueous two-phase partitioning. Reversed-phase chromatography on C-4 resin performed in micro-spin columns with stepwise elution by 2-propanol...

  4. Reduction of 2-chloro-N-phenylpropanamide and 2-methyl-N-phenylaziridine with lithium aluminium hydride

    DEFF Research Database (Denmark)

    Vilhelmsen, Mie Højer; Østergaard, Lars Frøsig; Nielsen, Mogens Brøndsted;

    2008-01-01

    -chloropropanamide, which indicates that Lewis acid catalysis (by aluminium chlorohydrides) facilitates the reduction of the aziridine. In addition, Lewis acid catalysis increases the relative yield of the propylamine product. The reduction of 2-chloro-N-phenylpropanamide furnishes 2-phenylamino-1-propanol as a by......-product, rather than the previously proposed 1-phenylamino-2-propanol....

  5. Stereo block copolymers of L- and D-lactides

    NARCIS (Netherlands)

    Yui, Nobuhiko; Dijkstra, Pieter J.; Feijen, Jan

    1990-01-01

    Sequential diblock copolymers composed of L- and D-lactic acid residues were synthesized through a living ring-opening polymerization of L- and D-lactide initiated by aluminium tris(2-propanolate). The composition of the block copolymers was varied by changing the reaction conditions and monomer ove

  6. Preparation of PtRu/C anode electrocatalysts using gamma radiation for methanol electro-oxidation; Preparacao de eletrocatalisadores PtRu/C utilizando radiacao gama para aplicacao como anodo na oxidacao direta de metanol

    Energy Technology Data Exchange (ETDEWEB)

    Silva, Dionisio Fortunato da

    2006-07-01

    Pt Ru/C (carbon-supported Pt Ru nanoparticles) anode electrocatalysts were prepared using radiolytic process (gamma radiation) and tested for methanol electro-oxidation. In this process, water/2-propanol and water/ethylene glycol solutions containing the metallic ions and the carbon support were submitted to gamma radiation under stirring. The water/alcohol ratio (v/v) and the total dose (kGy) were studied. A nominal Pt Ru atomic ratio of 50:50 were used in all experiments. The electrocatalysts were characterized by energy dispersive X-ray analysis (EDX), X-ray diffraction (XRD), transmission electron microscopy (TEM) and cyclic voltammetry (CV). The electro-oxidation of methanol was studied by cyclic voltammetry using the thin porous coating technique. The electrocatalysts prepared in water/2-propanol showed crystallite size in the range of 3-5 nm and Pt Ru atomic ratio of 50:50. The electrocatalysts prepared in water/ethylene glycol showed crystallite size (2-3 nm) smaller than the ones obtained in water/2-propanol, however, the Pt Ru atomic ratios obtained were approximately 80:20, showing that only part of ruthenium ions were reduced. For methanol oxidation the electrocatalytic activity depends on the water/2-propanol and water/ethylene glycol ratio used in the reaction medium. The electrocatalysts prepared in water/2-propanol showed inferior performance to the ones prepared in water/ethylene glycol, which showed similar or superior performances (amperes per gram of platinum) to the commercial electrocatalyst from E-TEK. (author)

  7. Hydrogen generation from renewable resources

    Energy Technology Data Exchange (ETDEWEB)

    Loges, Bjoern

    2009-09-04

    In this thesis, the hydrogen generation by dehydrogenation of 2-propanol and formic acid as model substances for renewable resources have been studied, which is of importance for hydrogen storage. For the base-assisted dehydrogenation of 2-propanol, a ruthenium diamine catalyst system has been investigated. For the selective decomposition of formic acid to hydrogen and carbon dioxide, a system has been established containing ruthenium catalysts and formic acid amine adducts as substrates. The best catalyst activity and productivity have been achieved with in situ generated ruthenium phosphine catalysts, e.g. [RuCl{sub 2}(benzene)]{sub 2} / dppe (TOF = 900 h{sup -1}, TON = 260,000). The gas evolved has been directly used in fuel cells. Furthermore, the influence of irradiation with visible light has been described for the ruthenium phosphine catalysts. (orig.)

  8. Visible-Light-Driven Selective Photocatalytic Hydrogenation of Cinnamaldehyde over Au/SiC Catalysts.

    Science.gov (United States)

    Hao, Cai-Hong; Guo, Xiao-Ning; Pan, Yung-Tin; Chen, Shuai; Jiao, Zhi-Feng; Yang, Hong; Guo, Xiang-Yun

    2016-08-01

    Highly selective hydrogenation of cinnamaldehyde to cinnamyl alcohol with 2-propanol was achieved using SiC-supported Au nanoparticles as photocatalyst. The hydrogenation reached a turnover frequency as high as 487 h(-1) with 100% selectivity for the production of alcohol under visible light irradiation at 20 °C. This high performance is attributed to a synergistic effect of localized surface plasmon resonance of Au NPs and charge transfer across the SiC/Au interface. The charged metal surface facilitates the oxidation of 2-propanol to form acetone, while the electron and steric effects at the interface favor the preferred end-adsorption of α,β-unsaturated aldehydes for their selective conversion to unsaturated alcohols. We show that this Au/SiC photocatalyst is capable of hydrogenating a large variety of α,β-unsaturated aldehydes to their corresponding unsaturated alcohols with high conversion and selectivity. PMID:27403658

  9. Chemical isomeric effects on propanol glassy structures

    CERN Document Server

    Cuello, G J; Bermejo, F J; Cabrillo, C

    2002-01-01

    We have studied the structure of both propanol isomers in their glassy and crystalline states by neutron diffraction. The glass-transition temperatures of 1- and 2-propanol are about 98 and 115 K, respectively and, surprisingly, even larger differences are observed for the melting temperatures of the stable crystals, which are 148 and 185 K, respectively. Their supercooled liquid phases show rather different relaxation spectra, 1-propanol manifesting strong deviations from Debye behavior, whereas 2-propanol shows a far weaker effect. We discuss the spectra obtained for the static structure factor and the static pair correlation function D(r). There is a noticeable difference in the position of the first sharp diffraction peak, which clearly indicates a density change, well correlated with the period of the intermolecular oscillations shown by D(r). (orig.)

  10. Direct effect of tetrahedral alcohol species on the SPB of gold colloids: a deconvolution study

    International Nuclear Information System (INIS)

    Aqueous gold colloids with a mean diameter of 15.4 ± 1.5 nm have been transferred into a range of water–alcohol mixtures. The influence of these mixtures (methanol, ethanol, 2-propanol, and tert-butanol), which present different hydrophobic properties, on the surface plasmon band of gold nanoparticles has been studied. Shifts of gold nanoparticles’ surface plasmon band (SPB) depend on the number of methyl groups and hydrophobic character of the alcohol molecule. Results from deconvolution analysis are explained considering variations on the grade of alcohol adsorption on the nanoparticle surface. TEM images indicate aggregation of the nanoclusters in mixtures of 2-propanol and tert-butanol. ζ potential measurements support the exchange of citrate ions by alcohol molecules, which in turn reflects the existence of an additional electrostatic component

  11. 双回流动态累积间歇精馏全过程的研究%Study on dynamic-accumulation batch distillation of a noveloperation tower with double-reflux

    Institute of Scientific and Technical Information of China (English)

    张兵; 陈立峰; 李文秀

    2011-01-01

    在动态累积间歇精馏塔中,采用双回流动态累积间歇精馏操作对正丙醇-异丙醇二元混合物系进行分离研究.主要考察了操作时间对塔顶整个过程产品浓度、温度变化的影响,并与塔顶回流动态累积间歇精馏操作的分离结果进行了比较,以及过渡馏分阶段操作时间对塔釜正丙醇浓度及温度变化的影响,同时,又对正丙醇的回收进行了研究.结果表明,在同样的产品采出要求条件下,双回流动态累积间歇精馏操作时,随原料中异丙醇含量的增加,所需的操作时间越长,产品的纯度越高,收率越高;操作时间节省166 min,原料中异丙醇质量分数为30%的条件下,所得回收正丙醇的纯度达到91.22%,正丙醇的回收率可达62.93%,原料中异丙醇质量分数别为30%、50%、70%时对应过渡馏分持续时间分别为40、47、58m in;原料中异丙醇质量分数越大,所得回收正丙醇产品的量越少,正丙醇的纯度越低,回收率越小.%A novel double-reflux operation mode by reflux at both top and bottom was applied in a dynamic-accumulation batch distillation tower. Binary mixture of 1-propanol and 2-propanol as the separated system,in the state progress the mass fraction change of 2-propanol and temperature with operation time at top was studied, while the effection was compared with the operation by reflux at top;during slop cut stage the mass fraction change of 1-propanol and temperature at bottom with operation time were mainly discussed. The recovery of 1-propanol was mainly considered. The experiment results indicate that the operation time, mass fraction of 2-propanol in product and yield of 2-propanol all increase with the mass fraction of 2-propanol added more in feed at the same condition of product quality. When mass fraction of 2-propanol in feed was 30% ,the mass fraction of 1-propanol in product was 91. 22% and yield of 1-propanol was 62. 93% . When mass fraction of 2-propanol

  12. Refractive indices of ternary liquid mixtures containing aliphatic alcohols at several temperatures

    Directory of Open Access Journals (Sweden)

    Sovilj Milan N.

    2005-01-01

    Full Text Available The refractive indices of ternary liquid mixtures (2-propanol+2-butanol+ethanol and (chloroform+2-propanol+2-butanol were measured at 20, 25, 30, and 35°C, and atmospheric pressure. The results were used to calculate the refractive index deviations over the entire mole fraction range for the mixtures. The refractive index deviations for the ternary mixtures were further fitted to empirical correlations (Cibulka Nagata-Tamura, and Lopez et al to estimate the ternary fitting parameters. Standard deviations and average percentage deviations from the regression lines are shown. The best fit was obtained by the Nagata-Tamura empirical correlation. Some of the existing predictive equations for the refractive index deviations (Tsao-Smith, Köhler, and Colinet were tested.

  13. Synthesis of high refractive spiro heterocyclic derivatives through thioacetalization of multi-carbonyl compounds

    Energy Technology Data Exchange (ETDEWEB)

    Ye, Jim Young; Maheswara, Muchchintala; Do, Jung Yun [Pusan National Univ., Busan (Korea, Republic of)

    2012-04-15

    Preparation of several new spirocyclic mercaptol derivatives is described. Thiol protection on multi-carbonyl compounds allows of high sulfur content necessary to induce high refractive index. Condensation of 1,3-dimercapto-2-propanol and cyclohexanone followed by successive oxidation and thioacetalization affords a dispiro cycle with four sulfurs. Selective S,S-protection of cyclohexane-1,4-dione is achieved with 1,3-dimercapto-2-propanol and 2,3-dimercapto-1-propanol to provide dispiro cycles with four sulfurs. Olefineoxidation of norbornene gives a useful dialdehyde intermediate which is transformed to 1,3-dithiolane for a linearly-bound-cyclic molecule. Refractive index of linearly-bound-cycles was below 1.60 and dispiro cycles exhibited high refractive index of 1.57-1.69.

  14. A 2D [Fe-II-bistetrazole] coordination polymer exhibiting spin-crossover properties

    NARCIS (Netherlands)

    Quesada, Manuel; Prins, Ferry; Roubeau, Olivier; Gamez, Patrick; Teat, Simon J.; van Koningsbruggen, Petra J.; Haasnoot, Jaap G.; Reedijk, Jan

    2007-01-01

    The reaction of 1,3-bis(tetrazol-1-yl)-2-propanol (btzpol) with Fe(BF4)(2) center dot 6H(2)O in acetonitrile yields the remarkable 2D coordination polymer [Fe-II(btzpol)(1.8)(btzpol-OBF3)(1.2)](BF4)(0.8) center dot (H2O)(0.8)(CH3CN) (1). This compound has been structurally characterized using an X-r

  15. Influencia del solvente en el espectro ultravioleta del 4-nitrobifenilo

    Directory of Open Access Journals (Sweden)

    Jaime de la Zerda L.

    2009-05-01

    Full Text Available Se estudiaron los efectos de solvente en la banda del 4-nitrobifenilo en los alcoholes metanol, etanol, I propanol, 2 propanol, 1-butanol, 2-metilpropanol, que fueron purificados cuidadosamente, determinándose luego el grado de pureza que resultó satisfactorio en casi todos los casos. Por ser el agua la impureza persistente en todos ellos, fue necesario estudiar su efecto con cierto detalle.

  16. Sonochemiluminescence of lucigenin: Evidence of superoxide radical anion formation by ultrasonic irradiation

    Science.gov (United States)

    Matsuoka, Masanori; Takahashi, Fumiki; Asakura, Yoshiyuki; Jin, Jiye

    2016-07-01

    The sonochemiluminescence (SCL) behavior of lucigenin (Luc2+) has been studied in aqueous solutions irradiated with 500 kHz ultrasound. Compared with the SCL of a luminol system, a tremendously increased SCL intensity is observed from 50 µM Luc2+ aqueous solution (pH =11) when small amounts of coreactants such as 2-propanol coexist. It is shown that SCL intensity strongly depends on the presence of dissolved gases such as air, O2, N2, and Ar. The highest SCL intensity is obtained in an O2-saturated solution, indicating that molecular oxygen is required to generate SCL. Since SCL intensity is quenched completely in the presence of superoxide dismutase (SOD), an enzyme that can catalyze the disproportionation of O2 •‑, the generation of O2 •‑ in the ultrasonic reaction field is important in the SCL of Luc2+. In this work, the evidence of O2 •‑ production is examined by a spectrofluorometric method using 2-(2-pyridyl)benzothiazoline as the fluorescent probe. The results indicate that the yield of O2 •‑ is markedly increased in the O2-saturated solutions when a small amount of 2-propanol coexists, which is consistent with the results of SCL measurements. 2-Propanol in the interfacial region of a cavitation bubble reacts with a hydroxyl radical (•OH) to form a 2-propanol radical, CH3C•(OH)CH3, which can subsequently react with dissolved oxygen to generate O2 •‑. The most likely pathways for SCL as well as the spatial distribution of SCL in a microreactor are discussed in this study.

  17. Alcohol and water adsorption in zeolitic imidazolate frameworks

    KAUST Repository

    Zhang, Ke

    2013-01-01

    Alcohol (methanol, ethanol, 1-propanol, 2-propanol and 1-butanol) and water vapor adsorption in zeolitic imidazolate frameworks (ZIF-8, ZIF-71 and ZIF-90) with similar crystal sizes was systematically studied. The feasibility of applying these ZIF materials to the recovery of bio-alcohols is evaluated by estimating the vapor-phase alcohol-water sorption selectivity. © 2013 The Royal Society of Chemistry.

  18. 1-(Piperidin-1-yl)-3-(2,4,6-trimethyl-phen-yl)propan-2-ol.

    Science.gov (United States)

    Maharramov, Abel M; Khalilov, Ali N; Gurbanov, Atash V; Allahverdiyev, Mirze A; Ng, Seik Weng

    2011-01-01

    The title compound, C(17)H(27)NO, features a bufferfly-shaped substituted 2-propanol having an aromatic ring on the 1-carbon and a piperidine ring on the 3-carbon. The piperidine ring adopts a chair conformation and its N atom shows a trigonal coordination. In the crystal, the hy-droxy group inter-acts with the N atom of an inversion-related mol-ecule, generating an O-H⋯N hydrogen-bonded dimer. PMID:21522478

  19. 1-(Piperidin-1-yl)-3-(2,4,6-trimethyl­phen­yl)propan-2-ol

    OpenAIRE

    Maharramov, Abel M.; Ali N. Khalilov; Atash V. Gurbanov; Allahverdiyev, Mirze A.; Ng, Seik Weng

    2011-01-01

    The title compound, C17H27NO, features a bufferfly-shaped substituted 2-propanol having an aromatic ring on the 1-carbon and a piperidine ring on the 3-carbon. The piperidine ring adopts a chair conformation and its N atom shows a trigonal coordination. In the crystal, the hy­droxy group inter­acts with the N atom of an inversion-related mol­ecule, generating an O—H⋯N hydrogen-bonded dimer.

  20. Catalysis in the alkylation reaction of 1-naphthol with epichlorohydrin

    Directory of Open Access Journals (Sweden)

    SLOBODANKA JOVANOVIC

    2006-09-01

    Full Text Available Two new and improved procedures were developed for the synthesis of 1-(1-naphthyloxy-2,3-epoxypropane as an important intermediate in the production of the beta-blocker and antioxidant, 1-[(1-methylethylamino]-3-(1-naphthyloxy-2-propanol (propranolol. Both base homogeneous and heterogeneous PTC catalysis were employed. High yields and remarkable selectivity were achieved. The improved purity is particularly important, in view of the quality requirements for propranolol hydrochloride as an active pharmaceutical ingredient.

  1. Re-Refining of Waste Lubricating Oil by Solvent Extraction

    OpenAIRE

    Hassan Ali Durrani; Muhammed Ibrahim Panhwar; Rafique Akthar Kazi

    2011-01-01

    Re-refining of waste lubricating oil by solvent extraction is one of the potential techniques. The advantages of solvent extraction technique practically offers from environmental and economic points of view have received due attention. In this paper selection of composite solvent and technique to upgrade the used lubricant oil into base oil has been made. The composite solvent 2-propanol, 1-butanol and butanone have two alcohols that make a binary system reasonably effective. ...

  2. Determining an Efficient Solvent Extraction Parameters for Re-Refining of Waste Lubricating Oils

    OpenAIRE

    Hassan Ali Durrani; Muhammed Ibrahim Panhwar; Rafique Akthar Kazi

    2012-01-01

    Re-refining of vehicle waste lubricating oil by solvent extraction is one of the efficient and cheapest methods. Three extracting solvents MEK (Methyl-Ethyl-Ketone), 1-butanol, 2-propanol were determined experimentally for their performance based on the parameters i.e. solvent type, solvent oil ratio and extraction temperature. From the experimental results it was observed the MEK performance was highest based on the lowest oil percent losses and highest sludge removal. Further, w...

  3. Novel pot-shaped carbon nanomaterial synthesized in a submarine-style substrate heating CVD method

    OpenAIRE

    Yokoi, Hiroyuki; Hatakeyama, Kazuto; Taniguchi, Takaaki; Koinuma, Michio; Hara, Masahiro; Matsumoto, Yasumichi; ヨコイ, ヒロユキ; ハタケヤマ, カズト; タニグチ, タカアキ; コイヌマ, ミチオ; ハラ, マサヒロ; マツモト, ヤスミチ; 横井, 裕之; 畠山, 一翔; 谷口, 貴章

    2016-01-01

    We have developed a new synthesis method that includes a chemical vapor deposition process in a chamber settled in organic liquid, and applied its nonequilibrium reaction field to the development of novel carbon nanomaterials. In the synthesis at 1110-1120 K, using graphene oxide as a catalyst support, iron acetate and cobalt acetate as catalyst precursors, and 2-propanol as a carbon source as well as the organic liquid, we succeeded to create carbon nanofiber composed of novel pot-shaped uni...

  4. Liquid-liquid extraction and adsorption on solid surfaces applied to used lubricant oils recovery

    OpenAIRE

    J. L. Assunção Filho; L. G. M. Moura; A.C.S. RAMOS

    2010-01-01

    In this work, the recovery of base oils from waste lubricants following the steps of solvent extraction, adsorption on solids and solvent removal by evaporation was evaluated. In the step of solvent extraction, the most efficient was 1-butanol, followed by tert-butanol, 2-propanol and ethanol; for the step of adsorption, activated carbon was the most effective solid for PAH removal, confirming the similarity of these compounds with petroleum aromatic fractions. Thus, the optimum solvent-adsor...

  5. Penggunaan Karboksimetil Kitosan Dari Cangkang Belangkas (Tachypleus Gigas) Sebagai Adsorben Untuk Menurunkan Konsentrasi Logam Pb

    OpenAIRE

    Ananda, Fatya

    2015-01-01

    Reaserch has been done on the using of carboxymethyl chitosan from horseshoe crab’s shells (Tachypleus gigas) as adsorbent to reduce concentration of Pb metal. Carboxymethyl chitosan was made by reacting chitosan sample with NaOH 40 % and monochloroacetic acid which dispersed in 2-propanol for 10 hours at room temperature that results in carboxymethyl chitosan shown by functional groups using FTIR. On the adsorption process using standard solution of Pb with concentration of 5 mg/L and variat...

  6. Design, synthesis and antifungal activity of novel triazole derivatives

    Institute of Scientific and Technical Information of China (English)

    Qing lie Zhao; Yan Song; Hong Gang Hu; Shi Chong Yu; Qiu Ye Wu

    2007-01-01

    Twenty-three 1 -(1H-1,2,4-triazole-1-yl)-2-(2,4-difluorophenyl)-3-(N-cycloproyl-N-substituted-amino)-2-propanols were designed and synthesized on the basis of the active site of lanosterol 14α-demethylase.In vitro antifungal activities showed that some of the title compounds had higher antifungal activity and broader antifungal spectrum than fluconazole.

  7. Hydroxymethylation beyond Carbonylation: Enantioselective Iridium-Catalyzed Reductive Coupling of Formaldehyde with Allylic Acetates via Enantiotopic π-Facial Discrimination.

    Science.gov (United States)

    Garza, Victoria J; Krische, Michael J

    2016-03-23

    Chiral iridium complexes modified by SEGPHOS catalyze the 2-propanol-mediated reductive coupling of branched allylic acetates 1a-1o with formaldehyde to form primary homoallylic alcohols 2a-2o with excellent control of regio- and enantioselectivity. These processes, which rely on enantiotopic π-facial discrimination of σ-allyliridium intermediates, represent the first examples of enantioselective formaldehyde C-C coupling beyond aldol addition. PMID:26958737

  8. Solvent-treated PEDOT:PSS on the improvement PTB7 based on polymer solar cells performance

    Science.gov (United States)

    Huang, Di; Xu, Zheng; Zhao, Suling; Li, Yang; Zhao, Ling; Jin, Shi Qi

    2015-10-01

    In this manuscript, the effect of the 2-propanol(IPA)-treated poly(3,4-ethylenedioxy-thiophene):poly(styrenesulfonate) (PEDOT:PSS) on the performance enhancement of polymer solar cells(PSCs) based on poly[[4,8-bis[(2-ethylhexyl)oxy]benzo[1,2-b:4,5-b‧]dithiophene-2,6-diyl][3-fluoro-2-[(2-ethylhexyl)carbonyl]thieno[3,4-b]thiophenediyl

  9. Systematic study of the thermal diffusion in associated mixtures

    OpenAIRE

    Polyakov, P.; Wiegand, S.

    2008-01-01

    We performed systematic temperature and concentration dependent measurements of the Soret coefficient in different associated binary mixtures of water, deuterated water, dimethyl sulfoxide (DMSO), methanol, ethanol, acetone, methanol, 1-propanol, 2-propanol, and propionaldehyde using the so-called thermal diffusion forced Rayleigh scattering method. For some of the associating binary mixtures such as ethanol/water, acetone/water, and DMSO/water, the concentration xw+/- at which the Soret coef...

  10. Kinetics and mechanism of photolysis and TiO2 photocatalysis of triclosan.

    Science.gov (United States)

    Son, Hyun-Seok; Ko, Gwangpyo; Zoh, Kyung-Duk

    2009-07-30

    The degradations of triclosan (5-chloro-2-(2,4-dichlorophenoxy)-phenol), a potent broad-spectrum antimicrobial agent, were compared in TiO2-only in the dark condition, photolysis, and TiO2 photocatalysis with a UV-A lamp. TiO2 photocatalysis more effectively degraded and mineralized triclosan compared to TiO2-only and photolysis conditions. While triclosan removed only 30% by TiO2-only condition within 20 min, the triclosan degradation in photolysis and photocatalysis at the same time was 75 and 82%, respectively, and TOC removal was significantly higher in photocatalysis than in photolysis. The data of kinetics showed that triclosan adsorption onto TiO2 was fitted to Langmuir isotherm, and TiO2 photocatalysis was fitted to Langmuir-Hinshelwood model (b=27.99 mM(-1), K(triclosan)=9.49 mM(-1)). The neutral range of pH was favorable to photocatalysis due to the charge effect between TiO2 and triclosan. The addition of 2-propanol, a radical scavenger, significantly reduced the degradation of triclosan both in photolysis and photocatalysis. Dioxin-type intermediates such as dibenzo-dichloro-p-dioxin (DCDD), dibenzo-p-dioxin were produced in photolysis with and without 2-propanol, and also in photocatalysis with 2-propanol, but these intermediates were not detected in photocatalysis without 2-propanol. This result indicates that the photocatalytic degradation of triclosan is mainly achieved by radicals, and these radicals can further degrade dioxin-type intermediates once they are produced in photocatalysis.

  11. Thermal Decomposition Reaction of Acetophenone Cyclic Diperoxide in Solvents of Different Physicochemical Properties

    Directory of Open Access Journals (Sweden)

    C. M. Mateo

    2000-03-01

    Full Text Available The thermal decomposition reaction of acetophenone cyclic diperoxide (trans-3,6-dimethyl-3,6-diphenyl-1,2,4,5-tetroxane; APDP at the initial concentration of c.a. 0.01 mol kg-1 and temperature ranges of 135.5 to 185.0° C has been investigated in dioxane and acetonitrile solutions, and in an 2-propanol/benzene mixture.

  12. (Vapor + liquid) equilibria of the binary mixtures of m-cresol with C1-C4 aliphatic alcohols at 95.5 kPa

    International Nuclear Information System (INIS)

    Bubble point temperatures at 95.5 kPa, over the entire composition range, are measured for the binary mixtures formed by m-cresol with: methanol, ethanol, 1-propanol, 2-propanol, and n-, iso-, sec-, and tert-butanols - using a Swietoslawski-type ebulliometer. The liquid phase composition - bubble point temperature measurements are well represented by the Wilson model. (Vapor + liquid) equilibria predicted from the model are presented

  13. Determination of some volatile compounds in fruit spirits produced from grapes (Vitis Vinifera L.) and plums (Prunus domestica L.) cultivars

    OpenAIRE

    Kostik, Vesna; Gjorgjeska, Biljana; Angelovska, Bistra; Kovacevska, Ivona

    2014-01-01

    Fruit spirits contain a large array of volatile compounds among which the important role from toxicological aspect besides ethanol has methanol, aliphatic esters and fusel alcohols. This study evaluates the content of ethanol, ethyl acetate, methanol, isopropyl alcohol (2-propanol), n-propyl alcohol (propan-l-ol), isobutyl alcohol (2-methylpropan-1-ol), n-butyl alcohol (1-butanol), isoamyl alcohol (3-methyl-1-butanol) and n-amyl alcohol (pentan-1-ol) in different grapes and plum brandies i...

  14. Rapid Estimation of Tocopherol Content in Linseed and Sunflower Oils-Reactivity and Assay

    Directory of Open Access Journals (Sweden)

    Tjaša Prevc

    2015-08-01

    Full Text Available The reactivity of tocopherols with 2,2-diphenyl-1-picrylhydrazyl (DPPH was studied in model systems in order to establish a method for quantifying vitamin E in plant oils. The method was optimized with respect to solvent composition of the assay medium, which has a large influence on the course of reaction of tocopherols with DPPH. The rate of reaction of α-tocopherol with DPPH is higher than that of γ-tocopherol in both protic and aprotic solvents. In ethyl acetate, routinely applied for the analysis of antioxidant potential (AOP of plant oils, reactions of tocopherols with DPPH are slower and concentration of tocopherols in the assay has a large influence on their molar reactivity. In 2-propanol, however, two electrons are exchanged for both α- and γ-tocopherols, independent of their concentration. 2-propanol is not toxic and is fully compatible with polypropylene labware. The chromatographically determined content of tocopherols and their molar reactivity in the DPPH assay reveal that only tocopherols contribute to the AOP of sunflower oil, whereas the contribution of tocopherols to the AOP of linseed oil is 75%. The DPPH assay in 2-propanol can be applied for rapid and cheap estimation of vitamin E content in plant oils where tocopherols are major antioxidants.

  15. Efficient photocatalytic degradation of organics present in gas and liquid phases using Pt-TiO2/Zeolite (H-ZSM).

    Science.gov (United States)

    Neppolian, B; Mine, Shinya; Horiuchi, Yu; Bianchi, C L; Matsuoka, M; Dionysiou, D D; Anpo, M

    2016-06-01

    TiO2-encapsulated H-ZSM photocatalysts were prepared by physical mixing of TiO2 and zeolites. Pt was immobilized on the surface of the TiO2-encapsulated zeolite (H-ZSM) catalysts by a simple photochemical reduction method. Different weight ratios of both TiO2 and Pt were hybridized with H-ZSM and the catalytic performance of the prepared catalysts was investigated for 2-propanol oxidation in liquid phase and acetaldehyde in gas phase reaction. Around 5-10 wt% TiO2-encapsulated H-ZSM catalysts was found to be optimal amount for the effective oxidation of the organics. Prior to light irradiation, Pt-TiO2-H-ZSM showed considerable amount of catalytic degradation of 2-propanol in the dark, forming acetone as an intermediate. In this study, Pt has played a major and important role on the total oxidation of 2-propanol as well as acetaldehyde. As a result, no residual organics were present in the pores of the zeolites. The catalysts could be reused more than three times without losing their catalytic activity in both phases. The Pt-TiO2-H-ZSM photocatalysts could overcome the problem of strong adsorption of organics in the zeolite pores (after the reaction). Thus, Pt-TiO2-H-ZSM can be used as a potential catalyst for both liquid and gas phase oxidation of organic pollutants.

  16. Conversion of alcohols ({alpha}-methylated series) on AlPO{sub 4} catalysts

    Energy Technology Data Exchange (ETDEWEB)

    Campelo, J.M.; Garcia, A.; Herencia, J.F. [Universidad de Cordoba (Spain)] [and others

    1995-02-01

    The conversion (dehydration/dehydrogenation) of alcohols in {alpha}-methylated series (methanol, ethanol, 2-propanol, and tert-butanol) on AlPO{sub 4} catalysts differently prepared has been studied by microcatalytic pulse reactor technique at different temperatures and flow rates. The kinetic parameters have been obtained by analysis of the data through the Bassett-Habgood equation. Dehydration to ether and/or olefin is the major reaction process. Dehydrogenation product was only scarcely found in 2-propanol conversion. The influence of the reaction temperature upon the conversion of alcohols and the selectivities of the products was investigated. Activity increases as a function of surface acidity of the AlPO{sub 4} catalyst as well as with the {alpha}-substitution in the alcohol. Moreover, selectivity studies indicated that ethanol and 2-propanol dehydration follows a combination pathway of parallel and consecutive reactions. A good correlation between the results of dehydration conversion and acid properties, gas-chromatographically measured through the irreversible adsorption of pyridine (473 and 573 K) and 2,6-dimethylpyridine (573 K), is observed. Also, activity poisoning results indicated that Broensted acid sites of AlPO{sub 4} catalyst participated in dehydradation processes, thus strengthening the carbenium ion reaction pathway in AlPO{sub 4} catalysts. 49 refs., 3 figs., 4 tabs.

  17. Alcohol--Induced Polyelectrolyte-Surfactant Complex Coacervate Systems: Characterization and Applications in Enzyme and Protein Extraction

    Science.gov (United States)

    Nejati Moshtaghin, Mahboubeh

    of FA, oppositely charged amphiphiles (surfactant-polyelectrolyte), and the charge ratio of the surfactant-polyelectrolyte on the extent of coacervation have been investigated. Furthermore, the chemical composition of each phase formed in the coacervate system was determined as a function of HFIP percentage. Phase diagrams of HFIP-PMA-CTAB and 2-propanol-PMA-CTAB were studied. The phase separation occurs over a wide range of polyelectrolyte, surfactant and alcohol concentration. In addition, a study of the dependence of coacervate volume on phase composition in different system (as defined by concentrations and mole charge ratio of amphihiles and alcohols) provided useful insight about possible underlying interactions and mechanisms. It has been concluded that neutralization favors coacervation in both systems. However, according to the compositional analysis of both HFIP and 2-propanol SPCC system, it seems that coacervation mechanisms are different. In Chapter III the properties of 2-propanol--SPCC, with analogous surfactant (CTAB) and polyelectrolyte (PMA) used in Chapter II, will be investigated. In particular, we are interested in examining the difference between the phase separation characteristics of the coacervates induced by 2-propanol and HFIP as coacervator. For this purpose, the phase behavior and the chemical composition of the phases will be analyzed as a function of 2-propanol and constituents concentrations. Chapter IV contains results of our investigations on the activity of a model enzyme (Trypsin) in 2-propanol- and FA-induced SPCC system. These investigations will facilitate understanding whether the aliphatic alcohol, AA- and FA-induced SPCC system denature the model enzymes. Such investigations also help in evaluation of the applicability of the coacervate systems developed in this work in proteomics where the proteolytic activity of enzymes is used for protein digestion. Finally, in Chapter V, the efficiency of the coacervate system (2-propanol

  18. Chemical strategies for modifications of the solar cell process, from wafering to emitter diffusion; Chemische Ansaetze zur Neuordnung des Solarzellenprozesses ausgehend vom Wafering bis hin zur Emitterdiffusion

    Energy Technology Data Exchange (ETDEWEB)

    Mayer, Kuno

    2009-11-06

    The paper describes the classic standard industrial solar cell based on monocrystalline silicon and describes new methods of fabrication. The first is an alternative wafering concept using laser microjet cutting instead of multiwire cutting. This method originally uses pure, deionized water; it was modified so that the liquid jet will not only be a liquid light conductor but also a transport medium for etching fluids supporting thermal abrasion of silicon by the laser jet. Two etching fluids were tested experimentally; it was found that water-free fluids based on perfluorinated solvents with very slight additions of gaseous chlorine are superior to all other options. In the second section, the wet chemical process steps between wafering and emitter diffusion (i.e. the first high-temperature step) was to be modified. Alternatives to 2-propanol were to be found in the experimental part. Purification after texturing was to be rationalized in order to reduce the process cost, either by using less chemical substances or by achieving shorter process times. 1-pentanol and p-toluolsulfonic acid were identified as two potential alternatives to 2-propanol as texture additives. Finally, it could be shown that wire-cut substrates processed with the new texturing agents have higher mechanical stabilities than substrates used with the classic texturing agent 2-propanol. [German] Im ersten Kapitel wird die klassische Standard-Industrie-Solarzelle auf der Basis monokristallinen Siliziums vorgestellt. Der bisherige Herstellungsprozess der Standard-Industrie-Solarzelle, der in wesentlichen Teilen darauf abzielt, diese Verluste zu minimieren, dient als Referenz fuer die Entwicklung neuer Fertigungsverfahren, wie sie in dieser Arbeit vorgestellt werden. Den ersten thematischen Schwerpunkt bildet die Entwicklung eines alternativen Wafering-Konzeptes zum Multi-Drahtsaegen. Die Basis des neuen, hier vorgestellten Wafering-Prozesses bildet das Laser-Micro-Jet-Verfahren. Dieses System

  19. Analysis of 3-MCPD and 1,3-DCP in Various Foodstuffs Using GC-MS

    OpenAIRE

    Kim, Wooseok; Jeong, Yun A; On, Jiwon; Choi, Ari; Lee, Jee-yeon; Lee, Joon Goo; Lee, Kwang-Geun; Pyo, Heesoo

    2015-01-01

    3-Monochloro-1,2-propanediol (3-MCPD) and 1,3-dichloro-2-propanol (1,3-DCP) are not only produced in the manufacturing process of foodstuffs such as hydrolyzed vegetable proteins and soy sauce but are also formed by heat processing in the presence of fat and low water activity. 3-MCPD exists both in free and ester forms, and the ester form has been also detected in various foods. Free 3-MCPD and 1,3-DCP are classified as Group 2B by the International Agency for Research on Cancer. Although th...

  20. Enantioselektive Transferhydrierung mit Ruthenium(II)-Komplexen

    OpenAIRE

    Henning, Frauke

    2003-01-01

    Eine Vielzahl chiraler Liganden und Komplexe wurden als Katalysatoren in der enantioselektiven Transferhydrierung von Acetophenon mit den Wasserstoffdonoren 2-Propanol und Ameisensäure getestet. Vier dreizähnige axial chirale Binaphthyle erzielen in situ mit Tris-(triphenylphosphanyl)ruthenium(II)-chlorid hohe Enantiomerenüberschüsse von bis zu 98% und Ausbeuten über 90% unter optimierten Reaktionsbedingungen. Es wird ein deutlicher OH-Effekt beobachtet, während ein NH-Effekt nicht bestätigt ...

  1. Polymerization of cardanol using soybean peroxidase and its potential application as anti-biofilm coating material.

    Science.gov (United States)

    Kim, Yong Hwan; An, Eun Suk; Song, Bong Keun; Kim, Dong Shik; Chelikani, Rahul

    2003-09-01

    Soybean peroxidase (20 mg) catalyzed the oxidative polymerization of cardanol in 2-propanol/phospate buffer solution (25 ml, 1:1 v/v) and yielded 62% polycardanol over 6 h. Cobalt naphthenate (0.5% w/w) catalyzed the crosslinking of polycardanol and the final hardness of crosslinked polycardanol film exceeded 9 H scale as pencil scratch hardness, which shows a high potential as a commercial coating material. In addition, it showed an excellent anti-biofouling activity to Pseudomonas fluorescens compared to other polymeric materials such as polypropylene. PMID:14571976

  2. Thermal performance of an open loop closed end pulsating heat pipe

    Science.gov (United States)

    Saha, Manabendra; Feroz, C. M.; Ahmed, F.; Mujib, T.

    2012-02-01

    This paper presents an experimental study of an open loop pulsating heat pipe (OLPHP) of 0.9 mm inner diameter. The performance characterization has been done using four working fluids at vertical and horizontal orientations. Water, Methanol, 2-Propanol and Acetone has been employed as the working fluid with 50% fill ratio. The experimental results indicate a strong influence of gravity and thermo physical properties of the working fluids on the performance of OLPHP. Considering all the working fluids used, Water has shown better thermal performance in vertical orientation while Methanol has shown better performance in horizontal orientation. All the working fluids perform better at horizontal orientation.

  3. Synthesis and Structure of a New Dinuclear Uranyl Complex

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    With a heptadentate compartmental Schiff-base ligand H3L (1, 3-di[o-(salicylimino) ph-enoxyl]-2-propanol), a new binuclear diuranyl complex [(UO2)2L(OH)]?3DMF, C38H45N5O13U2, was synthesized and the crystal structure was determined by X-ray diffraction techniques. The coordination geometry are two pentagonal bipyramids. In each pentagon four kinds of U-O (phenoxido, hydroxo, alkoxo and ether oxo) bonds are discussed.

  4. 1-(Piperidin-1-yl)-3-(2,4,6-trimethyl­phen­yl)propan-2-ol

    Science.gov (United States)

    Maharramov, Abel M.; Khalilov, Ali N.; Gurbanov, Atash V.; Allahverdiyev, Mirze A.; Ng, Seik Weng

    2011-01-01

    The title compound, C17H27NO, features a bufferfly-shaped substituted 2-propanol having an aromatic ring on the 1-carbon and a piperidine ring on the 3-carbon. The piperidine ring adopts a chair conformation and its N atom shows a trigonal coordination. In the crystal, the hy­droxy group inter­acts with the N atom of an inversion-related mol­ecule, generating an O—H⋯N hydrogen-bonded dimer. PMID:21522478

  5. Nichtklassische Rutheniumhydridkomplexe in Wasserstofftransfer-Reaktionen

    OpenAIRE

    Ahmad, Javed

    2012-01-01

    This work investigates the activity of pincer stabilised Ruthenium complexes. The main emphasis was put on the complexes [Ru(dtbpmp)(H2)H2] 2 and [Ru(dtbpoet)(H2)H2] 3, whose activity was compared with the well-known Chaudret complex [Ru(PCy3)2(H2)2H2] 1. Complexes 1 to 3 were active in the transfer hydrogenation of ketones, olefins and alpha,beta-unsaturated ketones with 2-propanol as hydrogen donor – without any base additives necessary. Thereby the activity for the reduction of ketones, wi...

  6. Ultrasonic and Volumetric Investigations of -Butyrolactone with Aliphatic Alcohols

    Directory of Open Access Journals (Sweden)

    Amara Jyothi Koppula

    2014-08-01

    Full Text Available Densities ( and speeds of sound (u have been determined for the binary liquid mixtures of -butyrolactone (GBL with 1-propanol (1-Pro, 2-propanol (2-Pro, 1-butanol (1-But and 2-butanol (2-But at 303.15, 308.15, and 313.15 K and entire composition range. From the experimental results, the excess molar volume (V E , and deviation in isentropic compressibility (s were calculated. The computed properties have been fitted to a Redlich-Kister type polynomial equation to derive binary coefficients and standard deviations.

  7. Characterization of catalytic supports based in mixed oxides for control reactions of NO and N2O

    International Nuclear Information System (INIS)

    The catalytic supports Al2O3, La2O3 and Al2O3-La2O3 were prepared by the Precipitation and Coprecipitation techniques. The catalytic supports Al2O3, La2O3 and Al2O3-La2O3 were characterized by several techniques to determine: texture (Bet), crystallinity (XRD), chemical composition (Sem)(Ftir) and it was evaluated their total acidity by reaction with 2-propanol. The investigation will be continued with the cobalt addition and this will be evaluated for its catalytic activity in control reactions of N O and N2O. (Author)

  8. Measurement and correlation of solubility of trans-resveratrol in 11 solvents at T = (278.2, 288.2, 298.2, 308.2, and 318.2) K

    Energy Technology Data Exchange (ETDEWEB)

    Sun Xilan; Peng Bin [Department of Chemistry, Zhejiang University, Hangzhou 310027 (China); Yan Weidong [Department of Chemistry, Zhejiang University, Hangzhou 310027 (China)], E-mail: yanweidong@zju.edu.cn

    2008-04-15

    The solubilities of trans-resveratrol in methanol, ethanol, 1-propanol, 2- propanol, 1-butanol, 1-pentanol, 1-hexanol, ethyl acetate, tetrahydrofuran, acetone, and water (pH 6.0) solvents were measured at T = (278.2, 288.2, 298.2, 308.2, and 318.2) K. The solubilities of trans-resveratrol in selected solvents increase with temperature, but decrease with increasing the number of carbon in alcohol solvents. The experimental data were correlated using a thermodynamic equation.

  9. Improved regioselectivity in pyrazole formation through the use of fluorinated alcohols as solvents: synthesis and biological activity of fluorinated tebufenpyrad analogs.

    Science.gov (United States)

    Fustero, Santos; Román, Raquel; Sanz-Cervera, Juan F; Simón-Fuentes, Antonio; Cuñat, Ana C; Villanova, Salvador; Murguía, Marcelo

    2008-05-01

    The preparation of N-methylpyrazoles is usually accomplished through reaction of a suitable 1,3-diketone with methylhydrazine in ethanol as the solvent. This strategy, however, leads to the formation of regioisomeric mixtures of N-methylpyrazoles, which sometimes are difficult to separate. We have determined that the use of fluorinated alcohols such as 2,2,2-trifluoroethanol (TFE) and 1,1,1,3,3,3-hexafluoro-2-propanol (HFIP) as solvents dramatically increases the regioselectivity in the pyrazole formation, and we have used this modification in a straightforward synthesis of fluorinated analogs of Tebufenpyrad with acaricide activity.

  10. Design synthesis and biological evaluation of 3-substituted triazole derivatives

    Institute of Scientific and Technical Information of China (English)

    Bao Gang Wang; Shi Chong Yu; Xiao Yun Chai; Yong Zheng Yan; Hong Gang Hu; Qiu Ye Wu

    2011-01-01

    Based on the active site of lanosterol 14α-demethylase of azole antifungal agents, sixteen l-(lH-l,2,4-triazole-l-yl)- 2-(2,4-difluorophenyl)-3-(N-n-butyl-N-l-substitutedbenzyl-4-methylene-lH-l,2,3-triazole)-2-propanols have been designed, synthesized and evaluated as antifungal agents. Results of preliminary antifungal tests against eight human pathogenic fungi in vitro showed that some of the compounds exhibited excellent activities with broad spectrum.

  11. Ionic association and solvation of the ionic liquid 1-hexyl-3-methylimidazolium chloride in molecular solvents revealed by vapor pressure osmometry, conductometry, volumetry, and acoustic measurements.

    Science.gov (United States)

    Sadeghi, Rahmat; Ebrahimi, Nosaibah

    2011-11-17

    A systematic study of osmotic coefficient, conductivity, volumetric and acoustic properties of solutions of ionic liquid 1-hexyl-3-methylimidazolium chloride ([C(6)mim][Cl]) in various molecular solvents has been made at different temperatures in order to study of ionic association and solvation behavior of [C(6)mim][Cl] in different solutions. Precise measurements on electrical conductances of solutions of [C(6)mim][Cl] in water, methanol, ethanol, 1-propanol, 2-propanol, 1-butanol, and acetonitrile at 293.15, 298.15, and 303.15 K are reported and analyzed with Barthel's low-concentration chemical model (lcCM) to obtain the limiting molar conductivities and association constants of this ionic liquid in the investigated solvents. Strong ion pairing was found for the ionic liquid in 2-propanol, 1-butanol, and 1-propanol, whereas ion association in acetonitrile, methanol and ethanol is rather weak and in water the ionic liquid is fully dissociated. In the second part of this work, the apparent molar volumes and isentropic compressibilities of [C(6)mim][Cl] in water, methanol, ethanol, acetonitrile, 1-propanol, 2-propanol, and 1-butanol are obtained at the 288.15-313.15 K temperature range at 5 K intervals at atmospheric pressure from the precise measurements of density and sound velocity. The infinite dilution apparent molar volume and isentropic compressibility values of the free ions and ion pairs of [C(6)mim][Cl] in the investigated solvents as well as the excess molar volume of the investigated solutions are determined and their variations with temperature and type of solvents are also studied. Finally, the experimental measurements of osmotic coefficient at 318.15 K for binary solutions of [C(6)mim][Cl] in water, methanol, ethanol, 2-propanol, and acetonitrile are taken using the vapor pressure osmometry (VPO) method and from which the values of the solvent activity, vapor pressure, activity coefficients, and Gibbs free energies are calculated. The results are

  12. Polycaprolactone-Chitin Nanofibrous Mats as Potential Scaffolds for Tissue Engineering

    OpenAIRE

    Min Sup Kim; Sang Jun Park; Bon Kang Gu; Chun-Ho Kim

    2012-01-01

    We describe here the preparation of poly(caprolactone) (PCL)-chitin nanofibrous mats by electrospinning from a blended solution of PCL and chitin dissolved in a cosolvent, 1,1,1,3,3,3-hexafluoro-2-propanol and trifluoroacetic acid. Scanning electron microscopy showed that the neutralized PCL-chitin nanofibrous mats were morphologically stable, with a mean diameter of 340.5±2.6 nm, compared with a diameter of 524.2±12.1 nm for PCL mats. The nanofibrous mats showed decreased water contact angle...

  13. Cyclic Tetranuclear and Hexanuclear Palladium(II) Complexes and Their Host-Guest Chemistry

    OpenAIRE

    Judith A. Walmsley; Zhu, Shourong; Matilla, Antonio; Donowick, Tiffanee G.; Cramp, Jessica E.; Tercero, Jose Manuel; Dalrymple, Tatyana

    2007-01-01

    Cyclic tetrameric complexes have been prepared by the reaction of Pd(en)Cl2 or Pd(dapol)Cl2, or their nitrato analogs, with Na2(5′GMP) in aqueous solution, where en = 1,2-diaminoethane, dapol = 1,3-diamino-2-propanol, 5′-GMP = guanosine 5′-monophosphate. Addition of certain small molecules containing hydrophobic groups resulted in the expansion of the tetramer to a cyclic hexamer with strong bonding of one guest per hexameric host. At pH 5-6, the guest molecule can be a cation, anion, or neut...

  14. Extended UNIQUAC Model for Correlation and Prediction of Vapor-Liquid-Liquid-Solid Equilibria in Aqueous Salt Systems Containing Non-Electrolytes. Part B. Alcohol (Ethanol, Propanols, Butanols) - Water-salt systems

    DEFF Research Database (Denmark)

    Thomsen, Kaj; Iliuta, Maria Cornelia; Rasmussen, Peter

    2004-01-01

    The Extended UNIQUAC model for electrolyte solutions is an excess Gibbs energy function consisting of a Debye-Huckel term and a term corresponding to the UNIQUAC equation. For vapor-liquid equilibrium calculations, the fugacities of gas-phase components are calculated with the Soave-Redlich-Kwong......-propanol, 2-methyl 2-propanol) and various ions (Na+, K+, NH4+, Cl-, NO3, SO42-, SO32-, HSO3-, CO32-, and HCO3-) shows the capability of the model to accurately represent the phase behavior of these kinds of systems. (C) 2004 Elsevier Ltd. All rights reserved....

  15. Stereo block copolymers of L- and D-lactides

    OpenAIRE

    Yui, Nobuhiko; Pieter J. Dijkstra; Feijen, Jan

    1990-01-01

    Sequential diblock copolymers composed of L- and D-lactic acid residues were synthesized through a living ring-opening polymerization of L- and D-lactide initiated by aluminium tris(2-propanolate). The composition of the block copolymers was varied by changing the reaction conditions and monomer over initiator ratio and confirmed by 1H NMR analysis, molecular weight determination and optical rotation measurements. Molecular weights ranged from 1,3 to 2,0 · 104 with 1,2 < Mw/Mn < 1,4. Stereoco...

  16. Enhanced Reactivity of [Hydroxy(tosyloxyiodo]benzene in Fluoroalcohol Media. Efficient Direct Synthesis of Thienyl(aryliodonium Salts

    Directory of Open Access Journals (Sweden)

    Toshifumi Dohi

    2010-03-01

    Full Text Available In this manuscript, we report clear evidence for the generation of aromatic cation radicals produced by using [hydroxy(tosyloxyiodo]benzene (HTIB in fluoroalcohol solvents such as 2,2,2-trifluoroethanol (TFE and 1,1,1,3,3,3-hexafluoro-2-propanol (HFIP. The single-electron-transfer (SET oxidation ability of HTIB to give cation radicals was first established by ESR and UV measurements. The reaction was broadly applied to various thiophenes, and unique thienyliodonium salts were directly synthesized by this method in excellent yields without the production of any harmful byproducts.

  17. New Chiral Metal Cluster Systems for Catalytic Asymmetric Syntheses of Chiral Alcohols

    Institute of Scientific and Technical Information of China (English)

    LI Yan-yun; CHEN Jian-shan; YANG Chuan-bo; DONG Zhen-rong; LI Bao-zhu; ZHANG Hui; GAO Jing-xing; TAKAO Ikariya

    2004-01-01

    The efficient chiral Ru3(CO)12 systems were prepared in situ from Ru3(CO)12 and various chiral diiminoor diamino-diphosphine tetradentate ligands. The systems have been used for the asymmetric transfer hydrogenation of propiophenone in 2-propanol, leading to 1-phenyl-1-propanol in a 98% yield and 96% e.e. The IR study suggests that the carbonyl hydride anion [HRu3(CO)11]- most probably exists as a principal species under the reaction conditions. The high chiral efficiency may be due to the synergetic effect produced by the neighboring ruthenium atoms and a special chiral micro-environment involving the polydentate ligand and the Ru3 framework.

  18. Efecto del método de preparación de los óxidos mixtos de Zr-Ti

    OpenAIRE

    J. Guzmán López; H. Pérez Pastenes; J. Trejo Gaytán; T. Viveros García

    2002-01-01

    Se sintetizaron óxidos mixtos de ZrO2-TiO2 con diferentes relaciones molares mediante los procesos de precipitación y sol-gel. Las muestras se analizaron mediante fisisorción de nitrógeno, difracción de rayos X, análisis térmicos diferencial y gravimétrico. Se realizaron reacciones de descomposición de 2-propanol para determinar la acidez y basicidad de los materiales mediante la deshidratación y la deshidrogenación del alcohol para producir propileno y acetona, respectivamente. Se encontró q...

  19. In vitro release studies of piroxicam from oil-in-water creams and hydroalcoholic gel topical formulations.

    Science.gov (United States)

    Rafiee-Tehrani, M; Mehramizi, A

    2000-04-01

    The importance of piroxicam, a therapeutic anti-inflammatory drug, is well known. Because of gastrointestinal disorders, dermatological dosage forms are recommended most. In our first studies, oil-in-water (O/W) creams of piroxicam (1% concentration) were prepared using glyceryl monostearate (GMS), stearic acid, and triethanolamine as additive ingredients. In our second studies, hydroalcoholic transparent gel formulations of this drug in a 0.5% concentration were prepared using hydroxypropylcellulose (HPC) as the gelling agent. The release of piroxicam from all formulations via dialysis through a cellulose membrane into phosphate buffer pH 6.8 at 37 degrees C was studied. The effects of additives such as propylene glycol and 2-propanol on the drug release were also investigated. The release profiles from the standpoint of diffusion-controlled processes, as well as zero-order and first-order kinetics, were evaluated, and relevant parameters, such as diffusion coefficient, permeability coefficient, and partition coefficient, were calculated. The release obeys both the diffusion mechanism and first-order kinetics. The drug release from gel formulations containing 10%, 20%, and 30% propylene glycol was decreased due to the enhancement of viscosity. However, the limpidity of these formulations was improved. Moreover, the release of drug from gel formulations containing 15% and 20% of 2-propanol was increased. These results show that a hydroalcoholic gel formulation with HPC is a more suitable preparation of piroxicam when compared with an O/W cream formulation.

  20. Effect of reduction enhancer on a radiolytic synthesis of carbon-supported Pt–Cu nanoparticles and their structural and electrochemical properties

    Energy Technology Data Exchange (ETDEWEB)

    Kugai, Junichiro, E-mail: jkugai@kobe-kosen.ac.jp [Kobe City College of Technology, Department of Applied Chemistry (Japan); Kubota, Chihiro; Okazaki, Tomohisa; Seino, Satoshi; Nakagawa, Takashi [Osaka University, Graduate School of Engineering (Japan); Nitani, Hiroaki [High Energy Accelerator Research Organization, Institute of Materials Structure Science (IMSS) (Japan); Yamamoto, Takao A. [Osaka University, Graduate School of Engineering (Japan)

    2015-06-15

    In order to clarify the effect of reduction enhancer on the nanoparticle formation process and their structural and catalytic properties, carbon-supported Pt–Cu nanoparticles were synthesized by electron beam irradiation on an aqueous precursor solution in the presence/absence of reduction enhancer. In the absence of reduction enhancer, tetravalent platinum oxide particles of approximately 1 nm in diameter were formed on carbon support with copper barely precipitated, while in the presence of 2-propanol or ethylene glycol or glucose both platinum and copper precipitated as few-nanometer-sized alloy particles together with copper oxides. It was suggested that the metal nuclei produced upon electron beam irradiation do not have enough lifetime without reduction enhancer due to fast oxidation of the nuclei by oxidizing radicals, while the reduction enhancer scavenges these oxidizing radicals preventing oxidation of metallic clusters and prolonging their lifetime. Ethylene glycol gave smaller and better alloyed particles with less copper oxides compared to 2-propanol since the carbonyl compounds derived from oxidation of ethylene glycol protect metallic clusters from oxidation further prolonging their lifetime. In the electrochemical measurements, the methanol oxidation activities of Pt–Cu/C catalysts were well explained by their structural characteristics.

  1. Response surface methodology for the optimization of dispersive liquid-liquid microextraction of chloropropanols in human plasma.

    Science.gov (United States)

    Gonzalez-Siso, Paula; Lorenzo, Rosa A; Regenjo, María; Fernández, Purificación; Carro, Antonia M

    2015-10-01

    Chloropropanols are processing toxicants with a potential risk to human health due to the increased intake of processed foods. A rapid and efficient method for the determination of three chloropropanols in human plasma was developed using ultrasound-assisted dispersive liquid-liquid microextraction. The method involved derivatization and extraction in one step followed by gas chromatography with tandem mass spectrometry analysis. Parameters affecting extraction, such as sample pH, ionic strength, type and volume of dispersive and extraction solvents were optimized by response surface methodology using a pentagonal design. The linear range of the method was 5-200 ng/mL for 1,3-dichloro-2-propanol, 10-200 ng/mL for 2,3-dichloro-2-propanol and 10-400 ng/mL for 3-chloropropane-1,2-diol with the determination coefficients between 0.9989 and 0.9997. The limits of detection were in the range of 0.3-3.2 ng/mL. The precision varied from 1.9 to 10% relative standard deviation (n = 9). The recovery of the method was between 91 and 101%. Advantages such as low consumption of organic solvents and short time of analysis make the method suitable for the biomonitoring of chloropropanols. PMID:26205350

  2. Effect of mixing, concentration and temperature on the formation of mesostructured solutions and their role in the nucleation of DL-valine crystals.

    Science.gov (United States)

    Jawor-Baczynska, Anna; Moore, Barry D; Sefcik, Jan

    2015-01-01

    We report investigations on the formation of mesostructured solutions in DL-valine-water-2-propanol mixtures, and the crystallization of DL-valine from these solutions. Mesostructured liquid phases, similar to those previously observed in aqueous solutions of glycine and DL-alanine, were observed using Dynamic Light Scattering and Brownian microscopy, in both undersaturated and supersaturated solutions below a certain transition temperature. Careful experimentation was used to demonstrate that the optically clear mesostructured liquid phase, comprising colloidal mesoscale clusters dispersed within bulk solution, is thermodynamically stable and present in equilibrium with the solid phase at saturation conditions. Solutions prepared by slow cooling contained mesoscale clusters with a narrow size distribution and a mean hydrodynamic diameter of around 200 nm. Solutions of identical composition prepared by rapid isothermal mixing of valine aqueous solutions with 2-propanol contained mesoscale clusters which were significantly larger than those observed in slowly cooled solutions. The presence of larger mesoscale clusters was found to correspond to faster nucleation. Observed induction times were strongly dependent on the rapid initial mixing step, although solutions were left undisturbed afterwards and the induction times observed were up to two orders of magnitude longer than the initial mixing period. We propose that mesoscale clusters above a certain critical size are likely to be the location of productive nucleation events.

  3. Influence of the composition of aqueous-alcohol solvents on the thermodynamic characteristics of L-phenylalanine dissolution at 298.15 K

    Energy Technology Data Exchange (ETDEWEB)

    Badelin, Valentin G. [Laboratory of Thermodynamics of Solutions of Non-electrolytes and Biologically Active Substances, Institute of Solution Chemistry, Russian Academy of Sciences, 1 Akademicheskaya Street, 153045, Ivanovo (Russian Federation); Smirnov, Valeriy I., E-mail: vis@isc-ras.ru [Laboratory of Thermodynamics of Solutions of Non-electrolytes and Biologically Active Substances, Institute of Solution Chemistry, Russian Academy of Sciences, 1 Akademicheskaya Street, 153045, Ivanovo (Russian Federation)

    2011-11-10

    Highlights: Black-Right-Pointing-Pointer Enthalpies of L-phenylalanine dissolution have been measured in aqueous methanol, ethanol, 1-propanol and 2-propanol. Black-Right-Pointing-Pointer The measured data were reported as functions of composition of water + alcohol mixtures. Black-Right-Pointing-Pointer Enthalpy coefficients of pair-wise interactions have been analyzed in terms of McMillan-Mayer theory. Black-Right-Pointing-Pointer A comparative analysis of the characteristics of dissolution of L-phenylalanine and some other L-amino acids in the similar systems has been made. - Abstract: The enthalpies of L-phenylalanine dissolution in aqueous methanol, ethanol, 1-propanol and 2-propanol have been determined by calorimetry at 298.15 K and alcohol mole fractions up to x{sub 2} {approx}0.4. The standard enthalpies of solution {Delta}{sub sol}H Degree-Sign and transfer {Delta}{sub tr}H Degree-Sign from water to the mixed solvent as well as the enthalpy coefficients of L-phenylalanine-alcohol pair-wise interactions were calculated. The interrelation of the enthalpies of dissolution and transfer for L-phenylalanine with structural features of alcohols has been determined. A comparative analysis of the thermodynamic characteristics of dissolution of L-phenylalanine and some other amino acids (glycine, L-alanine, L-threonine and L-valine) in the mixtures studied has been made.

  4. Steric vs. electronic effects in the Lactobacillus brevis ADH-catalyzed bioreduction of ketones.

    Science.gov (United States)

    Rodríguez, Cristina; Borzęcka, Wioleta; Sattler, Johann H; Kroutil, Wolfgang; Lavandera, Iván; Gotor, Vicente

    2014-01-28

    Lactobacillus brevis ADH (LBADH) is an alcohol dehydrogenase that is commonly employed to reduce alkyl or aryl ketones usually bearing a methyl, an ethyl or a chloromethyl as a small ketone substituent to the corresponding (R)-alcohols. Herein we have tested a series of 24 acetophenone derivatives differing in their size and electronic properties for their reduction employing LBADH. After plotting the relative activity against the measured substrate volumes we observed that apart from the substrate size other effects must be responsible for the activity obtained. Compared to acetophenone (100% relative activity), other small substrates such as propiophenone, α,α,α-trifluoroacetophenone, α-hydroxyacetophenone, and benzoylacetonitrile had relative activities lower than 30%, while medium-sized ketones such as α-bromo-, α,α-dichloro-, and α,α-dibromoacetophenone presented relative activities between 70% and 550%. Moreover, the comparison between the enzymatic activity and the obtained final conversions using an excess or just 2.5 equiv. of the hydrogen donor 2-propanol, denoted again deviations between them. These data supported that these hydrogen transfer (HT) transformations are mainly thermodynamically controlled. For instance, bulky α-halogenated derivatives could be quantitatively reduced by LBADH even employing 2.5 equiv. of 2-propanol independently of their kinetic values. Finally, we found good correlations between the IR absorption band of the carbonyl groups and the degrees of conversion obtained in these HT processes, making this simple method a convenient tool to predict the success of these transformations.

  5. Thermodynamic properties of binary liquid mixtures of diethylenetriamine with alcohols at different temperatures

    Energy Technology Data Exchange (ETDEWEB)

    Dubey, Gyan Prakash, E-mail: gyan.dubey@rediffmail.com [Department of Chemistry, Kurukshetra University, Kurukshetra 136119 (India); Kumar, Krishan [Department of Chemistry, Kurukshetra University, Kurukshetra 136119 (India)

    2011-09-20

    Highlights: {yields} Thermodynamic study of diethylenetriamine + 2-methyl-1-propanol, +2-propanol or +1-butanol have been made. {yields} Excess molar volumes and isentropic compressibility were determined. {yields} Types of interactions were discussed based on derived properties. - Abstract: Densities, {rho}, viscosities, {eta}, and speeds of sound, u, were measured for the binary liquid mixtures containing diethylenetriamine with 2-methyl-1-propanol, 2-propanol and 1-butanol at 293.15, 298.15, 303.15, 308.15 and 313.15 K. From density and speed of sound data, excess molar volumes, V{sub m}{sup E} and deviations in isentropic compressibility, {Delta}{kappa}{sub s}, and speed of sound, {Delta}u have been evaluated. Viscosity data were used to compute deviations in viscosity and excess Gibbs energy of activation of viscous flow {Delta}G*{sup E} at 298.15, 303.15 and 308.15 K. A Redlich-Kister type equation was applied to fit the excess molar volumes and deviations in isentropic compressibility, speed of sound and viscosity data. The viscosity data have been correlated with the equations of Grunberg-Nissan, Tamura-Kurata, Heric-Brewer and of Hind et al. All the binary systems of the present study have negative values of excess molar volumes and deviations in isentropic compressibility over whole composition range and at all temperatures which indicates strong interactions between the components of binary mixtures.

  6. Electron beam induced synthesis of uranium dioxide nanoparticles: Effect of solvent composition

    Science.gov (United States)

    Rath, M. C.; Keny, S. J.; Naik, D. B.

    2016-09-01

    The effect of various compositions of solvents was investigated on the electron beam induced synthesis of uranium dioxide, UO2 nanoparticles. The synthesis was carried out at different pHs from 2 to 7 in the aqueous solutions containing 10 mM uranyl nitrate and 10% 2-propanol. The formation of UO2 nanoparticles was found to occur only in the pH range from 2.5 to 3.7. Experiments were also carried out in the aqueous solutions containing various other alcohols (10% v/v) such as methanol, ethanol, 1-propanol, 1-butanol or tert-butanol as well as in solutions containing 10 mM sodium formate at pH 3.4. The formation of UO2 nanoparticles in the aqueous solutions was found to occur only in the presence of ethanol, 1-propanol, 2-propanol or 1-butanol. It is therefore confirmed that the electron beam induced synthesis of UO2 nanoparticles strongly depends on the solvent compositions as well as the pH of the medium.

  7. Adsorption and Reaction of C1-C3 Alcohols over CeOx(111) Thin Films

    Energy Technology Data Exchange (ETDEWEB)

    D Mullins; S Senanayake; T Chen

    2011-12-31

    This study reports the interaction of methanol, ethanol, 1-propanol, and 2-propanol with well-ordered CeO{sub 2}(111) thin film surfaces. All of the alcohols adsorb at low temperature by forming alkoxy and hydroxyl species on the surface. On fully oxidized CeO{sub 2}(111), recombination occurs between some of the alkoxys and hydroxyls, resulting in alcohol desorption near 220 K. At the same temperature, some of the surface hydroxyls disproportionate to produce water and the loss of lattice O. The remaining alkoxys react above 550 K. The primary alcohols favor dehydrogenation products (aldehydes). There is a net loss of O from the system, resulting in a reduction of the ceria. The secondary alcohol, 2-propanol, undergoes primarily dehydration, producing propene with no net change in the cerium oxidation state. Reduced CeO{sub x}(111) competes with the gaseous products for available O. Little or no water is produced. The reaction selectivity for the C{sub 2} and C{sub 3} alcohols shifts toward favoring dehydration products. The loss of O from the alcohols leads to oxidation of the reduced ceria. Compared with the oxidized surface, the alkene desorption shifts to lower temperature, whereas the aldehyde desorption shifts to higher temperature. This indicates that, on the reduced surface, it is easier to break the C-O bond but more difficult to break the O-substrate bond.

  8. Synthesis of sup 18 F-labeled fluconazole and positron emission tomography studies in rabbits

    Energy Technology Data Exchange (ETDEWEB)

    Livni, E. (Massachusetts General Hospital, Boston, MA (United States). Dept. of Radiology); Fischman, A.J. (Massachusetts General Hospital, Boston, MA (United States). Radiology Dept. Havard Medical School, Boston, MA (United States). Dept. of Radiology Havard Medical School, Boston, MA (United States). Dept. of Medicine)

    1992-02-01

    (4-{sup 18}F) 2-(2,4-difluorophenyl)-1,3-bis(1H-1,2,4-triazol-1-yl)-2-propanol ((4-{sup 18}F) fluconazole) was synthesized from its amino precursor. Fieldel-Crafts acylation of 3-fluoroacetanilide with chloroacetyl chloride produced 2'-fluoro-4'-aceteamido-2-(1H-1,2,4-triazole-1-yl) acetophenone in 12% yield. Sequential reaction with (1) dimethylsulphoxonium methylide and (2) 1,2,4-triazole followed by in situ hydrolysis resulted in 2-(2-fluoro-4-aminophenyl)-1,3-bis(1H-2,2,4-triazol-1-yl)-2-propanol in 19% yield. A modified Schiemann reaction on this product resulted in (4-{sup 18}F)fluconazole with a radiochemical yield of 1.0-2.0% (EOS) within 2h. (4-{sup 18}F)Fluconazole was used to measure the pharmacokinetics of fluconazole in rats by measurement of radioactivity in excised tissues and in rabbits by PET. In both species, there was rapid equilibration of (4-{sup 18}F)fluoconazole to a relatively uniform distribution of radioactivity in most organs. (Author).

  9. Enhancement of percutaneous absorption of finasteride by cosolvents, cosurfactant and surfactants.

    Science.gov (United States)

    Javadzadeh, Yousef; Shokri, Javad; Hallaj-Nezhadi, Somayeh; Hamishehkar, Hamed; Nokhodchi, Ali

    2010-12-01

    The enhancing effects of routinely used co-solvents, propylene glycol and 2-propanol, anionic and cationic surfactants and a co-surfactant with different concentrations were evaluated on the skin permeation of Finasteride. In vitro permeation experiments with rat skin revealed that the solvent mixture is a very important factor in the penetration of Finasteride through the skin. Unexpectedly, cationic and anionic surfactants in various concentrations did not show any enhancement effect on drug transdermal absorption but co-surfactant Transcutol P increased skin penetration of Finastride significantly. Transcutol P with 0.25% and 1% showed the best enhancement in the initial and final sampling time, respectively. Transcutol P in a concentration of 0.25% increased skin absorption of the drug nearly 3.6 times in the first 15 min. The highest enhancement ratio (ER) was gained in the presence of 1% Transcutol P (ER = 5.98). In this study, among the different topical Finastride formulations, Transcutol P 1% in combination with water, propylene glycol and 2-propanol (30, 10, and 60) showed the highest enhancement ratio. PMID:19929166

  10. Impact of growth kinetics on morphology and pore structure of TiO2-one-pot synthesis of macroporous TiO2 microspheres.

    Science.gov (United States)

    Zhong, Ziyi; Chen, Fengxi; Ang, Thiam-Peng; Han, Yifan; Lim, Weiqiang; Gedanken, Aharon

    2006-06-12

    Titanium dioxide was synthesized by the hydrolysis of titanium tetraisopropoxide (TTIP) in the presence of acetic acid, 2-propanol, and organic amines (octylamine, aniline, and isobutylamine). H2O was supplied by an esterification reaction between acetic acid and 2-propanol (denoted as H2Oe), and/or by intentionally adding it (denoted as H2Oa). It was found that the quantity of H2Oa plays a crucial role in the morphology and porous structure of the final TiO2 product. Without the addition of H2Oa, 1D and porous TiO2 was synthesized. With the addition of H2Oa, and when the H2Oa:TiO2 molar ratio was in the range of 1:1 to 60:1, macroporous TiO2 microspheres possessing a large surface area and high thermal stability were obtained. When the H2Oa:TiO2 molar ratio exceeded 60:1, porous TiO2 with an irregular shape was formed. The variation in the morphology and porous structure is attributed to the manipulation of the growth kinetics by the addition of water. PMID:16749824

  11. Hydrophobic and hydrophilic interactions in aqueous mixtures of alcohols at a hydrophobic surface.

    Science.gov (United States)

    Ballal, Deepti; Chapman, Walter G

    2013-09-21

    Aqueous solutions of alcohols are interesting because of their anomalous behavior that is believed to be due to the molecular structuring of water and alcohol around each other in solution. The interfacial structuring and properties are significant for application in alcohol purification processes and biomolecular structure. Here we study aqueous mixtures of short alcohols (methanol, ethanol, 1-propanol, and 2-propanol) at a hydrophobic surface using interfacial statistical associating fluid theory which is a perturbation density functional theory. The addition of a small amount of alcohol decreases the interfacial tension of water drastically. This trend in interfacial tension can be explained by the structure of water and alcohol next to the surface. The hydrophobic group of an added alcohol preferentially goes to the surface preserving the structure of water in the bulk. For a given bulk alcohol concentration, water mixed with the different alcohols has different interfacial tensions with propanol having a lower interfacial tension than methanol and ethanol. 2-propanol is not as effective in decreasing the interfacial tension as 1-propanol because it partitions poorly to the surface due to its larger excluded volume. But for a given surface alcohol mole fraction, all the alcohol mixtures give similar values for interfacial tension. For separation of alcohol from water, methods that take advantage of the high surface mole fraction of alcohol have advantages compared to separation using the vapor in equilibrium with a water-alcohol liquid.

  12. A Study of the Solvation Structure of L-Leucine in Alcohol-Water Binary Solvents through Molecular Dynamics Simulations and FTIR and NMR Spectroscopy.

    Science.gov (United States)

    Takamuku, Toshiyuki; Hatomoto, Yohei; Tonegawa, Junko; Tsutsumi, Youichi; Umecky, Tatsuya

    2015-10-26

    The solvation structures of l-leucine (Leu) in aliphatic-alcohol-water and fluorinated-alcohol-water solvents are elucidated for various alcohol contents by using molecular dynamics (MD) simulations and IR, and (1) H and (13) C NMR spectroscopy. The aliphatic alcohols included methanol, ethanol, and 2-propanol, whereas the fluorinated alcohols were 2,2,2-trifluoroethanol and 1,1,1,3,3,3-hexafluoro-2-propanol. The MD results show that the hydrophobic alkyl moiety of Leu is surrounded by the alkyl or fluoroalkyl groups of the alcohol molecules. In particular, TFE and HFIP significantly solvate the alkyl group of Leu. IR spectra reveal that the Leu C-H stretching vibration blueshifts in fluorinated alcohol solutions with increasing alcohol content, whereas the vibration redshifts in aliphatic alcohol solutions. When the C-H stretching vibration blueshifts in the fluorinated alcohol solutions, the hydrogen and carbon atoms of the Leu alkyl group are magnetically shielded. Consequently, TFE and HFIP molecules may solvate the Leu alkyl group through the blue-shifting hydrogen bonds.

  13. Temperature-induced inversion of elution order in the chromatographic enantioseparation of 1,1'-bi-2-naphthol on an immobilized polysaccharide-based chiral stationary phase.

    Science.gov (United States)

    Yao, Bixia; Zhan, Fengping; Yu, Guangyan; Chen, Zhifen; Fan, Wenjing; Zeng, Xiongping; Zeng, Qingle; Weng, Wen

    2009-07-10

    In this work, the enantioseparations of 1,1'-bi-2-naphthol (BINOL) and its three derivatives were performed on an immobilized polysaccharide-based chiral stationary phase, Chiralpak IA, under normal-phase mode. The effects of the content of polar modifier in the mobile phase and the column temperature on the retention and enantioseparation were investigated in detail. Temperature-induced inversion of elution order for BINOL was observed directly when n-hexane/2-propanol (92/8, v/v) was used as mobile phase. The isoenantioselective temperature (T(iso)) was calculated to be 31.4 degrees C. When n-hexane/2-propanol/THF (93/2/5, v/v/v) was used as mobile phase, the T(iso) value decreased to -8.2 degrees C. Entropically driven enantioseparation which had practical application was obtained successfully (separation factor being 1.189 and 1.332 at 25 degrees C and 50 degrees C, respectively). The corresponding thermodynamic parameters for other three binaphthyl compounds were compared with that for BINOL. Some inferences about chiral recognition mechanism were stressed.

  14. In vitro study on the disinfectability of two split-septum needle-free connection devices using different disinfection procedures

    Directory of Open Access Journals (Sweden)

    Engelhart, Steffen

    2015-12-01

    Full Text Available This in vitro study investigated the external disinfection of two needle-free connection devices (NFC using Octeniderm (spraying and wiping technique vs. Descoderm pads (wiping technique. The split-septum membrane of the NFC was contaminated with >10 CFU . The efficacy of the disinfection at 30 sec. exposure time was controlled by taking a swab sample and by flushing the NFC with sterile 0.9% sodium chloride solution. Disinfection with octenidine dihydrochloride 0.1 g, 1-Propanol 30.0 g, and 2-Propanol 45.0 g in solution was highly effective (CFU reduction ≥4 log against both microorganisms, whereas the use of 63.1 g 2-Propanol in 100 ml solution led to residual contamination with . Our investigation underlines that (i in clinical practice disinfection of NFCs before use is mandatory, and that (ii details of disinfection technique are of utmost importance regarding their efficacy. Our investigation revealed no significant differences between both split-septum NFC types. Clinical studies are needed to confirm a possible superiority of disinfectants with long-lasting residual antimicrobial activity.

  15. Effect of morphology and solvent on two-photon absorption of nano zinc oxide

    Energy Technology Data Exchange (ETDEWEB)

    Kavitha, M.K. [Department of Chemistry, Indian Institute of Space Science and Technology, Valiamala, Thiruvananthapuram 695547, Kerala (India); Haripadmam, P.C.; Gopinath, Pramod; Krishnan, Bindu [Department of Physics, Indian Institute of Space Science and Technology, Valiamala, Thiruvananthapuram 695547, Kerala (India); John, Honey, E-mail: honey@iist.ac.in [Department of Chemistry, Indian Institute of Space Science and Technology, Valiamala, Thiruvananthapuram 695547, Kerala (India)

    2013-05-15

    Highlights: ► ZnO nanospheres and triangular structures synthesis by novel precipitation technique. ► The effect of precursor concentration on the size and shape of nano ZnO. ► Open aperture Z-scan measurements of the ZnO nanoparticle dispersions. ► Nanospheres exhibit higher two photon absorption coefficient than triangular nanostructures. ► Nanospheres dispersed in water exhibit higher two photon absorption coefficient than its dispersion in 2-propanol. - Abstract: In this paper, we report the effect of morphology and solvent on the two-photon absorption of nano zinc oxide. Zinc oxide nanoparticles in two different morphologies like nanospheres and triangular nanostructures are synthesized by novel precipitation technique and their two-photon absorption coefficient is measured using open aperture Z-scan technique. Experimental results show that the zinc oxide nanospheres exhibit higher two-photon absorption coefficient than the zinc oxide triangular nanostructures. The zinc oxide nanospheres dispersed in water exhibit higher two-photon absorption coefficient than that of its dispersion in 2-propanol. The zinc oxide nanospheres dispersed in water shows a decrease in two-photon absorption coefficient with an increase in on-axis irradiance. The result confirms the dependence of shape and solvent on the two-photon absorption of nano zinc oxide.

  16. Liquid-Phase Catalytic Transfer Hydrogenation of Furfural over Homogeneous Lewis Acid-Ru/C Catalysts.

    Science.gov (United States)

    Panagiotopoulou, Paraskevi; Martin, Nickolas; Vlachos, Dionisios G

    2015-06-22

    The catalytic performance of homogeneous Lewis acid catalysts and their interaction with Ru/C catalyst are studied in the catalytic transfer hydrogenation of furfural by using 2-propanol as a solvent and hydrogen donor. We find that Lewis acid catalysts hydrogenate the furfural to furfuryl alcohol, which is then etherified with 2-propanol. The catalytic activity is correlated with an empirical scale of Lewis acid strength and exhibits a volcano behavior. Lanthanides are the most active, with DyCl3 giving complete furfural conversion and a 97 % yield of furfuryl alcohol at 180 °C after 3 h. The combination of Lewis acid and Ru/C catalysts results in synergy for the stronger Lewis acid catalysts, with a significant increase in the furfural conversion and methyl furan yield. Optimum results are obtained by using Ru/C combined with VCl3 , AlCl3 , SnCl4 , YbCl3 , and RuCl3 . Our results indicate that the combination of Lewis acid/metal catalysts is a general strategy for performing tandem reactions in the upgrade of furans.

  17. Construction of heterologous gene expression cassettes for the development of recombinant Clostridium beijerinckii.

    Science.gov (United States)

    Oh, Young Hoon; Eom, Gyeong Tae; Kang, Kyoung Hee; Joo, Jeong Chan; Jang, Young-Ah; Choi, Jae Woo; Song, Bong Keun; Lee, Seung Hwan; Park, Si Jae

    2016-04-01

    Gene-expression cassettes for the construction of recombinant Clostridium beijerinckii were developed as potential tools for metabolic engineering of C. beijerinckii. Gene expression cassettes containing ColE1 origin and pAMB origin along with the erythromycin resistance gene were constructed, in which promoters from Escherichia coli, Lactococcus lactis, Ralstonia eutropha, C. acetobutylicum, and C. beijerinckii are examined as potential promoters in C. beijerinckii. Zymogram analysis of the cell extracts and comparison of lipase activities of the recombinant C. beijerinckii strains expressing Pseudomonas fluorescens tliA gene suggested that the tliA gene was functionally expressed by all the examined promoters with different expression level. Also, recombinant C. beijerinckii expressing C. beijerinckii secondary alcohol dehydrogenase by the constructed expression cassettes successfully produced 2-propanol from glucose. The best promoter for TliA expression was the R. eutropha phaP promoter while that for 2-propanol production was the putative C. beijerinckii pta promoter. Gene expression cassettes developed in this study may be useful tools for the construction of recombinant C. beijerinckii strains as host strains for the valuable chemicals and fuels from renewable resources. PMID:26780375

  18. OPTIMIZING OF TIO2 SEPARATION FROM BANGKA ILMENITE BY LEACHING PROCESS USING HCL

    Directory of Open Access Journals (Sweden)

    Sayekti Wahyuningsih

    2016-09-01

    Full Text Available Separation of titanium dioxide (TiO2 from ilmenite Bangka has been done byleaching processusing HCl. Before the leaching process, ilmenite was roastedat 900oC for pre-oxidation (preliminary - oxidation. Leaching process carried out by variation of HCl concentration and Fe0 reducing agents. While the re-deposition of dissolved Ti4+ ion achieved by hydrolysis - condensation using 2-propanol-H2O solvents. Leaching the pre-oxidazed ilmenite shows the phase change of pseudobrokite (Fe2TiO5 into hematite (Fe2O3 and synthetic rutile (TiO2. Formation of the synthetic rutile was characterized by the loss of intensity of Fe2TiO5 at 26.65º and the increasing intensity of rutile TiO2 at 27.49º.The dissolution rate of both titanium and iron was found to be increased, generally, by increasing acid concentration in case of HCl as well as by increasing ilmenite: Fe0 ratio. Precipitation of the dissolved titania with 2-propanol -H2Oof 8:2(v /v produced anatase TiO2 due to the hydrolysis and condensation of Ti-tetra isopropoxide complexes.

  19. Contribution of Liver Alcohol Dehydrogenase to Metabolism of Alcohols in Rats

    Science.gov (United States)

    Plapp, Bryce V.; Leidal, Kevin G.; Murch, Bruce P.; Green, David W.

    2015-01-01

    The kinetics of oxidation of various alcohols by purified rat liver alcohol dehydrogenase (ADH) were compared with the kinetics of elimination of the alcohols in rats in order to investigate the roles of ADH and other factors that contribute to the rates of metabolism of alcohols. Primary alcohols (ethanol, 1-propanol, 1-butanol, 2-methyl-1-propanol, 3-methyl-1-butanol) and diols (1,3-propanediol, 1,3-butanediol, 1,4-butanediol, 1,5-pentanediol) were eliminated in rats with zero-order kinetics at doses of 5–20 mmole/kg. Ethanol was eliminated most rapidly, at 7.9 mmole/kg•h. Secondary alcohols (2-propanol-d7, 2-propanol, 2-butanol, 3-pentanol, cyclopentanol, cyclohexanol) were eliminated with first order kinetics at doses of 5–10 mmole/kg, and the corresponding ketones were formed and slowly eliminated with zero or first order kinetics. The rates of elimination of various alcohols were inhibited on average 73% (55% for 2-propanol to 90% for ethanol) by 1 mmole/kg of 4-methylpyrazole, a good inhibitor of ADH, indicating a major role for ADH in the metabolism of the alcohols. The Michaelis kinetic constants from in vitro studies (pH 7.3, 37 °C) with isolated rat liver enzyme were used to calculate the expected relative rates of metabolism in rats. The rates of elimination generally increased with increased activity of ADH, but a maximum rate of 6 ± 1 mmole/kg•h was observed for the best substrates, suggesting that ADH activity is not solely rate-limiting. Because secondary alcohols only require one NAD+ for the conversion to ketones whereas primary alcohols require two equivalents of NAD+ for oxidation to the carboxylic acids, it appears that the rate of oxidation of NADH to NAD+ is not a major limiting factor for metabolism of these alcohols, but the rate-limiting factors are yet to be identified. PMID:25641189

  20. Research Update: A hafnium-based metal-organic framework as a catalyst for regioselective ring-opening of epoxides with a mild hydride source

    International Nuclear Information System (INIS)

    Reaction of styrene oxide with sodium cyanoborohydride and a catalytic amount of Hf-NU-1000 yields the anti-Markovnikov product, 2-phenylethanol, with over 98% regioselectivity. On the other hand, propylene oxide is ring opened in a Markovnikov fashion to form 2-propanol with 95% regioselectivity. Both styrene oxide and propylene oxide failed to react with sodium cyanoborohydride without the addition of Hf-NU-1000 indicative of the crucial role of Hf-NU-1000 as a catalyst in this reaction. To the best of our knowledge, this is the first report of the use of a metal-organic framework material as a catalyst for ring-opening of epoxides with hydrides

  1. Thermodynamic Modeling of Several Aqueous Alkanol Solutions Containing Amino Acids with the Perturbed-Chain Statistical Associated Fluid Theory Equation of State

    DEFF Research Database (Denmark)

    Ferreira, Luisa; Breil, Martin Peter; Pinho, S. P.;

    2009-01-01

    The perturbed-chain statistical associated fluid theory EoS was applied to model the solubilities of glycine, DL-alanine, L-serine, L-threonine, and L-isoleucine in pure water, pure alcohols (ethanol, I-propanol, and 2-propanol) and in mixed solvent systems. Three pure component nonassociating...... parameters for the amino acids were fitted to the densities, activity and osmotic coefficients, vapor pressures, and water activity of their aqueous solutions. The solubilities of amino acids in pure and mixed solvent systems were calculated on the basis of the phase equilibrium conditions for a pure solid...... and a fluid phase. The hypothetical melting properties of each amino acid were fitted, to accurately correlate the solubilities in pure water. Only one temperature independent binary parameter is required for each amino acid/solvent pair. The model can accurately describe the solubility of the amino acids...

  2. Direct high-performance liquid chromatographic separation of the enantiomers of an aromatic amine and four aminoalcohols using polysaccharide chiral stationary phases and acidic additive.

    Science.gov (United States)

    Caccamese, Salvatore; Bianca, Salvatore; Carter, Guy T

    2007-08-01

    The HPLC enantiomeric separation of N-benzyl-alpha-methyl-benzylamine, phenylalaninol, tryptophanol, 2 (diphenylhydroxymethyl)pyrrolidine, and isoproterenol was accomplished in the normal-phase mode using two polysaccharide-derived chiral stationary phases (CSPs) and various n-hexane/2-propanol mobile phases with acidic (TFA) or basic (DEA) additive. The compounds were separated without any derivatization and separation factor range between 2.09 and 1.09 with resolution factor 3.4 and 0.4, respectively. The best separation of the enantiomers of the amine was achieved on amylose tris (3, 5-dimethylphenylcarbamate) CSP with TFA additive in the mobile phase; in acidic conditions, instead, the best enantioseparation of the aminoalcohols was achieved on cellulose tris (3, 5-dimethylphenilcarbamate). A long equilibration time of the CSP when switching from an undoped mobile phase to a doped one is required to obtain reproducible results. PMID:17568428

  3. Effect of temperature on the enthalpies of formation of water- o-xylene-Triton X-100 microemulsions

    Science.gov (United States)

    Batov, D. V.; Kartsev, V. N.; Shtykov, S. N.

    2013-03-01

    Enthalpies of solution for water- o-xylene-Triton X-100 (TX-100) microemulsions and their components in 2-propanol are determined thermochemically at 288.15, 298.15, and 313.15 K. Enthalpies of formation for the microemulsions are calculated using a thermochemical cycle. It is shown that the enthalpies of formation are negative and fall in moving from water/oil microemulsions to oil/water microemulsions. The obtained data show that strong molecular interactions between components in the investigated systems favor the formation of thermodynamically stable microemulsions. It is concluded that the spontaneous formation of the microemulsions can be due to both the entropy and enthalpy contributions to the change in free energy.

  4. LET and dose rate effect on radiation-induced copolymerization in physical gel

    Energy Technology Data Exchange (ETDEWEB)

    Nakagawa, Seiko, E-mail: Nakagawa.Seiko@iri-tokyo.jp [Tokyo Metropolitan Industrial Technology Research Institute, 2-4-10 Aomi, Koto-ku, Tokyo 135-0064 (Japan); Taguchi, Mitsumasa; Kimura, Atsushi; Nagasawa, Naotsugu; Hiroki, Akihiro [Environmental Radiation Processing Group, Environment and Industrial Materials Research Division, Quantum Beam Science Directorate, Japan Atomic Energy Agency, 1233 Watanuki, Takasaki, Gunma 370-1292 (Japan)

    2014-09-01

    Highlights: •LET and dose rate effect on polymerization in gel was almost the same as in solution. •The ratio of the dose rate effect in the gel was higher than that in solution. •The initiation and termination processes show the difference on the dose rate effect. -- Abstract: N{sub 2}-saturated 2-propanol solutions containing styrene and maleimide were gelled by the addition of hydroxypropylcellulose and irradiated by proton, He and C-ion beams. The trend in the dose rate and LET effects on the yield and molecular weight distribution of the polymer produced in the gel was almost the same in the solution. On the contrary, the dose rate effect in the gel was higher than that in the solution. This effect was accelerated for irradiations by proton as well as heavier ion with a higher LET value.

  5. Extruded expanded polystyrene sheets coated by TiO2 as new photocatalytic materials for foodstuffs packaging

    Science.gov (United States)

    Loddo, V.; Marcì, G.; Palmisano, G.; Yurdakal, S.; Brazzoli, M.; Garavaglia, L.; Palmisano, L.

    2012-11-01

    Nanostructured, photoactive anatase TiO2 sol prepared under very mild conditions using titanium tetraisopropoxide as the precursor is used to functionalise extruded expanded polystyrene (XPS) sheets by spray-coating resulting in stable and active materials functionalised by TiO2 nanoparticles. Photocatalytic tests of these sheets performed in a batch reactor in gas-solid system under UV irradiation show their successful activity in degrading probe molecules (2-propanol, trimethylamine and ethene). Raman spectra ensure the deposition of TiO2 as crystalline anatase phase on the polymer surface. The presence of TiO2 with respect to polymer surface can be observed in SEM images coupled to EDAX mapping allowing to monitor the surface morphology and the distribution of TiO2 particles. Finally thermoforming of these sheets in industrial standard equipment leads to useful containers for foodstuffs.

  6. Design and synthesis of novel triazole antifungal derivatives based on the active site of fungal lanosterol 14a-demethylase (CYP51)

    Institute of Scientific and Technical Information of China (English)

    Zhi Gang Dan; Jun Zhang; Shi Chong Yu; Hong Gang Hu; Xiao Yun Chai; Qing Yan Sun; Qiu Ye Wu

    2009-01-01

    A series of 1-(1H-1,2,4-triazole-1-yl)-2-(2,4-difluorophenyl)-3-(N-isoproyl-N-substituted-amino)-2-propanols have been designed and synthesized on the basis of the active site of lanosterol 14a-demethylase (CYP51). Their structures were confirmed by MS and 1H NMR. In vitro antifungal activities of these synthesized compounds were evaluated against eight human pathogenic fungi. The results showed that all title compounds exhibited activity against fungi tested to some extent. Compounds 3c, 3d, 7a, 7b and 7c exhibited more potent antifungal activities against nearly all fungi tested except Aspergillus fumigatus than fluconazole.

  7. Stability of ZnO quantum dots tuned by controlled addition of ethylene glycol during their growth

    Science.gov (United States)

    Zimmermann, Lizandra M.; Baldissera, Paulo V.; Bechtold, Ivan H.

    2016-07-01

    ZnO quantum dots were prepared via a sol–gel route from zinc acetate and sodium hydroxide. The influence of ethylene glycol addition during the first stages of reaction (1–5 min) as a stabilizer, as well as the influence of its concentration in 2-propanol were investigated. The optimization led to particles with enough stability and homogeneity around 3.7 nm of diameter to allow for quantum confinement effect. Spectroscopic UV–vis absorption measurements allowed to explore the underlying mechanism of nucleation and growth and to have the control of it. The emission of the ZnO nanoparticles was explored under experimental perturbations with addition of small amounts of water to investigate the interplay between surface defects and the excitonic effect. The results suggest that the water interferes directly on the defects first and later on the excitonic recombination. Their morphology was determined with transmission electron microscopy.

  8. Catalytic activity of carbon nanotubes in the conversion of aliphatic alcohols

    Science.gov (United States)

    Zhitnev, Yu. N.; Tveritinova, E. A.; Chernyak, S. A.; Savilov, S. V.; Lunin, V. V.

    2016-06-01

    Carbon nanotubes (CNTs) obtained via the catalytic pyrolysis of hexane at 750°C were studied as the catalysts in conversion of C2-C4 alcohols. The efficiency of CNTs as catalysts in dehydration and dehydrogenation of ethanol, 1-propanol, 2-propanol, 1-butanol, 2-butanol, and tert-butanol was studied by means of pulse microcatalysis. The surface and structural characteristics of CNTs are investigated via SEM, TEM, DTA, BET, and XPS. CNTs are shown to be effective catalysts in the conversion of alcohols and do not require additional oxidative treatment. The regularities of the conversion of aliphatic alcohols, related to the properties of the CNTs surface and the structure of the alcohols are identified.

  9. Enantiomeric resolution of p-toluenesulfonate of valine benzyl ester by preferential crystallizaion.

    Science.gov (United States)

    Munegumi, Toratane; Wakatsuki, Aiko; Takahashi, Yutaro

    2012-02-01

    Preferential crystallization of amino acid derivatives by seeding a pure enantiomer into racemic amino acid solutions has been studied for many years. However, few examples of valine derivatives have been reported so far. Although there have been some reports using valine hydrogen chloride with preferential crystallization, it is difficult to obtain optical isomers for valine derivatives using preferential crystallization. In this study, repeated preferential crystallization of p-toluenesulfonate valine benzyl ester with a 20% e.e. in 2-propanol gave a 94% e.e. on sonication. Sonication accelerated crystallization rate, but there was not a big difference in e.e. between with and without sonication. However, this research demonstrates the first preferential crystallization of p-toluenesulfonate of valine benzyl esters with an acceleration of crystallization using sonication.

  10. "Phase diagrams of Lecithin-based microemulsions containing Sodium Salicylate "

    Directory of Open Access Journals (Sweden)

    "Aboofazeli R

    2000-08-01

    Full Text Available Partial phase diagrams were constructed at 25°C to investigate the phase behaviour of systems composed of soybean lecithin, water, sodium salicylate, alcohol and isopropyl myristate. The lecithins used were the commercially available soy bean lecithins, namely E200 and E170 (phosphatidyl choline purities greater than 95% and 68-72% respectively. The cosurfactants employed were n-propanol, 2-propanol and n-butanol and these were used at lecithin/alcohol weight ratios (Km of 1:1 and 1.5:1. At a given Km, the aqueous phase consisted of a 2% w/w sodium salicylate solution. Phase diagrams showed the area of existence of a stable isotropic region along the surfactant/oil axis (i.e., reverse microemulsion area. The extension of the microemulsion domain was influenced by the purity of surfactant, the lecithin/alcohol weight ratios and the kind of the alcohol.

  11. Radiosynthesis of a chloroacetanilide herbicide ([phenyl-4-3 H] acetochlor) and a dichloroacetamide safener for herbicides [2,2-dimethyl-3 H]R-29148

    International Nuclear Information System (INIS)

    2-Chloro-N-(ethoxymethyl)-N-(2-ethyl-6-methylphenyl) acetamide (the chloroacetanilide herbicide acetochlor) and 3-(dichloroacetyl)-2,2,5-trimethyl-1, 3-oxazolidine (the dichloroacetamide safener R-29148) are required at high specific activity for studies on their metabolism and mode of action. [phenyl-4-3H]Acetochlor was obtained at 22 Ci/mmol in 71% yield by reductive dehalogenation of iodoacetochlor with tritium gas in ethanol in the presence of palladium on carbon and triethylamine. [2,2-dimethyl-3H]R-29148 was prepared at 15 Ci/mmol by treating acetone and 1-amino-2-propanol in pentane with two equivalents of NaOH in tritiated water (i.e. hydroxide ion-catalyzed enolization of acetone) followed by dichloroacetyl chloride. (Author)

  12. Thermodynamic properties of binary mixtures containing dimethyl carbonate+2-alkanol: Experimental data, correlation and prediction by ERAS model and cubic EOS

    Energy Technology Data Exchange (ETDEWEB)

    Almasi, Mohammad, E-mail: m.almasi@khouzestan.srbiau.ac.ir [Department of Chemistry, Science and Research Branch, Islamic Azad University, Khouzestan (Iran, Islamic Republic of)

    2013-03-01

    Densities and viscosities for binary mixtures of dimethyl carbonate with 2-propanol up to 2-heptanol were measured at various temperatures and ambient pressure. From experimental data, excess molar volumes, V{sub m}{sup E}. were calculated and correlated by the Redlich–Kister equation to obtain the binary coefficients and the standard deviations. Excess molar volumes, V{sub m}{sup E}, are positive for all studied mixtures over the entire range of the mole fraction. The ERAS-model has been applied for describing the binary excess molar volumes and also Peng–Robinson–Stryjek–Vera (PRSV) equation of state (EOS) has been used to predict the binary excess molar volumes and viscosities. Also several semi-empirical models were used to correlate the viscosity of binary mixtures.

  13. Derived thermodynamic properties of alcohol + cyclohexylamine mixtures

    Directory of Open Access Journals (Sweden)

    IVONA R. RADOVIĆ

    2010-02-01

    Full Text Available Thermal expansion coefficients, α, excess thermal expansion coefficients, αE, isothermal coefficients of pressure excess molar enthalpy, (∂HE/∂pT,x, partial molar volumes, , partial molar volumes at infinite dilution, , partial excess molar volumes, , and partial excess molar volumes at infinite dilution, , were calculated using experimental densities and excess molar volumes, , data. All calculations are performed for the binary systems of cyclohexylamine with 1-propanol or 1-butanol or 2-butanol or 2-methyl-2-propanol. The Redlich–Kister polynomial and the reduced excess molar volume approach were used in the evaluation of these properties. In addition, the aim of this investigation was to provide a set of various volumetric data in order to asses the influence of temperature, chain length and position of hydroxyl group in the alcohol molecule on the molecular interactions in the examined binary mixtures.

  14. Liquid-liquid extraction and adsorption on solid surfaces applied to used lubricant oils recovery

    Directory of Open Access Journals (Sweden)

    J. L. Assunção Filho

    2010-12-01

    Full Text Available In this work, the recovery of base oils from waste lubricants following the steps of solvent extraction, adsorption on solids and solvent removal by evaporation was evaluated. In the step of solvent extraction, the most efficient was 1-butanol, followed by tert-butanol, 2-propanol and ethanol; for the step of adsorption, activated carbon was the most effective solid for PAH removal, confirming the similarity of these compounds with petroleum aromatic fractions. Thus, the optimum solvent-adsorbent pair for the recovery of used lubricant oils through the proposed methodology was 1-butanol/activated carbon. At the end of the process, it was possible to establish a set of steps that permit the recovery of lubricant base oils with lower content of contaminants.

  15. Nitrogen-doped titanium dioxide photocatalysts for visible response prepared by using organic compounds

    Directory of Open Access Journals (Sweden)

    Yoshio Nosaka, Masami Matsushita, Junichi Nishino and Atsuko Y. Nosaka

    2005-01-01

    Full Text Available In order to utilize visible light in photocatalytic reactions, nitrogen atoms were doped in commercially available photocatalytic TiO2 powders by using an organic compound such as urea and guanidine. Analysis by X-ray photoelectron spectroscopy (XPS indicated that N atoms were incorporated into two different sites of the bulk phase of TiO2. A significant shift of the absorption edge to a lower energy and a higher absorption in the visible light region were observed. These N-doped TiO2 powders exhibited photocatalytic activity for the decomposition of 2-propanol in aqueous solution under visible light irradiation. The photocatalytic activity increased with the decrease of doped N atoms in O site, while decreased with decrease of the other sites. Degradation of photocatalytic activity based on the release of nitrogen atoms was observed for the reaction in the aqueous suspension system.

  16. Pharmacokinetic study of inosiplex tablets in healthy Chinese volunteers by hyphenated HPLC and tandem MS techniques

    Institute of Scientific and Technical Information of China (English)

    Mo Chen; Yuan Zhang; Xiao-Ting Que; Ya Ding; Lin Yang; Ai-Dong Wen; Tai-Jun Hang

    2013-01-01

    Inosiplex is a compound formulation composed of inosine and p-acetaminobenzoic acid (PABA) salt of N,N-dimethylamino-2-propanol (DIP). This study was to investigate the clinical plasma pharmacokinetic properties of DIP and PABA after single and multiple oral doses of inosiplex tablets in healthy Chinese volunteers. The established LC/MS/MS method for plasma DIP determination had a linear range of 0.02-10 mg/mL, and the HPLC method for plasma PABA determination had a linear range of 0.05-40 mg/mL. Linear pharmacokinetic characteristics were found with single oral doses of 0.5, 1.0 and 2.0 g. No obvious accumulation effects were observed for DIP and PABA.

  17. Preparation and Catalytic Properties of Polymer Supported Dendritic Metal Complex

    Institute of Scientific and Technical Information of China (English)

    LI Cui-ling; YANG Zhi-wang; KANG Qiao-xiang; MA Heng-chang; MA Xiao-peng; GAO Qi-kuan; GUO Zhen; LEI Zi-qiang

    2004-01-01

    Polymer supported materials are extensively used as oxidizing agent, reducing agent catalysts, photosensitizers ion exchange resins and agriculturally and pharmacologically active agents1. The application of polymer metal complexes has been widely investigated2. The polymer supported complex undergoes swelling in a suitable solvent medium and provides enough surface area in carrying out electron transfer reactions, which clearly emphasizes the influence of a polymer network in heterogeneous catalysis.In the present, we have succeeded in the grafting of "dendrimer-like" hyperbranched polymer onto the surface of chloromethyl polystyrene reactions.All the catalysts show promising catalytic activities for the oxidation of iso-propylbenzene in the mild reaction condition, in each case, hypnone 1, 2-phenyl-2-propanol 2 were obtained as the major products

  18. Dynamics of water and solute transport in polymeric reverse osmosis membranes via molecular dynamics simulations

    CERN Document Server

    Shen, Meng; Lueptow, Richard M

    2016-01-01

    The Angstrom-scale transport characteristics of water and six different solutes, methanol, ethanol, 2-propanol, urea, Na+, and Cl-, were studied for a polyamide reverse osmosis (RO) membrane, FT-30, using non-equilibrium molecular dynamics (NEMD) simulations. Results indicate that water transport increases with an increasing fraction of connected percolated free volume, or water-accessible open space, in the membrane polymer structure. This free volume is enhanced by the dynamic structure of the membrane at the molecular level as it swells when hydrated and vibrates due to molecular collisions allowing a continuous path connecting the opposite membrane surfaces. The tortuous paths available for transport of solutes result in Brownian motion of solute molecules and hopping from pore to pore as they pass through the polymer network structure of the membrane. The transport of alcohol solutes decreases for solutes with larger Van der Waals volume, which corresponds to less available percolated free volume, or sol...

  19. Degradation and miscibility of poly(DL-lactic acid)/poly(glycolic acid) composite films: Effect of poly(DL-lactic-co-glycolic acid)

    Indian Academy of Sciences (India)

    Zhigang Ma; Na Zhao; Chengdong Xiong

    2012-08-01

    The in vitro degradation behaviour of poly(glycolic acid) (PGA) and its composite films containing poly(DL-lactic acid) (PDLLA) and poly(DL-lactic-co-glycolic acid) (PDLGA) were investigated via mass loss, scanning electron microscopy (SEM) and differential scanning calorimetry (DSC). All the films were prepared by solution casting, using 1,1,1,3,3,3-hexafluoro-2-propanol (HFIP) as the solvent. Since the degradation rate of PDLLA is lower than that of PGA, those of the PDLLA/PGA composite films decreased. As a compatibilizer, PDLGA improved the compatibility and hydrolytic stability of PDLLA/PGA composite films. Changes in the composite films indicate that this kind of PGA-based composite biomaterial may be applicable to device design for clinical application in the future.

  20. Design, synthesis, and antifungal activities of novel triazole derivatives containing the benzyl group

    Directory of Open Access Journals (Sweden)

    Xu K

    2015-03-01

    Full Text Available Kehan Xu,1,* Lei Huang,1,* Zheng Xu,2 Yanwei Wang,1,3 Guojing Bai,1 Qiuye Wu,1 Xiaoyan Wang,1 Shichong Yu,1 Yuanying Jiang1 1School of Pharmacy, Second Military Medical University, Shanghai, 2Shanghai Changzheng Hospital, Second Military Medical University, Shanghai, 3Number 422 Hospital of PLA, Zhanjiang, People’s Republic of China *These authors contributed equally to this work Abstract: In previous studies undertaken by our group, a series of 1-(1H-1,2,4-triazole-1-yl-2-(2,4-difluorophenyl-3-substituted-2-propanols (1a–r, which were analogs of fluconazole, was designed and synthesized by click chemistry. In the study reported here, the in vitro antifungal activities of all the target compounds were evaluated against eight human pathogenic fungi. Compounds 1a, 1q, and 1r showed the more antifungal activity than the others. Keywords: triazole, synthesis, antifungal activity, CYP51

  1. Simple Synthesis of Sakuranetin and Selinone via a Common Intermediate, Utilizing Complementary Regioselectivity in the Deacetylation of Naringenin Triacetate.

    Science.gov (United States)

    Yamashita, Yasunobu; Hanaya, Kengo; Shoji, Mitsuru; Sugai, Takeshi

    2016-01-01

    Sakuranetin and selinone were successfully synthesized utilizing the regioselective deacetylation of naringenin triacetate. Deacetylation of the latter at C-7 with imidazole in 1,4-dioxane at 40°C furnished the corresponding diacetate in 80% yield. Methylation of the obtained free hydroxy group and subsequent removal of the remaining two acetyl groups gave sakuranetin, which was previously isolated as a phytoalexin against rice blast disease fungus, Pyricularia oryzae, in 71% overall yield. The same intermediate, naringenin triacetate, was subjected to transesterification with 2-propanol in tetrahydrofuran, catalyzed by Candida antarctica lipase B. A contrasting regioselective preference for C-4' deacetylation was observed, giving an isomeric diacetate in 82% yield. Prenylation of the free hydroxy group under Mitsunobu conditions and subsequent deprotection furnished selinone, which was previously isolated from Monotes engleri and exhibits antifungal activity against Candida albicans, in 55% overall yield. PMID:27373654

  2. Correlation and prediction of thermodynamic properties of binary mixtures from perturbed chain statistical associating fluid theory

    Science.gov (United States)

    Almasi, Mohammad

    2014-11-01

    Densities and viscosities for binary mixtures of Diethanolamine (DEA) + 2 alkanol (2 propanol up to 2 pentanol) were measured over the entire composition range and temperature interval of 293.15-323.15 K. From the density and viscosity data, values of various properties such as isobaric thermal expansibility, excess isobaric thermal expansibility, partial molar volumes, excess molar volumes and viscosity deviations were calculated. The observed variations of these parameters, with alkanols chain length and temperature, are discussed in terms of the intermolecular interactions between the unlike molecules of the binary mixtures. The ability of the perturbed chain statistical associating fluid theory (PC-SAFT) to correlate accurately the volumetric behavior of the binary mixtures is demonstrated.

  3. Successive cycles of utilization of novozym 435 in three different reaction systems

    Energy Technology Data Exchange (ETDEWEB)

    Lerin, L.; Oestreicher, E. G. [Universidade Federal do Rio de Janeiro (IQ/UFRJ), RJ (Brazil). Inst. de Quimica; Ceni, G.; Richett, A.; Kubiak, G.; Oliveira, J. Vladimir; Toniazzo, G.; Treichel, H.; Oliveira, D., E-mail: helen@uricer.ed [Universidade Regional Integrada do Alto Uruguai e das Missoes (URI), Erechim, RS (Brazil)

    2011-04-15

    The main focus of this work was to investigate the residual esterification activity and the product conversion after 10 successive cycles of utilization of a commercial lipase in three systems: esterification of 2-ethyl hexanol and palmitic acid in a solvent-free system; esterification of ascorbic acid and palmitic acid in tert-butanol; and transesterification of glycerol and methyl benzoate in 2-propanol. These systems were chosen based on previous results by our research group in terms of product conversion. Before scale-up, there is a need for evaluating several cycles of utilization of the biocatalyst. The esterification of 2-ethyl hexanol showed that after 10 cycles the enzyme retained 90% of its activity. The system consisting of ascorbic acid, palmitic acid, Novozym 435 and tert-butanol showed that a reduction in enzyme activity was accompanied by a reduction in reaction conversion; the same behavior was not observed for the third system. (author)

  4. Research Update: A hafnium-based metal-organic framework as a catalyst for regioselective ring-opening of epoxides with a mild hydride source

    Science.gov (United States)

    Stephenson, Casey J.; Hassan Beyzavi, M.; Klet, Rachel C.; Hupp, Joseph T.; Farha, Omar K.

    2014-12-01

    Reaction of styrene oxide with sodium cyanoborohydride and a catalytic amount of Hf-NU-1000 yields the anti-Markovnikov product, 2-phenylethanol, with over 98% regioselectivity. On the other hand, propylene oxide is ring opened in a Markovnikov fashion to form 2-propanol with 95% regioselectivity. Both styrene oxide and propylene oxide failed to react with sodium cyanoborohydride without the addition of Hf-NU-1000 indicative of the crucial role of Hf-NU-1000 as a catalyst in this reaction. To the best of our knowledge, this is the first report of the use of a metal-organic framework material as a catalyst for ring-opening of epoxides with hydrides.

  5. X-Ray structure and cytotoxic activity of a picolinate ruthenium(II–arene complex

    Directory of Open Access Journals (Sweden)

    IVANKA IVANOVIĆ

    2011-01-01

    Full Text Available A ruthenium(II–arene complex with picolinic acid, [(η6-p-cymeneRuCl(pico]∙H2O, was prepared by the reaction of [(η6-p-cymeneRuCl2]2 with picolinic acid in a 1:2 molar ratio in 2-propanol. The compound was characterized by elemental analysis, and IR and NMR spectroscopy. X-ray diffraction analysis showed that the molecule adopts a “three-leg piano-stool” geometry, which is common for this type of complexes. The cytotoxic activity of the complex was tested in two human cancer cell lines HeLa (cervix and FemX (melanoma by MTT assay. The IC50 values were at 82.0 and 36.2 µmol dm-3 for HeLa and FemX cells, respectively.

  6. Enantioselective and diastereoselective separation of synthetic pyrethroid insecticides on a novel chiral stationary phase by high-performance liquid chromatography.

    Science.gov (United States)

    Tan, Xulin; Hou, Shicong; Wang, Min

    2007-07-01

    A novel chiral packing material for high-performance liquid chromatography (HPLC) was prepared by connecting (R)-1-phenyl-2-(4-methylphenyl) ethylamine (PTE) amide derivative of (S)-isoleucine to aminopropyl silica gel through 2-amino-3,5-dinitro-1-carboxamido-benzene unit. This chiral stationary phase was applied to the enantioselective and diastereoselective separation of five pyrethroid insecticides by HPLC under normal phase condition. To achieve satisfactory baseline separation an optimization of the variables of mobile phase composition was required. The two enantiomers of fenpropathrin and four stereoisomers of fenvalerate were baseline separated using hexane-1,2-dichloroethane-2-propanol as mobile phase. The results show that the enantioselectivity of CSP is better than Pirkle type 1-A column for these compounds. Only partial separations for the cypermethrin and cyfluthrin stereoisomers were observed. Seven peaks and eight peaks were observed for cypermethrin and cyfluthrin, respectively. The elution orders were assigned by using different stereoisomer-enriched products.

  7. Development of carborane synthons: Synthesis and chemistry of (aminoalkyl)carboranes

    International Nuclear Information System (INIS)

    A number of (aminoalkyl)-1,2-closo-dodecaboranes have been synthesized to provide carboranes with a functional group for covalent incorporation into structures of potential use in the treatment of cancer by boron neutron capture therapy (BNCT). (Phthalimidoalkyl)acetylenes reacted with decaborane to give the corresponding carboranes; removal of the phthalimido group under mild conditions using sodium borohydride in 2-propanol furnished the (aminoalkyl)carboranes which were isolated as their hydrochloride salts. An alternative approach involved the conversion of an (iodoalkyl)- or a ((tosyloxy)alkyl)carborane to the azido derivative which gave the amine on hydrogenation. An effective way of attaching a carborane moiety to thiouracil, which is selectively taken up in melanoma cells, is illustrated by the acylation of two of these amines with thiouracil-5-carboxylic acid

  8. Thermodynamic properties of binary mixtures containing dimethyl carbonate+2-alkanol: Experimental data, correlation and prediction by ERAS model and cubic EOS

    Science.gov (United States)

    Almasi, Mohammad

    2013-03-01

    Densities and viscosities for binary mixtures of dimethyl carbonate with 2-propanol up to 2-heptanol were measured at various temperatures and ambient pressure. From experimental data, excess molar volumes, VmE. were calculated and correlated by the Redlich-Kister equation to obtain the binary coefficients and the standard deviations. Excess molar volumes, VmE, are positive for all studied mixtures over the entire range of the mole fraction. The ERAS-model has been applied for describing the binary excess molar volumes and also Peng-Robinson-Stryjek-Vera (PRSV) equation of state (EOS) has been used to predict the binary excess molar volumes and viscosities. Also several semi-empirical models were used to correlate the viscosity of binary mixtures.

  9. 利用二元体系的C-H红外光谱推算汽液平衡数据%Prediction of Vapor-Liquid Equilibrium Data from C-H Band Shift of IR Spectra in Some Binary Systems

    Institute of Scientific and Technical Information of China (English)

    朱霄; 姚加; 李浩然; 韩世钧

    2007-01-01

    Prediction of vapor-liquid equilibrium (VLE) is extremely necessary to separate liquid mixture in chemical production, especially when the required experimental data are difficult to measure, or the measurement is not economical. The infinite dilution activities can be used to predict VLE. However, it needs both thc ends of the activities that are difficult to obtain for many systems. In the present study, a new model is proposed for correlating the frequency shift of C-H stretching band of IR spectra over the whole concentration. Investigated mixtures include water/2-propanol, water/N, N-dimethylformamide (DMF), water/methanol, water/ethanol, water/1, 4-dioxane,and water/dimethylsulfoxidc (DMSO) systems. Simultaneous correlations of C-H frequency shift and VLE data arc made. Furthermore, the VLE data were predicted with satisfactory results by the parameters obtained from IR spectra coupled with one of the infinite dilution activity coefficients.

  10. Enantiomer Separation of α-Dimethyl Dicarboxylate Biphenyl and Related Biphenyl Compounds by Normal Phase HPLC on Polysaccharide Based Chiral Stationary Phases

    Institute of Scientific and Technical Information of China (English)

    LIU,Yue-Qi(刘月启); HAN,Xiao-Qian(韩小茜); Qi,Bang-Feng(齐邦峰); LIU,Chun-Hui(柳春辉); LI,Yong-Min(李永民); CHEN,Li-Ren(陈立仁)

    2002-01-01

    Cellulose tris(4-methylphenylcarbamate), amylose tris(3,5-dimethylpphenylcarbamate) and amylose tris (phenylcarbamate)were prepared by the method reported by Okamoto and were coated onto an aminopropylated mesoporous spherical silica gel. These final products were used as chiral stationary phases of high performance liquid chromatography for the eighteen structurally related biphenyl conmpounds. The resolution was made using normal-phase methodology with a mobile phase consisting of n-hexane-alcohol (ethanol, 1-propanol, 2-propanol or 1-butanol). The effects of various aliphatic alcohols in the mobile phase were studied. The structural features of the solutes that influence their k'were discussed. A dominant effect of trifluoroaetic acid on chiral separation of aacidicdic solutes was noted.

  11. The Role of Fluorinated Alcohols as Mobile Phase Modifiers for LC-MS Analysis of Oligonucleotides

    Science.gov (United States)

    Basiri, Babak; van Hattum, Hilde; van Dongen, William D.; Murph, Mandi M.; Bartlett, Michael G.

    2016-09-01

    Hexafluoroisopropanol (HFIP) has been widely used as an acidic modifier for mobile phases for liquid chromatography-mass spectrometry (LC-MS) analysis of oligonucleotides ever since the first report of its use for this purpose. This is not surprising, considering the exceptional performance of HFIP compared with carboxylic acids, which cause significant MS signal suppression in electrospray ionization. However, we have found that other fluorinated alcohols can also be utilized for mobile phase preparation and the choice of optimal fluorinated alcohol is determined by the ion-pairing (IP) agent. Although HFIP is a very good choice to be used alongside less hydrophobic IP agents, other fluorinated alcohols such as 1,1,1,3,3,3-hexafluoro-2-methyl-2-propanol (HFMIP) can significantly outperform HFIP when used with more hydrophobic IP agents. We also found that more acidic fluorinated alcohols assist with the transfer of oligonucleotides with secondary structure (e.g., folded strands and hairpins) into the gas phase.

  12. Hydrogen Peroxide in Fluorinated Alcohols: A Potent and Selective Oxidative System

    Institute of Scientific and Technical Information of China (English)

    Jernej Iskra

    2005-01-01

    @@ 1Introduction Fluorinated alcohols such as 1,1,1,3,3,3-hexafluoro-2-propanol and 2,2,2-trifluoroetanol have particular properties compared to non-fluorinated ones and could provoke changes in the course of reactions in these solvents. Their specific properties are connected mainly to the strong hydrogen bond donor ability and solvation of nuclephiles on one side, and weak hydrogen bond acceptor strength and weak solvation of electrophiles on the other. This dichotomy makes them very attractive solvents for various chemical reactions including cleavage of O - O and C - O bonds and cycloadditions[1]. At first they were used for solvolysis studies and stabilization of kationic intermediates and kation radicals, then their use was extended to various chemical synthesis and to biochemistry, where their effect on the formation of hydrogen bonds was used to alter the conformations of peptides and proteins[2].

  13. Determining an Efficient Solvent Extraction Parameters for Re-Refining of Waste Lubricating Oils

    Directory of Open Access Journals (Sweden)

    Hassan Ali Durrani

    2012-04-01

    Full Text Available Re-refining of vehicle waste lubricating oil by solvent extraction is one of the efficient and cheapest methods. Three extracting solvents MEK (Methyl-Ethyl-Ketone, 1-butanol, 2-propanol were determined experimentally for their performance based on the parameters i.e. solvent type, solvent oil ratio and extraction temperature. From the experimental results it was observed the MEK performance was highest based on the lowest oil percent losses and highest sludge removal. Further, when temperature of extraction increased the oil losses percent also decreased. This is due to the solvent ability that dissolves the base oil in waste lubricating oil and determines the best SOR (Solvent Oil Ratio and extraction temperatures.

  14. Effect of Pt:Sn atomic ratio on the preparation of PtSn/C electrocatalysts using electron beam irradiation

    International Nuclear Information System (INIS)

    PtSn/C electrocatalysts were prepared with Pt:Sn atomic ratios of 3:1, 1:1 and 1:3 in water/2-propanol using electron beam irradiation. The obtained materials were characterized by EDX, XRD and cyclic voltammetry. The ethanol electro-oxidation was studied by chronoamperometry. The XRD diffractograms of the PtSn/C electrocatalysts showed typical face-centered cubic (fcc) structure of platinum and the presence of a SnO2 phase (cassiterite). The mean crystallite sizes of Pt fcc phase was in the range of 3.0-3.5 nm. The PtSn/C electrocatalysts were active for ethanol electro-oxidation at room temperature and the material prepared with Pt:Sn atomic ratio of 1:1 showed the best activity. (author)

  15. Ruthenium-Catalyzed Transfer Hydrogenation for C-C Bond Formation: Hydrohydroxyalkylation and Hydroaminoalkylation via Reactant Redox Pairs.

    Science.gov (United States)

    Perez, Felix; Oda, Susumu; Geary, Laina M; Krische, Michael J

    2016-06-01

    Merging the chemistry of transfer hydrogenation and carbonyl or imine addition, a broad new family of redox-neutral or reductive hydrohydroxyalkylations and hydroaminomethylations have been developed. In these processes, hydrogen redistribution between alcohols and π-unsaturated reactants is accompanied by C-C bond formation, enabling direct conversion of lower alcohols to higher alcohols. Similarly, hydrogen redistribution between amines to π-unsaturated reactants results in direct conversion of lower amines to higher amines. Alternatively, equivalent products of hydrohydroxyalkylation and hydroaminomethylation may be generated through the reaction of carbonyl compounds or imines with π-unsaturated reactants under the conditions of 2-propanol-mediated reductive coupling. Finally, using vicinally dioxygenated reactants, that is, diol, ketols, or diones, successive transfer hydrogenative coupling occurs to generate 2 C-C bonds, resulting in products of formal [4+2] cycloaddition. PMID:27573275

  16. Analysis of iodine in food samples by inductively coupled plasma-mass spectrometry.

    Science.gov (United States)

    Todorov, Todor I; Gray, Patrick J

    2016-01-01

    This work shows a method for the determination of iodine in a variety of food samples and reference materials using inductively coupled plasma-mass spectrometry (ICP-MS) following alkaline extraction. Optimisation of the addition of organic carbon showed that a minimum of 3% 2-propanol was necessary for a constant ratio of iodine to internal standard. The limit of quantification (LOQ), calculated as 30σ for the method, was 36 ng g(-1) in solid food samples. For method validation, seven standard reference materials (SRM) and 21 fortified food samples were used. The precision (%RSD) of the measurements was in the 2-7% range. Accuracies for the SRMs were 85-105%, while the fortified food samples showed 81-119% recoveries, including a number of samples fortified at 50% of the LOQ.

  17. An Oxygen Reduction Study of Graphene-Based Nanomaterials of Different Origin

    Directory of Open Access Journals (Sweden)

    Jaana Lilloja

    2016-07-01

    Full Text Available The aim of this study is to compare the electrochemical behaviour of graphene-based materials of different origin, e.g., commercially available graphene nanosheets from two producers and reduced graphene oxide (rGO towards the oxygen reduction reaction (ORR using linear sweep voltammetry, rotating disc electrode and rotating ring-disc electrode methods. We also investigate the effect of catalyst ink preparation using two different solvents (2-propanol containing OH− ionomer or N,N-dimethylformamide on the ORR. The graphene-based materials are characterised by scanning electron microscopy, transmission electron microscopy, Raman spectroscopy and X-ray photoelectron spectroscopy. Clearly, the catalytic effect depends on the origin of graphene material and, interestingly, the electrocatalytic activity of the catalyst material for ORR is lower when using the OH− ionomer in electrode modification. The graphene electrodes fabricated with commercial graphene show better ORR performance than rGO in alkaline solution.

  18. Lipase-catalyzed biodiesel synthesis with different acyl acceptors

    Directory of Open Access Journals (Sweden)

    Ognjanović Nevena D.

    2008-01-01

    Full Text Available Biodiesel is an alternative fuel for diesel engine that is environmentally acceptable. Conventionally, biodiesel is produced by transesterification of triglycerides and short alcohols in the presence of an acid or an alkaline catalyst. There are several problems associated with this kind of production that can be resolved by using lipase as the biocatalyst. The aim of the present work was to investigate novel acyl acceptors for biodiesel production. 2-Propanol and n-butanol have a less negative effect on lipase stability, and they also improve low temperature properties of the fuel. However, excess alcohol leads to inactivation of the enzyme, and glycerol, a major byproduct, can block the immobilized enzyme, resulting in low enzymatic activity. This problem was solved by using methyl acetate as acyl acceptor. Triacetylglycerol is produced instead of glycerol, and it has no negative effect on the activity of the lipase.

  19. Effect of temperature on O anion radical reactions and equilibria: a pulse radiolysis study

    International Nuclear Information System (INIS)

    The pKa of the hydroxyl radical was measured over the 20-800C temperature range. At 200C, the pKa was 11.84 and fell to 10.81 at 800C. The dissociation constant for the ozonide anion (O2-anion radical ↔ O2 + O anion radical) was found to be 5.5 x 10-7 mol dm-3 at 200C and 46.2 x 10-7 mol dm-3 at 700C. The rate constants and activation energies for the reaction of O anion radical and OH with 2-propanol, methanol and 3-hexene-1,6-dicarboxylate ions have also been measured. (author)

  20. Effect of temperature on O⊘ reactions and equilibria: A pulse radiolysis study

    Science.gov (United States)

    Elliot, Allen John; McCracken, David Ritchie

    The p Ka of the hydroxyl radical was measured over the 20-80°C temperature range. At 20°C, the p Ka was 11.84 and fell to 10.81 at 80°C. The dissociation constant for the ozonide anion (O⊘ 3⇌O 2+O⊘) was found to be 5.5 × 10 -7 mol dm -3 at 20°C and 46.2 × 10 -7 mol dm -3 at 70°C. The rate constants and activation energies for the reaction of O⊘ and OH with 2-propanol, methanol and 3-hexene-1,6-dicarboxylate ions have also been measured.

  1. Optimization of ultrasound-assisted extraction of total monomeric anthocyanin (TMA) and total phenolic content (TPC) from eggplant (Solanum melongena L.) peel.

    Science.gov (United States)

    Dranca, Florina; Oroian, Mircea

    2016-07-01

    The present study describes the extraction of total monomeric anthocyanin (TMA) and total phenolic content (TPC) from eggplant peel using ultrasonic treatments and methanol and 2-propanol as extraction solvents. The extraction yields were optimized by varying the solvent concentration, ultrasonic frequency, temperature and time of ultrasonic treatment. Box-Behnken design was used to investigate the effect of process variables on the ultrasound-assisted extraction. The results showed that for TPC extraction the optimal condition were obtained with a methanol concentration of 76.6%, 33.88 kHz ultrasonic frequency, a temperature of 69.4 °C and 57.5 min extraction time. For TMA the optimal condition were the following: 54.4% methanol concentration, 37 kHz, 55.1 °C and process time of 44.85 min. PMID:26701808

  2. Direct optical observation of the formation of some aliphatic alcohol radicals. A pulse radiolysis study

    Indian Academy of Sciences (India)

    E Janata

    2002-12-01

    The kinetics of the reactions of hydroxyl radicals and hydrogen atoms with some aliphatic alcohols in aqueous solutions were studied using pulse radiolysis. Based on the increase in optical absorption in the UV region, the rate constants for the reaction of hydroxyl radicals and hydrogen atoms with methanol, ethanol, 2-propanol or -butyl alcohol were determined to be 9.0 × 108, 2.2 × 109, 2.0 × 109, 6.2 × 108 and 1.1 × 106, 1.8 × 107, 5.3 × 107, 2.3 × 105 dm3 mol-1 s-1 respectively. The bimolecular decay rate constants for the alcohol radicals produced in methanol and ethanol were evaluated to be 2 .4 × 109 and 1.5 × 109 dm3 mol-1 s-1. The values observed are in fairly good agreement with those reported earlier.

  3. The effect of the presence of alcohol in the dispersing phase of oxide sols on the properties of RuO2-TiO2/Ti anodes obtained by the sol–gel procedure

    Directory of Open Access Journals (Sweden)

    R. ATANASOSKI

    2000-09-01

    Full Text Available The effect of the addition of ethanol and 2-propanol to the dispersing phase of TiO2 and RuO2 sols mixture on the morphology and, consequently, on the electrochemical properties of the sol-gel obtained activated titanium anodes was investigated. The properties of the obtained anodes were compared to those obtained by the thermal decomposition of appropriate chloride salts. The morphology of the anode coatings was examined by scanning tunneling microscopy. The electrochemical behaviour was investigated by cyclic voltammetry and by polarization measurements. An accelerated stability test was used for the examination of the stability of the anodes under simultaneous oxygen and chlorine evolution reaction. A dependence of the anode stability on the type of added alcohol is indicated.

  4. A Convenient Synthesis of Octahydro-pyrazino [ 1,2- a ] pyrazine

    Institute of Scientific and Technical Information of China (English)

    LIANG Feng; WU Xiao-Jun; ZHANG Shi-Wei; WU Cheng-Tai

    2003-01-01

    @@ The recent research results suggest that a series of octahydro-pyrazino[ 1,2-a ]pyrazines are useful as antiallergic agents.[1] Gubert et al. [2] developed a route from 1,4-dibenzyl-2-ethoxycarbonylpiperazine for the synthesis of this ring system. Under their conditions, this ring system was obtained with a low overall yield in six steps. Optimization of synthetic route to this ring system is still desirable. In this paper, we presented an efficient synthesis of octahydropyrazino[1,2-a]pyrazine by a new and efficient method starting from 1,3-dichloro-2-propanol and N-tosylated diethylenetriamine. The structure of title compound was determined by spectroscopy and X-ray diffraction technique.

  5. Synthesis of TiO2 Nanoparticles via a Ti(Ⅳ) Complex with Stearic Acid and the Photocatalytic Activity for Organic Oxidation

    Institute of Scientific and Technical Information of China (English)

    XU,Yi-Ming(许宜铭); YU,Xiao-Han(于小涵); LIU,Hui-Jun(刘惠君)

    2002-01-01

    The nano-sized particles of TiO2 were prepared by thermal decomposition of titanium(Ⅳ) tetrabutanoxide complex with stearic acid at 450 ℃ in the air. It was observed that the amount of stearic acid, used initially for the complex synthesis in 2-propanol at 25 ℃, had great influence on the physical properties of the prepared TiO2 including crystal structure,the particle size, surface area and the adsorption capacity for organic substrate of a textile dye X3B in water, and thereafter the photocatalytic activity for the dye oxidation. Some samples displayed lower adsorption capacity for the organic substrate in water than a TiO2 of Degussa p25, but higher photocatalytic activity for the organic oxidation. Possible reason for the observed difference was discussed in the text.

  6. ANALYSIS OF OUT OF DATE MCU MODIFIER LOCATED IN SRNL

    Energy Technology Data Exchange (ETDEWEB)

    Crawford, C.

    2014-10-22

    SRNL recently completed density measurements and chemical analyses on modifier samples stored in drums within SRNL. The modifier samples date back to 2008 and are in various quantities up to 40 gallons. Vendor information on the original samples indicates a shelf life of 5 years. There is interest in determining if samples that have been stored for more than the 5 year shelf life are still acceptable for use. The Modular Caustic Side Solvent Extraction Unit (MCU) Solvent component Cs-7SB [(2,2,3,3- tetraflouropropoxy)-3-(4-sec-butylphenoxy)-2-propanol, CAS #308362-88-1] is used as a diluent modifier to increase extractant solubility and provide physical characteristics necessary for diluent trimming.

  7. Effect of solvents on propylene epoxidation over TS-1 catalyst

    Institute of Scientific and Technical Information of China (English)

    Yulong WU; Qingshan LIU; Xueli SU; Zhentao MI

    2008-01-01

    Solvents have an important effect on the epoxidation of propylene catalyzed by TS-1. The experimental results show that, in different solvents, the catalytic activity of epoxidation is in the following order: methanol > 2-propanol > 2-butanol > acetoni-trile > acetone > tetrahydrofuran. Based on the reaction mechanism, the effects of solvents on the epoxidation were studied from eight aspects, which included the electronic effect, the steric effect, the polarity of solvent, the effect of solvent on sorption and diffusion of reactant, the oxidation of alcohol, the etherification of PO, the deactivation of TS-1 and the solubility of propylene in the solvents. The electronic effect, steric effect and the polarity of solvent were considered to be the main aspects. This work may provide theoretical guidance for choosing solvents for these kinds of reactions and also may serve as basis for further industrialization.

  8. Transition metal complexes of 5-bromosalicylidene-4-amino-3-mercapto-1,2,4-triazine-5-one: Synthesis, characterization, catalytic and antibacterial studies

    Directory of Open Access Journals (Sweden)

    AYALOOR SUBRAMANIAN RAMASUBRAMANIAN

    2011-01-01

    Full Text Available Transition metal complexes of 5-bromosalicylidene-4-amino-3-mercapto-1,2,4-triazine-5-one with metal precursors, such as Cu(II, Ni(II, Co(II and Pd(II, were synthesized and characterized by physico–chemical and spectroscopic techniques. All the complexes are of the ML type. Based on analytical, spectral data and magnetic moments, the Co(II and Ni(II complexes were assigned octahedral geometries, while the Cu (II and Pd(II complexes square planar. A study on the catalytic oxidation of benzyl alcohol, cyclohexanol, cinnamyl alcohol, 2-propanol and 2-methyl-1-propanol was performed with N-methylmorpholine-N-oxide (NMO as co-oxidant. All the complexes and their parent organic moiety were screened for their biological activity on several pathogenic bacteria and were found to possess appreciable bactericidal properties.

  9. PREPARATION OF POLYETHERSULFONE ULTRAFILTRATION MEMBRANES FOR MILK CONCENTRATION AND EFFECTS OF ADDITIVES ON THEIR MORPHOLOGY AND PERFORMANCE

    Institute of Scientific and Technical Information of China (English)

    S.S. Madaeni; A. Rahimpour

    2005-01-01

    Polyethersulfone membranes were prepared from quaternary systems containing N,N-dimethylacetamide (DMAc) as solvent, polyvinylpyrrolidone (PVP) as constant additive and acetic acid, acetone and water as variable additives. Phase inversion via immersion precipitation was employed for manufacturing of membranes. The prepared films were immersed in the mixture of pure water and 2-propanol (30/70 vol%) as the non-solvent. Acetic acid caused an increment in the flux at high polymer concentration (16wt%) and a decline in the flux at low polymer concentrations (10 wt% and 13 wt%). Acetone and water as the solvent in the casting solution declined the flux at any polymer concentration tested. The morphology and performance of the prepared membranes were investigated by scanning electron microscopy and separation experiments using milk as the feed.

  10. Synergetic effect of TeMo5O16 and MoO3 phases in MoTeOx catalysts used for the partial oxidation of propylene

    Institute of Scientific and Technical Information of China (English)

    Yiming He; Ying Wu; Weizheng Weng; Huilin Wan

    2011-01-01

    A detailed study on the synergetic effect of TeMo5O16 and MoO3 phases in the MoTeOx catalysts for the partial oxidation of propylene to acrolein has been reported in this work. It was found that both propylene conversion and acrolein selectivity increased with the addition of MoO3 to TeMo5O16. Based on the results of N2 adsorption-desorption, XRD, XPS, in-situ XRD, O2-TPO, and 2-propanol decomposition reaction, the higher catalytic performance and synergetic effect could be attributed to the enhancement of acidity and the oxygen transfer from TeMo5O16 to MoO3 phase.

  11. Measurements of Conductivity for Low Concentration Strong- electrolytes in Organic Solvents (I) LiBr, LiCI, and LiNO3 in Alcohols%Measurements of Conductivity for Low Concentration Strong- electrolytes in Organic Solvents (I) LiBr, LiCI, and LiNO3 in Alcohols

    Institute of Scientific and Technical Information of China (English)

    陈红; 王利生; 姜波; 李弥异

    2012-01-01

    The conductivities of LiBr, LiCl, and LiNO 3 in methanol, ethanol, 1-propanol, and 2-propanol (with electrolyte concentrations 〈0.08 mol·L-1 ) were determined at 298.15 K, 313.15 K, and 323.15 K at atmosphere pressure separately by using a conductivity meter. The conductivity data were correlated with Foss-Chen-Justice (FCJ) equation and the limiting molar conductivities were obtained. The mean ionic activity coefficients of the salts in the organic solvents were calculated according to the Debye-Hückel limiting law and Onsager-Falkenhangen equations. The calculated results were compared with those activity coefficients in literature.

  12. Degradation of a recalcitrant xenobiotic compound: methyl tert-butyl ether (MTBE) metabolism by mycobacterium austroafricanum; Degradation d'un compose xenobiotique recalcitrant: metabolisme du methyl tert-butyl ether (MTBE) par mycobacterium austroafricanum IFP 2012

    Energy Technology Data Exchange (ETDEWEB)

    Francois, A.

    2002-11-01

    Methyl tert-butyl ether (MTBE) is introduced up to 15% (vol/vol) in gasoline in order to obtain a good octane number and to prevent carbon monoxide emissions. However, as a consequence of storage tanks leakage, MTBE became one of the major pollutants of aquifers because of its very low biodegradability. The present study aimed at investigating the biodegradation of MTBE by Mycobacterium austroafricanum IFP 2012. The MTBE metabolic pathway was partially elucidated owing to the identification of some intermediates (tert-butyl formate (TBF), tert-butyl alcohol (TBA), a-hydroxy-isobutyric acid and acetone) and some enzymatic activities (MTBE/TBA monooxygenase (non hemic and inducible), TBF esterase, 2-propanol: NDMA oxidoreductase and another monooxygenase involved in acetone degradation). The involvement of TBF and the requirement of cobalt could be explanations for the low natural attenuation of MTBE; whereas the methoxy group does not seem to be implicated. (author)

  13. One-step synthesis of graphene-Pt nanocomposites by gamma-ray irradiation

    Science.gov (United States)

    Tokai, Akihiro; Okitsu, Kenji; Hori, Fuminobu; Mizukoshi, Yoshiteru; Iwase, Akihiro

    2016-06-01

    We developed a one-step gamma-ray irradiation method to synthesize nanocomposites composed of graphene and Pt nanoparticles from aqueous solution containing graphene and Pt(IV) complex ions in the presence of 2-propanol (IPA) or sodium dodecyl sulfate (SDS). It was confirmed that gamma-ray irradiation provided carbonyl groups on graphene and Pt nanoparticles formed from the radiolytic reduction of Pt(IV) complex ions were deposited onto the carbonyl modified graphene. In the presence of IPA, small Pt nanoparticles were deposited on graphene, but large Pt nanoparticles were deposited in the presence of SDS: the size of Pt nanoparticles formed was larger in the presence of SDS than IPA. Based on the results, formation and deposition mechanisms of Pt nanoparticles were proposed.

  14. Lipase-catalyzed synthesis of fatty acid amide (erucamide) using fatty acid and urea.

    Science.gov (United States)

    Awasthi, Neeraj Praphulla; Singh, R P

    2007-01-01

    Ammonolysis of fatty acids to the corresponding fatty acid amides is efficiently catalysed by Candida antartica lipase (Novozym 435). In the present paper lipase-catalysed synthesis of erucamide by ammonolysis of erucic acid and urea in organic solvent medium was studied and optimal conditions for fatty amides synthesis were established. In this process erucic acid gave 88.74 % pure erucamide after 48 hour and 250 rpm at 60 degrees C with 1:4 molar ratio of erucic acid and urea, the organic solvent media is 50 ml tert-butyl alcohol (2-methyl-2-propanol). This process for synthesis is economical as we used urea in place of ammonia or other amidation reactant at atmospheric pressure. The amount of catalyst used is 3 %.

  15. Characterization of catalytic supports based in mixed oxides for control reactions of NO and N{sub 2}O; Caracterizacion de soportes cataliticos basados en oxidos mixtos para reacciones de control de NO y N{sub 2}O

    Energy Technology Data Exchange (ETDEWEB)

    Garcia C, M.A.; Perez H, R.; Gomez C, A.; Diaz, G. [Instituto Nacional de Investigaciones Nucleares, A.P. 18-1027, 11801 Mexico D.F. (Mexico)

    1999-07-01

    The catalytic supports Al{sub 2}O{sub 3}, La{sub 2}O{sub 3} and Al{sub 2}O{sub 3}-La{sub 2}O{sub 3} were prepared by the Precipitation and Coprecipitation techniques. The catalytic supports Al{sub 2}O{sub 3}, La{sub 2}O{sub 3} and Al{sub 2}O{sub 3}-La{sub 2}O{sub 3} were characterized by several techniques to determine: texture (Bet), crystallinity (XRD), chemical composition (Sem)(Ftir) and it was evaluated their total acidity by reaction with 2-propanol. The investigation will be continued with the cobalt addition and this will be evaluated for its catalytic activity in control reactions of N O and N{sub 2}O. (Author)

  16. Advances in the catalysts development in base of mixed oxides for control reactions of N{sub 2}O; Avances en el desarrollo de catalizadores a base de oxidos mixtos para reacciones de control de N{sub 2}O

    Energy Technology Data Exchange (ETDEWEB)

    Garcia, M.A.; Perez, R.; Gomez, A.; Diaz, G. [Instituto Nacional de Investigaciones Nucleares, A.P. 18-1027, C.P. 11801 Mexico D.F. (Mexico)

    2000-07-01

    The catalytic supports Al{sub 2}O{sub 3}, La{sub 2}O{sub 3} and Al{sub 2}O{sub 3}-La{sub 2}O{sub 3} were prepared by the precipitation and coprecipitation techniques. The catalytic supports Al{sub 2}O{sub 3}, La{sub 2}O{sub 3} and Al{sub 2}O{sub 3}-La{sub 2}O{sub 3} were characterized by several techniques for to determine texture (BET), crystallinity (XRD), chemical composition (SEM), FTIR and it was evaluated their total acidity by the reaction with 2-propanol. It was continued with the cobalt addition by Impregnation and coprecipitation and it was evaluated its catalytic activity in the N{sub 2}O decomposition reaction. Also it was realized the N{sub 2}O reduction with Co using these catalysts. (Author)

  17. A method suitable for DNA extraction from humus-rich soil.

    Science.gov (United States)

    Miao, Tianjin; Gao, Song; Jiang, Shengwei; Kan, Guoshi; Liu, Pengju; Wu, Xianming; An, Yingfeng; Yao, Shuo

    2014-11-01

    A rapid and convenient method for extracting DNA from soil is presented. Soil DNA is extracted by direct cell lysis in the presence of EDTA, SDS, phenol, chloroform and isoamyl alcohol (3-methyl-1-butanol) followed by precipitation with 2-propanol. The extracted DNA is purified by modified DNA purification kit and DNA gel extraction kit. With this method, DNA extracted from humus-rich dark brown forest soil was free from humic substances and, therefore, could be used for efficient PCR amplification and restriction digestion. In contrast, DNA sample extracted with the traditional CTAB-based method had lower yield and purity, and no DNA could be extracted from the same soil sample with a commonly-used commercial soil DNA isolation kit. In addition, this method is time-saving and convenient, providing an efficient choice especially for DNA extraction from humus-rich soils.

  18. Effect of the composition of a water-alcohol solvent on the thermodynamics of dissolution of DL-α-alanyl-β-alanine at 298.15 K

    Science.gov (United States)

    Smirnov, V. I.; Badelin, V. G.

    2014-12-01

    Enthalpies of solution for DL-α-alanyl-β-alanine in H2O-ethanol, H2O-1-propanol, and H2O-2-propanol mixed solvents with the alcohol mole fraction x 2 = 0-0.3 are measured at 298.15 K. Standard enthalpies of solution (Δsol H ∘), standard enthalpies of transfer of DL-α-alanyl-β-alanine from water to binary solvent (Δtr H ∘), and coefficients of enthalpies of pair interactions with alcohol molecules ( h xy) are calculated. The effect the structure and properties of alcohols and the composition of a water-alcohol mixture have on the enthalpy of dissolution for DL-α-alanyl-β-alanine are discussed. The h xy values for dipeptides of the alanine series in water-alcohol binary solvents are compared.

  19. Effect of solvent structure on election reactivity

    International Nuclear Information System (INIS)

    The reactivity of solvated electrons (es-) with efficient (nitrobenzene, acetone) and inefficient (phenol, toluene) scavengers is affected greatly by the solvent composition in 2-propanol/water mixed solvents. 2-Propanol is the only secondary alcohol that is completely miscible with water. The variation of the nitrobenzene rate constant k2 with solvent composition displays four viscosity zones, as in primary and tertiary alcohol/water mixtures. In zone (c), where the Stokes-Smoluchowski equation applies, the nitrobenzene k2 values in the secondary alcohol/water mixtures are situated between those in the primary and tertiary alcohols, due to the relative values of the dielectric permittivity ε. The charge-dipole attraction energy varies at ε-1. The two water-rich zones (c) and (d) are characterized by a large change of viscosity η and a small change in es- solvation energy (trap depth) Er; here k2 for all the scavengers correlates with the inverse of the viscosity. In the two alcohol-rich zones (a) and (b) the change of η is small but that of Er is large; here k2 of inefficient scavengers correlates with the inverse of Er, due to the difficulty of electron transfer out of deeper traps. Activation energies E2 and entropies ΔS2(double dagger) also show composition zone behaviour. The value of ΔS2(double dagger) is more negative for less efficient scavengers; E2 varies less and does not correlate with reactivity of Er. Electron transfer from solvent to inefficient scavenger is driven by solvent rearrangement around the reaction center, reflected in ΔS2(double dagger)

  20. Enhancement of the electrical characteristics of MOS capacitors by reducing the organic content of H{sub 2}O-diluted Spin-On-Glass based oxides

    Energy Technology Data Exchange (ETDEWEB)

    Molina, Joel, E-mail: jmolina@inaoep.mx [National Institute of Astrophysics, Optics and Electronics, Electronics Department, Luis Enrique Erro 1, PO BOX 51 and 216, Tonantzintla, Puebla 72000 (Mexico); Munoz, Ana; Torres, Alfonso; Landa, Mauro; Alarcon, Pablo; Escobar, Manuel [National Institute of Astrophysics, Optics and Electronics, Electronics Department, Luis Enrique Erro 1, PO BOX 51 and 216, Tonantzintla, Puebla 72000 (Mexico)

    2011-10-25

    In this work, the physical, chemical and electrical properties of Metal-Oxide-Semiconductor (MOS) capacitors with Spin-On-Glass (SOG)-based thin films as gate dielectric have been investigated. Experiments of SOG diluted with two different solvents (2-propanol and deionized water) were done in order to reduce the viscosity of the SOG solution so that thinner films (down to {approx}20 nm) could be obtained and their general characteristics compared. Thin films of SOG were deposited on silicon by the sol-gel technique and they were thermally annealed using conventional oxidation furnace and Rapid Thermal Processing (RTP) systems within N{sub 2} ambient after deposition. SOG dilution using non-organic solvents like deionized water and further annealing (at relatively high temperatures {>=}450 deg. C) are important processes intended to reduce the organic content of the films. Fourier-Transform Infrared (FTIR) Spectroscopy results have shown that water-diluted SOG films have a significant reduction in their organic content after increasing annealing temperature and/or dilution percentage when compared to those of undiluted SOG films. Both current-voltage (I-V) and capacitance-voltage (C-V) measurements show better electrical characteristics for SOG-films diluted in deionized water compared to those diluted in 2-propanol (which is an organic solvent). The electrical characteristics of H{sub 2}O-diluted SOG thin films are very similar to those obtained from high quality thermal oxides so that their application as gate dielectrics in MOS devices is promising. Finally, it has been demonstrated that by reducing the organic content of SOG-based thin films, it is possible to obtain MOS devices with better electrical properties.

  1. Metabolism of spacecraft cleaning reagents by Mars Odyssey and Phoenix-associated Acinetobacter

    Science.gov (United States)

    Mogul, Rakesh; Barding, Gregory; Baki, Ryan; Perkins, Nicole; Lee, Sooji; Lalla, Sid; Campos, Alexa; Sripong, Kimberly; Madrid, Steve

    2016-07-01

    The metabolomic and proteomic properties that promote microbial survival in spacecraft assembly facilities are important aspects to planetary protection and astrobiology. In this presentation, we will provide molecular and biological evidence that the spacecraft-associated Acinetobacter metabolize/degrade spacecraft cleaning reagents such as ethanol, 2-propanol, and Kleenol-30. Gas chromatography-mass spectrometry (GC-MS) studies on A. radioresistens 50v1 (Mars Odyssey) show that the metabolome is dependent upon growth conditions and that ^{13}C-labeled ethanol is incorporated into metabolites such as TCA/glyoxylate cycle intermediates, amino acids, monosaccharides, and disaccharides (e.g., trehalose). In fact, plate count assays show that ethanol is a sole carbon source under minimal conditions for several Mars Phoenix and Odyssey-associated Acinetobacter strains, which may explain why the Acinetobacter are among the most abundant genera found in spacecraft assembly facilities. Biochemical analyses support the enzymatic oxidation of ethanol and 2-propanol by a membrane-bound and NAD+/PQQ-dependent alcohol dehydrogenase, with current kinetic data providing similar apparent K _{M} and maximum growth rate values of ˜5 and 8 mM ethanol, respectively. Preliminary GC-MS analysis also suggests that Kleenol-30 is degraded by A. radioresistens 50v1 when grown in ethanol mixtures. Under minimal conditions, A. radioresistens 50v1 (˜10 ^{8} cfu/mL) also displays a remarkable oxidative extremotolerance (˜2-log reduction in 10 mM hydrogen peroxide), which suggests crucial roles for metabolites associated with oxidative stress (e.g., trehalose) and the observed appreciable catalase specific activities. In conclusion, these results provide key insights into the survival strategies of spacecraft-associated Acinetobacter and emphasize the importance of characterizing the carbon metabolism of forward contaminants.

  2. Influence of hydroxyl group position and temperature on thermophysical properties of tetraalkylammonium hydroxide ionic liquids with alcohols.

    Science.gov (United States)

    Attri, Pankaj; Baik, Ku Youn; Venkatesu, Pannuru; Kim, In Tae; Choi, Eun Ha

    2014-01-01

    In this work, we have explored the thermophysical properties of tetraalkylammonium hydroxide ionic liquids (ILs) such as tetrapropylammonium hydroxide (TPAH) and tetrabutylammonium hydroxide (TBAH) with isomers of butanol (1-butanol, 2-butanol and 2-methyl-2-propanol) within the temperature range 293.15-313.15 K, with interval of 5 K and over the varied concentration range of ILs. The molecular interactions between ILs and butanol isomers are essential for understanding the function of ILs in related measures and excess functions are sensitive probe for the molecular interactions. Therefore, we calculated the excess molar volume (V(E) ) and the deviation in isentropic compressibility (Δκs ) using the experimental values such as densities (ρ) and ultrasonic sound velocities (u) that are measured over the whole compositions range at five different temperatures (293.15, 298.15, 303.15, 308.15 and 313.15 K) and atmospheric pressure. These excess functions were adequately correlated by using the Redlich-Kister polynomial equation. It was observed that for all studied systems, the V(E) and Δκs values are negative for the whole composition range at 293.15 K. And, the excess function follows the sequence: 2-butanol>1-butanol>2-methyl-2-propanol, which reveals that (primary or secondary or tertiary) position of hydroxyl group influence the magnitude of interactions with ILs. The negative values of excess functions are contributions from the ion-dipole interaction, hydrogen bonding and packing efficiency between the ILs and butanol isomers. Hence, the position of hydroxyl group plays an important role in the interactions with ILs. The hydrogen bonding features between ILs and alcohols were analysed using molecular modelling program by using HyperChem 7. PMID:24489741

  3. Obtención de Dímeros por Termólisis de 1,2-Propanodiol Synthesis of Dimers from Thermolysis of 1,2-Propanediol

    Directory of Open Access Journals (Sweden)

    Nathaly Milanés

    2012-01-01

    Full Text Available Los compuestos dímeros 3-oxi-(bis-2-propanol, 2-(2-hidroxipropoxi-propanol y 2-oxi-(bis-propanol fueron obtenidos de la reacción de descomposición térmica del 1,2-propanodiol, realizada a 573.15 K y a su presión de vapor, utilizando un sistema de reacción a microescala, Los dímeros resultaron ser isómeros y fueron elucidados por cromatografía gaseosa acoplada a espectrometría de masas. E stos compuestos no han sido reportados en la literatura como productos de termólisis de polioles. La cinética y el mecanismo, fueron confirmados por cálculos computacionales utilizando el método de la Teoría del Funcional Densidad, DFT. E l mecanismo propuesto transcurrió a través de un proceso concertado de una sola etapa, que pasa por un estado de transición cíclico de cuatro miembros , compatible con cálculos cinéticos y termodinámicos.The dimers 3-oxy-(bys-2-propanol, 2-(2-hydroxypropoxy-propanol and 2-oxy-(bys-propanol were obtained from the thermal decomposition reaction of 1,2-propanediol , at 573.15 K and to its vapor pressure, and using microscale reaction system. The dimers resulted to be isomers and were elucidated by gas chromatography coupled to mass spectrometry. These compounds have not been reported in literature as products polyol thermolysis. The kinetic and the mechanism were validated by computational calculations using the Density Functional Theory, DFT. The proposed mechanism occurred in a single step concerted process that passes through a four member transition cyclical state that is compatible with kinetic and thermodynamic calculations.

  4. Influence of hydroxyl group position and temperature on thermophysical properties of tetraalkylammonium hydroxide ionic liquids with alcohols.

    Directory of Open Access Journals (Sweden)

    Pankaj Attri

    Full Text Available In this work, we have explored the thermophysical properties of tetraalkylammonium hydroxide ionic liquids (ILs such as tetrapropylammonium hydroxide (TPAH and tetrabutylammonium hydroxide (TBAH with isomers of butanol (1-butanol, 2-butanol and 2-methyl-2-propanol within the temperature range 293.15-313.15 K, with interval of 5 K and over the varied concentration range of ILs. The molecular interactions between ILs and butanol isomers are essential for understanding the function of ILs in related measures and excess functions are sensitive probe for the molecular interactions. Therefore, we calculated the excess molar volume (V(E and the deviation in isentropic compressibility (Δκs using the experimental values such as densities (ρ and ultrasonic sound velocities (u that are measured over the whole compositions range at five different temperatures (293.15, 298.15, 303.15, 308.15 and 313.15 K and atmospheric pressure. These excess functions were adequately correlated by using the Redlich-Kister polynomial equation. It was observed that for all studied systems, the V(E and Δκs values are negative for the whole composition range at 293.15 K. And, the excess function follows the sequence: 2-butanol>1-butanol>2-methyl-2-propanol, which reveals that (primary or secondary or tertiary position of hydroxyl group influence the magnitude of interactions with ILs. The negative values of excess functions are contributions from the ion-dipole interaction, hydrogen bonding and packing efficiency between the ILs and butanol isomers. Hence, the position of hydroxyl group plays an important role in the interactions with ILs. The hydrogen bonding features between ILs and alcohols were analysed using molecular modelling program by using HyperChem 7.

  5. Influence of hydroxyl group position and temperature on thermophysical properties of tetraalkylammonium hydroxide ionic liquids with alcohols.

    Science.gov (United States)

    Attri, Pankaj; Baik, Ku Youn; Venkatesu, Pannuru; Kim, In Tae; Choi, Eun Ha

    2014-01-01

    In this work, we have explored the thermophysical properties of tetraalkylammonium hydroxide ionic liquids (ILs) such as tetrapropylammonium hydroxide (TPAH) and tetrabutylammonium hydroxide (TBAH) with isomers of butanol (1-butanol, 2-butanol and 2-methyl-2-propanol) within the temperature range 293.15-313.15 K, with interval of 5 K and over the varied concentration range of ILs. The molecular interactions between ILs and butanol isomers are essential for understanding the function of ILs in related measures and excess functions are sensitive probe for the molecular interactions. Therefore, we calculated the excess molar volume (V(E) ) and the deviation in isentropic compressibility (Δκs ) using the experimental values such as densities (ρ) and ultrasonic sound velocities (u) that are measured over the whole compositions range at five different temperatures (293.15, 298.15, 303.15, 308.15 and 313.15 K) and atmospheric pressure. These excess functions were adequately correlated by using the Redlich-Kister polynomial equation. It was observed that for all studied systems, the V(E) and Δκs values are negative for the whole composition range at 293.15 K. And, the excess function follows the sequence: 2-butanol>1-butanol>2-methyl-2-propanol, which reveals that (primary or secondary or tertiary) position of hydroxyl group influence the magnitude of interactions with ILs. The negative values of excess functions are contributions from the ion-dipole interaction, hydrogen bonding and packing efficiency between the ILs and butanol isomers. Hence, the position of hydroxyl group plays an important role in the interactions with ILs. The hydrogen bonding features between ILs and alcohols were analysed using molecular modelling program by using HyperChem 7.

  6. Crystallization and identification of the glycosylated moieties of two isoforms of the main allergen Hev b 2 and preliminary X-ray analysis of two polymorphs of isoform II

    International Nuclear Information System (INIS)

    Crystallization of important glycoenzymes involved in IgE-mediated latex allergy. Latex from Hevea brasiliensis contains several allergenic proteins that are involved in type I allergy. One of them is Hev b 2, which is a β-1,3-glucanase enzyme that exists in different isoforms with variable glycosylation content. Two glucanase isoforms were isolated from trees of the GV-42 clone by gel filtration, affinity and ion-exchange chromatography. Isoform I had a carbohydrate content of about 20%, with N-linked N-acetyl-glucosamine, N-acetyl-galactosamine, fucose and galactose residues as the main sugars, while isoform II showed 6% carbohydrate content constisting of N-acetyl-glucosamine, fucose, mannose and xylose. Both isoforms were crystallized by the hanging-drop vapour-diffusion method. Isoform I crystals were grown using 0.2 M trisodium citrate dihydrate, 0.1 M Na HEPES pH 7.5 and 20%(v/v) 2-propanol, but these crystals were not appropriate for data collection. Isoform II crystals were obtained under two conditions and X-ray diffraction data were collected from both. In the first condition (0.2 M trisodium citrate, 0.1 M sodium cacodylate pH 6.5, 30% 2-propanol), crystals belonging to the tetragonal space group P41 with unit-cell parameters a = b = 150.17, c = 77.41 Å were obtained. In the second condition [0.2 M ammonium acetate, 0.1 M trisodium citrate dihydrate pH 5.6, 30%(w/v) polyethylene glycol 4000] the isoform II crystals belonged to the monoclinic space group P21, with unit-cell parameters a = 85.08, b = 89.67, c = 101.80 Å, β = 113.6°. Preliminary analysis suggests that there are four molecules of isoform II in both asymmetric units

  7. Photoinduced Electron Accumulation of Titanium Dioxide Nanoparticles Modified Electrodes

    Science.gov (United States)

    Miyoshi, Hirokazu; Sakamoto, Kensho; Kurashina, Masaru; Kanezaki, Eiji

    Titanium dioxide (TiO2) nanoparticles (Nps) were prepared by the hydrolysis of titanium tetraisopropoxide (TTIP) in 2-propanol with different water contents (0.5 vol% to 7.2 vol%) at 45 °C. The diameter of the Nps was estimated to be 1.5±0.5 nm (L-TiO2) and 3.0±0.6 nm (S-TiO2) from the onset wavelength in the absorption spectra and by transmission electron microscopy (TEM). A modified Pt electrode with a three-layered sandwich structure was prepared; the outermost and innermost layers were composed of S-TiO2 and L-TiO2, respectively, and the middle layer contained 1, 1'-dimethyl-4,4'-bipyridyl (MV2+)/Nafion®. Irradiation by a 500 W superhigh-pressure mercury lamp produced electrons in the conduction band of TiO2. An anodic current was observed after turning off the light. The mechanism by which anodic current is generated after turning off the radiation involves the reduction of MV2+ to MV+. by photogenerated electrons on the Nps and the diffusion of MV+. in the middle layer. After turning off the irradiation, MV+. transferred an electron to the Pt electrode via holes in the innermost layer or the conduction band of S-TiO2 coincidentally localized on the Pt electrode, resulting in the generation of the anodic current. The generation of MV+. was confirmed by the absorption spectra of MV+.. As a sacrificial reagent, 2-propanol (0.1 M) was used.

  8. Crystallization and identification of the glycosylated moieties of two isoforms of the main allergen Hev b 2 and preliminary X-ray analysis of two polymorphs of isoform II

    Energy Technology Data Exchange (ETDEWEB)

    Fuentes-Silva, D. [Instituto de Química, Universidad Nacional Autónoma de México, Circuito Exterior s/n, Cuidad Universitaria, Coyoacán, México, DF 04510 (Mexico); Mendoza-Hernández, G. [Facultad de Medicina, Universidad Nacional Autónoma de México, Circuito Exterior s/n, Cuidad Universitaria, Coyoacán, México, DF 04510 (Mexico); Stojanoff, V. [Brookhaven National Laboratory, National Synchrotron Light Source, Upton, NY (United States); Palomares, L. A. [Instituto de Biotecnología, Universidad Nacional Autónoma de México, Circuito Exterior s/n, Cuidad Universitaria, Coyoacán, México, DF 04510 (Mexico); Zenteno, E. [Facultad de Medicina, Universidad Nacional Autónoma de México, Circuito Exterior s/n, Cuidad Universitaria, Coyoacán, México, DF 04510 (Mexico); Torres-Larios, A. [Instituto de Fisiología Celular, Universidad Nacional Autónoma de México, Circuito Exterior s/n, Cuidad Universitaria, Coyoacán, México, DF 04510 (Mexico); Rodríguez-Romero, A., E-mail: adela@servidor.unam.mx [Instituto de Química, Universidad Nacional Autónoma de México, Circuito Exterior s/n, Cuidad Universitaria, Coyoacán, México, DF 04510 (Mexico)

    2007-09-01

    Crystallization of important glycoenzymes involved in IgE-mediated latex allergy. Latex from Hevea brasiliensis contains several allergenic proteins that are involved in type I allergy. One of them is Hev b 2, which is a β-1,3-glucanase enzyme that exists in different isoforms with variable glycosylation content. Two glucanase isoforms were isolated from trees of the GV-42 clone by gel filtration, affinity and ion-exchange chromatography. Isoform I had a carbohydrate content of about 20%, with N-linked N-acetyl-glucosamine, N-acetyl-galactosamine, fucose and galactose residues as the main sugars, while isoform II showed 6% carbohydrate content constisting of N-acetyl-glucosamine, fucose, mannose and xylose. Both isoforms were crystallized by the hanging-drop vapour-diffusion method. Isoform I crystals were grown using 0.2 M trisodium citrate dihydrate, 0.1 M Na HEPES pH 7.5 and 20%(v/v) 2-propanol, but these crystals were not appropriate for data collection. Isoform II crystals were obtained under two conditions and X-ray diffraction data were collected from both. In the first condition (0.2 M trisodium citrate, 0.1 M sodium cacodylate pH 6.5, 30% 2-propanol), crystals belonging to the tetragonal space group P4{sub 1} with unit-cell parameters a = b = 150.17, c = 77.41 Å were obtained. In the second condition [0.2 M ammonium acetate, 0.1 M trisodium citrate dihydrate pH 5.6, 30%(w/v) polyethylene glycol 4000] the isoform II crystals belonged to the monoclinic space group P2{sub 1}, with unit-cell parameters a = 85.08, b = 89.67, c = 101.80 Å, β = 113.6°. Preliminary analysis suggests that there are four molecules of isoform II in both asymmetric units.

  9. Crystallization and Identification of the Glycosylated Moieties of Two Isoforms of the Main Allergen Hev b 2 and Preliminary X-ray Analysis of Two Polymorphs of Isoform ll

    Energy Technology Data Exchange (ETDEWEB)

    Fuentes-Silva,D.; Mendoza-Hernandez, G.; Stojanoff, V.; Palomares, L.; Zenteno, E.; Torres-Larios, A.; Rodriguez-Romero, A.

    2007-01-01

    Latex from Hevea brasiliensis contains several allergenic proteins that are involved in type I allergy. One of them is Hev b 2, which is a {beta}-1,3-glucanase enzyme that exists in different isoforms with variable glycosylation content. Two glucanase isoforms were isolated from trees of the GV-42 clone by gel filtration, affinity and ion-exchange chromatography. Isoform I had a carbohydrate content of about 20%, with N-linked N-acetyl-glucosamine, N-acetyl-galactosamine, fucose and galactose residues as the main sugars, while isoform II showed 6% carbohydrate content consisting of N-acetyl-glucosamine, fucose, mannose and xylose. Both isoforms were crystallized by the hanging-drop vapor-diffusion method. Isoform I crystals were grown using 0.2 M trisodium citrate dihydrate, 0.1 M Na HEPES pH 7.5 and 20%(v/v) 2-propanol, but these crystals were not appropriate for data collection. Isoform II crystals were obtained under two conditions and X-ray diffraction data were collected from both. In the first condition (0.2 M trisodium citrate, 0.1 M sodium cacodylate pH 6.5, 30% 2-propanol), crystals belonging to the tetragonal space group P4{sub 1} with unit-cell parameters a = b = 150.17, c = 77.41 {angstrom} were obtained. In the second condition [0.2 M ammonium acetate, 0.1 M trisodium citrate dihydrate pH 5.6, 30%(w/v) polyethylene glycol 4000] the isoform II crystals belonged to the monoclinic space group P2{sub 1}, with unit-cell parameters a = 85.08, b = 89.67, c = 101.80 {angstrom}, {beta}= 113.6{sup o}. Preliminary analysis suggests that there are four molecules of isoform II in both asymmetric units.

  10. Enhancement and inhibition effects of water matrices during the sonochemical degradation of the antibiotic dicloxacillin.

    Science.gov (United States)

    Villegas-Guzman, Paola; Silva-Agredo, Javier; Giraldo-Aguirre, Ana L; Flórez-Acosta, Oscar; Petrier, Christian; Torres-Palma, Ricardo A

    2015-01-01

    The sonochemical degradation of dicloxacillin (DXC) was studied in both synthetic and natural waters. Degradation routes and the effect of experimental conditions such as pH, initial DXC concentration and ultrasonic power were evaluated. Experiments were carried out with a fixed frequency (600kHz). The best performances were achieved using acidic media (pH=3) and high power (60W). The degradation process showed pseudo-first order kinetics as described by the Okitsu model. To evaluate water matrix effects, substrate degradation, in the presence of Fe(2+) and organic compounds such as glucose and 2-propanol, was studied. A significant improvement was achieved with Fe(2+) (1.0mM). Inhibition of the degradation process was observed at a relatively high concentration of 2-propanol (4.9mM), while glucose did not show any effect. Natural water showed an interesting effect: for a low concentration of DXC (6.4μM), an improvement in the degradation process was observed, while at a higher concentration of DXC (0.43mM), degradation was inhibited. Additionally, the extent of degradation of the process was evaluated through the analysis of chemical oxygen demand (COD), antimicrobial activity, total organic carbon (TOC) and biochemical oxygen demand (BOD5). A 30% removal of COD was achieved after the treatment and no change in the TOC was observed. Antimicrobial activity was eliminated after 360min of ultrasonic treatment. After 480min of treatment, a biodegradable solution was obtained. PMID:25069890

  11. Synthesis and Catalytic Hydrogen Transfer Reaction of Ruthenium(II) Complex

    Energy Technology Data Exchange (ETDEWEB)

    Son, Jung Ik; Kim, Aram; Noh, Hui Bog; Lee, Hyun Ju; Shim, Yoon Bo; Park, Kang Hyun [Pusan National University, Busan (Korea, Republic of)

    2012-01-15

    The ruthenium(II) complex [Ru(bpy){sub 2}-(PhenTPy)] was synthesized, and used for the transfer hydrogenation of ketones and the desired products were obtained in good yield. Based on the presented results, transition-metal complexes can be used as catalysts for a wide range of organic transformations. The relationship between the electro-reduction current density and temperature are being examined in this laboratory. Attempts to improve the catalytic activity and determine the transfer hydrogenation mechanism are currently in progress. The catalytic hydrogenation of a ketone is a basic and critical process for making many types of alcohols used as the final products and precursors in the pharmaceutical, agrochemical, flavor, fragrance, materials, and fine chemicals industries. The catalytic hydrogenation process developed by Noyori is a very attractive process. Formic acid and 2-propanol have been used extensively as hydrogenation sources. The advantage of using 2-propanol as a hydrogen source is that the only side product will be acetone, which can be removed easily during the workup process. Hydrogen transfer (HT) catalysis, which generates alcohols through the reduction of ketones, is an attractive protocol that is used widely. Ruthenium(II) complexes are the most useful catalysts for the hydrogen transfer (HT) of ketones. In this method, a highly active catalytic system employs a transition metal as a catalyst to synthesize alcohols, and is a replacement for the hydrogen-using hydrogenation process. The most active system is based on Ru, Rh and Ir, which includes a nitrogen ligand that facilitates the formation of a catalytically active hydride and phosphorus.

  12. Synthesis and Catalytic Hydrogen Transfer Reaction of Ruthenium(II) Complex

    International Nuclear Information System (INIS)

    The ruthenium(II) complex [Ru(bpy)2-(PhenTPy)] was synthesized, and used for the transfer hydrogenation of ketones and the desired products were obtained in good yield. Based on the presented results, transition-metal complexes can be used as catalysts for a wide range of organic transformations. The relationship between the electro-reduction current density and temperature are being examined in this laboratory. Attempts to improve the catalytic activity and determine the transfer hydrogenation mechanism are currently in progress. The catalytic hydrogenation of a ketone is a basic and critical process for making many types of alcohols used as the final products and precursors in the pharmaceutical, agrochemical, flavor, fragrance, materials, and fine chemicals industries. The catalytic hydrogenation process developed by Noyori is a very attractive process. Formic acid and 2-propanol have been used extensively as hydrogenation sources. The advantage of using 2-propanol as a hydrogen source is that the only side product will be acetone, which can be removed easily during the workup process. Hydrogen transfer (HT) catalysis, which generates alcohols through the reduction of ketones, is an attractive protocol that is used widely. Ruthenium(II) complexes are the most useful catalysts for the hydrogen transfer (HT) of ketones. In this method, a highly active catalytic system employs a transition metal as a catalyst to synthesize alcohols, and is a replacement for the hydrogen-using hydrogenation process. The most active system is based on Ru, Rh and Ir, which includes a nitrogen ligand that facilitates the formation of a catalytically active hydride and phosphorus

  13. A survey of phthalate esters in consumer cosmetic products.

    Science.gov (United States)

    Hubinger, Jean C

    2010-01-01

    Certain phthalate esters have been shown to cause reproductive toxicity in animal models. For this reason, the FDA has been monitoring the use of phthalate esters in cosmetics. In this study, the U.S. Food and Drug Administration (FDA) conducted a limited survey of 84 adult-use and baby-care cosmetic products for the presence of five phthalate esters: dimethyl phthalate (DMP), diethyl phthalate (DEP), benzylbutyl phthalate (BBP), dibutyl phthalate (DBP), and diethylhexyl phthalate (DEHP) (Figure 1). The analytes were extracted from a cosmetic product/Celite mixture with hexane, and the extract was then analyzed using reversed-phase high-performance chromatography (HPLC) on an instrument equipped with an ultraviolet radiation (UV) detector set at 230 nm. The analytes were separated on a Partisil octadecylsilane (ODS)-3 column (250 mm × 4.6 mm I.D., 5μm). The mobile phase consisted of a mixture of 50% water, 34% acetonitrile, 13% 2-propanol, and 3% methanol that was changed linearly (35 minutes) to 15% water, 55% acetonitrile, 25% 2-propanol, and 5% methanol and held for an additional ten minutes. Spiked recoveries in antiperspirant and nail color ranged from 88% to 104%. Thirty-one of the 60 adult-use cosmetic products were found to contain at least one phthalate ester. Twenty products contained DEP and 11 nail products contained DBP. Concentrations of DBP ranged from 123 μg/g to 62,607 μg/g. Concentrations of DEP ranged from 80 μg/g to 36,006 μg/g. Five of the 24 baby-care products contained DEP at concentrations ranging from 10 μg/g to 274 μg/g.

  14. 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)

  15. Preparation and characterization of Pt catalysts supported on TiO{sub 2} and ZrO{sub 2} stabilized with La{sub 2}O{sub 3} for the elimination of nitric oxide; Preparacion y caracterizacion de catalizadores de Pt soportado en TiO{sub 2} y ZrO{sub 2} estabilizados con La{sub 2}O{sub 3} para la eliminacion de oxido nitrico

    Energy Technology Data Exchange (ETDEWEB)

    Aguilar V, A

    2001-07-01

    The objective of this work is the preparation and characterization of catalytic materials with a platinum base, supported in simple and mixed oxides of titanium (TiO{sub 2}) and zirconia (ZrO{sub 2}) which were stabilized with 10 % in mole of lanthanum (La{sub 2}O{sub 3}), the preparation technique of the supports is the one of precipitation, additioning a nominal charge of 1% in weight of active phase (Pt) by means of the impregnation method by conventional wetting. All the solids were calcinated at 500 Centigrade and subsequently reduced to the same temperature in air and hydrogen flow respectively. Their characterization was applying the techniques such as: Thermal gravimetric analysis (TGA), Differential scanning calorimetry (DSC), Surface area (BET), X-ray diffraction (XRD), Scanning electron microscopy (SEM), Decomposition of 2-propanol, Catalytic activity and selectivity. The application of these techniques allow to define and to explain the influence of the preparation method and of the thermal treatments to which were submitted the catalysts, in special the Surface area, X-ray diffraction and Scanning electron microscopy which demonstrated in evidence the morphologic structure and of crystalline phases present in the catalysts under study. The decomposition of 2-propanol, catalytic activity and selectivity show the supports and catalysts skill for the determination of acid or base sites, moreover of the selective reduction of nitric oxide respectively, the results seem to indicate that the preparation technique, precursors and the thermal treatments to what these materials were submitted have an influence on the catalyst and by consequence in the reduction reaction of nitric oxide. (Author)

  16. Preparation and characterization of Pt catalysts supported on TiO2 and ZrO2 stabilized with La2O3 for the elimination of nitric oxide

    International Nuclear Information System (INIS)

    The objective of this work is the preparation and characterization of catalytic materials with a platinum base, supported in simple and mixed oxides of titanium (TiO2) and zirconia (ZrO2) which were stabilized with 10 % in mole of lanthanum (La2O3), the preparation technique of the supports is the one of precipitation, additioning a nominal charge of 1% in weight of active phase (Pt) by means of the impregnation method by conventional wetting. All the solids were calcinated at 500 Centigrade and subsequently reduced to the same temperature in air and hydrogen flow respectively. Their characterization was applying the techniques such as: Thermal gravimetric analysis (TGA), Differential scanning calorimetry (DSC), Surface area (BET), X-ray diffraction (XRD), Scanning electron microscopy (SEM), Decomposition of 2-propanol, Catalytic activity and selectivity. The application of these techniques allow to define and to explain the influence of the preparation method and of the thermal treatments to which were submitted the catalysts, in special the Surface area, X-ray diffraction and Scanning electron microscopy which demonstrated in evidence the morphologic structure and of crystalline phases present in the catalysts under study. The decomposition of 2-propanol, catalytic activity and selectivity show the supports and catalysts skill for the determination of acid or base sites, moreover of the selective reduction of nitric oxide respectively, the results seem to indicate that the preparation technique, precursors and the thermal treatments to what these materials were submitted have an influence on the catalyst and by consequence in the reduction reaction of nitric oxide. (Author)

  17. Determination of Odor Release in Hydrocolloid Model Systems Containing Original or Carboxylated Cellulose at Different pH Values Using Static Headspace Gas Chromatographic (SHS-GC Analysis

    Directory of Open Access Journals (Sweden)

    Pahn-Shick Chang

    2013-02-01

    Full Text Available Static headspace gas chromatographic (SHS-GC analysis was performed to determine the release of 13 odorants in hydrocolloid model systems containing original or regio-selectively carboxylated cellulose at different pH values. The release of most odor compounds was decreased in the hydrocolloid solutions compared to control, with the amounts of 2-propanol, 3-methyl-1-butanol, and 2,3-butanedione released into the headspace being less than those of any other odor compound in the hydrocolloid model systems. However, there was no considerable difference between original cellulose-containing and carboxylated-cellulose containing systems in the release of most compounds, except for relatively long-chain esters such as ethyl caprylate and ethyl nonanoate. The release from the original and carboxylated cellulose solutions controlled to pH 10 was significantly higher than that from solutions adjusted to pH 4 and 7 in the case of some esters (ethyl acetate, methyl propionate, ethyl propionate, ethyl butyrate, butyl propionate, ethyl caproate and alcohols (2-propanol, 3-methyl-1-butanol, in particular, ethyl butyrate and 3-methyl-1-butanol. In contrast, the release of 2,3-butanedione from both the original and carboxylated cellulose solutions was increased at pH 4 and 7 compared to that at pH 10 by about 70% and 130%, respectively. Our study demonstrated that the release of some odorants could be changed significantly by addition of both original and carboxylated cellulose in hydrocolloid model systems, but only minor effect was observed in pH of the solution.

  18. Inactivation of murine norovirus by chemical biocides on stainless steel

    Directory of Open Access Journals (Sweden)

    Steinmann Jörg

    2009-07-01

    Full Text Available Abstract Background Human norovirus (NoV causes more than 80% of nonbacterial gastroenteritis in Europe and the United States. NoV transmission via contaminated surfaces may be significant for the spread of viruses. Therefore, measures for prevention and control, such as surface disinfection, are necessary to interrupt the dissemination of human NoV. Murine norovirus (MNV as a surrogate for human NoV was used to study the efficacy of active ingredients of chemical disinfectants for virus inactivation on inanimate surfaces. Methods The inactivating properties of different chemical biocides were tested in a quantitative carrier test with stainless steel discs without mechanical action. Vacuum-dried MNV was exposed to different concentrations of alcohols, peracetic acid (PAA or glutaraldehyde (GDA for 5 minutes exposure time. Detection of residual virus was determined by endpoint-titration on RAW 264.7 cells. Results PAA [1000 ppm], GDA [2500 ppm], ethanol [50% (v/v] and 1-propanol [30% (v/v] were able to inactivate MNV under clean conditions (0.03% BSA on the carriers by ≥ 4 log10 within 5 minutes exposure time, whereas 2-propanol showed a reduced effectiveness even at 60% (v/v. Furthermore, there were no significant differences in virus reduction whatever interfering substances were used. When testing with ethanol, 1- and 2-propanol, results under clean conditions were nearly the same as in the presence of dirty conditions (0.3% BSA plus 0.3% erythrocytes. Conclusion Products based upon PAA, GDA, ethanol and 1-propanol should be used for NoV inactivation on inanimate surfaces. Our data provide valuable information for the development of strategies to control NoV transmission via surfaces.

  19. Stoichiometric adsorption complexes in H-ZSM-5, H-ZSM-12, and H-mordenite zeolites

    Energy Technology Data Exchange (ETDEWEB)

    Kofke, T.J.G.; Gorte, R.J.; Kokotailo, G.T. (Univ. of Pennsylvania, Philadelphia (USA)); Farneth, W.E. (E.I. duPont de Nemours and Company, Wilmington, DE (USA))

    1989-01-01

    In order to understand the chemical properties of acid sites in zeolites, the authors have been examining the adsorption of simple molecules which can undergo classical acid-catalyzed chemistry in high-silica H-ZSM-5. For many molecules, including a series of alcohols, toluene, 2-propanamine, and 2-propanone, the authors have found that, following adsorption and evacuation, a well-defined adsorption complex corresponding to one molecule per Al site could be obtained. Furthermore, the unimolecular reactivities of the molecules in these 1 : 1 adsorption complexes were consistent with solution-phase, Bronsted acid-catalyzed chemistry and were unaffected by the Al concentration for SiO{sub 2}/Al{sub 2}O{sub 3} ratios from 38 to 520. These results imply that the active acid sites in H-ZSM-5 are identical and are present in a concentration of one/Al atom. This is consistent with conclusions reached from n-hexane cracking studies on H-ZSM-5. In order to examine the effect of solid-state structure on these acid sites, the authors extended their previous work to two other zeolites. H-ZSM-12 and H-mordenite. The adsorption of 2-propanol and 2-propanamine were chosen for study since the 1 : 1 complexes formed by these two molecules were the most distinctive in our previous adsorption studies. The authors show in this paper that 2-propanol and 2-propanamine also form clearly defined, 1 : 1 adsorption complexes with the Al site in H-ZSM-12 and H-mordenite. The reactivity of these adsorption complexes is identical to the reactivity of the 1 : 1 adsorption complexes formed by these molecules in H-ZSM-5. The complexes decompose at the same temperatures and form the same products on all three zeolites. This is strong evidence that the acid sites formed by isolated Al atoms in a zeolite lattice are chemically equivalent, independent of the structure of the lattice.

  20. Simultaneous derivatization and ultrasound-assisted dispersive liquid-liquid microextraction of chloropropanols in soy milk and other aqueous matrices combined with gas-chromatography-mass spectrometry.

    Science.gov (United States)

    Carro, A M; González, P; Lorenzo, R A

    2013-12-01

    A novel approach involving ultrasound-assisted dispersive liquid-liquid microextraction (UA-DLLME) and derivatization combined with gas chromatography-mass spectrometry was developed for the determination of chloropropanols in water and beverages. UA-DLLME was optimized as less solvent-consuming and cost-effective extraction method for water, fruit juice, milk and soy milk samples. The effect of parameters such as the type and volume of extraction solvent, the type and volume of dispersive solvent, amount of derivatization agent, temperature, pH of sample and ionic strength was investigated and optimized for each specimen, using experimental designs. By adding acetonitrile as dispersive solvent, N-heptafluorobutyrylimizadole (HFBI) as derivatization agent and chloroform as extraction solvent, the extraction-derivatization and preconcentration were simultaneously performed. The analytical concentration range was investigated in detail for each analyte in the different samples, obtaining linearity with R(2) ranging between 0.9990 and 0.9999. The method detection limits were in the range of 0.2-1.8μgL(-1) (water), 0.5-15μgL(-1) (fruit juices) and 0.9-3.6μgkg(-1) (milk) and 0.1-1.0μgkg(-1) (soy milk). The method was applied to the analysis of a variety of specimens, with recoveries of 98-101% from water, 97-102% from juices, 99-103% from milk and 97-105% from soy beverage. The relative standard deviation (precision, n=6) varied between 1.3 and 4.9%RSD in water, 2.3 and 5.8%RSD in juices, 1.0 and 5.7%RSD in milk and 3.9 and 9.3%RSD in soy milk. The proposed method was applied to analysis of twenty-eight samples. 1,3-Dichloro-2-propanol was found in an influent water sample from urban wastewater treatment plant (WWTP) (2.1±0.04mgL(-1)) but no chloropropanols were found in the corresponding effluent water sample. This result suggests that the purification system used in the WWTP has been effective for this compound. Moreover, the results revealed the presence of 3

  1. Soporte de Nuevas Películas de TiO2 y TiO2/SiO2 sobre Gránulos de Poliéster para Aplicación en Fotocatálisis Support of New TiO2 and TiO2/SiO2 Films on Polyester Granules for Photocatalytic Applications

    Directory of Open Access Journals (Sweden)

    Juan M Marín

    2008-01-01

    Full Text Available Películas de TiO2 o TiO2/SiO2 fueron soportadas sobre gránulos de poliéster usando mecanismos de difusión y posterior tratamiento térmico a 100ºC. Se emplearon dos clases de geles. El primero fue preparado usando diferentes cantidades de TiO2, cloruro de metileno y silicona líquida. El segundo fue obtenido por medio del método sol-gel, empleado para producir una matriz de sílice a partir de la hidrólisis el tetraetilo ortosilicato, en un medio orgánico de 2-propanol, en el cual se dispersó el fotocatalizador. Los precursores de cada sistema fueron agregados en diferentes relaciones para determinar su influencia en la estabilidad, propiedades y fotoactividad de las películas. La actividad fotocatalítica fue evaluada en la fotodegradación de metanol en fase gaseosa. Los resultados muestran la producción de materiales con alta resistencia, funcionalidad y actividad así como una fuerte relación entre la actividad fotocatalítica con las propiedades fisicoquímicas.Films of TiO2 and of TiO2/SiO2 were supported on polyester granules using a diffusion mechanism and a posterior thermal treatment to 100ºC. Two kinds of gels were used. The first one was prepared using different amounts of TiO2, methylene chloride and liquid silicone. The second one used the sol-gel method to produce a silica matrix by adding tetraethyl orthosilicate, water and 2- propanol. After that the photocatalyst was dispersed in the gel. The precursors of each system were added in different amounts to determine their influence in the stability, properties and photoactivity of the films. The photocatalytic activity was tested in the methanol photodegradation in gas phase. The results show the production of materials with high resistance, functionality and activity as well as a strong dependence between the photocatalityc activity and efficiency with the physicochemical properties of the films.

  2. Efecto del Potasio en Catalizadores CoMo/g-Al2O3-K(x sobre el Hidrotratamiento de Naftas Effect of Potassium in CoMo/g-Al2O3-K(x Catalysts on Naphtha Hydrotreating

    Directory of Open Access Journals (Sweden)

    David J Pérez-Martínez

    2009-01-01

    Full Text Available Se prepararon catalizadores CoMo soportados en g-Al2O3 modificada con potasio (K, 1, 3 y 5% en masa y se evaluaron en reacciones simultáneas de hidrodesulfuración (HDS de 2-metiltiofeno e hidrogenación de olefinas (trimetil-1-penteno y trimetil-2-penteno. Las propiedades ácido-base de los catalizadores se determinaron utilizando desorción de amoniaco con temperatura programada (TPD y la reacción de descomposición de 2-propanol. El área superficial BET y la acidez de los catalizadores CoMo/g-Al2O3-K(x disminuyeron con el incremento en el contenido de K, mientras que la selectividad hidrodesulfuración/hidrogenación de olefinas internas (HDS/HID aumentó. Sin embargo, la actividad de los catalizadores disminuyó en todas las reacciones. La comparación con la literatura permitió establecer que las modificaciones en la estructura y dispersión de la fase activa provocadas por la introducción del potasio no son las causantes de la disminución en la actividad.CoMo catalysts supported on g-Al2O3 modified with potassium (K, 1, 3 and 5 wt% were prepared and evaluated in simultaneous hydrodesulfurization (HDS of 2-methyltiophene and hydrogenation of olefins (trimethyl-1-pentene to trimethyl-2-pentene ratio reactions. The acid-base properties of the catalysts were measured by ammonia temperature-programmed desorption (TPD and by the decomposition reaction of 2-propanol. Results showed that the BET surface area and the acidity of catalysts modified with potassium decreased when the potassium concentration increased as long as hydrodesulfurization/ hidrogenation (HDS/HYD of internal olefins increased. However, the activity of the modified catalysts decreased for all reactions. Comparison with literature information allowed establishing that modifications in the structure and dispersion of the active phase caused by the introduction of potassium are not the responsible for the activity decrease.

  3. Assessment of lead distribution in aquatic plant Lemna minor, using sequential extraction procedure

    International Nuclear Information System (INIS)

    Complete text of publication follows. The contamination of water resources by toxic metals demands for attention since this kind of contamination, sometimes, is difficult to realize. Moreover, lead, for instance, has the capacity to be accumulated in fish and plants utilized in the food, and also in human beings, causing several disturbances. Phytoremediation is an emerging technology that employs the use of plants for the clean-up of contaminated environments. The model plant Lemna minor is a genera of Duckweed plant, and refers to a group of floating, flowering plants of the family Lemnaceae. The aquatic plant Lemna minor is relevant to many aquatic environments, including lakes, streams, effluent, rain, and sediment. The aquatic plant Lemna minor has been studied due its potential to extract lead from contaminated waters. The aim of this study was to determine the distribution of Pb in the aquatic plant Lemna minor under stress, using a modified sequential extraction with different solvents: hexane, ethyl acetate, 2-propanol, methanol, ethanol/water (1:1) and water. Non-extractable residues formed the last fraction. Elemental distributions in the plants were determined using flame atomic absorption spectroscopy (F AAS), and scanning electron microscopy coupled with energy dispersive X-ray microanalysis (SEM-EDX). It was found that the aquatic plant L. minor has the capacity to accumulate lead: in the first day of contamination, about 79% of lead had been intake by the plant. After 7 days, the Pb content was 142 mg Kg-1. After sequential extraction, the methanol and ethanol/water fractions were dominants: 27 and 45% of total content, respectively. In these fractions we can find acids that form specific chelating agents, such as oligopeptides (phytochelatins). The hexane, ethyl acetate, and 2-propanol fractions gave the smallest isolated fraction. These fractions consisted of non-polar lipid compounds. Elemental distribution by X-ray fluorescence spectra and maps

  4. 介质阻挡放电对湖泊水华蓝藻的去除%Removal of water bloom cyanobacteria in lake by dielectric barrer discharge

    Institute of Scientific and Technical Information of China (English)

    王家齐; 郑宾国; 刘群; 张继彪; 罗兴章; 郭飞宏; 郑正

    2012-01-01

    In this study, non-thermal plasma produced by dielectric barrer discharge (DBD) was employed to remove the water bloom cyanobacteria in Taihu Lake. The effects of discharge power, air flow rate, various additives (2-propanol and humic acid) on the removal efficiency of cyanobacteria were discussed. The result showed that the cyanobacteria could be removed by DBD. With 100 W of discharge power, 1.0 L/min of air flow rate, 18 min of discharge time, 2 000 lx of light intensity and $ d of culture time at 25~C , the removal efficiency over 87.8% (the initial Chl-a concentration of cyanobaeteria was 9.58 rag/L). The removal efficiency increased with the increasing of discharge power and air flow rate. The presences of humic acid enhanced the cyanobacteri- al removal, while the addition of 2-propanol inhibited the cyanobacterial removal. The concentrations of carote- noids and malondialdehyde, the activity of superoxide dismutase in cyanobacterial cell changed after treatment, the intracellular materials of cyanobacteria were damaged.%采用介质阻挡放电等离子体技术去除太湖水华蓝藻,考察了放电输出功率、空气流速、添加剂(异丙醇、腐植酸)等对蓝藻去除的影响。结果表明,介质阻挡放电能去除太湖水华蓝藻,放电功率100 W,空气流速1.0 L/min,放电18min,在光照强度2 000 lx和25℃下培养4 d,初始叶绿素a浓度为9.58 mg/L藻液中蓝藻去除率达87.8%。增加放电输出功率和空气流速能提高蓝藻的去除效率;腐植酸促进了介质阻挡放电对蓝藻的去除;而异丙醇添加剂抑制了介质阻挡放电的作用。放电处理后,蓝藻细胞内类胡萝卜素含量、SOD活性、MDA含量发生明显变化,介质阻挡放电破坏了蓝藻细胞内含物。

  5. Selective microwave sensors exploiting the interaction of analytes with trap states in TiO2 nanotube arrays

    Science.gov (United States)

    Zarifi, M. H.; Farsinezhad, S.; Abdolrazzaghi, M.; Daneshmand, M.; Shankar, K.

    2016-03-01

    Sensing of molecular analytes by probing the effects of their interaction with microwaves is emerging as a cheap, compact, label-free and highly sensitive detection and quantification technique. Microstrip ring-type resonators are particularly favored for this purpose due to their planar sensing geometry, electromagnetic field enhancements in the coupling gap and compatibility with established printed circuit board manufacturing. However, the lack of selectivity in what is essentially a permittivity-sensing method is an impediment to wider adoption and implementation of this sensing platform. By placing a polycrystalline anatase-phase TiO2 nanotube membrane in the coupling gap of a microwave resonator, we engineer selectivity for the detection and differentiation of methanol, ethanol and 2-propanol. The scavenging of reactive trapped holes by aliphatic alcohols adsorbed on TiO2 is responsible for the alcohol-specific detection while the different short chain alcohols are distinguished on the basis of differences in their microwave response. Electrodeless microwave sensors which allow spectral and time-dependent monitoring of the resonance frequency and quality factor provide a wealth of information in comparison with electrode-based resistive sensors for the detection of volatile organic compounds. A high dynamic range (400 ppm-10 000 ppm) is demonstrated for methanol detection.Sensing of molecular analytes by probing the effects of their interaction with microwaves is emerging as a cheap, compact, label-free and highly sensitive detection and quantification technique. Microstrip ring-type resonators are particularly favored for this purpose due to their planar sensing geometry, electromagnetic field enhancements in the coupling gap and compatibility with established printed circuit board manufacturing. However, the lack of selectivity in what is essentially a permittivity-sensing method is an impediment to wider adoption and implementation of this sensing platform

  6. Sol-gel processing of metal sulfides

    Science.gov (United States)

    Stanic, Vesha

    germanium mercaptide evolved during the sol-gel processing of GeSsb2. The titrations were performed in 2-propanol or in a 50-50 vol % mixture of 2-propanol and toluene. The ion selective Ag/Agsb2S electrode was used for equivalence point detection. Study of the Nernst equation shows that complexes were formed at the electrode surface. However, the titration equivalence point volume clearly demonstrates the formation of Agsb2S and Ge(SAg)sbn. In order to explain this discrepancy a new electrode reaction mechanism and a modified Ag/Agsb2S electrode potential equation are proposed. Effects of hydrogen sulfide and germanium ethoxide concentrations, the concentration ratio and temperature on the microstructure of the prepared GeSsb2 gels were studied. It was found that the concentrations of the reactants have the most significant influence on gel structure.

  7. Using a water-immiscible ionic liquid to improve asymmetric reduction of 4-(trimethylsilyl-3-butyn-2-one catalyzed by immobilized Candida parapsilosis CCTCC M203011 cells

    Directory of Open Access Journals (Sweden)

    Smith Thomas J

    2009-10-01

    Full Text Available Abstract Background Whole cells are usually employed for biocatalytic reduction reactions to ensure efficient coenzyme regeneration and to avoid problems with enzyme purification and stability. The efficiency of whole cell-catalyzed bioreduction is frequently restricted by pronounced toxicity of substrate and/or product to the microbial cells and in many instances the use of two-phase reaction systems can solve such problems. Therefore, we developed new, biphasic reaction systems with biocompatible water-immiscible ionic liquids (ILs as alternatives to conventional organic solvents, in order to improve the asymmetric reduction of 4-(trimethylsilyl-3-butyn-2-one (TMSB to (S-4-(trimethylsilyl-3-butyn-2-ol {(S-TMSBOL}, a key intermediate for synthesis of 5-lipoxygenase inhibitors, using immobilized Candida parapsilosis CCTCC M203011 cells as the biocatalyst. Results Various ILs exerted significant but different effects on the bioreduction. Of all the tested water-immiscible ILs, the best results were observed with 1-butyl-3-methylimidazolium hexafluorophosphate (C4MIM·PF6, which exhibited not only good biocompatibility with the cells but also excellent solvent properties for the toxic substrate and product, thus markedly improving the efficiency of the bioreduction and the operational stability of the cells as compared to the IL-free aqueous system. 2-Propanol was shown to be the most suitable co-substrate for coenzyme regeneration, and it was found that the optimum volume ratio of buffer to C4MIM·PF6, substrate concentration, buffer pH, 2-propanol concentration and reaction temperature were 4/1 (v/v, 24 mM, 5.5, 130 mM and 30°C, respectively. Under these optimized conditions, the maximum yield and the product e.e. wer 97.7% and >99%, respectively, which are much higher than the corresponding values previously reported. The efficient whole-cell biocatalytic process was shown to be feasible on a 250-mL scale. Conclusion The whole cell

  8. Industrial Acetogenic Biocatalysts: A Comparative Metabolic and Genomic Analysis

    Science.gov (United States)

    Bengelsdorf, Frank R.; Poehlein, Anja; Linder, Sonja; Erz, Catarina; Hummel, Tim; Hoffmeister, Sabrina; Daniel, Rolf; Dürre, Peter

    2016-01-01

    Synthesis gas (syngas) fermentation by anaerobic acetogenic bacteria employing the Wood–Ljungdahl pathway is a bioprocess for production of biofuels and biocommodities. The major fermentation products of the most relevant biocatalytic strains (Clostridium ljungdahlii, C. autoethanogenum, C. ragsdalei, and C. coskatii) are acetic acid and ethanol. A comparative metabolic and genomic analysis using the mentioned biocatalysts might offer targets for metabolic engineering and thus improve the production of compounds apart from ethanol. Autotrophic growth and product formation of the four wild type (WT) strains were compared in uncontrolled batch experiments. The genomes of C. ragsdalei and C. coskatii were sequenced and the genome sequences of all four biocatalytic strains analyzed in comparative manner. Growth and product spectra (acetate, ethanol, 2,3-butanediol) of C. autoethanogenum, C. ljungdahlii, and C. ragsdalei were rather similar. In contrast, C. coskatii produced significantly less ethanol and its genome sequence lacks two genes encoding aldehyde:ferredoxin oxidoreductases (AOR). Comparative genome sequence analysis of the four WT strains revealed high average nucleotide identity (ANI) of C. ljungdahlii and C. autoethanogenum (99.3%) and C. coskatii (98.3%). In contrast, C. ljungdahlii WT and C. ragsdalei WT showed an ANI-based similarity of only 95.8%. Additionally, recombinant C. ljungdahlii strains were constructed that harbor an artificial acetone synthesis operon (ASO) consisting of the following genes: adc, ctfA, ctfB, and thlA (encoding acetoacetate decarboxylase, acetoacetyl-CoA:acetate/butyrate:CoA-transferase subunits A and B, and thiolase) under the control of thlA promoter (PthlA) from C. acetobutylicum or native pta-ack promoter (Ppta-ack) from C. ljungdahlii. Respective recombinant strains produced 2-propanol rather than acetone, due to the presence of a NADPH-dependent primary-secondary alcohol dehydrogenase that converts acetone to 2

  9. Efeito da fertilização nitrogenada em videira sobre a formação de alguns compostos volatéis no vinho Effect of vineyard nitrogen fertilization on the formation of some wine volatile coumpounds

    Directory of Open Access Journals (Sweden)

    Lúcia Schuch Boeira

    1995-01-01

    Full Text Available Vitis vinifera cv. Gewürztraminer e Cabemet Sauvignon cultivadas em Santana do Livramento e Garibaldi foram submetidas a diferentes tratamentos nitrogenados realizados durante o período vegetativo de 1992-1993. Após a colheita e esmagamento o mosto obtido foi dividido em quatro lotes e fermentado com diferentes leveduras. As determinações dos compostos voláteis foram realizados através de cromatografia gasosa. Maiores valores de metanol foram encontrados nos vinhos de Cabemet Sauvignon (máximo 225,6mg/l. A fertilização nitrogenada provocou um aumento na concentração (mg/l de propanol-1 (min. 25 -máx. 78,2 e uma diminuição de metil-2 propanol-1 (min. 60,8 - máx. 125,9 e metil-3 + metil-2 butanol-1 (min. 85,8 - máx. 407,8 nos vinhos. Os álcoois superiores apresentaram também diferenças em relação à região, cultivar e levedura utilizada.Vitis vinifera Gewürztraminer (white variety and Cabemet Sauvignon (red growned in Santana do Livramento, RS, and Garibaldi, RS, were added with different nitrogen treatments in the vineyard during me 1992-1993 season. After harvest and crushing, the musts were divided into four lots each one added with a different yeast. The volatiles were analyzed through GC. Maximum amount of methanol was found with the red variety (225.6mg/l. Increasing nitrogen in the soil increased (mg/l propanol-1 (min. 25-max. 78.2 and decreased methyl-2 propanol-1 (min. 60.8-max. 125.9 and methyl-3+methyl-2 butanol-1 (min. 85.8-max. 407.8. The fusel alcohol fraction showed, also, differences between region,grape variety and yeast used.

  10. Catabolism of methyl ter-butyl ether (MTBE): characterization of the enzymes of Mycobacterium austroafricanum IFP 2012 involved in MTBE degradation; Catabolisme du methyl tert-butyl ether (MTBE): caracterisation des enzymes impliquees dans la degradation du MTBE chez Mycobacterium austroafricanum IFP 2012

    Energy Technology Data Exchange (ETDEWEB)

    Lopes Ferreira, N.

    2005-11-15

    Methyl tert-butyl ether (MTBE) is added to gasoline to meet the octane index requirement. its solubility in water and its poor biodegradability made the use of MTBE a great environmental concern, particularly regarding aquifers. We previously isolated M austroafricanum IFP 2012 able to use MTBE as a sole source of carbon and energy and the MTBE pathway was partially characterized. In the present study, which aimed at isolating the genes involved in MTBE biodegradation in order to use them for estimation of MTBE biodegradation capacities in contaminated environment, we isolated a new M. austroafricanum strain, IFP 2015. A new degradation intermediate, the 2-methyl 1,2-propane-diol (2-M1,2-PD), the product of tert-butanol (TBA) oxidation, was identified. We also determined the enzymes induced during growth of M. austroafricanum IFP 2012 on MTBF. Then, using the tools of protein analysis and of molecular biology, we isolated and cloned the mpd genes cluster in the plasmid pCL4D. Heterologous expression of the recombinant plasmid in M smegmatis tmc2 155, showed the involvement of an 2-M1,2-PD dehydrogenase (MpdB) and a hydroxy-iso-butyr-aldehyde dehydrogenase (MpdC), encoded by mpdB and mpdC, respectively. Both enzymes were responsible for the conversion of 2-M 1,2-PD to hydroxy-isobutyric acid (HIBA). A further survey of different M austroafricanum strains, including IFP 2012, IFP 2015 and JOBS (ex-M vaccae) showed the link between the ability to grow on C{sub 2} to C{sub 16} n-alkanes and the MTBE and TBA degradation capacities. The alkB gene was partially sequenced in all these strains. Expression of alkB was demonstrated in M. austroafricanum IFP 2012 after growth on propane, hexane, hexadecane and TBA. Finally, we identified 2-propanol as the intermediate of HIBA degradation. The gene encoding the 2-propanol:p-N,N'-dimethyl-4-nitroso-aniline (NDMA) oxidoreductase was detected M austroafricanum IFP 2012. (author)

  11. Extraction and separation of zinc and cadmium chlorides by TOPO from mixed media

    International Nuclear Information System (INIS)

    The effect of water-miscible alcohols and acetone on the extraction and separation of Cd and Zn chlorides by TOPO was systematically investigated. The maximum extraction of Zn chloride with 0.1 M TOPO decreases in the order: acetone > methanol > ethanol > 2-propanol > 2-butanol. For alcohols, the sequence of decreasing extractability is thus parallel to the order of their dielectric constants. This can be explained by the increase of HCl extraction by TOPO in the same direction. The presence of additives in the polar phase prevents the formation of a bulky white precipitate encountered during extraction of ZnCl2 from pure aqueous solutions. A decrease of Cd chloride extraction was generally noticed in presence of additives; this is more noticeable for the longer chain alcohols. The highest separation factor (E) for ZnCl2 and CdCl2 in 0.48 M HCl is obtained from 30% methanol (13.8 compared to about 3.8 in absence of methanol) and from 10-20% acetone where it reaches 30. (author)

  12. Identification of Wet-Spinning and Post-Spin Stretching Methods Amenable to Recombinant Spider Aciniform Silk.

    Science.gov (United States)

    Weatherbee-Martin, Nathan; Xu, Lingling; Hupe, Andre; Kreplak, Laurent; Fudge, Douglas S; Liu, Xiang-Qin; Rainey, Jan K

    2016-08-01

    Spider silks are outstanding biomaterials with mechanical properties that outperform synthetic materials. Of the six fibrillar spider silks, aciniform (or wrapping) silk is the toughest through a unique combination of strength and extensibility. In this study, a wet-spinning method for recombinant Argiope trifasciata aciniform spidroin (AcSp1) is introduced. Recombinant AcSp1 comprising three 200 amino acid repeat units was solubilized in a 1,1,1,3,3,3-hexafluoro-2-propanol (HFIP)/water mixture, forming a viscous α-helix-enriched spinning dope, and wet-spun into an ethanol/water coagulation bath allowing continuous fiber production. Post-spin stretching of the resulting wet-spun fibers in water significantly improved fiber strength, enriched β-sheet conformation without complete α-helix depletion, and enhanced birefringence. These methods allow reproducible aciniform silk fiber formation, albeit with lower extensibility than native silk, requiring conditions and methods distinct from those previously reported for other silk proteins. This provides an essential starting point for tailoring wet-spinning of aciniform silk to achieve desired properties.

  13. Factors controlling volatile organic compounds in dwellings in Melbourne, Australia.

    Science.gov (United States)

    Cheng, M; Galbally, I E; Molloy, S B; Selleck, P W; Keywood, M D; Lawson, S J; Powell, J C; Gillett, R W; Dunne, E

    2016-04-01

    This study characterized indoor volatile organic compounds (VOCs) and investigated the effects of the dwelling characteristics, building materials, occupant activities, and environmental conditions on indoor VOC concentrations in 40 dwellings located in Melbourne, Australia, in 2008 and 2009. A total of 97 VOCs were identified. Nine VOCs, n-butane, 2-methylbutane, toluene, formaldehyde, acetaldehyde, d-limonene, ethanol, 2-propanol, and acetic acid, accounted for 68% of the sum of all VOCs. The median indoor concentrations of all VOCs were greater than those measured outdoors. The occupant density was positively associated with indoor VOC concentrations via occupant activities, including respiration and combustion. Terpenes were associated with the use of household cleaning and laundry products. A petroleum-like indoor VOC signature of alkanes and aromatics was associated with the proximity of major roads. The indoor VOC concentrations were negatively correlated (P < 0.05) with ventilation. Levels of VOCs in these Australian dwellings were lower than those from previous studies in North America and Europe, probably due to a combination of an ongoing temporal decrease in indoor VOC concentrations and the leakier nature of Australian dwellings. PMID:25788118

  14. Magnetically responsive enzyme powders

    Energy Technology Data Exchange (ETDEWEB)

    Pospiskova, Kristyna, E-mail: kristyna.pospiskova@upol.cz [Regional Centre of Advanced Technologies and Materials, Palacky University, Slechtitelu 11, 783 71 Olomouc (Czech Republic); Safarik, Ivo, E-mail: ivosaf@yahoo.com [Regional Centre of Advanced Technologies and Materials, Palacky University, Slechtitelu 11, 783 71 Olomouc (Czech Republic); Department of Nanobiotechnology, Institute of Nanobiology and Structural Biology of GCRC, Na Sadkach 7, 370 05 Ceske Budejovice (Czech Republic)

    2015-04-15

    Powdered enzymes were transformed into their insoluble magnetic derivatives retaining their catalytic activity. Enzyme powders (e.g., trypsin and lipase) were suspended in various liquid media not allowing their solubilization (e.g., saturated ammonium sulfate and highly concentrated polyethylene glycol solutions, ethanol, methanol, 2-propanol) and subsequently cross-linked with glutaraldehyde. Magnetic modification was successfully performed at low temperature in a freezer (−20 °C) using magnetic iron oxides nano- and microparticles prepared by microwave-assisted synthesis from ferrous sulfate. Magnetized cross-linked enzyme powders were stable at least for two months in water suspension without leakage of fixed magnetic particles. Operational stability of magnetically responsive enzymes during eight repeated reaction cycles was generally without loss of enzyme activity. Separation of magnetically modified cross-linked powdered enzymes from reaction mixtures was significantly simplified due to their magnetic properties. - Highlights: • Cross-linked enzyme powders were prepared in various liquid media. • Insoluble enzymes were magnetized using iron oxides particles. • Magnetic iron oxides particles were prepared by microwave-assisted synthesis. • Magnetic modification was performed under low (freezing) temperature. • Cross-linked powdered trypsin and lipase can be used repeatedly for reaction.

  15. Single Pulse Remote Raman Detection of Minerals and Organics Under Illuminated Condition from 10 Meters Distance

    Science.gov (United States)

    Misra, A. K.; Sharma, S. K.; Lucey, P. G.

    2005-01-01

    A directly coupled portable remote Raman instrument developed by the University of Hawaii has been shown here to identify several minerals, chemicals and organics from a distance of 10 m using a single laser pulse in a well illuminated background. Raman spectra, obtained during a very short period of time, of common minerals e.g., dolomite, calcite, marble, barite, gypsum, quarts, rutile, fluorapatite etc. clearly show Raman features which could be used as fingerprints for mineral identification. Raman features of organics such as benzene, cyclohexane, 2-propanol, naphthalene, etc. and other chemicals containing various functional groups like oxides, silicates, sulphates, nitrates, phosphates and carbonates were also easily detected. Ability to measure Raman spectra with a single laser pulse would be promising for future space missions where power consumption is critical and a rapid survey of the minerals with moderate to high Raman cross section might be desirable for selecting rocks that would provide high scientific return or for acquiring rocks for sample return to the Earth.

  16. Novel Ordered Mesoporous Carbon Based Sulfonic Acid as an Efficient Catalyst in the Selective Dehydration of Fructose into 5-HMF: the Role of Solvent and Surface Chemistry.

    Science.gov (United States)

    Karimi, Babak; Mirzaei, Hamid M; Behzadnia, Hesam; Vali, Hojatollah

    2015-09-01

    Novel ionic liquid derived ordered mesoporous carbons functionalized with sulfonic acid groups IOMC-ArSO3H and GIOMC-ArSO3H were prepared, characterized, and examined in the dehydration reaction of fructose into 5-hydroxymethylfurfural (5-HMF) both in aqueous and nonaqueous systems. To study and correlate the surface properties of these carbocatalysts and some other SBA-15 typed solid acids with 5-HMF yield, hydrophilicity index (H-index) were employed in the fructose dehydration. Our study systematically declared that almost a criterion may be expected for application of solid acids in which by increasing H-index value up to 0.8 the HMF yield enhances accordingly. More increase in H-index up to 1.3 did not change the HMF yield profoundly. Although, it has been shown that the catalyst with larger H-index (∼1.3) resulted in higher activity both in aqueous and 2-propanol systems, during the recycling process deactivation occurs because of more water uptake and the catalysts with optimum amount of H-index (∼0.8) is more robust in the dehydration of fructose. PMID:26259108

  17. Determination and correlation of the solubility of four Brønsted-acidic ionic liquids based on benzothiazolium cations in six alcohols

    International Nuclear Information System (INIS)

    Highlights: • Solubility of four acidic benzothiazolium cations-based ILs was measured. • The solubilities vary with the polarity of the solvent. • The solubility of some ILs is with “temperature-sensitive” property. • The measured solubilities were correlated by Apelblat model and λh model. • The dissolution enthalpy and entropy of ILs were calculated using the van’t Hoff equation. - Abstract: Solubilities of four acidic ionic liquids based on benzothiazolium cations in six alcohols (methanol, ethanol, 1-propanol, 2-propanol, 1-butanol and 2-methyl-1-propanol) from at temperatures from (253 to 384) K were determined using a static equilibrium method under atmospheric pressure. The modified Apelblat equation and λh equation were employed to correlate the experimental data with good agreement. The solubilities of ILs increase with increasing temperature. It is interesting to find that the solubility of some ILs in alcohols are with “temperature-sensitive” properties. The solubility is related with the polarity and molecular structures of the solvent, as well as the strength of hydrogen bonding between alcohols and anionic groups of ILs. The dissolution enthalpy and entropy of ILs were calculated by the van’t Hoff equation. This study provides useful information for further research and application of the ionic liquids

  18. Electrophoretic deposition of ZnO nanostructures: Au nanoclusters on Si substrates induce self-assembled nanowire growth

    Energy Technology Data Exchange (ETDEWEB)

    Sandoval, Claudia [Laboratorio de Nanomateriales y Propiedades Dieléctricas, Facultad de Ciencias Exactas y Tecnología, Universidad Nacional de Tucumán, San Miguel de Tucumán (Argentina); Marin, Oscar [CONICET – LAFISO, Facultad de Ciencias Exactas y Tecnología, Universidad Nacional de Tucumán, San Miguel de Tucumán (Argentina); Real, Silvina [Laboratorio de Nanomateriales y Propiedades Dieléctricas, Facultad de Ciencias Exactas y Tecnología, Universidad Nacional de Tucumán, San Miguel de Tucumán (Argentina); Comedi, David [CONICET – LAFISO, Facultad de Ciencias Exactas y Tecnología, Universidad Nacional de Tucumán, San Miguel de Tucumán (Argentina); Tirado, Mónica, E-mail: mtirado@herrera.unt.edu.ar [Laboratorio de Nanomateriales y Propiedades Dieléctricas, Facultad de Ciencias Exactas y Tecnología, Universidad Nacional de Tucumán, San Miguel de Tucumán (Argentina)

    2014-09-15

    Highlights: • ZnO nanowires were grown on silicon substrate by electrophoretic deposition technique without use a porous template. • The growth was induced by Au nanoclusters and was performed at room temperature. • The photoluminescence spectrum for the nanowires obtained shows a broad UV-blue excitonic emission peak and a low emission in the green region. - Abstract: The present work reports the self-assembled growth of ZnO nanowires on silicon substrate with nanometer sized Au clusters using electrophoretic deposition technique at room temperature without a sacrificial template. A colloidal suspension of ≈5 nm sized ZnO nanoparticles dispersed in 2-propanol was used (nanoparticle bandgap of 3.47 eV as determined from absorbance measurements). The results show that the Au nanoclusters on the silicon substrate induce the self-assembly of the ZnO nanoparticles into vertically aligned ZnO nanowires. This effect is tentatively explained as being due to increased electric field intensities near the Au nanoclusters during the electrophoretic deposition. Photoluminescence measurements reveal the presence of quantum confined excitons and a relatively low concentration of deep defects in the nanowires. The electric field guided growth of semiconductor nanostructures at room temperature has great industrial potential as it minimizes production costs and enables the use of substrate materials not withstanding high temperatures.

  19. Large Mesopore Generation in an Amorphous Silica-Alumina by Controlling the Pore Size with the Gel Skeletal Reinforcement and Its Application to Catalytic Cracking

    Directory of Open Access Journals (Sweden)

    Hiroyuki Nasu

    2012-09-01

    Full Text Available Tetraethoxy orthosilicate (TEOS was used not only as a precursor of silica, but also as an agent which reinforces the skeleton of silica-gel to prepare an aerogel and resultant silica and silica-alumina with large pore size and pore volume. In this gel skeletal reinforcement, the strength of silica aerogel skeleton was enhanced by aging with TEOS/2-propanol mixed solution to prevent the shrink of the pores. When silica aerogel was reinforced by TEOS solution, the pore diameter and pore volume of calcined silica could be controlled by the amount of TEOS solution and reached 30 nm and 3.1 cm3/g. The results from N2 adsorption measurement indicated that most of pores for this silica consisted of mesopores. Silica-alumina was prepared by the impregnation of an aluminum tri-sec-butoxide/2-butanol solution with obtained silica. Mixed catalysts were prepared by the combination of β-zeolite (26 wt% and prepared silica-aluminas with large mesopore (58 wt% and subsequently the effects of their pore sizes on the catalytic activity and the product selectivity were investigated in catalytic cracking of n-dodecane at 500 °C. The mixed catalysts exhibited not only comparable activity to that for single zeolite, but also unique selectivity where larger amounts of branched products were formed.

  20. Bio-inspired 2-line ferrihydrite as a high-capacity and high-rate-capability anode material for lithium-ion batteries

    Science.gov (United States)

    Hashimoto, Hideki; Ukita, Masahiro; Sakuma, Ryo; Nakanishi, Makoto; Fujii, Tatsuo; Imanishi, Nobuyuki; Takada, Jun

    2016-10-01

    A high-capacity and high-rate-capability anode material for lithium-ion batteries, silicon-doped iron oxyhydroxide or 2-line ferrihydrite (2Fh), was prepared by mixing iron nitrate powder, tetraethyl orthosilicate, 2-propanol, and ammonium hydrogen carbonate powder at room temperature. The design of this material was inspired by a bacteriogenic product, a nanometric amorphous iron-based oxide material containing small amounts of structural Si. The atomistic structure of the prepared Si-doped 2Fh was strongly affected by the Si molar ratio [x = Si/(Fe + Si)]. Its crystallinity gradually decreased as the Si molar ratio increased, with a structural variation from nanocrystalline to amorphous at x = 0.25. The sample with x = 0.20 demonstrated the best Li storage performance. The developed material exhibited a high capacity of ∼400 mAh g-1 at the 25th cycle in the voltage range of 0.3-3.0 V and at a current rate of 9 A g-1, which was three times greater than that of the Si-free 2Fh. This indicates that Si-doping into the 2Fh structure realizes good rate capability, which are presumably because of the specific nanocomposite structure of iron-based electrochemical centers embedded in the Si-based amorphous matrix, generated by reversible Li insertion/deinsertion process.

  1. Improvement of the Dimensional Stability of Powder Injection Molded Compacts by Adding Swelling Inhibitor into the Debinding Solvent

    Science.gov (United States)

    Fan, Yang-Liang; Hwang, Kuen-Shyang; Su, Shao-Chin

    2008-02-01

    Defects are frequently found in powder injection molded (PIM) compacts during solvent debinding due to the swelling of the binders. This problem can be alleviated by adjusting the composition of the debinding solvent. In this study, 10 vol pct swelling inhibitors were added into heptane, and the in-situ amounts of swelling and sagging of the specimen in the solvent were recorded using a noncontacting laser dilatometer. The results show that the addition of ethanol, 2-propanol, 1-butanol, and 1-pentanol reduced the amounts of swelling by 31, 21, 17, and 11 pct, respectively. This was because the small molecule alcohols, which do not dissolve paraffin wax (PW) or stearic acid (SA) in the binder system, could diffuse easily into the specimen and increased the portion of the swelling inhibitor inside. The amount of the extracted PW and SA also decreased, but only by 8.3, 6.1, 4.3, and 2.4 pct, respectively. The solubility parameters of 1-bromopropane (n-PB) and ethyl acetate (EA) are between those of heptane and alcohols, and they also yielded a slight reduction in the amounts of swelling by 6 and 11 pct, respectively. These results suggest that to reduce defects caused by binder swelling during solvent debinding, alcohols with high solubility parameters can be added into heptane without sacrificing significantly on the debinding rate.

  2. Degradation of phorbol 12,13-diacetate in aqueous solution by gamma irradiation

    Science.gov (United States)

    Kongmany, Santi; Furuta, Masakazu; Matsuura, Hiroto; Okuda, Shuichi; Imamura, Kiyoshi; Maeda, Yasuaki

    2014-12-01

    Phorbol esters (PEs) are highly toxic compounds that cause skin irritation, inflammation, and tumor promotion upon contact with humans or animals. These compounds are naturally present in Jatropha curcas L. To promote the use of J. curcas seed oil in bio-diesel production industries and reduce environmental concerns, it is necessary to find methods of degrading PEs. In this study, the degradation of phorbol 12,13-diacetate (PDA), as a representative PE, in aqueous solution at a concentration of 10 mg/L by 60Co-γ-irradiation was investigated. The results demonstrate that PDA was effectively degraded by this treatment and the degradation efficiency increased with the absorbed dose within the range of 0.5-3 kGy. Complete degradation of PDA was achieved at a dose of 3 kGy. In the presence of radical scavengers (i.e., methanol, tert-butanol, 2-propanol), reactive species from water radiolysis were scavenged, and significant inhibition of PDA degradation was observed at absorbed doses less than 1 kGy. In the presence of nitrous oxide, the generation of hydroxyl radicals (rad OH) was promoted during gamma irradiation and PDA degradation was drastically enhanced.

  3. Effect of water miscible organic solvents on p-nitrophenol hydroxylase (CYP2E1 activity in rat liver microsomes

    Directory of Open Access Journals (Sweden)

    Pranali G Patil

    2015-01-01

    Full Text Available Organic solvents used for solubilization of the substrates/NCEs are known to affect the activity of cytochrome P450 enzymes. Further, this effect varies with the solvents used, the substrates and CYP450 isoforms in question. In the present study, we have investigated the effect of ten commonly used water miscible organic solvents (methanol, ethanol, 1-propanol, 2-propanol, acetonitrile, acetone, dimethyl sulphoxide, N,N-dimethyl formamide, dioxane and polyethylene glycol 400 on p-nitrophenol hydroxylase activity at 0, 0.1, 0.25, 0.5, 0.75 and 1% v/v concentration in rat liver microsomes. All the solvents studied showed concentration dependent inhibition of the p-nitrophenol hydroxylase activity except acetonitrile which showed activation of the activity at concentration range studied. Out of ten solvents studied, dioxane was found to be the most inhibitory solvent (inhibition >90% at 0.25% v/v concentration. Overall, solvents like dimethyl sulphoxide, dimethyl formamide and dioxane appeared to be unsuitable for characterizing p-nitrophenol hydroxylase (CYP2E1-mediated reactions due to a high degree of inhibition. On the other hand, methanol and acetonitrile at concentrations <0.5% v/v appeared to be appropriate solvents for substrate solubilization while evaluating CYP2E1-mediated catalysis. The results of this study imply that caution should be exercised while choosing solvents for dissolution of substrate during enzyme studies in liver microsomes.

  4. Fast gas chromatography and negative-ion chemical ionization tandem mass spectrometry for forensic analysis of cannabinoids in whole blood.

    Science.gov (United States)

    Thomas, Aurélien; Widmer, Christèle; Hopfgartner, Gérard; Staub, Christian

    2007-11-01

    The present work describes a fast gas chromatography/negative-ion chemical ionization tandem mass spectrometric assay (Fast GC/NICI-MS/MS) for analysis of tetrahydrocannabinol (THC), 11-hydroxy-tetrahydrocannabinol (THC-OH) and 11-nor-9-carboxy-tetrahydrocannabinol (THC-COOH) in whole blood. The cannabinoids were extracted from 500 microL of whole blood by a simple liquid-liquid extraction (LLE) and then derivatized by using trifluoroacetic anhydride (TFAA) and hexafluoro-2-propanol (HFIP) as fluorinated agents. Mass spectrometric detection of the analytes was performed in the selected reaction-monitoring mode on a triple quadrupole instrument after negative-ion chemical ionization. The assay was found to be linear in the concentration range of 0.5-20 ng/mL for THC and THC-OH, and of 2.5-100 ng/mL for THC-COOH. Repeatability and intermediate precision were found less than 12% for all concentrations tested. Under standard chromatographic conditions, the run cycle time would have been 15 min. By using fast conditions of separation, the assay analysis time has been reduced to 5 min, without compromising the chromatographic resolution. Finally, a simple approach for estimating the uncertainty measurement is presented. PMID:17913432

  5. Determination of calcium stearate in polyolefin samples by gas chromatographic technique after performing dispersive liquid-liquid microextraction.

    Science.gov (United States)

    Ranji, Ali; Ghorbani Ravandi, Mahboobeh; Farajzadeh, Mir Ali

    2008-05-01

    In this study, a gas chromatographic method is presented for the determination of calcium stearate after its conversion to stearic acid in a polymeric matrix. A solution of hydrochloric acid in 2-propanol is used as an extracting solvent of calcium stearate and its converter to stearic acid. For stearic acid preconcentration before its injection to a separation system, a recently presented extraction method, dispersive liquid-liquid microextraction, using carbon tetrachloride as an extracting solvent is used. Finally, 1 microL of the organic phase collected at the bottom of a conical test tube after centrifuging is injected into a gas chromatograph (GC) for quantification. This method has a relatively broad linear dynamic range (50 - 2000 mg/L) with a limit of detection (LOD) of 15 mg/L for stearic acid in solution. The LOD of the proposed method in a polymeric sample using 10 mg of polymer is 60 ppm as calcium stearate. Some effective parameters, such as the time and temperature of heating, the concentration of hydrochloric acid and the volume of distilled water, were studied. PMID:18469468

  6. Crystallization and preliminary characterization of three different crystal forms of human saposin C heterologously expressed in Pichia pastoris

    Energy Technology Data Exchange (ETDEWEB)

    Schultz-Heienbrok, Robert [Institut für Chemie und Biochemie/Kristallographie, Freie Universität Berlin (Germany); Remmel, Natascha; Klingenstein, R. [Kekule-Institut für Organische Chemie und Biochemie, Rheinische Friedrich-Wilhelms-Universität Bonn (Germany); Rossocha, Maksim [Institut für Chemie und Biochemie/Kristallographie, Freie Universität Berlin (Germany); Sandhoff, Konrad [Kekule-Institut für Organische Chemie und Biochemie, Rheinische Friedrich-Wilhelms-Universität Bonn (Germany); Saenger, Wolfram [Institut für Chemie und Biochemie/Kristallographie, Freie Universität Berlin (Germany); Maier, Timm, E-mail: timm.maier@mol.biol.ethz.ch [Institut für Chemie und Biochemie/Kristallographie, Freie Universität Berlin (Germany); Institute for Molecular Biology and Biophysics, Swiss Federal Institute of Technology, ETH Zürich (Switzerland)

    2006-02-01

    Three different crystal forms were obtained of human saposin C. The structures could not be determined by molecular replacement using known solution structures of the protein as search models, supporting the notion of a highly flexible protein. The amphiphilic saposin proteins (A, B, C and D) act at the lipid–water interface in lysosomes, mediating the hydrolysis of membrane building blocks by water-soluble exohydrolases. Human saposin C activates glucocerebrosidase and β-galactosylceramidase. The protein has been expressed in Pichia pastoris, purified and crystallized in three different crystal forms, diffracting to a maximum resolution of 2.5 Å. Hexagonal crystals grew from 2-propanol-containing solution and contain a single molecule in the asymmetric unit according to the Matthews coefficient. Orthorhombic and tetragonal crystals were both obtained with pentaerythritol ethoxylate and are predicted to contain two molecules in the asymmetric unit. Attempts to determine the respective crystal structures by molecular replacement using either the known NMR structure of human saposin C or a related crystal structure as search models have so far failed. The failure of the molecular-replacement method is attributed to conformational changes of the protein, which are known to be required for its biological activity. Crystal structures of human saposin C therefore might be the key to mapping out the conformational trajectory of saposin-like proteins.

  7. Phenol recovery by BPA tar hydrolysis in supercritical water; Chorinkaisuichu deno BPA tar no kasui bunkai ni yoru phenol no kaishu

    Energy Technology Data Exchange (ETDEWEB)

    Adschiri, T. Shibata, R.; Arai, K. [Tohoku University, Sendai (Japan). Faculty of Engineering

    1997-07-01

    Bisphenol-A (BPA) tar which is a heavy residue of petrochemical plant distillation is examined for efficient recovery in supercritical water. BPA is decomposed in supercritical water at 673K under 20-38MPa, when 2-(4-hydroxyphenyl)-2-propanol (HPP) and phenol are produced thanks to hydrolysis. HPP is further hydrolyzed for the production of phenol or 4-isopropylphenol. With an increase in supercritical water, the hydrolysis of HPP grows dominant, enabling a high yield of phenol. This is because an increase in water density results in an increase the dielectric constant, which stabilizes polar-activated intermediates for the acceleration of hydrolysis. Even in the actual processing of BPA tar, hydrolysis can procede while the formation of polymers is suppressed, and this reaction advances more efficiently when the water density is higher. The maximum phenol yield is 40wt% or higher against the raw material, equivalent to a phenol structure recovery rate of 60mol%. 12 refs., 9 figs., 1 tab.

  8. Photodegradation of estrone enhanced by dissolved organic matter under simulated sunlight

    KAUST Repository

    Caupos, Emilie

    2011-05-01

    In the present work the degradation of estrone (E1) a natural estrogenic hormone has been studied under simulated solar irradiation. The photodegradation of E1 has been investigated in the absence and in the presence of 7.7-8.9 mg L-1 of dissolved organic carbon (DOC), under solar light simulation with irradiance approximating that of the sun. DOC extracts from different origins have been used. Half-lives ranging between 3.9 h and 7.9 h were observed. Results indicated that E1 was photodegraded even in the absence of DOC. The presence of DOC was found to enhance the degradation of E1. Experiments performed with the addition of reactive species scavengers (azide ions and 2-propanol) have shown that these two species play a significant role in the photodegradation. Some experiments have been performed with a DOC previously submitted to solar irradiation. Changes in optical and physico-chemical properties of DOC strongly affect its photoinductive properties, and hence its efficiency on E1 degradation. A part of the study consisted in the investigation of photoproducts structures. Five photoproducts were shown by chromatographic analysis: one arising from direct photolysis and the four others from DOC photoinduced degradation. © 2011 Elsevier Ltd.

  9. Desalination of aqueous solutions by LTA and MFI zeolite membranes using pervaporation method

    Directory of Open Access Journals (Sweden)

    A. Malekpour

    2011-12-01

    Full Text Available LTA and MFI zeolite membranes were hydrothermally grown on the surface of an α-alumina porous support. The synthesized membranes were used for removal of cationic and anionic species from aqueous solutions by the pervaporation method. The perfection of the membranes was improved by employing the multi-stage synthesis method. The membranes were characterized by XRD, SEM and IR methods. The membranes were initially evaluated by the pervaporation separation of water from aqueous 2-propanol mixtures. The separation factors obtained were 7081 and 105 for NaA and ZSM-5 membranes, respectively. The ability of membranes for desalination of some aqueous solutions containing I-, Cs+ and Sr2+ ions was examined in various conditions. These ionic species were chosen because of their importance in the nuclear sciences. Both membranes effectively removed (more than 99 wt% I-, Cs+ and Sr2+ from their singlesalt solutions (0.001mol dm-3 over a temperature range of 298-338 K. The effects of parameters such as time and temperature on the separation factors and fluxes were investigated. This work shows that, due to their excellent chemical, thermal and mechanical stability, the zeolitic membranes are useful for desalination of aqueous solutions and treating saline wastewaters by pervaporation. Therefore, this method has the ability to desalinate harsh environment solutions involving strong solvent and radioactive components.

  10. High-Quality Perovskite Films Grown with a Fast Solvent-Assisted Molecule Inserting Strategy for Highly Efficient and Stable Solar Cells.

    Science.gov (United States)

    Yuan, Shuai; Qiu, Zhiwen; Gao, Chaomin; Zhang, Hailiang; Jiang, Yanan; Li, Cuncheng; Yu, Jinghua; Cao, Bingqiang

    2016-08-31

    The performance of organolead halide perovskites based solar cells has been enhanced dramatically due to the morphology control of the perovskite films. In this paper, we present a fast solvent-assisted molecule inserting (S-AMI) strategy to grow high-quality perovskite film, in which the methylammonium iodide/2-propanol (MAI/IPA) solution is spin-coated onto a dimethylformamide (DMF) wetted mixed lead halide (PbX2) precursor film. The DMF can help the inserting of MAI molecules into the PbX2 precursor film and provide a solvent environment to help the grain growth of the perovskite film. The perovskite film grown by the S-AMI approach shows large and well-oriented grains and long carrier lifetime due to the reduced grain boundary. Solar cells constructed with these perovskite films yield an average efficiency over 17% along with a high average fill factor of 80%. Moreover, these unsealed solar cell devices exhibit good stability in an ambient atmosphere. PMID:27526617

  11. Understanding Solvent Effects on the Properties of Two-Dimensional Transition Metal Dichalcogenides.

    Science.gov (United States)

    Choi, Jungwook; Zhang, Hanyu; Du, Haodong; Choi, Jong Hyun

    2016-04-13

    Two-dimensional (2D) transition metal dichalcogenides (TMDCs) have emerged as attractive direct bandgap semiconducting materials with remarkable properties. Recently, TMDC-based electronic and optoelectronic systems have been demonstrated with various chemical doping and functionalization approaches for modulating their physical properties and enhancing device performances. However, the dependence of intrinsic properties of TMDCs on diverse solvents, which are used necessarily in fabrication processes and chemical doping, remains largely unaddressed. Here we report a charge transfer mechanism in TMDCs by commonly used solvents such as chloroform, toluene, acetone, and 2-propanol, which significantly changes the physical properties of monolayer MoS2 and WSe2. We find that the relative difference in electronegativity between solvents and TMDCs drives the transfer of electrons from or to the TMDCs, which results in photoluminescence (PL) enhancement or quenching depending on the change of carrier density in TMDCs. The analysis of exciton and trion spectral weights in MoS2 as a function of solvent electronegativity provides evidence of charge transfer. Finally, conductive atomic force microscopy (C-AFM) on TMDCs before and after immersion in the solvents further supports the charge transfer mechanism and resulting changes in carrier density. Our results highlight the importance of selection of solvents for solution-processed 2D TMDC devices and systems. PMID:27018600

  12. Effect of the propanol-water volume ratios on the properties of SnO2 nanocrystals

    Science.gov (United States)

    Rakgalakane, B. P.; Sikhwivhilu, L. M.; Moloto, M. J.; van Wyk, J.; Moloto, N.

    2015-01-01

    Herein we report on the tuning of the morphologies of SnO2 nanocrystals (NCs) by varying the water-propanol volume ratios during the microwave synthesis. Our results show the change in morphology from spherical, when pure water is a solvent, to oriented attachment and then nanotubes, as the solvent mixture is increased from 1:1 to 2:3 to 3:2 propanol-water volume ratios. Furthermore electrical properties of solution processed thin films of the as-prepared SnO2 NCs were investigated. The 2:3 ratio sample showed the lowest resistivity of 0.95 mΩ cm. Annealing of the sample at different temperatures had an effect in electrical properties with an oscillatory trend with annealing temperature being observed. In addition there was an initial decrease in particle size upon annealing and the oriented attachment mechanism seen at room temperature was dismantled. There was subsequent increase in particle size with an increase on temperature due to Ostwald ripening.

  13. Extruded expanded polystyrene sheets coated by TiO{sub 2} as new photocatalytic materials for foodstuffs packaging

    Energy Technology Data Exchange (ETDEWEB)

    Loddo, V.; Marci, G. [Schiavello-Grillone Photocatalysis Group - Dipartimento di Ingegneria Elettrica, Elettronica e delle Telecomunicazioni, di tecnologie Chimiche, Automatica e modelli Matematici - Universita degli Studi di Palermo, Viale delle Scienze (Ed. 6) - 90128 Palermo (Italy); Palmisano, G., E-mail: giovanni_palmisano@yahoo.it [Schiavello-Grillone Photocatalysis Group - Dipartimento di Ingegneria Elettrica, Elettronica e delle Telecomunicazioni, di tecnologie Chimiche, Automatica e modelli Matematici - Universita degli Studi di Palermo, Viale delle Scienze (Ed. 6) - 90128 Palermo (Italy); Yurdakal, S. [Kimya Boeluemue, Fen-Edebiyat Fakueltesi, Afyon Kocatepe Ueniversitesi - Ahmet Necdet Sezer Kampuesue - 03200 Afyon (Turkey); Brazzoli, M.; Garavaglia, L. [Sirap-Gema S.p.A. - Via Industriale, 1/3 - 25028 Verolanuova (Brescia) (Italy); Palmisano, L., E-mail: leonardo.palmisano@unipa.it [Schiavello-Grillone Photocatalysis Group - Dipartimento di Ingegneria Elettrica, Elettronica e delle Telecomunicazioni, di tecnologie Chimiche, Automatica e modelli Matematici - Universita degli Studi di Palermo, Viale delle Scienze (Ed. 6) - 90128 Palermo (Italy)

    2012-11-15

    Highlights: Black-Right-Pointing-Pointer An extruded polystyrene has been functionalised by TiO{sub 2}. Black-Right-Pointing-Pointer A photocatalytic polymer has been developed via a sol-gel method. Black-Right-Pointing-Pointer Thermoformed packagings for foodstuffs application have been prepared. - Abstract: Nanostructured, photoactive anatase TiO{sub 2} sol prepared under very mild conditions using titanium tetraisopropoxide as the precursor is used to functionalise extruded expanded polystyrene (XPS) sheets by spray-coating resulting in stable and active materials functionalised by TiO{sub 2} nanoparticles. Photocatalytic tests of these sheets performed in a batch reactor in gas-solid system under UV irradiation show their successful activity in degrading probe molecules (2-propanol, trimethylamine and ethene). Raman spectra ensure the deposition of TiO{sub 2} as crystalline anatase phase on the polymer surface. The presence of TiO{sub 2} with respect to polymer surface can be observed in SEM images coupled to EDAX mapping allowing to monitor the surface morphology and the distribution of TiO{sub 2} particles. Finally thermoforming of these sheets in industrial standard equipment leads to useful containers for foodstuffs.

  14. Enhanced photo-degradation of paracetamol on n-platinum-loaded TiO2: The effect of ultrasound and OH/hole scavengers.

    Science.gov (United States)

    Ziylan-Yavaş, Asu; Ince, Nilsun H

    2016-11-01

    Elimination/mineralization of paracetamol (PCT) was investigated by catalytic oxidation under ultrasound, UV and both. The catalyst was synthesized by immobilization of nPt on TiO2 to benefit from the ability of Pt to facilitate charge transfer processes and to separate e(-)/h(+) pairs. It was found that increasing the Pt-loading enhanced the rate of sonochemical reactions, but retarded that of photolytic reactions, due to reduced UV absorption on the surface. Simultaneous application of sonolysis and photolysis was synergistic due to disaggregation of the particles and homogenization of the active species over the catalyst surface. The decay of PCT was highly dependent on the availability of OH, as the reactions were nearly terminated in the presence of a strong OH scavenger-2-propanol. However, a remarkable rate enhancement was observed in the presence of a suitable dose of I(-), which scavenges both OH and hvb(+). The result was explained by the production of excess radicals upon sonolysis of iodide solutions, and the reactivity of PCT with them. Finally, carbon mineralization was significantly hindered in the presence of both scavengers due to increased competition for OH and inefficient formation of hydroquinone arising from reduced availability of hvb(+). PMID:27518924

  15. Molecular level water and solute transport in reverse osmosis membranes

    Science.gov (United States)

    Lueptow, Richard M.; Shen, Meng; Keten, Sinan

    2015-11-01

    The water permeability and rejection characteristics of six solutes, methanol, ethanol, 2-propanol, urea, Na+, and Cl-, were studied for a polymeric reverse osmosis (RO) membrane using non-equilibrium molecular dynamics simulations. Results indicate that water flux increases with an increasing fraction of percolated free volume in the membrane polymer structure. Solute molecules display Brownian motion and hop from pore to pore as they pass through the membrane. The solute rejection depends on both the size of the solute molecule and the chemical interaction of the solute with water and the membrane. When the open spaces in the polymeric structure are such that solutes have to shed at least one water molecule from their solvation shell to pass through the membrane molecular structure, the water-solute pair interaction energy governs solute rejection. Organic solutes more easily shed water molecules than ions to more readily pass through the membrane. Hydrogen-bonding sites for molecules like urea also lead to a higher rejection. These findings underline the importance of the solute's solvation shell and solute-water-membrane chemistry in solute transport and rejection in RO membranes. Funded by the Institute for Sustainability and Energy at Northwestern with computing resources from XSEDE (NSF grant ACI-1053575).

  16. Calcium phosphate/microgel composites for 3D powderbed printing of ceramic materials.

    Science.gov (United States)

    Birkholz, Mandy-Nicole; Agrawal, Garima; Bergmann, Christian; Schröder, Ricarda; Lechner, Sebastian J; Pich, Andrij; Fischer, Horst

    2016-06-01

    Composites of microgels and calcium phosphates are promising as drug delivery systems and basic components for bone substitute implants. In this study, we synthesized novel composite materials consisting of pure β-tricalcium phosphate and stimuli-responsive poly(N-vinylcaprolactam-co-acetoacetoxyethyl methacrylate-co-vinylimidazole) microgels. The chemical composition, thermal properties and morphology for obtained composites were extensively characterized by Fourier transform infrared, X-ray photoelectron spectroscopy, IGAsorp moisture sorption analyzer, thermogravimetric analysis, granulometric analysis, ESEM, energy dispersive X-ray spectroscopy and TEM. Mechanical properties of the composites were evaluated by ball-on-three-balls test to determine the biaxial strength. Furthermore, initial 3D powderbed-based printing tests were conducted with spray-dried composites and diluted 2-propanol as a binder to evaluate a new binding concept for β-tricalcium phosphate-based granulates. The printed ceramic bodies were characterized before and after a sintering step by ESEM. The hypothesis that the microgels act as polymer adhesive agents by efficient chemical interactions with the β-tricalcium phosphate particles was confirmed. The obtained composites can be used for the development of new scaffolds. PMID:25870955

  17. Determination of alcohol compounds using corona discharge ion mobility spectrometry

    Institute of Scientific and Technical Information of China (English)

    HAN Hai-yan; HUANG Guo-dong; JIN Shun-ping; ZHENG Pei-chao; XU Guo-hua; LI Jian-quan; WANG Hong-mei; CHU Yan-nan

    2007-01-01

    Ion mobility spectrometry (IMS) is a very fast, highly sensitive, and inexpensive technique, it permits efficient monitoring of volatile organic compounds like alcohols. In this article, positive ion mobility spectra for six alcohol organic compounds have been systematically studied for the first time using a high-resolution IMS apparatus equipped with a discharge ionization source. Utilizing protonated water cluster ions (H2O)nH+ as the reactant ions and clean air as the drift gas, alcohol organic compounds, ethanol, 1-propanol, 2-propanol, 1-butanol, 1-pentanol and 2-octanol, all exhibit product ion characteristic peaks in their respective ion mobility spectrometry, that is a result of proton transfer reactions between the alcohols and reaction ions (H2O)nH+. The mixture of these alcohols, including two isomers, has been detected, and the result shows that they can also be distinguished effectively in the ion mobility spectrum. The reduced mobility values have been determined, which are in very well agreement with the traditional 63Ni-IMS experimental values. The exponential dilution method was used to calibrate the alcohol concentrations, and a detection limit available for the alcohols is in order of magnitude of a few ng/L.

  18. Enhanced bioactivity of ZnO nanoparticles-an antimicrobial study

    Energy Technology Data Exchange (ETDEWEB)

    Padmavathy, Nagarajan; Vijayaraghavan, Rajagopalan [School of Science and Humanities-Materials Division, VIT University, Vellore - 632 014, Tamil Nadu (India)], E-mail: rvijayaraghavan@vit.ac.in

    2008-07-01

    In this study, we investigate the antibacterial activity of ZnO nanoparticles with various particle sizes. ZnO was prepared by the base hydrolysis of zinc acetate in a 2-propanol medium and also by a precipitation method using Zn(NO{sub 3}){sub 2} and NaOH. The products were characterized by x-ray diffraction (XRD) analysis, transmission electron microscopy (TEM) and photoluminescence (PL) spectroscopy. Bacteriological tests such as minimum inhibitory concentration (MIC) and disk diffusion were performed in Luria-Bertani and nutrient agar media on solid agar plates and in liquid broth systems using different concentrations of ZnO by a standard microbial method for the first time. Our bacteriological study showed the enhanced biocidal activity of ZnO nanoparticles compared with bulk ZnO in repeated experiments. This demonstrated that the bactericidal efficacy of ZnO nanoparticles increases with decreasing particle size. It is proposed that both the abrasiveness and the surface oxygen species of ZnO nanoparticles promote the biocidal properties of ZnO nanoparticles.

  19. Simulated moving bed separation of tocopherol homologues: simulation and experiments

    Institute of Scientific and Technical Information of China (English)

    Yu-bin L(U); Bao-gen SU; Yi-wen YANG; Qi-long REN; Ping-dong WU

    2009-01-01

    Chromatograms of tocopherol homologues were obtained by a column of analytical size(inner diameter(ID)0.46 cm cm× 10 cm)packed with silica gel.Adsorption isotherms and film mass-transfer coefficient were estimated from the chromatograms by using a general rate model.which considers axial dispersion,external mass-transfer and intraparticle diffusion.Based on the obtained isotherms and mass-transfer coefficient.the separation process of tocopherol homologues on simulated moving impurities was separated on an SMB equipment.The SMB equipment was composed of 8 columns of ID 2 cm× 10 cm.with 2 columns in each section.The solid phase was silica gel,and the mobile phase was n-hexane/2-propanol(99/1 by volume).γ-and δ-tocopherols of purity greater than 98% were obtained with recovery greater than 98%.The effects of operating conditions (flow rates and switching time)on the performance of SMB were studied by both simulation and experiments.It was found that all the simulation results were quite close to the experimental results.We conclude that process development and optimization of operating conditions of SMB by simulation are feasible.

  20. Identification of volatile markers in potato brown rot and ring rot by combined GC-MS and PTR-MS techniques: study on in vitro and in vivo samples.

    Science.gov (United States)

    Blasioli, Sonia; Biondi, Enrico; Samudrala, Devasena; Spinelli, Francesco; Cellini, Antonio; Bertaccini, Assunta; Cristescu, Simona M; Braschi, Ilaria

    2014-01-15

    Ralstonia solanacearum (Rs) and Clavibacter michiganensis subsp. sepedonicus (Cms) are the bacterial causal agents of potato brown and ring rot, respectively, and are included in the A2 list of quarantine pathogens in Europe. Identification by GC-MS analysis of volatile organic compounds from Rs or Cms cultured on different nutrient media was performed. GC-MS and PTR-MS analysis were carried out also on unwounded potato tubers infected with the same pathogens. Infected tubers were produced by experimental inoculations of the plants. In in vitro experiments, Rs or Cms emitted volatile compounds, part of which were specific disease markers of potato (2-propanol and 3-methylbutanoic acid), mainly originating from bacterial metabolism (i.e., amino acid degradation, carbohydrate and fatty acid oxidation). In potato tubers, pathogen metabolism modified the volatile compound pattern emitted from healthy samples. Both bacteria seem to accelerate metabolic processes ongoing in potatoes and, in the case of Rs, disease markers (1-hepten-3-ol, 3,6-dimethyl-3-octanone, 3-ethyl-3-methylpentane, 1-chloroctane, and benzothiazole) were identified. PMID:24313381

  1. Thematic outlook. Technical outlook for the fuel-cell research network (PACo). August 8, 2002 update, no. 7; Veille thematique. La veille technique pour le reseau PACo. Actualisation du 8 aout 2002, no. 7

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2002-08-01

    This report brings together a compilation of abstracts of articles about some recent research works carried out in the domain of fuel cells, hydrogen production and hydrogen storage: characteristics of a PEM fuel cell submitted to a transient increase of CO concentration; perspectives of the different fuel cell technologies in transport applications; development of a portable fuel cell system for the soldier's equipment; direct 2-propanol low temperature fuel cell; a fuel cell system quasi-directly supplied with methanol and based on a mixture of electrolytic polymers; catalysis in low temperature fuel cells (part.1: the cathode stakes); manufacturing and performance of the new multi-layer cathodes for SOFCs; patent about intermediate plates for the limitation of the movement of the bolts used for the fastening of a fuel cell core; the Paul Sherrer institute is testing a zinc and synthetic gas production process that use solar energy, natural gas and zinc oxide; experimental evaluation of a combined plasma/catalyst system for the production of hydrogen from the partial oxidation of hydrocarbons; hydrogen production using a new chemo-organo-trophic bacteria: Citrobacter sp. Y19; hydrogen as energy vector: competition or complementarity with fossil fuels; hydrogen storage in general and in light monocrystalline metal hydrides in particular; the nuclear option for the production of hydrogen as energy of the future. (J.S.)

  2. Nanomaterials for the cleaning and pH adjustment of vegetable-tanned leather

    Science.gov (United States)

    Baglioni, Michele; Bartoletti, Angelica; Bozec, Laurent; Chelazzi, David; Giorgi, Rodorico; Odlyha, Marianne; Pianorsi, Diletta; Poggi, Giovanna; Baglioni, Piero

    2016-02-01

    Leather artifacts in historical collections and archives are often contaminated by physical changes such as soiling, which alter their appearance and readability, and by chemical changes which occur on aging and give rise to excessive proportion of acids that promote hydrolysis of collagen, eventually leading to gelatinization and loss of mechanical properties. However, both cleaning and pH adjustment of vegetable-tanned leather pose a great challenge for conservators, owing to the sensitivity of these materials to the action of solvents, especially water-based formulations and alkaline chemicals. In this study, the cleaning of historical leather samples was optimized by confining an oil-in-water nanostructured fluid in a highly retentive chemical hydrogel, which allows the controlled release of the cleaning fluid on sensitive surfaces. The chemical gel exhibits optimal viscoelasticity, which facilitates its removal after the application without leaving residues on the object. Nanoparticles of calcium hydroxide and lactate, dispersed in 2-propanol, were used to adjust the pH up to the natural value of leather, preventing too high alkalinity which causes swelling of fibers and denaturation of the collagen. The treated samples were characterized using scanning electron microscopy, controlled environment dynamic mechanical analysis, and infrared spectroscopy. The analytical assessment validated the use of tools derived from colloid and materials science for the preservation of collagen-based artifacts.

  3. Synthesis, characterization and application of naïve and nano-sized titanium dioxide as a photocatalyst for degradation of methylene blue

    Directory of Open Access Journals (Sweden)

    Arpita Pandey

    2015-09-01

    Full Text Available In the present work, photocatalytic degradation of methylene blue has been carried out using naïve titanium dioxide, nano-sized titanium dioxide and H2O2 under visible light. The catalysts, naïve and nano-sized titanium dioxide were prepared by the sol–gel method. Characterization of synthesized catalysts has been done by scanning electron microscopy (SEM, X-ray diffraction (XRD and UV–Visible spectroscopy. The rate of degradation of dye was monitored spectrophotometrically by measuring absorbance of dye at regular time intervals. The effect of various parameters such as pH, concentration of dye, amount of catalyst, amount of H2O2 and light intensity on the rate of reaction has been studied. Various parameters like chemical oxygen demand (COD, conductance, pH, TDS, salinity and dissolved oxygen (DO for the reaction mixture have also been determined. A tentative mechanism for degradation of dye has been proposed involving ·−OH radical as an oxidant. The participation of ·−OH radical has been confirmed by using 2-propanol (scavenger as the rate of reaction was drastically reduced in its presence.

  4. Oxygen Storage Capacity and Oxygen Mobility of Co-Mn-Mg-Al Mixed Oxides and Their Relation in the VOC Oxidation Reaction

    Directory of Open Access Journals (Sweden)

    María Haidy Castaño

    2015-05-01

    Full Text Available Co-Mn-Mg-Al oxides were synthesized using auto-combustion and co-precipitation techniques. Constant ratios were maintained with (Co + Mn + Mg/Al equal to 3.0, (Co + Mn/Mg equal to 1.0 and Co/Mn equal to 0.5. The chemical and structural composition, redox properties, oxygen storage capacity and oxygen mobility were analyzed using X-ray fluorescence (XRF, X-ray diffraction (XRD, Raman spectroscopy, scanning electron microscopy (SEM, temperature-programmed reduction of hydrogen (H2-TPR, oxygen storage capacity (OSC, oxygen storage complete capacity (OSCC and isotopic exchange, respectively. The catalytic behavior of the oxides was evaluated in the total oxidation of a mixture of 250 ppm toluene and 250 ppm 2-propanol. The synthesis methodology affected the crystallite size, redox properties, OSC and oxide oxygen mobility, which determined the catalytic behavior. The co-precipitation method got the most active oxide in the oxidation of the volatile organic compound (VOC mixture because of the improved mobility of oxygen and ability to favor redox processes in the material structure.

  5. Development and characterization of coaxially electrospun gelatin coated poly (3-hydroxybutyric acid) thin films as potential scaffolds for skin regeneration

    Energy Technology Data Exchange (ETDEWEB)

    Nagiah, Naveen [Bioproducts Lab, Central Leather Research Institute, Adyar, Chennai (India); Madhavi, Lakshmi; Anitha, R. [CavinKare Research Centre, Ekkattuthangal, Chennai (India); Anandan, C. [National Aerospace Laboratory, Banglore (India); Srinivasan, Natarajan Tirupattur, E-mail: naveen.nagiah@gmail.com [Conducting Polymers Lab, Department of Physics, Indian Institute of Technology Madras, Chennai (India); Sivagnanam, Uma Tirichurapalli, E-mail: suma67@gmail.com [Bioproducts Lab, Central Leather Research Institute, Adyar, Chennai (India)

    2013-10-01

    The morphology of fibers synthesized through electrospinning has been found to mimic extracellular matrix. Coaxially electrospun fibers of gelatin (sheath) coated poly (3-hydroxybutyric acid) (PHB) (core) was developed using 2,2,2 trifluoroethanol(TFE) and 1,1,1,3,3,3 hexafluoro-2-propanol(HFIP) as solvents respectively. The coaxial structure and coating of gelatin with PHB fibers was confirmed through transmission electron microscopy (TEM), scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). Thermal stability of the coaxially electrospun fibers was analyzed using thermogravimetric analysis(TGA), differential scanning calorimetry(DSC) and differential thermogravimetric analysis(DTA). Complete evaporation of solvent and gelatin grafting over PHB fibers was confirmed through attenuated total reflection-Fourier transformed infrared spectroscopy (ATR-FTIR). The coaxially electrospun fibers exhibited competent tensile properties for skin regeneration with high surface area and porosity. In vitro degradation studies proved the stability of fibers and its potential applications in tissue engineering. The fibers supported the growth of human dermal fibroblasts and keratinocytes with normal morphology indicating its potential as a scaffold for skin regeneration. - Highlights: • Coaxial electrospinning was employed to develop core-shell fibers of PHB and gelatin. • The scaffold has competent physicochemical properties. • Developed scaffold will have high impact as a dermal substitute in skin regeneration.

  6. Chain Confinement in Electrospun Nanocomposites: using Thermal Analysis to Investigate Polymer-Filler Interactions

    Energy Technology Data Exchange (ETDEWEB)

    Q Ma; B Mao; P Cebe

    2011-12-31

    We investigate the interaction of the polymer matrix and filler in electrospun nanofibers using advanced thermal analysis methods. In particular, we study the ability of silicon dioxide nanoparticles to affect the phase structure of poly(ethylene terephthalate), PET. SiO{sub 2} nanoparticles (either unmodified or modified with silane) ranging from 0 to 2.0 wt% in PET were electrospun from hexafluoro-2-propanol solutions. The morphologies of both the electrospun (ES) nanofibers and the SiO{sub 2} powders were observed by scanning and transmission electron microscopy, while the amorphous or crystalline nature of the fibers was determined by real-time wide-angle X-ray scattering. The fractions of the crystal, mobile amorphous, and rigid amorphous phases of the non-woven, nanofibrous composite mats were quantified by using heat capacity measurements. The amount of the immobilized polymer layer, the rigid amorphous fraction, was obtained from the specific reversing heat capacity for both as-spun amorphous fibers and isothermally crystallized fibers. Existence of the rigid amorphous phase in the absence of crystallinity was verified in nanocomposite fibers, and two origins for confinement of the rigid amorphous fraction are proposed. Thermal analysis of electrospun fibers, including quasi-isothermal methods, provides new insights to quantitatively characterize the polymer matrix phase structure and thermal transitions, such as devitrification of the rigid amorphous fraction.

  7. Linear and nonlinear optical studies of bare and copper doped TiO2 nanoparticles via sol gel technique

    Science.gov (United States)

    Rajamannan, B.; Mugundan, S.; Viruthagiri, G.; Praveen, P.; Shanmugam, N.

    2014-01-01

    In general, the nanoparticles of TiO2 may exist in the phases of anatase, rutile and brookite. In the present work, we used titanium terta iso propoxide and 2-propanol as a common starting material to prepare the precursors of bare and copper doped nanosized TiO2. Then the synthesized products were calcinated at 500 °C and after calcination the pure TiO2 nanoparticles in anatase phase were harvested. The crystallite sizes of bare and copper doped TiO2 nanoparticles were calculated from X-ray diffraction analysis. The existence of functional groups of the samples was identified by Fourier transform infrared spectroscopy. The optical properties of bare and doped samples were carried out using UV-DRS and photoluminescence measurements. The surface morphology and the element constitution of the copper doped TiO2 nanoparticles were studied by scanning electron microscope fitted with energy dispersive X-ray spectrometer arrangement. The nonlinear optical properties of the products were confirmed by Kurtz second harmonic generation (SHG) test and the output power generated by the nanoparticle was compared with that of potassium di hydrogen phosphate (KDP).

  8. Enhanced bioactivity of ZnO nanoparticles—an antimicrobial study

    Directory of Open Access Journals (Sweden)

    Nagarajan Padmavathy and Rajagopalan Vijayaraghavan

    2008-01-01

    Full Text Available In this study, we investigate the antibacterial activity of ZnO nanoparticles with various particle sizes. ZnO was prepared by the base hydrolysis of zinc acetate in a 2-propanol medium and also by a precipitation method using Zn(NO32 and NaOH. The products were characterized by x-ray diffraction (XRD analysis, transmission electron microscopy (TEM and photoluminescence (PL spectroscopy. Bacteriological tests such as minimum inhibitory concentration (MIC and disk diffusion were performed in Luria-Bertani and nutrient agar media on solid agar plates and in liquid broth systems using different concentrations of ZnO by a standard microbial method for the first time. Our bacteriological study showed the enhanced biocidal activity of ZnO nanoparticles compared with bulk ZnO in repeated experiments. This demonstrated that the bactericidal efficacy of ZnO nanoparticles increases with decreasing particle size. It is proposed that both the abrasiveness and the surface oxygen species of ZnO nanoparticles promote the biocidal properties of ZnO nanoparticles.

  9. Enhanced bioactivity of ZnO nanoparticles—an antimicrobial study

    Science.gov (United States)

    Padmavathy, Nagarajan; Vijayaraghavan, Rajagopalan

    2008-07-01

    In this study, we investigate the antibacterial activity of ZnO nanoparticles with various particle sizes. ZnO was prepared by the base hydrolysis of zinc acetate in a 2-propanol medium and also by a precipitation method using Zn(NO3)2 and NaOH. The products were characterized by x-ray diffraction (XRD) analysis, transmission electron microscopy (TEM) and photoluminescence (PL) spectroscopy. Bacteriological tests such as minimum inhibitory concentration (MIC) and disk diffusion were performed in Luria-Bertani and nutrient agar media on solid agar plates and in liquid broth systems using different concentrations of ZnO by a standard microbial method for the first time. Our bacteriological study showed the enhanced biocidal activity of ZnO nanoparticles compared with bulk ZnO in repeated experiments. This demonstrated that the bactericidal efficacy of ZnO nanoparticles increases with decreasing particle size. It is proposed that both the abrasiveness and the surface oxygen species of ZnO nanoparticles promote the biocidal properties of ZnO nanoparticles.

  10. A simple and sensitive spectrofluorimetric method for analysis of some nitrofuran drugs in pharmaceutical preparations.

    Science.gov (United States)

    Belal, Tarek Saied

    2008-09-01

    A simple, rapid, selective and sensitive spectrofluorimetric method was described for the analysis of three nitrofuran drugs, namely, nifuroxazide (NX), nitrofurantoin (NT) and nitrofurazone (NZ). The method involved the alkaline hydrolysis of the studied drugs by warming with 0.1 M sodium hydroxide solution then dilution with distilled water for NX or 2-propanol for NT and NZ. The formed fluorophores were measured at 465 nm (lambda (Ex) 265 nm), 458 nm (lambda (Ex) 245 nm) and 445 nm (lambda (Ex) 245 nm) for NX, NT and NZ, respectively. The reaction pathway was discussed and the structures of the fluorescent products were proposed. The different experimental parameters were studied and optimized. Regression analysis showed good correlation between fluorescence intensity and concentration over the ranges 0.08-1.00, 0.02-0.24 and 0.004-0.050 microg ml(-1) for NX, NT and NZ, respectively. The limits of detection of the method were 8.0, 1.9 and 0.3 ng ml(-1) for NX, NT and NZ, respectively. The proposed method was validated in terms of accuracy, precision and specificity, and it was successfully applied for the assay of the three nitrofurans in their different dosage forms. No interference was observed from common pharmaceutical adjuvants. The results were favorably compared with those obtained by reference spectrophotometric methods. PMID:18246413

  11. The effect of nitroimidazole and nitroxyl radiosensitizers on the post-irradiation synthesis of DNA

    International Nuclear Information System (INIS)

    The modification of DNA damage by three radiosensitizing drugs, present during γ-irradiation of hypoxic Chinese hamster cells, was investigated. Both 2-methyl-5-nitroimidazole-1-ethanol (metronidazole) and 1-(2-nitro-1-imidazole)-3-methoxy-2-propanol (Ro-07-0582) were found to cause large increases in the yield of DNA single-strand breaks (SSB); triacetoneamine-N-oxyl (TAN) was found to have only a small effect on SSB production. The three drugs tested did not inhibit the rejoining of SSB. A pulse label and chase procedure was used to examine post-irradiation DNA synthesis. TAN present during irradiation under hypoxia was found to cause interruptions in subsequent DNA synthesis. Metronidazole and Ro-07-0582 had no effect on post-irradiation DNA synthesis. In addition, the effects of pre- and post-irradiation exposure to TAN were investigated, since these treatments have shown increased cell-killing in survival studies. TAN pre- and post-treatments were found to have no significant effect on subsequent DNA synthesis. (author)

  12. Sustained release of vancomycin from novel biodegradable nanofiber-loaded vascular prosthetic grafts: in vitro and in vivo study

    Directory of Open Access Journals (Sweden)

    Liu KS

    2015-01-01

    Full Text Available Kuo-Sheng Liu,1 Cheng-Hung Lee,2 Yi-Chuan Wang,3 Shih-Jung Liu3 1Department of Thoracic and Cardiovascular Surgery, Chang Gung Memorial Hospital, Linkou, Taiwan; 2Division of Cardiology, Department of Internal Medicine, Chang Gung Memorial Hospital, Linkou, Taiwan; 3Department of Mechanical Engineering, Chang Gung University, Tao-Yuan, Taiwan Abstract: This study describes novel biodegradable, drug-eluting nanofiber-loaded vascular prosthetic grafts that provide local and sustained delivery of vancomycin to surrounding tissues. Biodegradable nanofibers were prepared by first dissolving poly(D,L-lactide-co-glycolide and vancomycin in 1,1,1,3,3,3-hexafluoro-2-propanol. The solution was then electrospun into nanofibers onto the surface of vascular prostheses. The in vitro release rates of the pharmaceutical from the nanofiber-loaded prostheses was characterized using an elution method and a high-performance liquid chromatography assay. Experimental results indicated that the drug-eluting prosthetic grafts released high concentrations of vancomycin in vitro (well above the minimum inhibitory concentration for more than 30 days. In addition, the in vivo release behavior of the drug-eluting grafts implanted in the subcutaneous pocket of rabbits was also documented. The drug-eluting grafts developed in this work have potential applications in assisting the treatment of vascular prosthesis infection and resisting reinfection when an infected graft is to be exchanged. Keywords: drug-eluting prosthetic graft, vascular prosthesis infection, release characteristics

  13. Magnetically responsive enzyme powders

    International Nuclear Information System (INIS)

    Powdered enzymes were transformed into their insoluble magnetic derivatives retaining their catalytic activity. Enzyme powders (e.g., trypsin and lipase) were suspended in various liquid media not allowing their solubilization (e.g., saturated ammonium sulfate and highly concentrated polyethylene glycol solutions, ethanol, methanol, 2-propanol) and subsequently cross-linked with glutaraldehyde. Magnetic modification was successfully performed at low temperature in a freezer (−20 °C) using magnetic iron oxides nano- and microparticles prepared by microwave-assisted synthesis from ferrous sulfate. Magnetized cross-linked enzyme powders were stable at least for two months in water suspension without leakage of fixed magnetic particles. Operational stability of magnetically responsive enzymes during eight repeated reaction cycles was generally without loss of enzyme activity. Separation of magnetically modified cross-linked powdered enzymes from reaction mixtures was significantly simplified due to their magnetic properties. - Highlights: • Cross-linked enzyme powders were prepared in various liquid media. • Insoluble enzymes were magnetized using iron oxides particles. • Magnetic iron oxides particles were prepared by microwave-assisted synthesis. • Magnetic modification was performed under low (freezing) temperature. • Cross-linked powdered trypsin and lipase can be used repeatedly for reaction

  14. Application of the ERAS model to volumetric properties of binary mixtures of banana oil with primary and secondary alcohols (C1-C4) at different temperatures

    Energy Technology Data Exchange (ETDEWEB)

    Behroozi, Mahboobe [Faculty of Chemistry, Bu-Ali Sina University, Hamedan (Iran, Islamic Republic of); Zarei, Hosseinali, E-mail: zareih@basu.ac.i [Faculty of Chemistry, Bu-Ali Sina University, Hamedan (Iran, Islamic Republic of)

    2011-05-15

    The densities of binary mixtures of {l_brace}isoamyl acetate + alcohols (methanol, ethanol, 1-propanol, 2-propanol, 1-butanol, and 2-butanol){r_brace}, including those of pure liquids, over the entire composition range were measured at temperatures (293.15 to 333.15) K and atmospheric pressure by means of a vibrating-tube densimeter. The excess molar volume, V{sub m}{sup E}, thermal expansion coefficients, {alpha}, and their excess values, {alpha}{sup E}, were calculated from density data. The V{sub m}{sup E} values are positive over the entire range of composition and temperature and become more positive with increasing temperature for all of the mixtures except for the (isoamyl acetate + methanol) mixture. The V{sub m}{sup E} values were correlated by Redlich-Kister equation and the extended real associated solution (ERAS) model was used for describing V{sub m}{sup E} values at T = 303.15 K.

  15. Microemulsion System for Topical Delivery of Thai Mango Seed Kernel Extract: Development, Physicochemical Characterisation and Ex Vivo Skin Permeation Studies

    Directory of Open Access Journals (Sweden)

    Jiraporn Leanpolchareanchai

    2014-10-01

    Full Text Available A microemulsion system containing Thai mango seed kernel extract (MSKE, cultivar “Fahlun” was developed and characterised for the purpose of topical skin delivery. The MSKE-loaded microemulsions were prepared by using the spontaneous emulsification method. Isopropyl myristate (IPM was selected as the oil phase. A polyoxyethylene sorbitan monooleate and sorbitan monododecanoate (1:1, w/w system was used as the surfactant phase; an aqueous mixture of different cosurfactants (absolute ethanol, 96.3% v/v ethanol, 1-propanol, 2-propanol or 1,2-propanediol at a weight ratio of 1:1 was used as the aqueous phase. Among the cosurfactants studied, the 1-propanol aqueous mixture had the largest microemulsion region (48.93% in the pseudo-ternary phase diagram. Microemulsions containing 1% MSKE demonstrated good physicochemical stability during a six-month study period at 25 ± 2 °C/60% ± 5% RH. The ex vivo skin permeation study demonstrated that the microemulsions exhibited a potent skin enhancement effect allowing MSKE to penetrate skin layers up to 60-fold higher compared with the control. Neither skin irritation nor skin corrosion was observed in ex vivo studies. The present study revealed that IPM-based microemulsion systems may be promising carriers to enhance skin penetration and delivering MSKE for topical treatment.

  16. Analysis of wax esters by silver-ion high-performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Vrkoslav, Vladimír; Urbanová, Klára; Háková, Matina; Cvačka, Josef

    2013-08-01

    Wax esters (WEs), esters of long-chain fatty acids and long-chain alcohols, were analysed by Ag-HPLC/APCI-MS/MS. Two ChromSpher Lipids columns connected in series (a total length of 50cm) and hexane-2-propanol-acetonitrile mobile phases were used to achieve good separation of the molecular species. The chromatographic behaviour of WEs was studied under optimised conditions: retention increased with the number of double bonds and with the temperature (15-35°C); retention times were affected by the double-bond position, trans isomers eluted earlier than cis isomers, and the WEs were partially separated depending on the aliphatic-chain length. The WEs provided simple APCI spectra with [M+H](+) ions, the MS/MS spectra showed fragments, which allowed their identification. The method was applied for an analysis of the WE mixtures from jojoba oil and human hair and the results were compared with analogous data from an optimised RP-HPLC system.

  17. 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

  18. Combined AC electroosmosis and dielectrophoresis for controlled rotation of microparticles.

    Science.gov (United States)

    Walid Rezanoor, Md; Dutta, Prashanta

    2016-03-01

    Electrorotation is widely used for characterization of biological cells and materials using a rotating electric field. Generally, multiphase AC electric fields and quadrupolar electrode configuration are needed to create a rotating electric field for electrorotation. In this study, we demonstrate a simple method to rotate dielectrophoretically trapped microparticles using a stationary AC electric field. Coplanar interdigitated electrodes are used to create a linearly polarized nonuniform AC electric field. This nonuniform electric field is employed for dielectrophoretic trapping of microparticles as well as for generating electroosmotic flow in the vicinity of the electrodes resulting in rotation of microparticles in a microfluidic device. The rotation of barium titanate microparticles is observed in 2-propanol and methanol solvent at a frequency below 1 kHz. A particle rotation rate as high as 240 revolutions per minute is observed. It is demonstrated that precise manipulation (both rotation rate and equilibrium position) of the particles is possible by controlling the frequency of the applied electric field. At low frequency range, the equilibrium positions of the microparticles are observed between the electrode edge and electrode center. This method of particle manipulation is different from electrorotation as it uses induced AC electroosmosis instead of electric torque as in the case of electrorotation. Moreover, it has been shown that a microparticle can be rotated along its own axis without any translational motion. PMID:27014394

  19. Oxidation, Reduction, and Condensation of Alcohols over (MO3)3 (M=Mo, W) Nanoclusters

    Energy Technology Data Exchange (ETDEWEB)

    Fang, Zongtang; Li, Zhenjun; Kelley, Matthew S.; Kay, Bruce D.; Li, Shenggang; Hennigan, Jamie M.; Rousseau, Roger J.; Dohnalek, Zdenek; Dixon, David A.

    2014-10-02

    The reactions of deuterated methanol, ethanol, 1-propanol, 1-butanol, 2-propanol, 2-butanol and t-butanol over cyclic (MO3)3 (M = Mo, W) clusters were studied experimentally with temperature programmed desorption (TPD) and theoretically with coupled cluster CCSD(T) theory and density functional theory. The reactions of two alcohols per M3O9 cluster are required to provide agreement with experiment for D2O release, dehydrogenation and dehydration. The reaction begins with the elimination of water by proton transfers and forms an intermediate dialkoxy species which can undergo further reaction. Dehydration proceeds by a β hydrogen transfer to a terminal M=O. Dehydrogenation takes place via an α hydrogen transfer to an adjacent MoVI = O atom or a WVI metal center with redox involved for M = Mo and no redox for M = W. The two channels have comparable activation energies. H/D exchange to produce alcohols can take place after olefin is released or via the dialkoxy species depending on the alcohol and the cluster. The Lewis acidity of the metal center with WVI being larger than MoVI results in the increased reactivity of W3O9 over Mo3O9 for dehydrogenation and dehydration.

  20. Deacidification of oils and fats of biological origine by aqueous solutions of tertiary amines*

    Directory of Open Access Journals (Sweden)

    Peter Siegfried

    2001-01-01

    Full Text Available Deacidification of triacylglycerols by extraction is investigated using aqueous solutions of amines as extractants. Tertiary amines with boiling points ranging between 100° and 170°C, such as 2-methylamino-diethanol, 2-dimethylamino-ethanol, 4-methylmorpholine, 1-dimethylamino-2-propanol etc. were found to be suitable substances. Especially the deacidification by aqueous solutions of 2-dimethylamino-ethanol (DMAE was amply investigated as it is used as an active agent in remedies. Amazingly gelatinous soap stocks are not formed, when the concentration of DMAE exceeds 20% if the free fatty acid content of the oil is below 15%. Two liquid phases are formed in systems composed of triacylglyceroles and aqueous solutions containing 20 to 80% DMAE. Palm oil containing 4.3 wt.% free fatty acids was mixed with an equal amount of an aqueous solution of 30 wt.% DMAE at 60°C. In equilibrium an extract containing 86 wt.% free fatty acids (solvents deducted and a raffinate of 0.09 wt.% free fatty acids are obtained. Loss of neutral oil being 0.7 wt.%.

  1. Case study of the sonochemical decolouration of textile azo dye Reactive Black 5

    Energy Technology Data Exchange (ETDEWEB)

    Vajnhandl, Simona [University of Maribor, Faculty of Mechanical Engineering, Smetanova 17, 2000 Maribor (Slovenia)]. E-mail: simona.vajnhandl@uni-mb.si; Le Marechal, Alenka Majcen [University of Maribor, Faculty of Mechanical Engineering, Smetanova 17, 2000 Maribor (Slovenia)

    2007-03-06

    The decolouration and mineralization of reactive dye C.I. Reactive Black 5, a well-known representative of non-biodegradable azo dyes, by means of ultrasonic irradiation at 20, 279 and 817 kHz has been investigated with emphasis on the effect of various parameters on decolouration and degradation efficiency. Characterization of the used ultrasound systems was performed using calorimetric measurements and oxidative species monitoring using Fricke and iodine dosimeter. Experiments were carried out with low frequency probe type, and a high-frequency plate type transducer at 50, 100 and 150 W of acoustic power and within the 5-300 mg/L initial dye concentration range. Decolouration, as well as radical production, increased with increasing frequency, acoustic power, and irradiation time. Any increase in initial dye concentration results in decreased decolouration rates. Sonochemical decolouration was substantially depressed by the addition of 2-methyl-2-propanol as a radical scavenger, which suggests radical-induced reactions in the solution. Acute toxicity to marine bacteria Vibrio fischeri was tested before and after ultrasound irradiation. Under the conditions employed in this study, no toxic compounds were detected after 6 h of irradiation. Mineralization of the dye was followed by TOC measurements. Relatively low degradation efficiency (50% after 6 h of treatment) indicates that ultrasound is rather inefficient in overall degradation, when used alone.

  2. Gene-specific amplicons from metagenomes as an alternative to directed evolution for enzyme screening: a case study using phenylacetaldehyde reductases.

    Science.gov (United States)

    Itoh, Nobuya; Kazama, Miki; Takeuchi, Nami; Isotani, Kentaro; Kurokawa, Junji

    2016-06-01

    Screening gene-specific amplicons from metagenomes (S-GAM) is a highly promising technique for the isolation of genes encoding enzymes for biochemical and industrial applications. From metagenomes, we isolated phenylacetaldehyde reductase (par) genes, which code for an enzyme that catalyzes the production of various Prelog's chiral alcohols. Nearly full-length par genes were amplified by PCR from metagenomic DNA, the products of which were fused with engineered par sequences at both terminal regions of the expression vector to ensure proper expression and then used to construct Escherichia coli plasmid libraries. Sequence- and activity-based screening of these libraries identified different homologous par genes, Hpar-001 to -036, which shared more than 97% amino acid sequence identity with PAR. Comparative characterization of these active homologs revealed a wide variety of enzymatic properties including activity, substrate specificity, and thermal stability. Moreover, amino acid substitutions in these genes coincided with those of Sar268 and Har1 genes, which were independently engineered by error-prone PCR to exhibit increased activity in the presence of concentrated 2-propanol. The comparative data from both approaches suggest that sequence information from homologs isolated from metagenomes is quite useful for enzyme engineering. Furthermore, by examining the GAM-based sequence dataset derived from soil metagenomes, we easily found amino acid substitutions that increase the thermal stability of PAR/PAR homologs. Thus, GAM-based approaches can provide not only useful homologous enzymes but also an alternative to directed evolution methodologies. PMID:27419059

  3. Computational and experimental studies of 2-[(E)-hydrazinylidenemethyl]-6-methoxy-4-[(E)-phenyldiazenyl]phenol and its tautomers

    Science.gov (United States)

    Sayin, Koray; Kurtoglu, Nurcan; Kose, Muhammet; Karakas, Duran; Kurtoglu, Mukerrem

    2016-09-01

    A new azo-chromophore group containing a hydrazine-Schiff base compound, 2-[(E)-hydrazinylidenemethyl]-6-methoxy-4-[(E)-phenyldiazenyl]phenol, was synthesized and structurally characterized by single crystal X-ray diffraction study. The compound was found to crystallise in orthorhombic crystal system with Pca2(1) space group. In the structure, the molecule exhibits a phenol-imine intramolecular hydrogen bond and the sbnd NH2 group also involves in intermolecular hydrogen bonding with one of the nitrogen atom of the azo group (-Ndbnd N-) forming a 1D zigzag chain. Computational studies were performed on the titled compound and its tautomers. As computationally, this compound and its tautomers were optimized by using M062X/6-311G(d,p) level. According to thermodynamic parameters, the most stable tautomer was found to be azo-enol form. This result was then taken into account and spectral studies, which are IR, UV-Vis and NMR spectra, of this compound were performed and examined in detail. All calculations were performed at gas phase (ε = 1.000), 2-propanol (ε = 19.264), 1,2-ethanediol (ε = 40.245), water (ε = 78.355), formamide (ε = 108.940) and N-methylformamide-mixture (ε = 181.560).

  4. High-performance liquid chromatography-ionspray mass spectrometry for the specific determination of digoxin and some related cardiac glycosides in human plasma.

    Science.gov (United States)

    Tracqui, A; Kintz, P; Ludes, B; Mangin, P

    1997-04-25

    An original method based upon high-performance liquid chromatography coupled to ionspray mass spectrometry (HPLC-ISP-MS) has been developed for the identification and quantification in plasma of several cardiac glycosides, namely digoxin, digitoxin, lanatoside C and acetyldigitoxin. After single-step liquid-liquid extraction by chloroform-2-propanol (95:5, v/v) at pH 9.5 using oleandrin as an internal standard, solutes are separated on a 4 microm NovaPak C18 (Waters) column (150x2.0 mm, I.D.), using a gradient of acetonitrile-2 mM NH4COOH, pH 3 buffer (flow-rate 200 microl/min, post-column split 1:3). Detection is done by a Perkin-Elmer Sciex API-100 mass analyzer equipped with an ISP interface. In most instances the major ion observed is not [M+H]+ as expected, but [M+NH4]+. The mean retention times (min) are: lanatoside C, 5.74; digoxin, 6.00; digitoxin, 8.08, oleandrin, 8.30, acetyldigitoxin, 8.66 and 9.01 (isomers alpha and beta, respectively). The lower limits of detection in single ion monitoring mode range from 0.15 ng/ml (alpha- and beta-acetyldigitoxin) to 0.60 ng/ml (lanatoside C), making the method less sensitive than radioimmunoassay, whereas it is much more specific.

  5. Charge-transfer complexes of 4-nitrocatechol with some amino alcohols

    Science.gov (United States)

    Baniyaghoob, Sahar; Najafpour, Mohammad Mahdi; Boghaei, Davar M.

    2010-03-01

    Charge-transfer (CT) complexes formed from the reactions of 4-nitropyrocatechol (4-nCat) as an electron acceptor with four amino alcohols: 2-aminoethanol, 1-amino-2-propanol, 4-aminobutanol and N-(2-hydroxyethyl)-1,3-diaminopropane (NHEDAP) as electron donors, have been studied spectrophotometrically in H 2O and H 2O/EtOH at 20, 25, 30, 35 and 40 °C. The calculated values of the oscillator strength and transition moment confirm the formation of CT-complexes. The thermodynamic and spectroscopic parameters were also evaluated for the formation of CT-complexes. The equilibrium constants ranged from 9.00 to 2.20 l mol -1 (M -1). These interactions are exothermic and have relatively large standard enthalpy and entropy changes (Δ H values ranged from -15.58 to -3.10 kJ mol -1; Δ S ranged from 26.81 to -3.25 J K -1 mol -1). The solid CT-complexes have been synthesized and characterized by IR, NMR, mass spectrometry and thermal analysis. The photometric titration curves and other spectrometric data for the reactions indicated that the data obtained refer to the formation of 1:1 charge-transfer complex of [(4-nCat) (NHEDAP)] and 1:2 charge-transfer complexes of other amino alcohols [(4-nCat) (amino alcohol) 2]. The effect of alkali and alkaline earth metals on increasing the equilibrium constant of the CT-complexation was also investigated.

  6. Fiber content of diet affects exhaled breath volatiles in fasting and postprandial state in a pilot crossover study.

    Science.gov (United States)

    Raninen, Kaisa J; Lappi, Jenni E; Mukkala, Maria L; Tuomainen, Tomi-Pekka; Mykkänen, Hannu M; Poutanen, Kaisa S; Raatikainen, Olavi J

    2016-06-01

    Our pilot study examined the potential of exhaled breath analysis in studying the metabolic effects of dietary fiber (DF). We hypothesized that a high-fiber diet (HFD) containing whole grain rye changes volatile organic compound (VOC) levels in exhaled breath and that consuming a single meal affects these levels. Seven healthy men followed a week-long low-fiber diet (17 g/d) and HFD (44 g/d) in a randomized crossover design. A test meal containing 50 g of the available carbohydrates from wheat bread was served as breakfast after each week. Alveolar exhaled breath samples were analyzed at fasting state and 30, 60, and 120 minutes after this meal parallel to plasma glucose, insulin, and serum lipids. We used solid-phase microextraction and gas chromatography-mass spectrometry for detecting changes in 15 VOCs. These VOCs were acetone, ethanol, 1-propanol, 2-propanol, 1-butanol, acetic acid, propionic acid, butyric acid, valeric acid, isovaleric acid, 2-methylbutyric acid, hexanoic acid, acetoin, diacetyl, and phenol. Exhaled breath 2-methylbutyric acid in the fasting state and 1-propanol at 120 minutes decreased (P = .091 for both) after an HFD. Ingestion of the test meal increased ethanol, 1-propanol, acetoin, propionic acid, and butyric acid levels while reducing acetone, 1-butanol, diacetyl, and phenol levels. Both DF diet content and having a single meal affected breathVOCs. Exploring exhaled breath further could help to develop tools for monitoring the metabolic effects of DF. PMID:27188907

  7. Study the interactions between human serum albumin and two antifungal drugs: fluconazole and its analogue DTP.

    Science.gov (United States)

    Zhang, Shao-Lin; Yao, Huankai; Wang, Chenyin; Tam, Kin Y

    2014-11-01

    Binding affinities of fluconazole and its analogue 2-(2,4-dichlorophenyl)-1,3-di(1H-1,2,4-triazol-yl)-2-propanol (DTP) to human serum albumin (HSA) were investigated under approximately human physiological conditions. The obtained result indicated that HSA could generate fluorescent quenching by fluconazole and DTP because of the formation of non-fluorescent ground-state complexes. Binding parameters calculated from the Stern-Volmer and the Scatchard equations showed that fluconazole and DTP bind to HSA with binding affinities of the order 10(4)L/mol. The thermodynamic parameters revealed that the binding was characterized by negative enthalpy and positive entropy changes, suggesting that the binding reaction was exothermic. Hydrogen bonds and hydrophobic interaction were found to be the predominant intermolecular forces stabilizing the drug-protein. The effect of metal ions on the binding constants of fluconazole-HSA complex suggested that the presence of Mg(2+) and Zn(2+) ions could decrease the free drug level and extend the half-life in the systematic circulation. Docking experiments revealed that fluconazole and DTP binds in HSA mainly by hydrophobic interaction with the possibility of hydrogen bonds formation between the drugs and the residues Arg 222, Lys 199 and Lys 195 in HSA.

  8. Determination of the mixture in a reaction of glycerol with hydrochloric acid by gas chromatography%气相色谱法测定甘油与盐酸反应过程的混合物

    Institute of Scientific and Technical Information of China (English)

    尤小姿; 李华荣; 罗正鸿

    2009-01-01

    采用气相色谱方法分析了甘油与盐酸反应过程中的主要物质. 使用KB-WAX毛细管柱及FID检测器, 以乙二醇作内标和甲醇定容, 并用内标法计算. 结果表明, 在程序升温下, 气相色谱内标法能使GLY, DCP, CPD等几种物质达到基线分离, 该方法能满足测试要求.%In this paper, a simple gas chromatographic method for the identification of glycerol (GLY), 1,3-dichloropropanol-2-propanol,(DCP) and 3-chloro-1,2-propandiol (CPD) in GLY chlorination reaction is described. The results are detected by KB-WAX capillary column with a flame ionization detector (FID) and calculated by an internal stand method. Glycol is used as an internal standard, and the samples are diluted with methanol. This method is simple, rapid and the results are reliable.

  9. Overexpression, purification, crystallization and preliminary structural studies of p-coumaric acid decarboxylase from Lactobacillus plantarum

    Energy Technology Data Exchange (ETDEWEB)

    Rodríguez, Héctor; Rivas, Blanca de las; Muñoz, Rosario [Instituto de Fermentaciones Industriales, CSIC, Juan de la Cierva 3, 28006 Madrid (Spain); Mancheño, José M., E-mail: xjosemi@iqfr.csic.es [Grupo de Cristalografía Macromolecular y Biología Estructural, Instituto Rocasolano, CSIC, Serrano 119, 28006 Madrid (Spain); Instituto de Fermentaciones Industriales, CSIC, Juan de la Cierva 3, 28006 Madrid (Spain)

    2007-04-01

    The enzyme p-coumaric acid decarboxylase (PDC) from L. plantarum has been recombinantly expressed, purified and crystallized. The structure has been solved at 2.04 Å resolution by the molecular-replacement method. The substrate-inducible p-coumaric acid decarboxylase (PDC) from Lactobacillus plantarum has been overexpressed in Escherichia coli, purified and confirmed to possess decarboxylase activity. The recombinant His{sub 6}-tagged enzyme was crystallized using the hanging-drop vapour-diffusion method from a solution containing 20%(w/v) PEG 4000, 12%(w/v) 2-propanol, 0.2 M sodium acetate, 0.1 M Tris–HCl pH 8.0 with 0.1 M barium chloride as an additive. Diffraction data were collected in-house to 2.04 Å resolution. Crystals belonged to the tetragonal space group P4{sub 3}, with unit-cell parameters a = b = 43.15, c = 231.86 Å. The estimated Matthews coefficient was 2.36 Å{sup 3} Da{sup −1}, corresponding to 48% solvent content, which is consistent with the presence of two protein molecules in the asymmetric unit. The structure of PDC has been determined by the molecular-replacement method. Currently, the structure of PDC complexed with substrate analogues is in progress, with the aim of elucidating the structural basis of the catalytic mechanism.

  10. Improved Polymerase Chain Reaction-restriction Fragment Length Polymorphism Genotyping of Toxic Pufferfish by Liquid Chromatography/Mass Spectrometry.

    Science.gov (United States)

    Miyaguchi, Hajime

    2016-09-20

    An improved version of a polymerase chain reaction (PCR)-restriction fragment length polymorphism (RFLP) method for genotyping toxic pufferfish species by liquid chromatography/electrospray ionization mass spectrometry (LC/ESI-MS) is described. DNA extraction is carried out using a silica membrane-based DNA extraction kit. After the PCR amplification using a detergent-free PCR buffer, restriction enzymes are added to the solution without purifying the reaction solution. A reverse-phase silica monolith column and a Fourier transform high resolution mass spectrometer having a modified Kingdon trap analyzer are employed for separation and detection, respectively. The mobile phase, consisting of 400 mM 1,1,1,3,3,3-hexafluoro-2-propanol, 15 mM triethylamine (pH 7.9) and methanol, is delivered at a flow rate of 0.4 ml/min. The cycle time for LC/ESI-MS analysis is 8 min including equilibration of the column. Deconvolution software having an isotope distribution model of the oligonucleotide is used to calculate the corresponding monoisotopic mass from the mass spectrum. For analysis of oligonucleotides (range 26-79 nucleotides), mass accuracy was 0.62 ± 0.74 ppm (n = 280) and excellent accuracy and precision were sustained for 180 hr without use of a lock mass standard.

  11. Synthesis and characterization of mesoporous TiO{sub 2} assembled as microspheres

    Energy Technology Data Exchange (ETDEWEB)

    Beitollahi, Ali, E-mail: beitolla@iust.ac.i [Nanomaterial Research Group, Dept. of Metallurgy and Materials Eng., Iran University of Science and Technology (IUST), Narmak, Farjam, Tehran (Iran, Islamic Republic of); Daie, Amir Hossein Haj [Nanomaterial Research Group, Dept. of Metallurgy and Materials Eng., Iran University of Science and Technology (IUST), Narmak, Farjam, Tehran (Iran, Islamic Republic of); Samie, Leyla [Nanomaterial Research Group, Dept. of Metallurgy and Materials Eng., Iran University of Science and Technology (IUST), Narmak, Farjam, Tehran (Iran, Islamic Republic of); Research Institute of Petroleum Industries, Tehran (Iran, Islamic Republic of); Akbarnejad, Mohammad Mehdi [Research Institute of Petroleum Industries, Tehran (Iran, Islamic Republic of)

    2010-02-04

    In the work presented here, we report the successful synthesis of highly porous (219 m{sup 2}/g) mesostructured titania powder assembled as microspheres of uniform wormlike channels of {approx}6-7 nm widths by spray pyrolysis of a titania sol prepared by templating approach using P123 pluronic block copolymer (BC). This method involves the preparation of a Ti{sup 4+}-sol containing titanium tertraisopropoxide (TTIP), pluronic BC P123, 2-propanol, acetyl acetonate (ACAC) and hydrochloric acid (HCl) as well as H{sub 2}O followed by spray pyrolysis of the obtained sol into the hot zone of a pre-heated reactor at 800 deg. C, 900 deg. C and 1000 deg. C. For all of these pyrolyzed samples, the formation of anatase as the major phase along with rutile as the minor one could be confirmed. The appearance of wormlike mesopores rather than highly ordered cubic or hexagonal mesostructures is related to the lack of appropriate drying conditions normally applied to induce self assembly as well as formation of rather large titania crystallite sizes.

  12. A new sol-gel processing routine without chelating agents for preparing highly transparent solutions and nanothin films: engineering the role of chemistry to design the process

    Science.gov (United States)

    Ashiri, Rouholah

    2015-01-01

    The great sensitivity of titanium alkoxides to hydrolysis makes their sol-gel transformation very fast and thus difficult to control. A method was proposed to alleviate this drawback. Preparation of highly transparent solutions and nanothin films is another objective of the present research. Employing nanoemulsion method and optimizing the processing conditions, a clear solution of well-dispersed nanosized particles was obtained. With the proposed process BaTiO3 precursor sols and nanothin films with enhanced optical transparency towards the visible were prepared. The optimal formulation of the sol consists of acetic acid, barium acetate, 2-propanol, TTIP and deionized water with 6:1:1:1:150 M ratios, respectively. It was found that the reduction of the temperature in the initial stage of mixing of precursors controls the size of the forming species and accordingly improves the stability and transparency of the sol. The results also showed that the applied modifications and optimizations significantly downsize the particles within the sol to the nanometric scale and accordingly result in a significant improvement in the optical response of the products.

  13. Microemulsion system for topical delivery of thai mango seed kernel extract: development, physicochemical characterisation and ex vivo skin permeation studies.

    Science.gov (United States)

    Leanpolchareanchai, Jiraporn; Padois, Karine; Falson, Françoise; Bavovada, Rapepol; Pithayanukul, Pimolpan

    2014-01-01

    A microemulsion system containing Thai mango seed kernel extract (MSKE, cultivar "Fahlun") was developed and characterised for the purpose of topical skin delivery. The MSKE-loaded microemulsions were prepared by using the spontaneous emulsification method. Isopropyl myristate (IPM) was selected as the oil phase. A polyoxyethylene sorbitan monooleate and sorbitan monododecanoate (1:1, w/w) system was used as the surfactant phase; an aqueous mixture of different cosurfactants (absolute ethanol, 96.3% v/v ethanol, 1-propanol, 2-propanol or 1,2-propanediol) at a weight ratio of 1:1 was used as the aqueous phase. Among the cosurfactants studied, the 1-propanol aqueous mixture had the largest microemulsion region (48.93%) in the pseudo-ternary phase diagram. Microemulsions containing 1% MSKE demonstrated good physicochemical stability during a six-month study period at 25 ± 2 °C/60% ± 5% RH. The ex vivo skin permeation study demonstrated that the microemulsions exhibited a potent skin enhancement effect allowing MSKE to penetrate skin layers up to 60-fold higher compared with the control. Neither skin irritation nor skin corrosion was observed in ex vivo studies. The present study revealed that IPM-based microemulsion systems may be promising carriers to enhance skin penetration and delivering MSKE for topical treatment. PMID:25347456

  14. Synthesis and Anticancer Activity of Some New S-Glycosyl and S-Alkyl 1,2,4-Triazinone Derivatives

    Directory of Open Access Journals (Sweden)

    Hosam A. Saad

    2011-07-01

    Full Text Available A series of S-glycosyl and S-alkyl derivatives of 4-amino-3-mercapto-6-(2-(2-thienylvinyl-1,2,4-triazin-5(4H-one (1 were synthesized using different halo compounds such as preacetylated sugar bromide, 4-bromobutylacetate, 2-acetoxyethoxy-methyl bromide, 3-chloropropanol, 1,3-dichloro-2-propanol, epichlorohydrin, allyl bromide, propargyl bromide, phthalic and succinic acids in POCl3. The structures of the synthesized compounds have been deduced from their elemental analysis and spectral (IR, 1H-NMR, and 13C-NMR data. Some of the synthesized compounds were screened as anticancer agents. Significant anticancer activities were observed in vitro for some members of the series, and compounds 4-Amino-3-(3-hydroxypropylthio-6-(2-(2-thienylvinyl-1,2,4-triazin-5(4H-one (12 and 3-(4-Oxo-3-(2-(2-thienylvinyl-4H-[1,3,4]thiadiazolo-[2,3-c][1,2,4]tr-iazin-7-ylpropanoic acid (18 are active cytotoxic agents against different cancer cell lines.

  15. Room temperature alcohol sensing by oxygen vacancy controlled TiO{sub 2} nanotube array

    Energy Technology Data Exchange (ETDEWEB)

    Hazra, A.; Dutta, K.; Bhowmik, B.; Bhattacharyya, P., E-mail: pb-etc-besu@yahoo.com [Nano-Thin Films and Solid State Gas Sensor Devices Laboratory, Department of Electronics and Telecommunication Engineering, Indian Institute of Engineering Science and Technology (IIEST), Shibpur, Howrah (India); Chattopadhyay, P. P. [Department of Metallurgy and Materials Engineering, Indian Institute of Engineering Science and Technology (IIEST), Shibpur, Howrah (India)

    2014-08-25

    Oxygen vacancy (OV) controlled TiO{sub 2} nanotubes, having diameters of 50–70 nm and lengths of 200–250 nm, were synthesized by electrochemical anodization in the mixed electrolyte comprising NH{sub 4}F and ethylene glycol with selective H{sub 2}O content. The structural evolution of TiO{sub 2} nanoforms has been studied by field emission scanning electron microscopy. Variation in the formation of OVs with the variation of the structure of TiO{sub 2} nanoforms has been evaluated by photoluminescence and X-ray photoelectron spectroscopy. The sensor characteristics were correlated to the variation of the amount of induced OVs in the nanotubes. The efficient room temperature sensing achieved by the control of OVs of TiO{sub 2} nanotube array has paved the way for developing fast responding alcohol sensor with corresponding response magnitude of 60.2%, 45.3%, and 36.5% towards methanol, ethanol, and 2-propanol, respectively.

  16. An organic solvent-stable lipase from a newly isolated Staphylococcus aureus ALA1 strain with potential for use as an industrial biocatalyst.

    Science.gov (United States)

    Ben Bacha, Abir; Moubayed, Nadine Ms; Al-Assaf, Alaa

    2016-05-01

    In this study, a new strain, ALA1, was identified as Staphylococcus aureus by biochemical tests, and its 16S ribosomal DNA sequence was isolated from dromedary milk. ALA1 lipase production was optimized in shake flask experiments and measured with varying pH (3-11), temperature (20-55 °C) and substrate concentrations. The maximum lipase production was recorded at pH 8 and 30 °C for up to 30 H of culture period for the S. aureus ALA1 strain. Among the substrates tested, selected carbon sources, xylose, nitrogen source, yeast extract, and olive oil (1%) were suitable for maximizing lipase production. The effects of surfactants were investigated and showed that Tween 20, Tween 80, and Triton X-100 prevented lipase production. Interestingly, isolate ALA1 was able to grow in high concentrations of benzene or toluene (up to 50% (v/v)). Moreover, the lipolytic activity of the S. aureus ALA1 lipase was stimulated by diethyl ether, whereas almost 100% of S. aureus ALA1 lipase activity was retained in 25% acetone, acetonitrile, benzene, 2-propanol, ethanol, methanol, or toluene. Because of its stability in organic solvent, the S. aureus ALA1 lipase was used as a biocatalyst to synthesize high levels of added value molecules. S. aureus ALA1 lipase could be considered as an ideal choice for applications in detergent formulations because of its high stability and compatibility with various surfactants, oxidizing agents, and commercial detergents. PMID:25828848

  17. Production of selective membranes using plasma deposited nanochanneled thin films

    Directory of Open Access Journals (Sweden)

    Rodrigo Amorim Motta Carvalho

    2006-12-01

    Full Text Available The hydrolization of thin films obtained by tetraethoxysilane plasma polymerization results in the formation of a nanochanneled silicone like structure that could be useful for the production of selective membranes. Therefore, the aim of this work is to test the permeation properties of hydrolyzed thin films. The films were tested for: 1 permeation of polar organic compounds and/or water in gaseous phase and 2 permeation of salt in liquid phase. The efficiency of permeation was tested using a quartz crystal microbalance (QCM technique in gas phase and conductimetric analysis (CA in liquid phase. The substrates used were: silicon for characterization of the deposited films, piezoelectric quartz crystals for tests of selective membranes and cellophane paper for tests of permeation. QCM analysis showed that the nanochannels allow the adsorption and/or permeation of polar organic compounds, such as acetone and 2-propanol, and water. CA showed that the films allow salt permeation after an inhibition time needed for hydrolysis of the organic radicals within the film. Due to their characteristics, the films can be used for grains protection against microorganism proliferation during storage without preventing germination.

  18. SÍNTESIS SELECTIVA DE BENZALDEHÍDO USANDO ZEOLITAS MODIFICADAS CON METALES DE TRANSICIÓN

    Directory of Open Access Journals (Sweden)

    Clara Saux

    2012-01-01

    Full Text Available Se estudió la oxidación selectiva de estireno para la obtención de benzaldehído sobre zeolitas ZSM-5 modificadas con diferentes metales de transición (cromo, cobalto, hierro, zinc, manganeso y cobre y utilizando peróxido de hidrógeno como oxidante. Dado que los mejores resultados se obtuvieron utilizando Cr-ZSM-5, estos materiales se estudiaron evaluando el efecto del tiempo de reacción, la masa de catalizador, la relación molar estireno/hidroperóxido, la naturaleza del solvente y la temperatura de reacción. Los mejores resultados de las condiciones evaluadas se obtuvieron trabajando con una relación molar sustrato/oxidante de 0,45 y utilizando acetonitrilo como solvente, dado su carácter aprótico y de mayor polaridad de los solventes evaluados (acetonitrilo, acetona, 2-butanol y 2-propanol. El aumento en la temperatura de reacción mostró un incremento en la conversión de estireno, el cual se desaceleró al superar los 60 oC por descomposición térmica del peróxido de hidrógeno.

  19. Determining indoor air quality and identifying the origin of odour episodes in indoor environments

    Institute of Scientific and Technical Information of China (English)

    Eva Gallego; Xavier Roca; Jose Francisco Perales; Xavier Guardino

    2009-01-01

    A methodology for identifying volatile organic compounds (VOC) and determining air quality of indoor air has been developed. The air samples are collected using pump samplers by the inhabitants when they perceive odorous and/or discomfort episodes. Glass multi-sorbent tubes are connected to the pump samplers for the retention of VOC. The analysis is performed by automatic thermal desorption (ATD) coupled with gas chromatography-mass spectrometry (GC/MS). This methodology can be applied in cases of sick building syndrome (SBS) evaluation, in which building occupants experience a series of varied symptoms that appear to be linked to time spent in the building. Chemical pollutants concentrations (e.g., VOC) have been described to contribute to SBS. To exemplify the methodology, a qualitative determination and an evaluation of VOC present were performed in a dwelling where the occupants experienced the SBS symptoms. Higher total VOC (TVOC) value was detected in episodes in indoor air (1.33 ( 1.53 mg/m3) compared to outdoor air (0.71 ( 0.46 mg/m3). The concentrations of individual VOCs, such as ethanol, acetone, isopropanol, 1-butanol, acetic acid, acetonitrile and 1-metoxy-2-propanol, were also higher than the expected for a standard dwelling. The external source of VOC was found to be a not declared activity of storage and manipulation of solvents located at the bottom of a contiguous building.

  20. Separation of alcohol-water mixtures using salts

    Energy Technology Data Exchange (ETDEWEB)

    Card, J. C.; Farrell, L. M.

    1982-04-01

    Use of a salt (KF or Na/sub 2/SO/sub 4/) to induce phase separation of alcohol-water mixtures was investigated in three process flowsheets to compare operating and capital costs with a conventional distillation process. The process feed was the Clostridia fermentation product, composed of 98 wt % water and 2 wt % solvents (70% 1-butanol, 27% 2-propanol, and 3% ethanol). The design basis was 150 x 10/sup 6/ kg/y of solvents. Phase equilibria and tieline data were obtained from literature and experiments. Three separation-process designs were developed and compared by an incremental economic analysis (+-30%) with the conventional separation technique using distillation alone. The cost of salt recovery for recycle was found to be the critical feature. High capital and operating costs make recovery of salt by precipitation uneconomical; however, a separation scheme using multiple-effect evaporation for salt recovery has comparable incremental capital costs ($1.72 x 10/sup 6/ vs $1.76 x 10/sup 6/) and lower incremental operating costs ($2.14 x 10/sup 6//y vs $4.83 x 10/sup 6//y) than the conventional separation process.

  1. Simultaneous determination of neonicotinoid insecticides in human serum and urine using diatomaceous earth-assisted extraction and liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Yamamuro, Tadashi; Ohta, Hikoto; Aoyama, Mika; Watanabe, Daisuke

    2014-10-15

    A rapid and sensitive analytical method was developed for simultaneous determination of eight neonicotinoid insecticides (acetamiprid, clothianidin, dinotefuran, flonicamid, imidacloprid, nitenpyram, thiacloprid and thiamethoxam) and three specific metabolites of acetamiprid (N-desmethylacetamiprid, 5-(N-acetyl-N-methylaminomethyl)-2-chloropyridine and 5-(N-acetylaminomethyl)-2-chloropyridine) in human serum and urine. A diatomaceous earth-assisted extraction using Extrelut NT3 column with chloroform/2-propanol (3:1, v/v) as eluent was selected for the single step cleanup procedure for all the target compounds. Qualitative and quantitative analyses were conducted by liquid chromatography-tandem mass spectrometry with multiple reaction monitoring mode. The limits of detection and the limits of quantification of eleven compounds were in the ranges of 0.1-0.2ng/mL and 0.5-10ng/mL for serum, 0.1-1ng/mL and 1-10ng/mL for urine, respectively. The extraction recoveries were between 80.9% and 101.8% for serum samples, 91.9% and 106% for urine samples. The intra-day RSDs and the inter-day RSDs were less than 11.5% and 13.2% for serum, less than 8.3% and 8.8% for urine. The proposed procedure will be suitable for forensic investigations of human poisoning cases with neonicotinoid insecticides. This is the first report of simultaneous determination of eight neonicotinoids in serum and urine samples.

  2. Effects of crystallization in the presence of the diastereomer on the crystal properties of (SS)-(+)-pseudoephedrine hydrochloride.

    Science.gov (United States)

    Gu, C H; Grant, D J

    2000-01-01

    The formation and separation of diastereomers is widely used to resolve enantiomers. However, during crystallization of a chiral compound from a solution containing its diastereomer, the diastereomer may be incorporated as an impurity into the host crystal lattice, leading to changes in the thermodynamic properties and intrinsic dissolution rate of the host crystals. This hypothesis was tested by growing crystals of (SS)-(+)-pseudoephedrine hydrochloride (+PC) from aqueous solution containing various amounts of (RS)-(-)-ephedrine hydrochloride (-EC). Although the melting phase diagram of these two solid compounds, determined by differential scanning calorimetry (DSC), shows eutectic behavior, 0.034-2.4 mol% of -EC was incorporated into the crystal lattice of +PC during crystallization to form terminal solid solutions with a segregation coefficient of 0.31. In a single batch, the larger crystals contain more incorporated impurities than smaller crystals. The enthalpy and entropy of fusion measured by DSC decrease with increasing incorporation of the guest molecules into the host, indicating increases in the enthalpy and entropy of the solid. The disruption index, which indicates the disruptive effect of guest molecules in the host crystal lattice, is 60 at lattice. The average intrinsic dissolution rate of impure crystals in 2-propanol is 15.8% lower than that of pure host crystals, suggesting the formation of stable solid solutions.

  3. High catalytic activity of magnetic CuFe2O4/graphene oxide composite for the degradation of organic dyes under visible light irradiation

    Science.gov (United States)

    Chen, Peng; Xing, Xiang; Xie, Huifang; Sheng, Qi; Qu, Hongxia

    2016-09-01

    Magnetic CuFe2O4/graphene oxide composite (CuFe2O4/GO) has been synthesized by hydrothermal method and showed excellent visible-light-photocatalytic activity for the degradation of different dyes as Rhodamine B (RhB) and acid orange II (AO7) with no need of H2O2. The Structure and morphology were investigated by XRD, FTIR and TEM and the performance of the catalyst was systematically investigated under various experimental conditions as pH, the dosage of catalyst, dye initial concentration, etc. The dyes degradation on CuFe2O4/GO was also remained in a level in the presence of OH2- radical scavenger (2-propanol), while it decreased in the presence of O2- radical scavenger (benzoquinone) and h+ radical scavenger (ammonium oxalate), indicating that O2- and h+ radicals were responsible for the dye degradation. The magnetic CuFe2O4/GO composite shows potential applications in organic dye water treatment due to its magnetically recyclability and powerful visible-light-photocatalytic activity.

  4. Outgrowth inhibition of Clostridium beijerinckii spores by a bacteriocin-producing lactic culture in ovine milk cheese.

    Science.gov (United States)

    Garde, Sonia; Avila, Marta; Arias, Ramón; Gaya, Pilar; Nuñez, Manuel

    2011-10-17

    In the manufacture of model cheeses, ovine milk was deliberately contaminated with spores of Clostridium beijerinckii INIA 63, a wild isolate from Manchego cheese with late blowing defect, and inoculated with nisin- and lacticin 481-producing Lactococcus lactis subsp. lactis INIA 415 as starter, to test its potential to prevent the late blowing defect, or with L. lactis subsp. lactis INIA 415-2, a spontaneous mutant not producing bacteriocins. Cheeses made individually with the lactococcal strains, without clostridial spores, served as controls. Cheese made with clostridial spores and L. lactis subsp. lactis INIA 415-2 showed late blowing defect after 120days of ripening. Spoilt cheese also showed lower concentrations of lactic acid, and higher levels of acetic, propionic and butyric acids, and of other volatile compounds such as 2-propanol and 1-butanol, than control cheese. In addition, cheese made with the bacteriocin producer did not show any late blowing symptoms, despite its spore counts similar to those of blown cheese, pointing to outgrowth inhibition of C. beijerinckii spores by bacteriocins. Besides, cheese made with the bacteriocin producer showed similar concentrations of lactic acid and volatile compounds than control cheese. Inclusion of L. lactis subsp. lactis INIA 415 in starter cultures seems a feasible method to prevent late blowing defect in cheese without altering its sensory characteristics. PMID:21849216

  5. Oxidation and β-Alkylation of Alcohols Catalysed by Iridium(I) Complexes with Functionalised N-Heterocyclic Carbene Ligands.

    Science.gov (United States)

    Jiménez, M Victoria; Fernández-Tornos, Javier; Modrego, F Javier; Pérez-Torrente, Jesús J; Oro, Luis A

    2015-12-01

    The borrowing hydrogen methodology allows for the use of alcohols as alkylating agents for CC bond forming processes offering significant environmental benefits over traditional approaches. Iridium(I)-cyclooctadiene complexes having a NHC ligand with a O- or N-functionalised wingtip efficiently catalysed the oxidation and β-alkylation of secondary alcohols with primary alcohols in the presence of a base. The cationic complex [Ir(NCCH3 )(cod)(MeIm(2- methoxybenzyl))][BF4 ] (cod=1,5-cyclooctadiene, MeIm=1-methylimidazolyl) having a rigid O-functionalised wingtip, shows the best catalyst performance in the dehydrogenation of benzyl alcohol in acetone, with an initial turnover frequency (TOF0 ) of 1283 h(-1) , and also in the β-alkylation of 2-propanol with butan-1-ol, which gives a conversion of 94 % in 10 h with a selectivity of 99 % for heptan-2-ol. We have investigated the full reaction mechanism including the dehydrogenation, the cross-aldol condensation and the hydrogenation step by DFT calculations. Interestingly, these studies revealed the participation of the iridium catalyst in the key step leading to the formation of the new CC bond that involves the reaction of an O-bound enolate generated in the basic medium with the electrophilic aldehyde. PMID:26493780

  6. Quantitative evaluation of size selective precipitation of Mn-doped ZnS quantum dots by size distributions calculated from UV/Vis absorbance spectra

    International Nuclear Information System (INIS)

    We demonstrate the quantitative evaluation of the sharp classification of manganese-doped zinc sulfide (ZnS:Mn) quantum dots by size selective precipitation. The particles were characterized by the direct conversion of absorbance spectra to particle size distributions (PSDs) and high-resolution transmission electron micrographs (HRTEM). Gradual addition of a poor solvent (2-propanol) to the aqueous colloid led to the flocculation of larger particles. Though the starting suspension after synthesis had an already narrow PSD between 1.5 and 3.2 nm, different particle size fractions were subsequently isolated by the careful adjustment of the good solvent/poor solvent ratio. Moreover, due to the fact that for the analysis of the classification results the size distributions were available, an in-depth understanding of the quality of the distinct classification steps could be achieved. From the PSDs of the feed, as well as the coarse and the fine fractions with their corresponding yields determined after each classification step, an optimum after the first addition of poor solvent was identified with a maximal separation sharpness κ as high as 0.75. Only by the quantitative evaluation of classification results leading to an in-depth understanding of the relevant driving forces, a future transfer of this lab scale post-processing to larger quantities will be possible.

  7. Ligand centered radical pathway in catechol oxidase activity with a trinuclear zinc-based model: Synthesis, structural characterization and luminescence properties

    Science.gov (United States)

    Pal, Sukanta; Chowdhury, Biswajit; Patra, Moumita; Maji, Milan; Biswas, Bhaskar

    2015-06-01

    A new trinuclear zinc(II) complex, [Zn3(L)(NCS)2](NO3)2·CH3OH·H2O (1), of a (N,O)-donor compartmental Schiff base ligand (H2L = N,N‧-bis(3-methoxysalicylidene)-1,3-diamino-2-propanol), has been synthesized in crystalline phase. The zinc(II) complex has been characterized by elemental analysis, IR spectroscopy, UV-Vis spectroscopy, powder X-ray diffraction study (PXRD), 1H NMR, EI mass spectrometry and thermogravimetric analysis. PXRD revealed that 1 crystallizes in P - 1 space group with a = 9.218 Å, b = 10.849 Å, c = 18.339 Å, with unit cell volume is 2179.713 (Å)3. Fluorescence spectra in methanolic solution reflect that intensity of emission for 1 is much higher compared to H2L and both the compounds exhibit good fluorescence properties. The complex 1 exhibits significant catalytic activities of biological relevance, viz. catechol oxidase. In methanol, it efficiently catalyzes the oxidation of 3,5-di-tert-butylcatechol (3,5-DTBC) to corresponding quinone via formation of a dinuclear species as [Zn2(L)(3,5-DTBC)]. Electron Paramagnetic Resonance (EPR) experiment suggests generation of radicals in the presence of 3,5-DTBC and it may be proposed that the radical pathway is probably responsible for conversion of 3,5-DTBC to 3,5-DTBQ promoted by complex of redox-innocent Zn(II) ion.

  8. Expression, purification and preliminary crystallographic studies of human ketohexokinase.

    Science.gov (United States)

    Kozak, M; Hayward, B; Borek, D; Bonthron, D T; Jaskólski, M

    2001-04-01

    Ketohexokinase (KHK; E.C. 2.7.1.3) catalyses the (reversible) phosphorylation of fructose to fructose-1-phosphate. KHK is the first enzyme in a specialized catabolic pathway metabolizing dietary fructose to the glycolytic intermediate glyceraldehyde-3-phosphate. Mutations inactivating KHK underlie the metabolic disorder essential fructosuria. The primary structure of KHK shows no significant homology to other mammalian hexokinases. It is most similar to prokaryotic ribokinases, but catalyses a distinct phosphorylation reaction. Recombinant human KHK has been crystallized in the orthorhombic form (space group P2(1)2(1)2 or P2(1)2(1)2(1)). Single crystals of this polymorph suitable for X-ray diffraction have been obtained by vapour diffusion using 2-propanol and MPD as precipitants (pH 7.5). The crystals have unit-cell parameters a = 93.4, b = 121.5, c = 108.4 A. Diffraction data were collected to 4.3 A resolution. The asymmetric unit contains four protein molecules.

  9. Osmotic coefficients and apparent molar volumes of 1-hexyl-3-methylimidazolium trifluoromethanesulfonate ionic liquid in alcohols

    International Nuclear Information System (INIS)

    Highlights: • Physical and osmotic properties of [HMim][TfO] in alcohols are reported. • Apparent molar properties and osmotic coefficients were obtained. • Apparent molar volumes were fitted using a Redlich–Meyer type equation. • The osmotic coefficients were modeled with the Extended Pitzer and the MNRTL models. -- Abstract: In this work, density for the binary mixtures of 1-hexyl-3-methylimidazolium trifluoromethanesulfonate in alcohols (1-propanol, or 2-propanol, or 1-butanol, or 2-butanol, or 1-pentanol) was measured at T = 323.15 K and atmospheric pressure. From this property, the corresponding apparent molar volumes were calculated and fitted to a Redlich–Meyer type equation. For these mixtures, the osmotic and activity coefficients, and vapor pressures of these binary systems were also determined at the same temperature using the vapor pressure osmometry technique. The experimental osmotic coefficients were modeled by the Extended Pitzer model of Archer. The parameters obtained in this correlation were used to calculate the mean molal activity coefficients and the excess Gibbs free energy for the studied mixtures

  10. Osmotic and apparent molar properties of binary mixtures alcohol + 1-butyl-3-methylimidazolium trifluoromethanesulfonate ionic liquid

    International Nuclear Information System (INIS)

    Highlights: ► Osmotic and physical properties of binary mixtures {alcohol + [BMim][TfO]} were measured. ► From experimental data, apparent molar properties and osmotic coefficients were calculated. ► The apparent properties were fitted using a Redlich–Meyer type equation. ► The osmotic coefficients were correlated using the Extended Pitzer model. -- Abstract: In this work, physical properties (densities and speeds of sound) for the binary systems {1-propanol, or 2-propanol, or 1-butanol, or 2-butanol, or 1-pentanol + 1-butyl-3-methylimidazolium trifluoromethanesulfonate} were experimentally measured from T = (293.15 to 323.15) K and at atmospheric pressure. These data were used to calculate the apparent molar volume and apparent molar isentropic compression which were fitted to a Redlich–Meyer type equation. This fit was used to obtain the corresponding apparent molar properties at infinite dilution. On the other hand, the osmotic and activity coefficients and vapor pressures of these binary mixtures were also determined at T = 323.15 K using the vapor pressure osmometry technique. The Extended Pitzer model of Archer was employed to correlate the experimental osmotic coefficients. From the parameters obtained in the correlation, the mean molal activity coefficients and the excess Gibbs free energy for the studied mixtures were calculated

  11. Synthesis and characterization of undoped and cobalt-doped TiO2 nanoparticles via sol-gel technique

    Science.gov (United States)

    Mugundan, S.; Rajamannan, B.; Viruthagiri, G.; Shanmugam, N.; Gobi, R.; Praveen, P.

    2015-04-01

    TiO2 nanoparticles doped with different concentrations of cobalt (4, 8, 12 and 16 %) were synthesized by sol-gel method at room temperature with appropriate reactants. In general, TiO2 can exist in anatase, rutile, and brookite phases. In this present study, we used titanium tetra iso propoxide and 2-propanol as a common starting materials and the obtained products were calcined at 500 °C and 800 °C to get anatase and rutile phases, respectively. The crystalline sizes of the doped and undoped TiO2 nanoparticles were observed with X-ray diffraction (XRD) analysis. The functional groups of the samples were identified by Fourier transform infrared spectroscopy (FTIR). From UV-VIS diffuse reflectance spectra (DRS), the band gap energy and excitation wavelength of doped and undoped TiO2 nanoparticles were identified. The defect oriented emissions were seen from photoluminescence (PL) study. The spherical uniform size distribution of particles and elements present in the samples was determined using two different techniques viz., scanning electron microscopy (SEM) with energy-dispersive spectrometer (EDX) and transmission electron microscope (TEM) with selected area electron diffraction (SAED) pattern. The second harmonic generation (SHG) efficiency was also found and the obtained result was compared with potassium di hydrogen phosphate (KDP).

  12. The Influence of Crown Ether and Alcohol on Unsaturation and Molar Mass of Poly(propylene oxide)s Prepared by Use of Potassium t-Butoxide: Reinvestigation of Chain Transfer Reactions

    Science.gov (United States)

    Jurek-Suliga, Justyna; Skrzeczyna, Kinga; Gabor, Jadwiga; Łężniak, Marta

    2016-01-01

    Potassium t-butoxide dissolved in tetrahydrofuran effectively initiates homogeneous polymerization of propylene oxide at room temperature. Unsaturation and molar mass (Mn) of the polymers prepared depend on the presence of additives, such as macrocyclic ligand 18-crown-6 (L) and t-butanol. Application of the ligand alone results in distinct increase of unsaturation and decrease of Mn, whereas use of t-BuOH leads to simultaneous decrease of unsaturation and Mn. Activation of t-BuOK/t-BuOH system with the ligand causes further decrease of unsaturation, that is, from 12.0 to 3.5 mol % for OK/OH (1/3) and OK/OH/L (1/3/2) systems, respectively. Unexpectedly, Mn of the polymers obtained does not practically change (~4800). This result differs from that reported earlier for neat PO polymerization initiated potassium 1-methoxy-2-propoxide/1-methoxy-2-propanol, in which in the presence of the same ligand Mn increases to ~12 400 for the same ratio of reagents. The mechanism of studied processes was discussed. PMID:27528874

  13. Fabrication and Intermolecular Interactions of Silk Fibroin/Hydroxybutyl Chitosan Blended Nanofibers

    Directory of Open Access Journals (Sweden)

    Xiu-Mei Mo

    2011-03-01

    Full Text Available The native extracellular matrix (ECM is composed of a cross-linked porous network of multifibril collagens and glycosaminoglycans. Nanofibrous scaffolds of silk fibroin (SF and hydroxybutyl chitosan (HBC blends were fabricated using 1,1,1,3,3,3-hexafluoro-2-propanol (HFIP and trifluoroacetic acid (TFA as solvents to biomimic the native ECM via electrospinning. Scanning electronic microscope (SEM showed that relatively uniform nanofibers could be obtained when 12% SF was blended with 6% HBC at the weight ratio of 50:50. Meanwhile, the average nanofibrous diameter increased when the content of HBC in SF/HBC blends was raised from 20% to 100%. Fourier transform infrared spectra (FTIR and 13C nuclear magnetic resonance (NMR showed SF and HBC molecules existed in hydrogen bonding interactions but HBC did not induce conformation of SF transforming from random coil form to β-sheet structure. X-ray diffraction (XRD confirmed the different structure of SF/HBC blended nanofibers from both SF and HBC. Thermogravimetry-Differential thermogravimetry (TG-DTG results demonstrated that the thermal stability of SF/HBC blend nanofibrous scaffolds was improved. The results indicated that the rearrangement of HBC and SF molecular chain formed a new structure due to stronger hydrogen bonding between SF and HBC. These electrospun SF/HBC blended nanofibers may provide an ideal tissue engineering scaffold and wound dressing.

  14. A robust whole-cell biocatalyst that introduces a thermo- and solvent-tolerant lipase into Aspergillus oryzae cells: characterization and application to enzymatic biodiesel production.

    Science.gov (United States)

    Adachi, Daisuke; Koh, FookHee; Hama, Shinji; Ogino, Chiaki; Kondo, Akihiko

    2013-05-10

    To develop a robust whole-cell biocatalyst that works well at moderately high temperature (40-50°C) with organic solvents, a thermostable lipase from Geobacillus thermocatenulatus (BTL2) was introduced into an Aspergillus oryzae whole-cell biocatalyst. The lipase-hydrolytic activity of the immobilized A. oryzae (r-BTL) was highest at 50°C and was maintained even after an incubation of 24-h at 60°C. In addition, r-BTL was highly tolerant to 30% (v/v) organic solvents (dimethyl carbonate, ethanol, methanol, 2-propanol or acetone). The attractive characteristics of r-BTL also worked efficiently on palm oil methanolysis, resulting in a nearly 100% conversion at elevated temperature from 40 to 50°C. Moreover, r-BTL catalyzed methanolysis at a high methanol concentration without a significant loss of lipase activity. In particular, when 2 molar equivalents of methanol were added 2 times, a methyl ester content of more than 90% was achieved; the yield was higher than those of conventional whole-cell biocatalyst and commercial Candida antarctica lipase (Novozym 435). On the basis of the results regarding the excellent lipase characteristics and efficient biodiesel production, the developed whole-cell biocatalyst would be a promising biocatalyst in a broad range of applications including biodiesel production. PMID:23608501

  15. Catalyst-Free Synthesis of ZnO Nanowires on Oxidized Silicon Substrate for Gas Sensing Applications.

    Science.gov (United States)

    Behera, B; Chandra, S

    2015-06-01

    In the present work, we report the synthesis of nanostructured ZnO by oxidation of zinc film without using a seed or catalyst layer. The zinc films were deposited on oxidized Si substrates by RF magnetron sputtering process. These were oxidized in dry and wet air/oxygen ambient. The optimized process yielded long nanowires of ZnO having diameter of around 60-70 nm and spread uniformly over the surface. The effect of oxidation temperature, time, Zn film thickness and the ambient has strong influence on the morphology of resulting nanostruxctured ZnO film. The films were characterized by scanning electron microscopy for morphological studies and X-ray diffraction (XRD) analysis to study the phase of the nanostructured ZnO. Room temperature photoluminescence (PL) measurements of the nanowires show UV and green emission. A sensor was designed and fabricated using nanostructured ZnO film, incorporating inter-digital-electrode (IDE) for the measurement of resistance of the sensing layer. The gas sensing properties were investigated from the measurement of change in resistance when exposed to vapours of different volatile organic compound (VOC) such as acetone, ethanol, methanol and 2-propanol. The results suggest that ZnO nanowires fabricated by this method have potential application in gas sensors.

  16. Picosecond pulse radiolysis study of primary reactions in solutions

    International Nuclear Information System (INIS)

    Following the discovery of ionizing radiations and their chemical effects, it was important to study and comprehend the formation mechanisms of short lived free radicals and molecular products. In order to perform such studies, researchers and research groups worked on developing tools allowing both formation and detection of those species at short time scales. Nowadays, pulse radiolysis imposed itself as a fundamental and efficient tool allowing scientists to probe chemical effects as well as reaction mechanisms in studied media. The Laboratoire de Chimie Physique d'Orsay 'LCP' is an interdisciplinary laboratory hosting the platform of fast kinetics known as 'ELYSE'. Due to its femtosecond laser and its picosecond electron accelerator, we have the possibility to study chemical effects of ionizing radiations interaction with media at ultrashort times up to ∼5 ps.Knowing that we are interested in primary reactions induced in aqueous media by ionizing radiations, ELYSE represents the essential tool in performing our studies. The obtained results concern:- First direct determination of hydroxyl radical 'HO*' radiolytic yield as function of time at picosecond time scale;- Direct effect of ionizing radiation in highly concentrated aqueous solutions as well as investigation of the ultrafast electron transfer reaction between solute molecules and positive holes 'H2O*+' formed upon water radiolysis;- Study at room temperature of electron transfer reaction between solvated electron (electron donor) and organic solutes (electron acceptors) en viscous medium;- Study at room temperature of electron's solvation dynamics in ethylene glycol and 2-propanol. (author)

  17. Electrospun silk fibroin-hydroxybutyl chitosan nanofibrous scaffolds to biomimic extracellular matrix.

    Science.gov (United States)

    Zhang, Kuihua; Qian, Yongfang; Wang, Hongsheng; Fan, Linpeng; Huang, Chen; Mo, Xiumei

    2011-01-01

    Silk fibroin (SF)-hydroxybutyl chitosan (HBC) blend nanofibrous scaffolds were fabricated using 1,1,1,3,3,3-hexafluoro-2-propanol (HFIP) and trifluoroacetic acid (TFA) as solvents to biomimic the native ECM by electrospinning. SEM results showed that the average nanofibrous diameter increased when the content of HBC was raised from 20% to 100%. Whereas water contact angle measurements confirmed that SF/HBC nanofibrous scaffolds with different weight ratios were of good hydrophilicity. Both the tensile strength and the elongation at break were improved obviously when the weight ratio of SF to HBC was 20:80. (13)C-NMR clarified that SF and HBC molecules existed in H-bond interactions, but HBC did not induce SF conformation to transform from random coil form to β-sheet structure. Moreover, the use of genipin vapour not only induced conformation of SF to convert from random coil to β-sheet structure but also acted as a cross-linking agent for SF and HBC. Cell viability studies demonstrated that SF/HBC nanofibrous scaffolds presented good cellular compatibility. Thus, electrospun SF/HBC blended nanofibres may provide an ideal biomimic tissue-engineering scaffold. PMID:20615313

  18. Synthesis of {sup 14}C-labelled hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX), 2,4,6-trinitrotoluene (TNT), nitrocellulose (NC) and glycidyl azide polymer (GAP) for use in assessing the biodegradation potential of these energetic compounds

    Energy Technology Data Exchange (ETDEWEB)

    Ampleman, G.; Thiboutot, S.; Lavigne, J.; Marois, A. [Defence Research Establishment Valcartier, Courcelette, PQ (Canada); Hawari, J.; Jones, A.M.; Rho, D. [National Research Council of Canada, Ottawa, ON (Canada)

    1995-06-01

    Within the framework of an R and D project on bioremediation of soils contaminated with energetic compounds, the biodegradation of energetic products such as hexogen (RDX), trinitrotoluene (TNT), nitrocellulose (NC) and glycidyl azide polymer (GAP) is under study. Microcosm assays must be performed with radioactive carbon-14 labelled products in order to follow the biodegradation process. {sup 14}C-RDX was prepared by nitration of hexamethylenetetramine (HMTA) according to the Hale process. {sup 14}C-ring and methyl labelled TNTs synthesized according to the Dorey and Carper procedure. {sup 14}C-cellulose was synthesized from {sup 14}C-glucose by Acetobacter xylinum. Nitration of the {sup 14}C-cellulose yielded {sup 14}C-nitrocellulose. {sup 14}C-glycidyl azide polymer was obtained by polymerization and azidation of {sup 14}C-epichlorohydrin (ECH) which was synthesized from {sup 14}C-glycerol. Hydrochlorination of {sup 14}C-glycerol and epoxidation of the resulting {sup 14}C-1,3-dichloro 2-propanol yielded {sup 14}C-ECH. The syntheses of these {sup 14}C-labelled explosives are described in this paper. (Author).

  19. Calcium phosphate/microgel composites for 3D powderbed printing of ceramic materials.

    Science.gov (United States)

    Birkholz, Mandy-Nicole; Agrawal, Garima; Bergmann, Christian; Schröder, Ricarda; Lechner, Sebastian J; Pich, Andrij; Fischer, Horst

    2016-06-01

    Composites of microgels and calcium phosphates are promising as drug delivery systems and basic components for bone substitute implants. In this study, we synthesized novel composite materials consisting of pure β-tricalcium phosphate and stimuli-responsive poly(N-vinylcaprolactam-co-acetoacetoxyethyl methacrylate-co-vinylimidazole) microgels. The chemical composition, thermal properties and morphology for obtained composites were extensively characterized by Fourier transform infrared, X-ray photoelectron spectroscopy, IGAsorp moisture sorption analyzer, thermogravimetric analysis, granulometric analysis, ESEM, energy dispersive X-ray spectroscopy and TEM. Mechanical properties of the composites were evaluated by ball-on-three-balls test to determine the biaxial strength. Furthermore, initial 3D powderbed-based printing tests were conducted with spray-dried composites and diluted 2-propanol as a binder to evaluate a new binding concept for β-tricalcium phosphate-based granulates. The printed ceramic bodies were characterized before and after a sintering step by ESEM. The hypothesis that the microgels act as polymer adhesive agents by efficient chemical interactions with the β-tricalcium phosphate particles was confirmed. The obtained composites can be used for the development of new scaffolds.

  20. Identification of Wet-Spinning and Post-Spin Stretching Methods Amenable to Recombinant Spider Aciniform Silk.

    Science.gov (United States)

    Weatherbee-Martin, Nathan; Xu, Lingling; Hupe, Andre; Kreplak, Laurent; Fudge, Douglas S; Liu, Xiang-Qin; Rainey, Jan K

    2016-08-01

    Spider silks are outstanding biomaterials with mechanical properties that outperform synthetic materials. Of the six fibrillar spider silks, aciniform (or wrapping) silk is the toughest through a unique combination of strength and extensibility. In this study, a wet-spinning method for recombinant Argiope trifasciata aciniform spidroin (AcSp1) is introduced. Recombinant AcSp1 comprising three 200 amino acid repeat units was solubilized in a 1,1,1,3,3,3-hexafluoro-2-propanol (HFIP)/water mixture, forming a viscous α-helix-enriched spinning dope, and wet-spun into an ethanol/water coagulation bath allowing continuous fiber production. Post-spin stretching of the resulting wet-spun fibers in water significantly improved fiber strength, enriched β-sheet conformation without complete α-helix depletion, and enhanced birefringence. These methods allow reproducible aciniform silk fiber formation, albeit with lower extensibility than native silk, requiring conditions and methods distinct from those previously reported for other silk proteins. This provides an essential starting point for tailoring wet-spinning of aciniform silk to achieve desired properties. PMID:27387592

  1. Natural organic matter and sunlight accelerate the degradation of 17ss-estradiol in water

    Energy Technology Data Exchange (ETDEWEB)

    Leech, Dina M. [Institute of Marine Sciences, University of North Carolina at Chapel Hill, 3431 Arendell Street, Morehead City, NC 28557 (United States)], E-mail: dmleech@email.unc.edu; Snyder, Matthew T.; Wetzel, Robert G. [Department of Environmental Sciences and Engineering, School of Public Health, University of North Carolina at Chapel Hill, Chapel Hill, NC 27599 (United States)

    2009-03-01

    Nanomolar concentrations of steroid hormones such as 17{beta}-estradiol can influence the reproductive development and sex ratios of invertebrate and vertebrate populations. Thus their release into surface and ground waters from wastewater facilities and agricultural applications of animal waste is of environmental concern. Many of these compounds are chromophoric and susceptible to photolytic degradation. High intensity UV-C radiation has been demonstrated to degrade some of these compounds in engineered systems. However, the degradation efficacy of natural solar radiation in shallow fresh waters is less understood. Here photolytic experiments with 17{beta}-estradiol demonstrated modest photodegradation ({approx} 26%) when exposed to simulated sunlight between 290 and 720 nm. Photodegradation significantly increased ({approx} 40-50%) in the presence of 2.0-15.0 mg/l of dissolved organic carbon (DOC) derived from humic acids of the Suwannee River, GA. However, rates of photodegradation reached a threshold at approximately 5.0 mg/l DOC. Observed suppression of photolysis in the presence of a radical inhibitor (i.e. 2-propanol) indicated that a significant proportion of the degradation was due to radicals formed from the photolysis of DOC. Although photodegradation was greatest in full sunlight containing UV-B (290-320 nm), degradation was also detected with UV-A (320-400 nm) and visible light (400-720 nm) alone.

  2. Influence of the structure of polyfluorinated alcohols on Brønsted acidity/hydrogen-bond donor ability and consequences on the promoter effect.

    Science.gov (United States)

    Vuluga, Daniela; Legros, Julien; Crousse, Benoit; Slawin, Alexandra M Z; Laurence, Christian; Nicolet, Pierre; Bonnet-Delpon, Danièle

    2011-02-18

    The influence of substituents on the properties of tri- and hexafluorinated alcohols derived from 2,2,2-trifluoroethanol (TFE) and 1,1,1,3,3,3-hexafluoro-2-propanol (HFIP) was examined. Measurements of specific solvent-solute interactions revealed that H-bond donation (HBD) of fluorinated alcohols is sensitive to the steric hindrance of the OH group, whereas their Brønsted acidity is dependent only on the number of fluorine atoms. For hexafluorinated alcohols (HFAs), their association with amines characterized by X-ray diffraction showed that the balance between HBD and acidity is influenced by their structure. Moreover, the ability of HFAs to donate H-bonds is exerted in synclinal (sc), synperiplanar (sp), and also antiperiplanar (ap) conformations along the C-O bond. Comparison of the effects of fluorinated alcohols as promoting solvents in three reactions is reported. The positive correlation between rate constants and H-bonding donation ability for sulfide oxidation and imino Diels-Alder reaction brings to light the role of this property, while acidity might have a minor influence. In the third reaction, epoxide opening by piperidine, none of these properties can clearly be put forward at this stage.

  3. Decellularized omentum as novel biologic scaffold for reconstructive surgery and regenerative medicine

    Directory of Open Access Journals (Sweden)

    A. Porzionato

    2013-01-01

    Full Text Available Homologous tissues, such as adipose tissue, may be an interesting source of acellular scaffolds, maintaining a complex physiological three-dimensional (3D structure, to be recellularized with autologous cells. The aim of the present work is to evaluate the possibility of obtaining homologous acellular scaffolds from decellularization of the omentum, which is known to have a complex vascular network. Adult rat and human omenta were treated with an adapted decellularization protocol involving mechanical rupture (freeze-thaw cycles, enzymatic digestion (trypsin, lipase, deoxyribonuclease, ribonuclease and lipid extraction (2-propanol. Histological staining confirmed the effectiveness of decellularization, resulting in cell-free scaffolds with no residual cells in the matrix. The complex 3D networks of collagen (azan-Mallory, elastic fibers (Van Gieson, reticular fibers and glycosaminoglycans (PAS were maintained, whereas Oil Red and Sudan stains showed the loss of lipids in the decellularized tissue. The vascular structures in the tissue were still visible, with preservation of collagen and elastic wall components and loss of endothelial (anti-CD31 and -CD34 immunohistochemistry and smooth muscle (anti-alpha smooth muscle actin cells. Fat-rich and well vascularized omental tissue may be decellularized to obtain complex 3D scaffolds preserving tissue architecture potentially suitable for recellularization. Further analyses are necessary to verify the possibility of recolonization of the scaffold by adipose-derived stem cells in vitro and then in vivo after re-implantation, as already known for homologus implants in regenerative processes.

  4. Development of fast and robust multiresidual LC-MS/MS method for determination of pharmaceuticals in soils.

    Science.gov (United States)

    Golovko, Oksana; Koba, Olga; Kodesova, Radka; Fedorova, Ganna; Kumar, Vimal; Grabic, Roman

    2016-07-01

    The aim of this study was to develop a simple extraction procedure and a multiresidual liquid chromatography-tandem mass spectrometry method for determination of a wide range of pharmaceuticals from various soil types. An extraction procedure for 91 pharmaceuticals from 13 soil types, followed by liquid chromatography-tandem mass spectrometry analysis, was optimized. The extraction efficiencies of three solvent mixtures for ultrasonic extraction were evaluated for 91 pharmaceuticals. The best results were obtained using acetonitrile/water (1/1 v/v with 0.1 % formic acid) followed by acetonitrile/2-propanol/water (3/3/4 v/v/v with 0.1 % formic acid) for extracting 63 pharmaceuticals. The method was validated at three fortification levels (10, 100, and 1000 ng/g) in all types of representative soils; recovery of 44 pharmaceuticals ranged between 55 and 135 % across all tested soils. The method was applied to analyze actual environmental samples of sediments, soils, and sludge, and 24 pharmaceuticals were found above limit of quantification with concentrations ranging between 0.83 ng/g (fexofenadine) and 223 ng/g (citalopram). PMID:27044290

  5. Modelling On Photogeneration Of Hydroxyl Radical In Surface Waters And Its Reactivity Towards Pharmaceutical Wastes

    Science.gov (United States)

    Das, Radha; Vione, Davide; Rubertelli, Francesca; Maurino, Valter; Minero, Claudio; Barbati, Stéphane; Chiron, Serge

    2010-10-01

    This paper reports a simple model to describe the formation and reactivity of hydroxyl radicals in the whole column of freshwater lakes. It is based on empirical irradiation data and is a function of the water chemical composition (the photochemically significant parameters NPOC, nitrate, nitrite, carbonate and bicarbonate), the lake conformation best expressed as the average depth, and the water absorption spectrum in a simplified Lambert-Beer approach. The purpose is to derive the lifetime of dissolved molecules, due to reaction with •OH, on the basis of their second-order rate constants with the hydroxyl radical. The model was applied to two compounds of pharmaceutical wastes ibuprofen and carbamazepine, for which the second-order rate constants for reaction with the hydroxyl radical were measured by means of the competition kinetics with 2-propanol. The measured values of the rate constants are 1.0×1010 and 1.6×1010M-1 s-1 for ibuprofen and carbamazepine, respectively. The model suggests that the lifetime of a given compound can be very variable in different lakes, even more than the lifetime of different compounds in the same lake. It can be concluded that as far as the reaction with •OH, is concerned the concepts of photolability and photostability, traditionally attached to definite compounds, are ecosystem-dependent at least as much as they depend on the molecule under consideration.

  6. Acid lipase from Candida viswanathii: production, biochemical properties, and potential application.

    Science.gov (United States)

    de Almeida, Alex Fernando; Tauk-Tornisielo, Sâmia Maria; Carmona, Eleonora Cano

    2013-01-01

    Influences of environmental variables and emulsifiers on lipase production of a Candida viswanathii strain were investigated. The highest lipase activity (101.1 U) was observed at 210 rpm, pH 6.0, and 27.5°C. Other fermentation parameters analyzed showed considerable rates of biomass yield (Y L/S = 1.381 g/g), lipase yield (Y L/S = 6.892 U/g), and biomass productivity (P X = 0.282 g/h). Addition of soybean lecithin increased lipase production in 1.45-fold, presenting lipase yield (Y L/S ) of 10.061 U/g. Crude lipase presented optimal activity at acid pH of 3.5, suggesting a new lipolytic enzyme for this genus and yeast in general. In addition, crude lipase presented high stability in acid conditions and temperature between 40 and 45°C, after 24 h of incubation in these temperatures. Lipase remained active in the presence of organic solvents maintaining above 80% activity in DMSO, methanol, acetonitrile, ethanol, acetone, 1-propanol, isopropanol, and 2-propanol. Effectiveness for the hydrolysis of a wide range of natural triglycerides suggests that this new acid lipase has high potential application in the oleochemical and food industries for hydrolysis and/or modification of triacylglycerols to improve the nutritional properties. PMID:24350270

  7. Dual delivery of active antibactericidal agents and bone morphogenetic protein at sustainable high concentrations using biodegradable sheath-core-structured drug-eluting nanofibers

    Science.gov (United States)

    Hsu, Yung-Hen; Lin, Chang-Tun; Yu, Yi-Hsun; Chou, Ying-Chao; Liu, Shih-Jung; Chan, Err-Cheng

    2016-01-01

    In this study, we developed biodegradable sheath-core-structured drug-eluting nanofibers for sustainable delivery of antibiotics (vancomycin and ceftazidime) and recombinant human bone morphogenetic protein (rhBMP-2) via electrospinning. To prepare the biodegradable sheath-core nanofibers, we first prepared solutions of poly(d,l)-lactide-co-glycolide, vancomycin, and ceftazidime in 1,1,1,3,3,3-hexafluoro-2-propanol and rhBMP-2 in phosphate-buffered solution. The poly(d,l)-lactide-co-glycolide/antibiotics and rhBMP-2 solutions were then fed into two different capillary tubes controlled by two independent pumps for coaxial electrospinning. The electrospun nanofiber morphology was observed under a scanning electron microscope. We further characterized the in vitro antibiotic release from the nanofibers via high-performance liquid chromatography and that of rhBMP-2 via enzyme-linked immunosorbent assay and alkaline phosphatase activity. We showed that the biodegradable coaxially electrospun nanofibers could release high vancomycin/ceftazidime concentrations (well above the minimum inhibition concentration [MIC]90) and rhBMP-2 for >4 weeks. These experimental results demonstrate that novel biodegradable nanofibers can be constructed with various pharmaceuticals and proteins for long-term drug deliveries. PMID:27574423

  8. Bimodal fibrous structures for tissue engineering: Fabrication, characterization and in vitro biocompatibility.

    Science.gov (United States)

    Tiwari, Arjun Prasad; Joshi, Mahesh Kumar; Kim, Jeong In; Unnithan, Afeesh Rajan; Lee, Joshua; Park, Chan Hee; Kim, Cheol Sang

    2016-08-15

    We report for the first time a polycaprolactone-human serum albumin (PCL-HSA) membrane with bimodal structures comprised of spider-web-like nano-nets and conventional fibers via facile electro-spinning/netting (ESN) technique. Such unique controllable morphology was developed by electrospinning the blend solution of PCL (8wt% in HFIP 1,1,1,3,3,3,-Hexafluoro-2-propanol) and HSA (10wt% deionized water). The phase separation during electrospinning caused the formation of bimodal structure. Various processing factors such as applied voltage, feeding rate, and distance between nozzle tip and collector were found responsible for the formation and distribution of the nano-nets throughout the nanofibrous mesh. Field emission electron microscopy (FE-SEM) confirmed that the nano-nets were composed of interlinked nanowires with an ultrathin diameter (10-30nm). When compared with a pure PCL membrane, the membrane containing nano-nets was shown to have better support for cellular activities as determined by cell viability and attachment assays. These results revealed that the blending of albumin, a hydrophilic biomolecule, with PCL, a hydrophobic polymer, proves to be an outstanding approach to developing membranes with controlled spider-web-like nano-nets for tissue engineering. PMID:27179176

  9. A thermodynamic study of ketoreductase-catalyzed reactions 5. Reduction of substituted ketones in n-hexane

    Energy Technology Data Exchange (ETDEWEB)

    Tewari, Yadu B. [Biochemical Science and Analytical Chemistry Division, National Institute of Standards and Technology, Gaithersburg, MD 20899 (United States)], E-mail: yadu.tewari@nist.gov; Vanderah, David J. [Biochemical Science and Analytical Chemistry Division, National Institute of Standards and Technology, Gaithersburg, MD 20899 (United States)], E-mail: david.vanderah@nist.gov; Schantz, Michele M. [Biochemical Science and Analytical Chemistry Division, National Institute of Standards and Technology, Gaithersburg, MD 20899 (United States)], E-mail: michele.schantz@nist.gov; Goldberg, Robert N. [Biochemical Science and Analytical Chemistry Division, National Institute of Standards and Technology, Gaithersburg, MD 20899 (United States)], E-mail: robert.goldberg@nist.gov; Rozzell, J. David [Codexis, Inc., 129 N. Hill Avenue, Pasadena, CA 91106 (United States)], E-mail: david.rozzell@codexis.com; Liebman, Joel F. [Department of Chemistry and Biochemistry, University of Maryland, Baltimore County, Baltimore, MD 21250 (United States)], E-mail: jliebman@umbc.edu; Hui, Raymond Wai-Man; Nissenbaum, Yitzy; Parniani, Ahmad Reza [Department of Chemistry and Biochemistry, University of Maryland, Baltimore County, Baltimore, MD 21250 (United States)

    2008-04-15

    The equilibrium constants K for the ketoreductase-catalyzed reduction reactions of 1-benzyl-3-pyrrolidinone, ethyl 2-oxo-4-phenylbutyrate, ethyl 4-chloroacetoacetate, 1-benzyl-4-piperidone, and 1-benzyl-3-piperidone were measured in n-hexane at T = 298.15 K by using gas chromatography. The equilibrium constants for the reaction involving 1-benzyl-4-piperidone were also measured as a function of temperature (288.15 to 308.05) K. The calculated thermodynamic quantities for the reaction (1-benzyl-4-piperidone + 2-propanol = 1-benzyl-4-hydroxypiperidine + acetone) reaction carried out in n-hexane at T = 298.15 K are: K = (26.2 {+-} 1.7); {delta}{sub r}G{sub m}{sup 0}=-(8.10{+-}0.16)kJ.mol{sup -1}; {delta}{sub r}H{sub m}{sup 0}=-(3.44{+-}0.42)kJ.mol{sup -1}; and {delta}{sub r}S{sub m}{sup 0}=(15.6{+-}1.4)J.K{sup -1}.mol{sup -1}. The chirality of the hydroxyl products of the reactions has also been investigated. The results showed that the stereoselectivity of the hydroxyl products formed can be controlled by the selection of the solvent and enzyme used in these reactions. The thermochemical results for these reactions are compared with the results for reactions that have analogous structural features as well as with the results of quantum chemical calculations.

  10. Close correlation between heat shock response and cytotoxicity in Neurospora crassa treated with aliphatic alcohols and phenols

    Energy Technology Data Exchange (ETDEWEB)

    Meyer, U.; Schweim, P.; Fracella, F.; Rensing, L. [Univ. of Bremen (Germany)

    1995-03-01

    In Neurospora crassa the aliphatic alcohols methanol, ethanol, 1-propanol, 2-propanol, 1-butanol, 2-butanol, isobutanol, ethylene glycol, glycerol, and allyl alcohol and the phenolic compounds phenol, hydroquinone, resorcinol, pyrogallol, phloroglucinol, sodium salicylate, and acetylsalicylic acid were analyzed with respect to their capacities to induce heat shock proteins (HSP) and to inhibit protein synthesis. Both the alcohols and phenols showed the greatest levels of HSP induction at concentrations which inhibited the overall protein synthesis by about 50%. The abilities of the different alcohols to induce the heat shock response are proportional to their lipophilicities: the lipophilic alcohol isobutanol is maximally inductive at about 0.6 M, whereas the least lipophilic alcohol, methanol, causes maximal induction at 5.7 M. The phenols, in general, show a higher capability to induce the heat shock response. The concentrations for maximal induction range between 25 mM (sodium salicylate) and 100 mM (resorcinol). Glycerol (4.1 M) shifted the concentration necessary for maximal HSP induction by hydroquinone from 50 to 200 mM. The results reveal that the induction of HSP occurs under conditions which considerably constrain cell metabolism. The heat shock response, therefore, does not represent a sensitive marker for toxicity tests but provides a good estimate for the extent of cell damage.

  11. Intercalation Pseudocapacitance in Ultrathin VOPO4 Nanosheets: Toward High-Rate Alkali-Ion-Based Electrochemical Energy Storage.

    Science.gov (United States)

    Zhu, Yue; Peng, Lele; Chen, Dahong; Yu, Guihua

    2016-01-13

    There is a growing need for energy storage devices in numerous applications where a large amount of energy needs to be either stored or delivered quickly. The present paper details the study of alkali-ion intercalation pseudocapacitance in ultrathin VOPO4 nanosheets, which hold promise in high-rate alkali-ion based electrochemical energy storage. Starting from bulk VOPO4·2H2O chunks, VOPO4 nanosheets were obtained through simple ultrasonication in 2-propanol. These nanosheets as the cathode exhibit a specific capacity of 154 and 136 mAh/g (close to theoretical value 166 mAh/g) for lithium and sodium storage devices at 0.1 C and 100 and ∼70 mAh/g at 5 C, demonstrating their high rate capability. Moreover, the capacity retention is maintained at 90% for lithium ion storage and 73% for sodium ion storage after 500 cycles, showing their reasonable stability. The demonstrated alkali-ion intercalation pseudocapacitance represents a promising direction for developing battery materials with promising high rate capability.

  12. Chromatographic analyses of fatty acid methyl esters by HPLC-UV and GC-FID

    Energy Technology Data Exchange (ETDEWEB)

    Carvalho, Myller S.; Pinho, David M.M.; Suarez, Paulo A.Z., E-mail: psuarez@unb.br [Laboratorio de Materiais e Combustiveis, Instituto de Quimica, Universidade de Brasilia, DF (Brazil); Mendonca, Marcio A. [Faculdade de Agronomia e Medicina Veterinaria, Universidade de Brasilia, DF (Brazil); Resck, Ines S. [Laboratorio de Ressonancia Magnetica Nuclear, Universidade de Brasilia, DF (Brazil)

    2012-04-15

    An analytical method using high performance liquid chromatography with UV detection (HPLC-UV) (method A) was used for simultaneous determination of total amounts of triacylglycerides, diacylglycerides, monoacylglycerides and fatty acid methyl esters in alcoholysis of different oil (cotton, canola, sunflower, corn and soybean) samples. Analyses were carried out at 40 deg C for 20 min using a gradient of methanol (MeOH) and 2-propanol-hexane 5:4 (v/v) (PrHex): 100% of MeOH in 0 min, 50% of MeOH and 50% of PrHex in 10 min maintained with isocratic elution for 10 min. Another HPLC-UV method (method B) with acetonitrile isocratic elution for 34 min was used to determine the fatty acid composition of oils analyzing their methyl ester derivatives. Contents were determined with satisfactory repeatability (relative standard deviation, RSD < 3%), linearity (r{sup 2} > 0.99) and sensitivity (limit of quantification). Method B was compared with an official gas chromatographic method with flame ionization detection (GC-FID) from American Oil Chemists' Society (AOCS) in the determination of fatty acid methyl esters (FAME) in biodiesel real samples. (author)

  13. A Novel Aqueous Two Phase System Composed of a Thermo-Separating Polymer and an Organic Solvent for Purification of Thermo-Acidic Amylase Enzyme from Red Pitaya (Hylocereus polyrhizus Peel

    Directory of Open Access Journals (Sweden)

    Mehrnoush Amid

    2014-05-01

    Full Text Available The purification of thermo-acidic amylase enzyme from red pitaya (Hylocereus polyrhizus peel for the first time was investigated using a novel aqueous two-phase system (ATPS consisting of a thermo-separating copolymer and an organic solvent. The effectiveness of different parameters such as molecular weight of the thermo-separating ethylene oxide-propylene oxide (EOPO copolymer and type and concentration of organic solvent on the partitioning behavior of amylase was investigated. In addition, the effects of phase components, volume ratio (VR, pH and crude load of purification factor and yield of amylase were evaluated to achieve the optimum partition conditions of the enzyme. In the novel ATPS method, the enzyme was satisfactorily partitioned into the polymer-rich top phase in the system composed of 30% (w/w EOPO 2500 and 15% (w/w 2-propanol, at a volume ratio of 1.94 and with a crude load scale of 25% (w/w at pH 5.0. Recovery and recycling of components was also measured in each successive step of the ATPS process. The enzyme was successfully recovered by the method with a high purification factor of 14.3 and yield of 96.6% and copolymer was also recovered and recycled at a rate above 97%, making the method was more economical than the traditional ATPS method.

  14. PHOTOREDUCTIVE SEQUESTRATION OF CO2 TO FORM C1 PRODUCTS AND FUEL

    Energy Technology Data Exchange (ETDEWEB)

    Theodore Mill; Haruthai Tungudomwongsa

    2003-03-13

    Analytical methods for determining formic and oxalic acids, formaldehyde and methanol have been evaluated and/or optimized for measuring products from photoreduction of CO{sub 2} in illuminated, aqueous suspensions of photocatalysts. An electrophoretic analysis method can detect aqueous formate and oxalate ions at 3 and 1 {micro}M respectively. Recalibration of the Nash formaldehyde determination shows that as little as 0.5 {micro}M can be detected spectrally. Several experiments using suspensions of TiO{sub 2}, SrTiO{sub 3} and SrTiO{sub 3} with Cr and Sb were tested in CO{sub 2} saturated solutions. No formate was detected in most experiments. However adding 2-propanol to a CO{sub 2}/TiO{sub 2} suspension gave significant amounts of formate and some formaldehyde by blocking the re-oxidation of formate by semiconductor holes. Loss of C{sub 1} products by re-oxidation is probably an important process limiting the accumulation of formate, formaldehyde and methanol.

  15. Platinum-Niobium(V Oxide/Carbon Nanocomposites Prepared By Microwave Synthesis For Ethanol Oxidation

    Directory of Open Access Journals (Sweden)

    Virginija KEPENIENĖ

    2016-05-01

    Full Text Available In the present work, Pt nanoparticles were deposited by means of microwave synthesis on the primary carbon supported Nb2O5 composite which was prepared in two different ways: (A by dispersion of Nb2O5 and carbon with the mass ratio equal to 1:1 in a 2-propanol solution by ultrasonication for 30 min. with further desiccation of the mixture and (B by heating the Nb2O5/C composite obtained according to the procedure (A at 500 °C for 2 h. The transmission electron microscopy was used to determine the shape and the size of catalyst particles. X-ray diffraction and inductively coupled plasma optical emission spectroscopy were employed to characterize the structure and composition of the synthesized catalysts. The electrocatalytic activity of the synthesized catalysts towards the oxidation of ethanol in an alkaline medium was investigated by means of cyclic voltammetry.DOI: http://dx.doi.org/10.5755/j01.ms.22.2.8609

  16. Steam reforming of cyclic model compounds of bio-oil over Ni-based catalysts: Product distribution and carbon formation

    DEFF Research Database (Denmark)

    Trane-Restrup, Rasmus; Jensen, Anker Degn

    2015-01-01

    Steam reforming (SR) and oxidative steam reforming (OSR) of furfural, 2-methylfuran, and guaiacol have been investigated in the temperature range 400-800°C at a steam to carbon (S/C)-ratio of 5 and oxygen to carbon (O/C)-ratio of 0.2-1.4 over Ni/CeO2-K/MgAl2O4. Carbon oxides and H2 were the major...... products in the SR of 2-methylfuran and furfural, while the by-products were methane, ethanol, 2-propanol, and acetone. Temperatures of 500°C or above were needed to minimize the formation of by-products in the SR of 2-methylfuran and furfural. Phenolics, like benzenediols and phenol, were produced in high...... yields in the SR of guaiacol and temperatures of 780°C were needed to totally convert guaiacol to carbon oxides and H2.Carbon deposition was observed in the SR of all three model compounds and was most severe for guaiacol followed by furfural and 2-methylfuran. The carbon deposition could be reduced...

  17. Photochemical-spectrofluorimetric method for the determination of benzoylurea insecticides: applications in river water samples and in technical formulations.

    Science.gov (United States)

    Gil-Garcia, M D; Martínez-Galera, M; López-López, T; Martínez-Vidal, J L; Mahedero, M C; Salinas, F

    2001-01-26

    Ultraviolet (UV) irradiation was used to obtain fluorescent photoproducts from four non-fluorescent benzoylurea (BU) insecticides (flufenoxuron (FLF), lufenuron (LUF), hexaflumuron (HF) and triflumuron (TRF)). The effect of solvent, pH (in aqueous solutions), organic solvent percentage and UV irradiation time on the excitation and emission wavelengths and fluorescence intensity were investigated. The largest fluorescence signals and the shortest UV irradiation time were obtained in methanol, ethanol and 2-propanol. Linear calibration graphs were established in the interval between 0.025 and 1.000 microg ml(-1) from FLF and TRF and between 0.050 and 1.000 microg ml(-1) from LUF and HF with regression coefficients larger than 0.99. A method based on the use of the first-derivative of the spectra of photoproducts was applied to the determination of BU insecticides in river water samples and in technical formulations. The mean recoveries ranged from 95.0% to 110.0% in river water samples and from 92.0% to 101.0% in technical formulations, according to the compound. A preconcentration step, using LLE, allowed to reach the concentration levels established by the EU directive for pesticides in drinking water. PMID:18968181

  18. HPLC Analysis of Egg Yolk Phosphatidylcholine by Evaporative Light Scattering Detector

    Institute of Scientific and Technical Information of China (English)

    周婧; 胡仙妹; 王田心; 梁浩; 袁其朋

    2012-01-01

    Egg yolk phosphatidylcholine(EYPC) is being widely used in food and pharmaceutical industries nowadays owing to its surface activity,pharmaceutical usefulness,and so on.Common determination methods of phospholipids were based on the American Oil Chemists' Society(AOCS) Official Method Ja7b-91,in which n-hexane/2-propanol/acetate buffer was used as the mobile phase.In order to achieve desired results,gradient elu-tion or buffer solution was used,which made the detection process more complicated.Moreover,water or buffer solution could affect the silica gel column both on its lifespan and the separation efficiency significantly.In this study,different mobile phase and detector were used to simplify EYPC analyzing process instead of using water within the mobile phase.The optimized HPLC operating conditions are as follows:pure methanol as a mobile phase,flow rate of 1.0 ml·min-1,silica gel column(250 mm×4.6 mm,5 μm,Inertsil GLTM),column temperature 30 ℃ and low temperature evaporative light scattering detector(40 ℃,0.35 MPa) as used.Under this optimal condition,the linear relative coefficient of the standard curve is 0.998 and the recovery was in the range of 96.83%-101.58% with a relative standard deviation of 1.79%(n=6).

  19. Acid Lipase from Candida viswanathii: Production, Biochemical Properties, and Potential Application

    Directory of Open Access Journals (Sweden)

    Alex Fernando de Almeida

    2013-01-01

    Full Text Available Influences of environmental variables and emulsifiers on lipase production of a Candida viswanathii strain were investigated. The highest lipase activity (101.1 U was observed at 210 rpm, pH 6.0, and 27.5°C. Other fermentation parameters analyzed showed considerable rates of biomass yield ( g/h. Addition of soybean lecithin increased lipase production in 1.45-fold, presenting lipase yield ( of 10.061 U/g. Crude lipase presented optimal activity at acid pH of 3.5, suggesting a new lipolytic enzyme for this genus and yeast in general. In addition, crude lipase presented high stability in acid conditions and temperature between 40 and 45°C, after 24 h of incubation in these temperatures. Lipase remained active in the presence of organic solvents maintaining above 80% activity in DMSO, methanol, acetonitrile, ethanol, acetone, 1-propanol, isopropanol, and 2-propanol. Effectiveness for the hydrolysis of a wide range of natural triglycerides suggests that this new acid lipase has high potential application in the oleochemical and food industries for hydrolysis and/or modification of triacylglycerols to improve the nutritional properties.

  20. Acid lipase from Candida viswanathii: production, biochemical properties, and potential application.

    Science.gov (United States)

    de Almeida, Alex Fernando; Tauk-Tornisielo, Sâmia Maria; Carmona, Eleonora Cano

    2013-01-01

    Influences of environmental variables and emulsifiers on lipase production of a Candida viswanathii strain were investigated. The highest lipase activity (101.1 U) was observed at 210 rpm, pH 6.0, and 27.5°C. Other fermentation parameters analyzed showed considerable rates of biomass yield (Y L/S = 1.381 g/g), lipase yield (Y L/S = 6.892 U/g), and biomass productivity (P X = 0.282 g/h). Addition of soybean lecithin increased lipase production in 1.45-fold, presenting lipase yield (Y L/S ) of 10.061 U/g. Crude lipase presented optimal activity at acid pH of 3.5, suggesting a new lipolytic enzyme for this genus and yeast in general. In addition, crude lipase presented high stability in acid conditions and temperature between 40 and 45°C, after 24 h of incubation in these temperatures. Lipase remained active in the presence of organic solvents maintaining above 80% activity in DMSO, methanol, acetonitrile, ethanol, acetone, 1-propanol, isopropanol, and 2-propanol. Effectiveness for the hydrolysis of a wide range of natural triglycerides suggests that this new acid lipase has high potential application in the oleochemical and food industries for hydrolysis and/or modification of triacylglycerols to improve the nutritional properties.

  1. Catalytic Hydrogenation of Methanol-Containing Eflfuent from Epoxidation of Propylene

    Institute of Scientific and Technical Information of China (English)

    Cheng Ke

    2015-01-01

    This paper describes the hydrogenation of impurities in the methanol-containing eflfuent from the propylene epoxidation process with hydrogen peroxide. The effects of reaction temperature, pressure, weight hourly space velocity (WHSV) and H2/methanol ratio on the concentration of various impurities in methanol solvent were investigated. It was found out that the aldehyde, hydrogen peroxide and nitro compounds in the methanol solvent could be completely hydroge-nated over the Ni catalyst under proper reaction conditions. 90%of acetone and up to 50%of acetals (ketals) existing in the methanol solvent could be hydrogenated. No signiifcant change was observed for the rest of the impurities that were present in the methanol solvent (i. e., 1-methoxy-2-propanol, 2-methoxy-1-propanol and 1,2-propanediol). The H2O2 decomposition reaction was enhanced using Ni catalyst, through the formation of NioOH, but no oxygen was found in the off-gas of hy-drogenation reaction since NioH could react on NioOH formed via dissociative adsorption of hydrogen peroxide, or on NioO formed via adsorption of oxygen.

  2. Fotólise no estado estacionário e com pulso de laser de 1-benzociclanonas e de seus derivados a,a -dimetilados Steady-state and laser flash photolysis of 1 - benzocyclanones and their a,a -dimethyl derivatives

    Directory of Open Access Journals (Sweden)

    José Carlos Netto-Ferreira

    1999-07-01

    Full Text Available Laser excitation of 0.01 M solutions of 1-indanone (Ia, 1-tetralone (Ib, 1-benzosuberone (Ic, and their a,a -dimethyl derivatives IIa-c, respectively, in benzene, produced transients with maximum absorption at 425 nm, and lifetimes ranging from 62 ns (IIa to 5.5ms (Ic. Quenching studies using well known triplet quenchers such as 1,3-cyclohexadiene and oxygen demonstrated the triplet nature of these transients. In the presence of hydrogen donors, such as 2-propanol, the triplet state decay of the ketones Ia-c leads to the formation of the corresponding ketyl radicals, i.e. IIIa-c, which show absorption spectra very similar to the parent ketone, with lmax at 430 nm and lifetime in excess of 20 ms. Steady state irradiations show that the a,a -dimethyl ketones IIa and IIc form ortho-alkyl benzaldehydes probably derived from an initial a-cleavage of the corresponding triplet excited states.

  3. Determination and Correlation of Solubilities of Four Novel Benzothiazolium Ionic Liquids with 6PF- in Six Alcohols

    Institute of Scientific and Technical Information of China (English)

    何志坚; 王小敏; 姚田; 宋航; 姚舜

    2014-01-01

    Four novel benzothiazolium ionic liquids with 6PF- ([C1Bth][PF6], [C4Bth][PF6], [C5Bth][PF6] and [C6Bth][PF6]) were synthesized, and the rang of their melting points were determined between 358.35 K-424.05 K. The relationship of their melting points and the length of the straight alkyl chain on cation reflected‘S’ type ten-dency. Then, the solubilities of the four ionic liquids in six lower alcohols (methanol, ethanol, 1-propanol, 2-propanol, 1-butanol and 2-methyl-1-propanol) were measured in the temperature rang of 253.15-383.15 K at at-mospheric pressure with static analytical method, respectively. It was found that [C6Bth][PF6] in all investigated ionic liquids had the largest solubility in six alcohols and the solubility of [C4Bth][PF6] in methanol was very sensi-tive for temperature in 313.15-333.15 K, which was so-called “temperature-sensitivity”. This feature is of great significance to their application of catalyzing reaction or extraction process, and makes the recovery and reuse of ionic liquids (ILs) become easier. Moreover, the experimental solubility data were correlated with the modified Apelblat equation andλh equation, respectively. It was found that the result of correlation using two divided tem-perature ranges was better than that of using the whole temperature range.

  4. Morphological Effect of CNT/TiO2 Nanocomposite Photoelectrodes Dye-Sensitized Solar Cell on Photovoltaic Performance with Various Annealing Temperatures

    Directory of Open Access Journals (Sweden)

    Mohd Zikri Razali

    2015-01-01

    Full Text Available This research focused on the fabrication of dye-sensitized solar cell based on a photoanode of carbon nanotube/titanium dioxide (CNT/TiO2 nanocomposite photoanode synthesized through acid-catalyzed sol-gel method. The results show the improvement of the chemical and electrical properties of the solar cells annealed at different temperatures. The CNT/TiO2 colloidal solution was synthesized using titanium tetraisopropoxide and CNT/2-propanol solution. The thin films were doctor-bladed on a fluorine tin oxide glass before being annealed at 550, 650, and 750°C. The field emission scanning electron microscopy morphological images show that the thin films were homogenously distributed and maintained their spherical structures. The X-ray diffraction patterns show that the films consisted of anatase and rutile phases with large crystallite sizes due to temperature increment. The atomic force microscopy analysis presents the thin film roughness in terms of root mean square roughness. The photovoltaic performance was analyzed using IV curve and electrochemical impedance spectroscopy (EIS. The thin films annealed at 750°C had the highest energy conversion efficiency at 5.23%. The EIS analysis estimated the values of the effective electron lifetime (τeff, effective electron diffusion coefficient, effective electron diffusion (Ln, and effective recombination rate constant (keff. A large τeff, small keff, and longer Ln can improve photovoltaic performance efficiency.

  5. Synthesis and pervaporation performance of high-reproducibility silicalite-1 membranes

    Institute of Scientific and Technical Information of China (English)

    CHEN HongLiang; LI YanShuo; Zhu GuangQi; LIU Jie; YANG WeiShen

    2008-01-01

    High-reproducibility silicalite-1 membranes were synthesized on silica tubes by in-situ hydrothermal synthesis, and the relative standard deviation (R.S.D.) of average separation factor for eight membranes was only 7.5%. By using an effective method called "solution-filling (SF)", the average flux of membranes prepared with SF method was improved by about 49% compared to membranes prepared without SF method, and the highest flux of membrane prepared with SF method towards ethanol/H2O mixture at 80℃ was 1.49 kg/(m2·h). Pervaporation experiments showed that the fluxes of silicalite-1 membranes at 60℃ were 2.63, 0.87, 0.24, and 0.20 kg/(m2·h) towards methanol/H2O, ethanol/H2O,2-propanol/H2O, and 1-propanol/H2O mixtures, respectively, and the corresponding separation factors were 22, 69, 81, and159, respectively.

  6. Polycaprolactone-Chitin Nanofibrous Mats as Potential Scaffolds for Tissue Engineering

    Directory of Open Access Journals (Sweden)

    Min Sup Kim

    2012-01-01

    Full Text Available We describe here the preparation of poly(caprolactone (PCL-chitin nanofibrous mats by electrospinning from a blended solution of PCL and chitin dissolved in a cosolvent, 1,1,1,3,3,3-hexafluoro-2-propanol and trifluoroacetic acid. Scanning electron microscopy showed that the neutralized PCL-chitin nanofibrous mats were morphologically stable, with a mean diameter of 340.5±2.6 nm, compared with a diameter of 524.2±12.1 nm for PCL mats. The nanofibrous mats showed decreased water contact angles as the proportion of chitin increased. However, the tensile properties of nanofibrous mats containing 30~50% (wt/wt chitin were enhanced compared with PCL-only mats. In vitro studies showed that the viability of human dermal fibroblasts (HDFs for up to 7 days in culture was higher on composite (OD value: 1.42±0.09 than on PCL-only (0.51±0.14 nanofibrous mats, with viability correlated with chitin concentration. Together, our results suggest that PCL-chitin nanofibrous mats can be used as an implantable substrate to modulate HDF viability in tissue engineering.

  7. Separación de las clases de lípidos neutros de polen apícola mediante cromatografía líquida de alta resolución (HPLC

    Directory of Open Access Journals (Sweden)

    Muniategui, S.

    1991-08-01

    Full Text Available A fast method for the separation of neutral lipid classes of bee-collected pollen by isocratic HPLC is described using ultraviolet detection at 206 nm and direct injection of the sample into a silica column. The mobile phase was n-hexane-2-propanolacetic acid (100:0.5:0.1. Three fractions of neutral lipids were isolated from 35 samples: Sterol esters and other nonpolar compounds such as carotenoids and waxes; triglycerides; and fatty acids.

    Se describe un método rápido mediante HPLC para la separación de las diferentes clases de lípidos neutros del polen apícola en condiciones isocráticas, con detección UV a 206 nm e inyección directa de la muestra en columna de sílica. Como fase móvil se usa n-hexano-2-propanol-ácido acético (100:0,5:0,1. Se aislaron 3 fracciones de lípidos neutros en las 35 muestras analizadas: Esteres de esteroles y otros componentes no polares tales como carotenoides y ceras; triglicéridos y ácidos grasos.

  8. Optimal oxidative folding of the novel antimicrobial cyclotide from Hedyotis biflora requires high alcohol concentrations.

    Science.gov (United States)

    Wong, Clarence T T; Taichi, Misako; Nishio, Hideki; Nishiuchi, Yuji; Tam, James P

    2011-08-23

    Hedyotide B1, a novel cyclotide isolated from the medicinal plant Hedyotis biflora, contains a cystine knot commonly found in toxins and plant defense peptides. The optimal oxidative folding of a cystine knot encased in the circular peptide backbone of a cyclotide poses a challenge. Here we report a systematic study of optimization of the oxidative folding of hedyotide B1, a 30-amino acid cyclic peptide with a net charge of +3. The linear precursor of hedyotide B1, synthesized as a thioester by solid phase synthesis, was cyclized quantitatively by a thia-zip cyclization to form the circular backbone and then subjected to oxidative folding in a thiol-disulfide redox system under 38 different conditions. Of the oxidative conditions examined, the nature of the organic cosolvent appeared to be critical, with the use of 70% 2-propanol affording the highest yield (48%). The disulfide connectivity of the folded hedyotide was identical to that of the native form as determined by partial acid hydrolysis. The use of such a high alcohol concentration suggests that a partial denaturation may be necessary for the oxidative folding of a cyclotide with the inverse orientation of hydrophobic side chains that are externalized to the solvent face to permit the formation of the interior cystine core in the circularized backbone. We also show that synthetic hedyotide B1 is an antimicrobial, exhibiting minimal inhibitory concentrations in the micromolar range against both Gram-positive and -negative bacteria. PMID:21776968

  9. Dual delivery of active antibactericidal agents and bone morphogenetic protein at sustainable high concentrations using biodegradable sheath-core-structured drug-eluting nanofibers.

    Science.gov (United States)

    Hsu, Yung-Hen; Lin, Chang-Tun; Yu, Yi-Hsun; Chou, Ying-Chao; Liu, Shih-Jung; Chan, Err-Cheng

    2016-01-01

    In this study, we developed biodegradable sheath-core-structured drug-eluting nanofibers for sustainable delivery of antibiotics (vancomycin and ceftazidime) and recombinant human bone morphogenetic protein (rhBMP-2) via electrospinning. To prepare the biodegradable sheath-core nanofibers, we first prepared solutions of poly(d,l)-lactide-co-glycolide, vancomycin, and ceftazidime in 1,1,1,3,3,3-hexafluoro-2-propanol and rhBMP-2 in phosphate-buffered solution. The poly(d,l)-lactide-co-glycolide/antibiotics and rhBMP-2 solutions were then fed into two different capillary tubes controlled by two independent pumps for coaxial electrospinning. The electrospun nanofiber morphology was observed under a scanning electron microscope. We further characterized the in vitro antibiotic release from the nanofibers via high-performance liquid chromatography and that of rhBMP-2 via enzyme-linked immunosorbent assay and alkaline phosphatase activity. We showed that the biodegradable coaxially electrospun nanofibers could release high vancomycin/ceftazidime concentrations (well above the minimum inhibition concentration [MIC]90) and rhBMP-2 for >4 weeks. These experimental results demonstrate that novel biodegradable nanofibers can be constructed with various pharmaceuticals and proteins for long-term drug deliveries. PMID:27574423

  10. Statistical Approach for Optimization of Physiochemical Requirements on Alkaline Protease Production from Bacillus licheniformis NCIM 2042

    Directory of Open Access Journals (Sweden)

    Biswanath Bhunia

    2012-01-01

    Full Text Available The optimization of physiochemical parameters for alkaline protease production using Bacillus licheniformis NCIM 2042 were carried out by Plackett-Burman design and response surface methodology (RSM. The model was validated experimentally and the maximum protease production was found 315.28 U using optimum culture conditions. The protease was purified using ammonium sulphate (60% precipitation technique. The HPLC analysis of dialyzed sample showed that the retention time is 1.84 min with 73.5% purity. This enzyme retained more than 92% of its initial activity after preincubation for 30 min at 37∘C in the presence of 25% v/v DMSO, methanol, ethanol, ACN, 2-propanol, benzene, toluene, and hexane. In addition, partially purified enzyme showed remarkable stability for 60 min at room temperature, in the presence of anionic detergent (Tween-80 and Triton X-100, surfactant (SDS, bleaching agent (sodium perborate and hydrogen peroxide, and anti-redeposition agents (Na2CMC, Na2CO3. Purified enzyme containing 10% w/v PEG 4000 showed better thermal, surfactant, and local detergent stability.

  11. Chiral separation of a diketopiperazine pheromone from marine diatoms using supercritical fluid chromatography.

    Science.gov (United States)

    Frenkel, Johannes; Wess, Carsten; Vyverman, Wim; Pohnert, Georg

    2014-03-01

    The proline derived diketopiperazine has been identified in plants, insects and fungi with unknown function and was recently also reported as the first pheromone from a diatom. Nevertheless the stereochemistry and enantiomeric excess of this natural product remained inaccessible using direct analytical methods. Here we introduce a chiral separation of this metabolite using supercritical fluid chromatography/mass spectrometry. Several chromatographic methods for chiral analysis of the diketopiperazine from the diatom Seminavis robusta and synthetic enantiomers have been evaluated but neither gas chromatography nor high performance liquid chromatography on different chiral cyclodextrin phases were successful in separating the enantiomers. In contrast, supercritical fluid chromatography achieved baseline separation within four minutes of run time using amylose tris(3,5-dimethylphenylcarbamate) as stationary phase and 2-propanol/CO2 as mobile phase. This very rapid chromatographic method in combination with ESI mass spectrometry allowed the direct analysis of the cyclic dipeptide out of the complex sea water matrix after SPE enrichment. The method could be used to determine the enantiomeric excess of freshly released pheromone and to follow the rapid degradation observed in diatom cultures. Initially only trace amounts of c(d-Pro-d-Pro) were found besides the dominant c(l-Pro-l-Pro) in the medium. However the enantiomeric excess decreased upon pheromone degradation within few hours indicating that a preferential conversion and thus inactivation of the l-proline derived natural product takes place.

  12. Evaluation of certain food additives and contaminants.

    Science.gov (United States)

    2002-01-01

    This report represents the conclusions of a Joint FAO/WHO Expert Committee convened to evaluate the safety of various food additives and contaminants, with a view to recommending Acceptable Daily Intakes (ADIs) and tolerable intakes, respectively, and to prepare specifications for the identity and purity of food additives. The first part of the report contains a general discussion of the principles governing the toxicological evaluation of food additives (including flavouring agents) and contaminants, assessments of intake, and the establishment and revision of specifications for food additives. A summary follows of the Committee's evaluations of toxicological and intake data on various specific food additives (diacetyltartaric and fatty acid esters of glycerol, quillaia extracts, invertase from Saccharomyces cerevisiae, beta-carotene from Blakeslea trispora, curcumin, phosphates, diphosphates and polyphosphates, hydrogenated poly-1-decene, natamycin, D-tagatose, carrageenan, processed Eucheuma seaweed, curdlan, acetylated oxidized starch, alpha-cyclodextrin and sodium sulfate), flavouring agents and contaminants (3-chloro-1,2-propanediol, 1,3-dichloro-2-propanol, and a large number of polychlorinated dibenzodioxins, polychlorinated dibenzofurans and coplanar polychlorinated biphenyls). Annexed to the report are tables summarizing the Committee's recommendations for ADIs of the food additives and tolerable intakes of the contaminants considered, changes in the status of specifications of these food additives and specific flavouring agents, and further information required or desired. PMID:12564044

  13. Expression, purification, crystallization and preliminary X-ray analysis of the PaaI-like thioesterase SAV0944 from Staphylococcus aureus.

    Science.gov (United States)

    Khandokar, Yogesh B; Roman, Noelia; Smith, Kate M; Srivastava, Parul; Forwood, Jade K

    2014-02-01

    Staphylococcus aureus is the causative agent of many diseases, including meningitis, bacteraemia, pneumonia, food poisoning and toxic shock syndrome. Structural characterization of the PaaI-like thioesterase SAV0944 (SaPaaI) from S. aureus subsp. aureus Mu50 will aid in understanding its potential as a new therapeutic target by knowledge of its molecular details and cellular functions. Here, the recombinant expression, purification and crystallization of SaPaaI thioesterase from S. aureus are reported. This protein initially crystallized with the ligand coenzyme A using the hanging-drop vapour-diffusion technique with condition No. 40 of Crystal Screen from Hampton Research at 296 K. Optimal final conditions consisting of 24% PEG 4000, 100 mM sodium citrate pH 6.5, 12% 2-propanol gave single diffraction-quality crystals. These crystals diffracted to beyond 2 Å resolution at the Australian Synchrotron and belonged to space group P12(1)1, with unit-cell parameters a = 44.05, b = 89.05, c = 60.74 Å, β = 100.5°. Initial structure determination and refinement gave an R factor and R(free) of 17.3 and 22.0%, respectively, confirming a positive solution in obtaining phases using molecular replacement.

  14. Detergent-Stable Salt-Activated Proteinases from Virgibacillus halodenitrificans SK1-3-7 Isolated from Fish Sauce Fermentation.

    Science.gov (United States)

    Montriwong, Aungkawipa; Rodtong, Sureelak; Yongsawatdigul, Jirawat

    2015-05-01

    The NaCl-activated and detergent-stable proteinases from Virgibacillus halodenitrificans SK1-3-7 isolated from fish sauce fermentation were purified and characterized. The enzymes with molecular masses of 20 and 36 kDa showed caseinolytic activity on a zymogram. Optimum azocaseinolytic activity was at 60 °C and pH 9. The proteolytic activity increased in the presence of 10 mM CaCl2 and 0.5 M NaCl and showed high stability at 0-2 M NaCl. The enzymes were stable at pH 4-10 and 10-50 °C. The enzymes preferably hydrolyzed Suc-Ala-Ala-Pro-Phe-pNA and were completely inhibited by phenylmethanesulfonyl fluoride (PMSF), showing subtilisin-like characteristics. Activity and stability remained high in the presence of H2O2 and various surfactants. The enzymes exhibited high stability (>95%) in various organic solvents (DMSO, butanol, ethanol, 2-propanol, and acetonitrile) at concentration of 50%. The V. halodenitrificans SK1-3-7 proteinases showed potential as a biocatalyst in aqueous-organic solvent systems and as an additive in laundry detergent. PMID:25820449

  15. Preparation, structural and morphological studies of Ni doped titania nanoparticles.

    Science.gov (United States)

    Rajamannan, B; Mugundan, S; Viruthagiri, G; Shanmugam, N; Gobi, R; Praveen, P

    2014-07-15

    TiO2 nanoparticles doped with different weight percentages (4%, 8%, 12% and 16%) of nickel contents were prepared by a modified sol-gel method using Titanium tetra iso propoxide and nickel nitrate as precursors and 2-propanol as a solvent. X-ray diffraction studies show that the as prepared and annealed products show anatase structure with average particle sizes running between of 8 and 16 nm. FTIR results demonstrate the presence of strong chemical bonding at the interface of TiO2 nanoparticles. The optical properties of bare and doped samples were carried out using UV-DRS and photoluminescence measurements. The surface morphology and the element constitution of the nickel doped TiO2 nanoparticles were studied by scanning electron microscope attached with energy dispersive X-ray spectrometer arrangement. The non linear optical properties of the products were confirmed by Kurtz second harmonic generation (SHG) test and the output power generated by the nanoparticle was compared with that of potassium di hydrogen phosphate (KDP).

  16. Characterization of a Membrane Interface for Analysis of Air Samples Using Time-of-flight Mass Spectrometry

    International Nuclear Information System (INIS)

    In the present study, we constructed a membrane inlet assembly for selective permeation of volatile airborne organic compounds for subsequent analysis by time-of-flight mass spectrometry. The time-dependent diffusion of analytes through a 75 μm thick polydimethylsiloxane membrane was measured by monitoring the ion signal after a step change in the sample concentration. The results fit well to a non-steady-state permeation equation. The diffusion coefficient, response time, and sensitivity were determined experimentally for a range of polar (halogenated) and nonpolar (aromatic) compounds. We found that the response times for several volatile organic compounds were greatly influenced by the alkyl chain length as well as the size of the substituted halogen atoms. The detection limits for benzene, ethylbenzene, and 2-propanol were 0.2 ppm, 0.1 ppm, and 3.0 ppm by volume, respectively, with a linear dynamic range greater than three orders of magnitude. These results indicate that the membrane inlet/time-of-flight mass spectrometry technique will be useful for a wide range of applications, particularly for in situ environmental monitoring

  17. Natural organic matter and sunlight accelerate the degradation of 17ss-estradiol in water

    International Nuclear Information System (INIS)

    Nanomolar concentrations of steroid hormones such as 17β-estradiol can influence the reproductive development and sex ratios of invertebrate and vertebrate populations. Thus their release into surface and ground waters from wastewater facilities and agricultural applications of animal waste is of environmental concern. Many of these compounds are chromophoric and susceptible to photolytic degradation. High intensity UV-C radiation has been demonstrated to degrade some of these compounds in engineered systems. However, the degradation efficacy of natural solar radiation in shallow fresh waters is less understood. Here photolytic experiments with 17β-estradiol demonstrated modest photodegradation (∼ 26%) when exposed to simulated sunlight between 290 and 720 nm. Photodegradation significantly increased (∼ 40-50%) in the presence of 2.0-15.0 mg/l of dissolved organic carbon (DOC) derived from humic acids of the Suwannee River, GA. However, rates of photodegradation reached a threshold at approximately 5.0 mg/l DOC. Observed suppression of photolysis in the presence of a radical inhibitor (i.e. 2-propanol) indicated that a significant proportion of the degradation was due to radicals formed from the photolysis of DOC. Although photodegradation was greatest in full sunlight containing UV-B (290-320 nm), degradation was also detected with UV-A (320-400 nm) and visible light (400-720 nm) alone

  18. Synthesis and swelling behavior of polyurethane networks based on hyperbranched polymer

    Directory of Open Access Journals (Sweden)

    Džunuzović Jasna V.

    2011-01-01

    Full Text Available A series of six polyurethane (PU networks was synthesized from BoltornR hydroxy-functional hyperbranched polyester (HBP of the second pseudo generation as a crosslinking agent, α,ω- dihydroxy-(ethylene oxide-poly(dimethylsiloxane-ethylene oxide (EO-PDMS-EO and 4,4’- methylenediphenyl diisocyanate, by a two-step polymerization in solution. Each sample of the prepared PUs had different EO-PDMS-EO content. The chemical structure of the synthesized networks was analyzed by FTIR spectroscopy. The influence of the EO-PDMS-EO content and type of the solvent on the swelling behavior of the PUs in 2-propanol and toluene was investigated. During the swelling measurements certain amount of sol fractions was extracted from the PUs by solvents. According to the 1H NMR results, sol fractions are mainly composed of the soluble hyperbranched PU, formed during the polymerization by partial modification of the end hydroxyl groups of HBP with NCO-terminated prepolymer synthesized in the first step of the reaction. Chains of the so reacted prepolymer can then fold back and form cyclic products by reaction of the free -NCO group from the NCO-terminated prepolymer with free -OH group of HBP. As the EO-PDMS-EO content increases the amount of the sol fractions and swelling degree also increased, indicating that networks with lower EO-PDMS-EO content are more crosslinked and have higher solvent resistance.

  19. Asymmetric transfer hydrogenation of prochiral ketone catalyzed over Fe-CS/SBA-15 catalyst

    Institute of Scientific and Technical Information of China (English)

    XUE Ping; WU Tao

    2007-01-01

    A heterogeneous chiral catalyst Fe(Ⅲ)-CS (chitosan)complex/mesoporous molecular sieve SBA-15 (Santa Barbara Amorphous) was prepared.The asymmetric transfer hydrogenations of prochiral acetophenone and 4-methyl-2-pentanone to corresponding chiral alcohols were carried out on Fe-CS/SBA-15 at atmosphere pressure using 2-propanol as hydrogen donor.Effects of Fe content in catalyst,reaction temperature,reaction time and promoter KOH concentration on the conversion of substrates and enantioselectivity were investigated.Fe-CS/SBA-15 with 2.2%mass fraction Fe exhibits considerable enantioselectivity and catalytic activity for the asymmetric transfer hydrogenations of aromatic ketone and aliphatic ketone.Under optimal reaction conditions:KOH concentration 0.03 mol/L,reaction temperature 70℃ and reaction time 4 h,enantiomer excess(ee)of (R)-1-phenylethanol and conversion of acetophenone can reach 87.4%and 27.7%,respectively.Under the above KOH concentration and reaction temperature and reaction time of 8 h,the ee of(R)-4-methyl-2-pentanol and conversion 4-methyl-2-pentanone amounted to 50.2%and 25.5%,respectively.

  20. Decay kinetics of benzophenone triplets and corresponding free radicals in soft and rigid polymers studied by laser flash photolysis.

    Science.gov (United States)

    Levin, Peter P; Efremkin, Alexei F; Sultimova, Natalie B; Kasparov, Valery V; Khudyakov, Igor V

    2014-01-01

    The kinetics of transients formed under photoexcitation of benzophenone (B) dissolved in three different polymers was studied by ns laser flash photolysis. These polymers were the soft rubbers poly (ethylene-co-butylene) (EB), polystyrene block-poly(ethylene-ran-butylene)-block-polystyrene (SEBS) and hard polystyrene (PS). We monitored the decay kinetics of triplet state (3)B(*) and of ketyl radicals BH(●). We observed exponential decay of (3)B(*) and two-stage decay kinetics of BH(●) in EB. The first stage is a fast cage recombination of a radical pair (BH(●), radical of polymer R(●)). The second slow stage of BH(●) decay follows the second-order law with a relatively high rate constant, which corresponds to recombination of BH(●) in a homogeneous liquid with a viscosity of only ~0.1 P (about five times of 2-propanol viscosity). Application of a magnetic field (MF) of 0.2 T leads to deceleration of both stages of BH(●) decay in EB by approximately 20%. Decay kinetics of both transients were observed in SEBS. There was no MF effect on BH(●) decay in SEBS. We only observed (3)B(*) in PS. Decay kinetics of (3)B(*) in this case were described as polychromatic dispersive first-order kinetics. We discuss the effects of polymer structure on transient kinetics and the MF effect.

  1. Solid phase microextraction and gas chromatography-mass spectrometry methods for residual solvent assessment in seized cocaine and heroin.

    Science.gov (United States)

    Cabarcos, Pamela; Herbello-Hermelo, Paloma; Álvarez-Freire, Iván; Moreda-Piñeiro, Antonio; Tabernero, María Jesús; Bermejo, Ana María; Bermejo-Barrera, Pilar

    2016-09-01

    A simple sample pre-treatment method based on solid phase microextraction (SPME) and gas chromatography-mass spectrometry (GC-MS) has been optimized and validated for the assessment of 15 residual solvents (2-propanol, 2-methylpentane, 3-methylpentane, acetone, ethyl acetate, benzene, hexane, methylcyclohexane, methylcyclopentane, m-xylene, propyl acetate, toluene, 1,2,4-trimethylbenzene, dichloromethane, and ethylbenzene) in seized illicit cocaine and heroin. DMSO and DMF as sample diluents were found to offer the best residual solvent transference to the head space for further adsorption onto the SPME fiber, and the developed method therefore showed high sensitivity and analytical recovery. Variables affecting SPME were fully evaluated by applying an experimental design approach. Best conditions were found when using an equilibration time of 5 min at 70 °C and headspace sampling of residual solvents at the same temperature for 15 min. Method validation, performed within the requirements of international guidelines, showed excellent sensitivity, as well as intra- and inter-day precision and accuracy. The proposed methodology was applied to 96 cocaine samples and 14 heroin samples seized in Galicia (northwestern Spain) within 2013 and 2014. PMID:27405875

  2. Cloud point measurements of 1-butyl-2,3-dimethylimidazolium tetrafluoroborate with alcohols

    Energy Technology Data Exchange (ETDEWEB)

    Li Xiaoli [Department of Chemistry and Chemical Engineering, Division of Material Sciences, Graduate School of Natural Science and Technology, Kanazawa University, Kakuma-machi, Kanazawa 920-1192 (Japan); Tamura, Kazuhiro, E-mail: tamura@t.kanazawa-u.ac.j [Department of Chemistry and Chemical Engineering, Division of Material Sciences, Graduate School of Natural Science and Technology, Kanazawa University, Kakuma-machi, Kanazawa 920-1192 (Japan)

    2010-12-15

    Mutual solubility data of imidazolium-based ionic liquid, 1-butyl-2,3-dimethylimidazolium tetrafluoroborate ([bmmim][BF{sub 4}]) with the alcohols, 1-propanol, 2-propanol, 1-butanol, 1-pentanol, and 1-hexanol were obtained by a cloud point method. The upper critical solution temperatures of the ionic liquid and alcohol mixtures were determined from the mutual solubility data. The upper critical solution temperature of the binary mixtures gradually increased as the chain length of the alcohol increased. The mutual solubility data of binary systems ([bmmim][BF{sub 4}] + alcohols) have been correlated by the original UNIQUAC model as well as the extended and modified form of the UNIQUAC model. The temperature dependence of the mutual solubility data could be represented in terms of the temperature dependence of the binary energy parameters obtained from the correlation. Additionally the influence of water contamination on the ionic liquid mixture was shown experimentally by adding pure water into the binary mixture ([bmmim][BF{sub 4}] + 1-butanol).

  3. Crystallization and preliminary X-ray characterization of two thermostable DNA nucleases

    International Nuclear Information System (INIS)

    Two thermostable DNA nucleases from archaea were crystallized in different space groups; the crystals were suitable for X-ray analysis. Temperature-tolerant organisms are an important source to enhance the stability of enzymes used in biotechnological processes. The DNA-cleaving enzyme exonuclease III from Escherichia coli is used in several applications in gene technology. A thermostable variant could expand the applicability of the enzyme in these methods. Two homologous nucleases from Archaeoglobus fulgidus (ExoAf) and Methanothermobacter thermoautrophicus (ExoMt) were studied for this purpose. Both enzymes were crystallized in different space groups using (poly)ethylene glycols, 2,4-methyl pentandiol, dioxane, ethanol or 2-propanol as precipitants. The addition of a 10-mer DNA oligonucleotide was important to obtain monoclinic crystals of ExoAf and ExoMt that diffracted to resolutions better than 2 Å using synchrotron radiation. The crystal structures of the homologous proteins can serve as templates for genetic engineering of the E. coli exonuclease III and will aid in understanding the different catalytic properties of the enzymes

  4. 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.

  5. VGF and striatal cell damage in in vitro and in vivo models of Huntington's disease.

    Science.gov (United States)

    Noda, Yasuhiro; Shimazawa, Masamitsu; Tanaka, Hirotaka; Tamura, Shigeki; Inoue, Teruyoshi; Tsuruma, Kazuhiro; Hara, Hideaki

    2015-06-01

    Huntington's disease (HD) is an inherited genetic disorder, characterized by cognitive dysfunction and abnormal body movements, and at present there is no effective treatment for HD. Therapeutic options for HD are limited to symptomatic treatment approaches and there is no cure for this devastating disease. Here, we examined whether SUN N8075, (2S)-1-(4-amino-2,3,5-trimethylphenoxy)-3-{4-[4-(4-fluorobenzyl)phenyl]-1-piperazinyl}-2-propanol dimethanesulfonate, which exerts neuroprotective effects by antioxidant effects and induction of VGF nerve growth factor inducible (VGF), has beneficial effects in STHdh cells derived from striatum of knock-in HD mice and R6/2 HD mice. In an in vitro study, SUN N8075 inhibited the cell death caused by mutant huntingtin (mHtt) and upregulated the VGF mRNA level via the phosphorylation of extracellular signal-regulated kinase 1/2 (ERK1/2). Furthermore, 30 amino acid of VGF C-terminal peptide, AQEE-30 inhibited the cell death and the aggregation of mHtt. In an in vivo study, SUN N8075 improved the survival and the clasping response in the R6/2 mice. Furthermore, SUN N8075 increased the number of surviving neurons in the striatum of the R6/2 mice. These findings suggest that SUN N8075 may be an effective candidate for HD treatments.

  6. Improved Polymerase Chain Reaction-restriction Fragment Length Polymorphism Genotyping of Toxic Pufferfish by Liquid Chromatography/Mass Spectrometry.

    Science.gov (United States)

    Miyaguchi, Hajime

    2016-01-01

    An improved version of a polymerase chain reaction (PCR)-restriction fragment length polymorphism (RFLP) method for genotyping toxic pufferfish species by liquid chromatography/electrospray ionization mass spectrometry (LC/ESI-MS) is described. DNA extraction is carried out using a silica membrane-based DNA extraction kit. After the PCR amplification using a detergent-free PCR buffer, restriction enzymes are added to the solution without purifying the reaction solution. A reverse-phase silica monolith column and a Fourier transform high resolution mass spectrometer having a modified Kingdon trap analyzer are employed for separation and detection, respectively. The mobile phase, consisting of 400 mM 1,1,1,3,3,3-hexafluoro-2-propanol, 15 mM triethylamine (pH 7.9) and methanol, is delivered at a flow rate of 0.4 ml/min. The cycle time for LC/ESI-MS analysis is 8 min including equilibration of the column. Deconvolution software having an isotope distribution model of the oligonucleotide is used to calculate the corresponding monoisotopic mass from the mass spectrum. For analysis of oligonucleotides (range 26-79 nucleotides), mass accuracy was 0.62 ± 0.74 ppm (n = 280) and excellent accuracy and precision were sustained for 180 hr without use of a lock mass standard. PMID:27684516

  7. Extraction and recovery of 2-butoxyethanol from aqueous phases containing high saline concentration

    Directory of Open Access Journals (Sweden)

    Katherine E. Manz

    2016-09-01

    Full Text Available Ethylene glycol monobutyl ether (EGBE, also known as 2-butoxyethanol (2-BE, has been identified as a contaminant in hydraulic fracturing fluids. In order to determine the presence of 2-BE in hydraulic fracturing chemical additives, a reliable method for recovering 2-BE from aqueous phases by liquid-liquid extraction combined with gas chromatography/mass spectrometry (GC/MS was established. The liquid-liquid extraction method was applied to samples matrices containing various amounts of salt. Using methylene chloride for liquid-liquid extraction in a sample to solvent ratio of 1:3, ≥99% 2-BE recovery may be achieved with less than 5% standard error. The limit of detection was determined to be 0.957 mg L−1 2-BE. Accuracy was determined to be 2.58% and precision was determined using the coefficient of variation, which was 3.5%. The method was used to recover 2-BE in a hydraulic fracturing chemical additive called Revert Flow and to quantify the weight percent of 2-BE in the chemical additive. Weight percent of two additional components of Revert Flow, D-limonene and 1-butoxy-2-propanol, were also determined. We also used the method to determine the abiotic of 2-BE in water, which was 5.55 days. The persistence of 2-BE in hydraulic fracturing fluid was also investigated and determined that 2-BE is more persistent in this environment.

  8. Analysis of 3-MCPD and 1,3-DCP in Various Foodstuffs Using GC-MS.

    Science.gov (United States)

    Kim, Wooseok; Jeong, Yun A; On, Jiwon; Choi, Ari; Lee, Jee-Yeon; Lee, Joon Goo; Lee, Kwang-Geun; Pyo, Heesoo

    2015-09-01

    3-Monochloro-1,2-propanediol (3-MCPD) and 1,3-dichloro-2-propanol (1,3-DCP) are not only produced in the manufacturing process of foodstuffs such as hydrolyzed vegetable proteins and soy sauce but are also formed by heat processing in the presence of fat and low water activity. 3-MCPD exists both in free and ester forms, and the ester form has been also detected in various foods. Free 3-MCPD and 1,3-DCP are classified as Group 2B by the International Agency for Research on Cancer. Although there is no data confirming the toxicity of either compound in humans, their toxicity was evidenced in animal experimentation or in vitro. Although few studies have been conducted, free 3-MCPD has been shown to have neurotoxicity, reproductive toxicity, and carcinogenicity. In contrast, 1,3-DCP only has mutagenic activity. The purpose of this study was to analyze 3-MCPD and 1,3-DCP in various foods using gas chromatography -mass spectrometry. 3-MCPD and 1,3-DCP were analyzed using phenyl boronic acid derivatization and the liquid-liquid extraction method, respectively. The analytical method for 3-MCPD and 1,3-DCP was validated in terms of linearity, limit of detection (LOD), limit of quantitation, accuracy and precision. Consequently, the LODs of 3-MCPD and 1,3-DCP in various matrices were identified to be in the ranges of 4.18~10.56 ng/g and 1.06~3.15 ng/g, respectively. PMID:26483891

  9. Determination of cocaine and its metabolites in plasma by porous membrane-protected molecularly imprinted polymer micro-solid-phase extraction and liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Sánchez-González, Juan; García-Carballal, Sara; Cabarcos, Pamela; Tabernero, María Jesús; Bermejo-Barrera, Pilar; Moreda-Piñeiro, Antonio

    2016-06-17

    A selective molecularly imprinted polymer synthesized for the selective retention of cocaine (COC) and its metabolites [benzoylecgonine (BZE), ecgonine methyl ester (EME), and cocaethylene (CE)] was used as a solid adsorbent for assessing cocaine abuse by plasma analysis. The MIP beads (50mg) were loaded inside a cone shaped device made of a polypropylene (PP) membrane for micro-solid-phase extraction (μ-SPE). High performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was used for quantifying the analytes after MIP-μ-SPE. The best retention capabilities were reached when loading plasma samples (within the 0.1-5.0mL range), previously adjusted to pH 5.5 by orbital-horizontal shaking (150rpm, 50°C) for 10min. Analyte elution was achieved by subjecting the MIP-μ-SPE device to ultrasound (37kHz, 325W) with 10mL of dichloromethane/2-propanol/ammonium hydroxide (76:20:4) for 8min. After eluate evaporation to dryness and re-dissolution in 100μL of mobile phase, the MIP-μ-SPE method yielded a pre-concentration factor of 50. Precision was assessed by intra-day and inter-day assays, and accuracy (intraday and inter-day analytical recovery, as well as the analysis of a BTMF 1/11-B control serum sample) show that the developed method is highly precise and accurate. In addition, the limits of detection, ranging from 0.061ngmL(-1) for COC to 0.87ngmL(-1) for BZE, were low enough for confirmative conclusions regarding cocaine abuse. The method was used for screening/quantifying cocaine and metabolites in plasma samples from poly-drug abusers. PMID:27207577

  10. Titania modification with a ruthenium(II) complex and gold nanoparticles for photocatalytic degradation of organic compounds.

    Science.gov (United States)

    Zheng, Shuaizhi; Wei, Zhishun; Yoshiiri, Kenta; Braumüller, Markus; Ohtani, Bunsho; Rau, Sven; Kowalska, Ewa

    2016-01-01

    Titania of fine anatase nanoparticles (ST01) was modified successively with two components, i.e., a ruthenium(II) complex with phosphonic anchoring groups [Ru(bpy)2(4,4'-(CH2PO3H2)2bpy)](2+) bpy = 2,2'-bipyridine (Ru(II)CP) and gold nanoparticles (Au). Various compositions of two titania modifiers were investigated, i.e., Au, Au + Ru(II)CP, Au + 0.5Ru(II)CP, Ru(II)CP, 0.5Ru(II)CP and 0.25Ru(II)CP, where Au and Ru(II)CP correspond to 0.81 mol% and 0.34 mol% (with respect to titania), respectively. In the case of hybrid photocatalysts, the sequence of modification (ruthenium(II) complex adsorption or gold deposition) was investigated to check its influence on the resultant properties and thus photocatalytic performance. Diffuse reflectance spectroscopy (DRS), X-ray photoelectron spectroscopy (XPS) and scanning transmission electron microscopy (STEM) were applied to characterize the structural properties of the prepared photocatalysts, which confirmed the successful introduction of modifiers of the ruthenium(II) complex and/or gold NPs. Different distributions of gold particle sizes and chemical compositions were obtained for the hybrid photocatalysts prepared with an opposite sequence. It was found that photocatalytic activities depended on the range of used irradiation (UV/vis or vis) and the kind of modifier in different ways. Gold NPs improved the photocatalytic activities, while Ru(II)CP inhibited the reactions under UV/vis irradiation, i.e., methanol dehydrogenation and acetic acid degradation. Oppositely, Ru(II)CP greatly enhanced the photocatalytic activities for 2-propanol oxidation under visible light irradiation. PMID:26661372

  11. Synthesis 1-(5-oxohexyl)-3,7-dimethyl-xanthyne labelled with tritium into 8 position from purinic ring

    International Nuclear Information System (INIS)

    This paper presents the work on synthesis of 1-(5-oxohexyl)-3,7-dimethyl-xanthyne labelled with tritium into 8 position from purinic ring. The obtaining of tritium labelled compound is realized by initial labelling of theobromine with tritium into 8 position and by coupling the purinic derivative to 1-Br-5-hexanone. Theobromine-8- 3 H was obtained by the bromination of theobromine with elementary bromine and after that the bromine was substituted with tritium i.e.: C7H8O2N4 theobromine Br2/(-HBr) C7H7O2N4 Br (8-Br-theobromine) (3 H2/cat)/(-KOH) C7H73 HO2N4 (theobromine-8- 3 H). Theobromine-8- 3 H was purified by thin layer chromatography with a solvent system i.e. n-BuOH:AcOH:H2O (4:1:1, v/v/v) and characterized radiochemically. It was then diluted by unlabelled theobromine to specific activity of 50 mCi/g. After dilution, theobromine-8-3 H was coupled to 1-Br-5-hexanone i.e.: C7H73 HO2N4 (theobromine-8- 3 H) + Br-(CH2)4-CO-CH3 (1-Br-5-hexanone) (NaOH)/(CH3OH) C13 H173 HO3N4 (1-(5-oxohexyl)- 3,7-dimethyl-xanthine-8- 3 H). The raw compound was purified by recrystallization from 2-propanol and it was characterized radiochemically. (authors)

  12. Synthesis of levan in water-miscible organic solvents.

    Science.gov (United States)

    Castillo, E; López-Munguía, A

    2004-10-19

    The synthesis of levan using a levansucrase from a strain of Bacillus subtilis was studied in the presence of the water-miscible solvents: acetone, acetonitrile and 2-methyl-2-propanol (2M2P). It was found that while the enzyme activity is only slightly affected by acetone and acetonitrile, 2M2P has an activating effect increasing the total activity 35% in 40-50% (v/v) 2M2P solutions at 30 degrees C. The enzyme is highly stable in water at 30 degrees C; however, incubation in the presence of 15 and 50% (v/v) 2M2P reduced the half-life time to 23.6 and 1.8 days, respectively. This effect is reversed in 83% 2M2P, where a half-life time of 11.8 days is observed. The presence of 2M2P in the system increases the transfer/hydrolysis ratio of levansucrase. As the reaction proceeds with 10% (w/v) sucrose in 50/50 water/2M2P sucrose is converted to levan and an aqueous two-phase system (2M2P/Levan) is formed and more sucrose can be added in a fed batch mode. It is shown that high molecular weight levan is obtained as an hydrogel and may be easily recovered from the reaction medium. However, when high initial sucrose concentrations (40% (w/v) in 50/50 water/2M2P) are used, an aqueous two-phase system (2M2P/sucrose) is induce, where the synthesized levan has a similar molecular weight distribution as in water and remains in solution. PMID:15464614

  13. Histology without xylene.

    Science.gov (United States)

    Buesa, René J; Peshkov, Maxim V

    2009-08-01

    After the hazardous effects of xylene became indisputable in the 1970s, many potential substitutes became available, some with as many if not more hazards. This article discusses the inadequacy of 5 vegetable oils as substitutes, as well as the characteristics of 22 D-limonene-based substitutes, all less effective in their chemical role, some capable of inducing health problems, and costing more than twice as much as xylene. Some of the 35 alkane-based substitutes discussed are effective for tissue processing, less toxic, with a cost about the same as xylene, but are not very effective for dewaxing and other staining tasks. Isopropanol (2-propanol) alone or mixed with molten paraffin is a technically acceptable and cost-effective substitute for xylene for tissue processing, but in this study, we demonstrate that the best clearing agents from the sectioning quality and diagnostic value point of view, with automated or manual protocols, are mixtures of 5:1 and 2:1 isopropanol and mineral oil, followed by undiluted mineral oil, all at 50 degrees C, making them a safer and cheaper substitute than xylene. Using a 1.7% dishwasher soap aqueous solution at 90 degrees C to dewax before staining and oven drying the stained sections before coverslipping will eliminate xylene from the staining tasks. Tissue processors retorts and conduits can be dewaxed with a 2% solution of a strong glassware laboratory detergent. These 4 methodologies will make the histology laboratory xylene-free but, due to the natural resistance to change, many histotechs will be reluctant to adopt them if they think that their technical expertise could be jeopardized, and the only way these changes will succeed is if the pathologists, as stewards of the histology laboratory, commit to their implementation.

  14. Breathomics for Gastric Cancer Classification Using Back-propagation Neural Network.

    Science.gov (United States)

    Daniel, D Arul Pon; Thangavel, K

    2016-01-01

    Breathomics is the metabolomics study of exhaled air. It is a powerful emerging metabolomics research field that mainly focuses on health-related volatile organic compounds (VOCs). Since the quantity of these compounds varies with health status, breathomics assures to deliver noninvasive diagnostic tools. Thus, the main aim of breathomics is to discover patterns of VOCs related to abnormal metabolic processes occurring in the human body. Classification systems, however, are not designed for cost-sensitive classification domains. Therefore, they do not work on the gastric carcinoma (GC) domain where the benefit of correct classification of early stages is more than that of later stages, and also the cost of wrong classification is different for all pairs of predicted and actual classes. The aim of this work is to demonstrate the basic principles for the breathomics to classify the GC, for that the determination of VOCs such as acetone, carbon disulfide, 2-propanol, ethyl alcohol, and ethyl acetate in exhaled air and stomach tissue emission for the detection of GC has been analyzed. The breath of 49 GC and 30 gastric ulcer patients were collected for the study to distinguish the normal, suspected, and positive cases using back-propagation neural network (BPN) and produced the accuracy of 93%, sensitivity of 94.38%, and specificity of 89.93%. This study carries out the comparative study of the result obtained by the single- and multi-layer cascade-forward and feed-forward BPN with different activation functions. From this study, the multilayer cascade-forward outperforms the classification of GC from normal and benign cases. PMID:27563574

  15. Synthesis of Biodiesel from the Oily Content of Marine Green Alga Ulva fasciata

    International Nuclear Information System (INIS)

    The present study is focused on the chemical transformation of oils derived from the marine green alga Ulva fasciata Delile to biodiesel. The transesterification of algal oil was performed with a variety of alcohols using Na metal and NaOH as catalysts. Transesterification of algal oil by mechanical stirring yielded significant biodiesel within an hour at 60 degree C with NaOH and at room temperature with Na metal. In addition, microwave irradiated transesterification produced significant amount of biodiesel with NaOH and Na metal within 1-5 minutes. However, reaction of sodium metal in microwave oven was highly exothermic and uncontrollable that could also damage the radiation source. The reactivity order of alcohols was found to be methanol > ethanol > benzyl alcohol > 1-propanol > 1-butanol > 1-pentanol > 1-hexanol > 2-propanol. Isopropyl alcohol was found to be least reactive due to steric hindrance. Benzyl alcohol was found to be more reactive than 1-propyl alcohol due to the electron withdrawing effect of benzene ring. The highest % conversion of FAME and FAEE were found to be 97% and 98% respectively using Na metal through mechanical stirring. Biodiesel production was confirmed by thin layer chromatography (TLC). Furthermore, the fuel properties including density, kinematics viscosity, high heating value, acid value, free fatty acid (%), cloud point and pour point of U. fasciata oil and all the esters were determined and compared with the standard limits of biodiesel. Fatty acid methyl, ethyl, 1-propyl, 2-propyl, 1-butyl, 1-pentyl and 1-hexyl esters showed the fuel properties within the biodiesel standard limits therefore all of them were considered as the substitute of biodiesel. On the other hand, the fuel properties of benzyl ester were found to be above the limits of biodiesel specifications and thus it could not be considered as biodiesel. This research article will be helpful to overcome the current challenges of energy crisis, global warming and

  16. Ultrastructure of Escherichia coli cells under the action of a novel derivative of aryl aliphatic aminoalcohols

    Directory of Open Access Journals (Sweden)

    Dronova M.L.

    2014-12-01

    Full Text Available Background. Novel derivatives of aryl aliphatic aminoalcohols were examined for antimicrobial activity. Compound KVM-114 (4-(1,1,3,3-tetrabutyl phenoxy-3-dimethylamino-2-propanol hydrochloride was found as a selective against gram-negative bacteria. Objective. Investigation of compound KVM-114 influence on E. coli ultrastructure. Methods. Minimum inhibitory concentrations were determined by serial dilution method in Muller-Hinton broth. Bacteria (Escherichia coli for transmission electron microscopy samples preparation was grown to exponential phase and then was exposed to the subinhibitory concentration of KVM-114 for 1 h and 24 h. Results. Intact E. coli cells were rod-shaped with rounded ends. A light layer, allowing clear visualization of the cell wall, was observed between the сytoplasm and cytoplasmic membrane. Lipopolysaccharide layer was well distinguished as well. Cytoplasm was filled with ribosomes and polyribosomes. 1 hour exposition to KVM-114 at a subinhibitory concentration resulted in the absence of polyribosomes in the cytoplasm. Increase of electron density of lipopolysaccharide layer and cell wall indicate alteration of cell envelope. Prolongation of the incubation period to 24 hours led to cell recovery: no changes were observed, compared to control cells. The data obtained suggest compound’s ability to alter cell envelope and metabolic activity, however, subinhibitory concentration is apparently not sufficient for total inhibition of E. coli growth. Conclusion. The derivative of aryl aliphatic aminoalcohols, compound KVM-114, possesses inhibitory activity against gram-negative bacteria. E. coli treatment with this compound resulted in structural changes of the cell wall and alteration of intracellular processes. Citation: Dronova ML, Voychuk SI, Vrynchanu NO. [Ultrastructure of Escherichia coli cells under the action of a novel derivative of aryl aliphatic aminoalcohols]. Morphologia. 2014;8(4:26-9. Ukrainian.

  17. Comparative study of photoinduced wettability conversion between [PW{sub 12}O{sub 40}]{sup 3−}/brookite and [SiW{sub 12}O{sub 40}]{sup 4−}/brookite hybrid films

    Energy Technology Data Exchange (ETDEWEB)

    Pruethiarenun, Kunchaya; Isobe, Toshihiro; Matsushita, Sachiko [Department of Metallurgy and Ceramic Science, Graduate School of Science and Engineering, Tokyo Institute of Technology, 2-12-1 O-okayama, Meguro-ku, Tokyo 152-8552 (Japan); Ye, Jinhua [Environmental Remediation Materials Unit, Environment and Energy Materials Division, National Institute for Materials Science, 1-1 Namiki, Tsukuba, Ibaraki 305-0044 (Japan); Nakajima, Akira, E-mail: anakajim@ceram.titech.ac.jp [Department of Metallurgy and Ceramic Science, Graduate School of Science and Engineering, Tokyo Institute of Technology, 2-12-1 O-okayama, Meguro-ku, Tokyo 152-8552 (Japan)

    2014-04-01

    Two tungsten-based Keggin-type heteropolyacids (PW{sub 12}: ([PW{sub 12}O{sub 40}]{sup 3−}) and SiW{sub 12}: ([SiW{sub 12}O{sub 40}]{sup 4−})) were hybridized with brookite-type TiO{sub 2}. Then photocatalytic decomposition activity, photoinduced hydrophilicity, and sustainability of the hydrophilicity in the dark were evaluated using gaseous 2-propanol (IPA) decomposition and sessile drop method. The obtained films were transparent in the visible wavelength range. Both hybrid films exhibited higher photocatalytic decomposition activity and had higher photoinduced hydrophilicizing rates than pure brookite films under UV illumination. The PW{sub 12}/TiO{sub 2} film exhibited better photocatalytic performance than the SiW{sub 12}/TiO{sub 2} film did. Atmosphere dependence, XPS analysis, and electrochemical experiments indicated the cause of these two films' different levels of sustainability of hydrophilicity to be differences in their electron storage capability. Results show that the electron scavenger capability and reoxidation efficiency of the heteropolyacid are key factors affecting the overall performance of wettability conversion of this hybrid film system before and after UV illumination. - Highlights: • Transparent PW{sub 12}/brookite(TTP) and SiW{sub 12}/brookite(TTS) films were prepared. • Both films exhibited better photocatalytic performance than pure brookite film. • The TTP film exhibited more sustainable hydrophilicity than the TTS film did. • Reoxidation efficiency of HPAs is a key factor for wettability conversion.

  18. An Integrated Theory of Adsorption and Partition Mechanism and Eash Contribution to Solute Retention in Reversed Phase Liquid Chromatography

    Institute of Scientific and Technical Information of China (English)

    耿信笃; 弗莱德依瑞格涅尔

    2003-01-01

    With the combination of the the stoichiometric displacement model for retention (SDM-R) in reversed phase liquid chromatography (RPLC) and the stoichiometric displacement model for adsorption (SDM-A) in physical chemistry,the total number of moles of the re-solvated methanol of stationary phase side.nr,and that of solute side in the mobile phase,q,corresponding the one mole of the desorbing solute,were separately determined and referred as the characterization parameters of the contributions of the adsorption mechanism and partition mechanism to the solute retention,respectively.A chromatographic system of insulin,using mobile phase consisting of the pseudo-homologue of alcohols(methanol,ethanol and 2-propanol)-water and trifluoroacetic acid was employed.The maximum number of the methanol layers on the stationary phase surface was found to be 10.6,only 3 of which being valid in usual RPLC,traditionally referred as a volume process in partition mechanism.However,it still follows the SDM-R.Both of q and nr of insulin were found not to be zero,indicating that the retention mechanism of insulin is a mixed mode of partition mechanism and adsorption mechanism.When methanol is used as the organic modifier,the ratio of q/nr was 1.13,indicating the contribution to insulin retention due to partition mechanism being a bit greater than that due to adsorption mechanism.A linear relationship between q,or nr and the carbon number of the pseudo-homologue in the mobile phase was also found.As a methodology for investigating the retention mechanism retention and behavior of biopolymers.a homologue of organic solvents as the organic modifier in mobile phase has also been explored.

  19. Physico-chemical properties of Pd nanoparticles produced by Pulsed Laser Ablation in different organic solvents

    International Nuclear Information System (INIS)

    Palladium nanoparticles are arousing an increasing interest because of their strong activity in heterogeneous catalysis in a wide range of reactions. Driven by the interest of producing Pd nanoparticles to be deposited for catalysis over hydrophobic supports, we investigated their synthesis via Pulsed Laser Ablation in Liquid in several organic solvents, as acetone, ethanol, 2-propanol, toluene, n-hexane. The colloids were produced by using a Nd:YAG ns laser and without the addition of surfactant agents. The morphology, composition, stability and oxidation state of the obtained nanoparticles were investigated by TEM-EDS analysis, UV-vis spectroscopy, X-ray Photoelectron Spectroscopy and micro-Raman spectroscopy. The results evidence that the nature of the solvent influences both the yield and the physico-chemical properties of the produced nanoparticles. While in acetone and alcohols spheroidal, non aggregated and stable particles are obtained, in case of toluene and n-hexane few unstable particles surrounded by a gel-like material are produced. Raman/XPS measurements suggest the presence of amorphous or graphitic carbon onto crystalline Pd nanoparticles, which could have hindered their growth and determined the observed smaller sizes if compared to nanoparticles produced in water. The stability of Pd colloids obtained in acetone and alcohols was attributed to adsorbed anions like enolates or alcoholates; non polar solvents like toluene and n-hexane, unable to give rise to adsorbed anionic species, cannot provide any stabilization to the palladium nanoparticles. XPS analyses also evidenced a partial oxidation of particles surface, with a ratio Pd2+:Pd0 of 1:2.5 and 1:4 in acetone and ethanol, respectively.

  20. Efficacy of ethanol-based hand foams using clinically relevant amounts: a cross-over controlled study among healthy volunteers

    Directory of Open Access Journals (Sweden)

    Marschall Sigunde

    2010-03-01

    Full Text Available Abstract Background Foams containing 62% ethanol are used for hand decontamination in many countries. A long drying time may reduce the compliance of healthcare workers in applying the recommended amount of foam. Therefore, we have investigated the correlation between the applied amount and drying time, and the bactericidal efficacy of ethanol foams. Methods In a first part of tests, four foams (Alcare plus, Avagard Foam, Bode test foam, Purell Instant Hand Sanitizer containing 62% ethanol, which is commonly used in U.S. hospitals, were applied to 14 volunteers in a total of seven variations, to measure drying times. In a second part of tests, the efficacy of the established amount of foam for a 30 s application time of two foams (Alcare plus, Purell Instant Hand Sanitizer and water was compared to the EN 1500 standard of 2 × 3 mL applications of 2-propanol 60% (v/v, on hands artificially contaminated with Escherichia coli. Each application used a cross-over design against the reference alcohol with 15 volunteers. Results The mean weight of the applied foam varied between 1.78 and 3.09 g, and the mean duration to dryness was between 37 s and 103 s. The correlation between the amount of foam applied and time until hands felt dry was highly significant (p 10-reduction: 3.05 ± 0.45 and Alcare plus (3.58 ± 0.71 was significantly less effective than the reference disinfection (4.83 ± 0.89 and 4.60 ± 0.59, respectively; p 10-reduction of 2.39 ± 0.57. Conclusions When using 62% ethanol foams, the time required for dryness often exceeds the recommended 30 s. Therefore, only a small volume is likely to be applied in clinical practice. Small amounts, however, failed to meet the efficacy requirements of EN 1500 and were only somewhat more effective than water.

  1. Physico-chemical properties of Pd nanoparticles produced by Pulsed Laser Ablation in different organic solvents

    Energy Technology Data Exchange (ETDEWEB)

    Cristoforetti, Gabriele, E-mail: gabriele.cristoforetti@cnr.it [National Institute of Optics, Research Area of National Research Council, Via G. Moruzzi 1, 56124 Pisa (Italy); Pitzalis, Emanuela; Spiniello, Roberto [Institute of Chemistry of OrganoMetallic Compounds, Research Area of National Research Council, Via G. Moruzzi 1, 56124 Pisa (Italy); Ishak, Randa [Department of Chem. Eng. And Material Science, University of Pisa, Via Diotisalvi 2, 56126 Pisa (Italy); Giammanco, Francesco [Department of Physics, University of Pisa, Largo B. Pontecorvo 3, 56127 Pisa (Italy); Muniz-Miranda, Maurizio; Caporali, Stefano [Department of Chemistry, University of Florence, Via della Lastruccia 3, 50019 Sesto Fiorentino (Italy)

    2012-01-15

    Palladium nanoparticles are arousing an increasing interest because of their strong activity in heterogeneous catalysis in a wide range of reactions. Driven by the interest of producing Pd nanoparticles to be deposited for catalysis over hydrophobic supports, we investigated their synthesis via Pulsed Laser Ablation in Liquid in several organic solvents, as acetone, ethanol, 2-propanol, toluene, n-hexane. The colloids were produced by using a Nd:YAG ns laser and without the addition of surfactant agents. The morphology, composition, stability and oxidation state of the obtained nanoparticles were investigated by TEM-EDS analysis, UV-vis spectroscopy, X-ray Photoelectron Spectroscopy and micro-Raman spectroscopy. The results evidence that the nature of the solvent influences both the yield and the physico-chemical properties of the produced nanoparticles. While in acetone and alcohols spheroidal, non aggregated and stable particles are obtained, in case of toluene and n-hexane few unstable particles surrounded by a gel-like material are produced. Raman/XPS measurements suggest the presence of amorphous or graphitic carbon onto crystalline Pd nanoparticles, which could have hindered their growth and determined the observed smaller sizes if compared to nanoparticles produced in water. The stability of Pd colloids obtained in acetone and alcohols was attributed to adsorbed anions like enolates or alcoholates; non polar solvents like toluene and n-hexane, unable to give rise to adsorbed anionic species, cannot provide any stabilization to the palladium nanoparticles. XPS analyses also evidenced a partial oxidation of particles surface, with a ratio Pd{sup 2+}:Pd{sup 0} of 1:2.5 and 1:4 in acetone and ethanol, respectively.

  2. p-Aminophenylacetic acid-mediated synthesis of monodispersed titanium oxide hybrid microspheres in ethanol solution.

    Science.gov (United States)

    Zhang, Hongye; Xie, Yun; Liu, Zhimin; Tao, Ranting; Sun, Zhenyu; Ding, Kunlun; An, Guimin

    2009-10-15

    Monodispersed TiO2 hybrid microspheres were prepared via the hydrolysis of titanium isopropoxide (TTIP) in ethanol solution containing p-aminophenylacetic acid (APA). The effects of the APA:TTIP molar ratio, water content, reaction time and reaction temperature on the morphology of the resultant spheres were investigated. The products were characterized by scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy, thermogravimetric analysis, and X-ray diffraction. It was demonstrated that the diameters of the resultant TiO2 spheres could be tuned in the range of 380-800 nm by changing the APA:TTIP molar ratio (1:3 to 3:1) and water content (1-3 v/v%) in the reaction medium, and that increasing the APA:TTIP molar ratio led to larger TiO2 hybrid spheres while increasing the water content decreased their size. The loading content of APA in the hybrid spheres could reach 20 wt.% as they were prepared with the APA:TTIP ratio of 3:1. The possible formation mechanism of the hybrid spheres was also investigated. It was found that APA slowed down the hydrolysis rate of the titanium precursor so that resulted in the formation of the TiO2 spheres. In addition, the APA present in TiO2 spheres acted as a reducing agent to in situ convert HAuCl4 into metallic Au on the surface of the TiO2 spheres. The catalytic activity of the resultant Au/APA-TiO2 composite was examined using transfer hydrogenation of phenylacetone with 2-propanol, and it was indicated that the catalyst displayed high efficiency for this reaction. PMID:19616218

  3. Crystal structures of halohydrin hydrogen-halide-lyases from Corynebacterium sp. N-1074.

    Science.gov (United States)

    Watanabe, Fumiaki; Yu, Fujio; Ohtaki, Akashi; Yamanaka, Yasuaki; Noguchi, Keiichi; Yohda, Masafumi; Odaka, Masafumi

    2015-12-01

    Halohydrin hydrogen-halide-lyase (H-Lyase) is a bacterial enzyme that is involved in the degradation of halohydrins. This enzyme catalyzes the intramolecular nucleophilic displacement of a halogen by a vicinal hydroxyl group in halohydrins to produce the corresponding epoxides. The epoxide products are subsequently hydrolyzed by an epoxide hydrolase, yielding the corresponding 1, 2-diol. Until now, six different H-Lyases have been studied. These H-Lyases are grouped into three subtypes (A, B, and C) based on amino acid sequence similarities and exhibit different enantioselectivity. Corynebacterium sp. strain N-1074 has two different isozymes of H-Lyase, HheA (A-type) and HheB (B-type). We have determined their crystal structures to elucidate the differences in enantioselectivity among them. All three groups share a similar structure, including catalytic sites. The lack of enantioselectivity of HheA seems to be due to the relatively wide size of the substrate tunnel compared to that of other H-Lyases. Among the B-type H-Lyases, HheB shows relatively high enantioselectivity compared to that of HheBGP1 . This difference seems to be due to amino acid replacements at the active site tunnel. The binding mode of 1, 3-dicyano-2-propanol at the catalytic site in the crystal structure of the HheB-DiCN complex suggests that the product should be (R)-epichlorohydrin, which agrees with the enantioselectivity of HheB. Comparison with the structure of HheC provides a clue for the difference in their enantioselectivity.

  4. Rapid Synthesis and Antiviral Activity of (Quinazolin-4-YlaminoMethyl-Phosphonates Through Microwave Irradiation

    Directory of Open Access Journals (Sweden)

    Baoan Song

    2012-06-01

    Full Text Available This study describes the simple synthesis of new (quinazolin-4-ylamino methylphosphonates via microwave irradiation. Substituted-2-aminobenzonitrile reacted with 1,1-dimethoxy-N,N-dimethylmethanamine at a reflux condition to obtain N'-(substituted-2-cyanophenyl-N,N-dimethylformamidine (1. The subsequent reaction of this intermediate product with α-aminophosphonate (2 in a solution containing glacial acetic acid in 2-propanol through microwave irradiation resulted in the formation of (quinazolin-4-ylaminomethyl-phosphonate derivatives 3a to 3x, which were unequivocally characterized by the spectral data and elemental analysis. The influence of the reaction conditions on the yield of 3a was investigated to optimize the synthetic conditions. The relative optimal conditions for the synthesis of 3a include a 1:1 molar ratio of N’-(2-cyanophenyl-N,N-dimethylformamidine to diethyl amino(phenylmethylphosphonate and a 4:1 volume ratio of isopropanol to HOAc in the solvent mixture, at a reaction temperature of 150 °C, with a microwave power of 100 W and a corresponding pressure of 150 psi for 20 min in the microwave synthesizer. The yield of 3a was approximately 79%, whereas those of 3b to 3x were approximately 77% to 86%. Some of the synthesized compounds displayed weak to good anti-Tobacco mosaic virus (TMV activity.

  5. Indoor air quality in hair salons: Screening of volatile organic compounds and indicators based on health risk assessment

    Science.gov (United States)

    de Gennaro, Gianluigi; de Gennaro, Lucrezia; Mazzone, Antonio; Porcelli, Francesca; Tutino, Maria

    2014-02-01

    Volatile organic compounds (VOCs) are common ingredients in cosmetic products which can impact human health. This study monitored 12 hairdressing salons in order to assess the individual exposure of the people working in or frequenting these environments as well as identify the main products or activities responsible for the presence of these compounds. In each site halogenated, oxygenated, aliphatic and aromatic compounds were monitored during the work week with diffusive samplers suitable for thermal desorption and analysed using GC-MS. The study of indoor-outdoor concentration ratios and a knowledge of the composition of most of the products, whether ecological or traditional, used in the hair salons verified the presence of compounds linked to hairdressing activities. In particular, compounds widely used in products for hair care as spray lacquer and foam (butane), shampoo, balms, hair masks and oils (camphene, camphor, limonene, eucalyptol, alpha pinene, 1-methoxy-2-propanol, n-butanol and menthol), and hair dye (benzyl alcohol, isopropanol, limonene, hexane and methyl ethyl ketone) were found at much higher levels inside rather than outside the salons (mean I/O > 10). The importance of this finding is linked to the potential health hazards of some of the VOCs detected. Integrated indicators of health risk were proposed in this study to assess the criticality level and rank the investigated environments accordingly. The results of this study indicate that the level of VOC concentrations was most affected by the type of products used while the size of the environment, the efficiency of air exchange and the number of customers had less impact on those levels.

  6. Mechanistic Insight into Peroxydisulfate Reactivity: Oxidation of the cis,cis-[Ru(bpy)2(OH2)]2O(4+) "Blue Dimer".

    Science.gov (United States)

    Hurst, James K; Roemeling, Margo D; Lymar, Sergei V

    2015-06-18

    One-electron oxidation of the μ-oxo dimer (cis,cis-[Ru(III)(bpy)2(OH2)]2O(4+), {3,3}) to {3,4} by S2O8(2-) can be described by three concurrent reaction pathways corresponding to the three protic forms of {3,3}. Free energy correlations of the rate constants, transient species dynamics determined by pulse radiolysis, and medium and temperature dependencies of the alkaline pathway all suggest that the rate-determining step in these reactions is a strongly nonadiabatic dissociative electron transfer within a precursor ion pair leading to the {3,4}|SO4(2-)|SO4(•-) ion triple. As deduced from the SO4(•-) scavenging experiments with 2-propanol, the SO4(•-) radical then either oxidizes {3,4} to {4,4} within the ion triple, effecting a net two-electron oxidation of {3,3}, or escapes in solution with ∼25% probability to react with additional {3,3} and {3,4}, that is, effecting sequential one-electron oxidations. The reaction model presented also invokes rapid {3,3} + {4,4} → 2{3,4} comproportionation, for which kcom ∼5 × 10(7) M(-1) s(-1) was independently measured. The model provides an explanation for the observation that, despite favorable energetics, no oxidation beyond the {3,4} state was detected. The indiscriminate nature of oxidation by SO4(•-) indicates that its fate must be quantitatively determined when using S2O8(2-) as an oxidant. PMID:25819370

  7. Pt/Al/sub 2/O/sub 3/- carbon nanocomposite as a catalyst for fuel cells

    International Nuclear Information System (INIS)

    Catalysts comprising platinum nanoparticles (Pt NPs) on carbon support are used in fuel cells for the hydrogen and electricity production by electrochemical oxidation of methanol. However, the catalyst is not the best in terms of its performance. Considering role of the support as significant towards efficiency and durability of the catalyst, there is need for introducing novel support materials to replace carbon alone. Deposition of various metallic NPs on ceramic-carbon (hybrid) supports has been reported to improve thermal, mechanical, electrical and chemical properties of different types of catalyst. In search of better performing catalysts for proton exchange membrane fuel cells (PEMFCs), hybrid supports having different ceramic materials should be synthesized. In this regard Pt/Al/sub 2/O/sub 3/-Carbon (nanocomposites) have been synthesized and applied as promising catalysts in the PEMFCs; results obtained for the nanocomposites were compared with Pt/carbon and Pt/Al/sub 2/O/sub 3/. Vulcan carbon was purified and functionalized prior to use; presence of oxygen containing functional groups on carbon was established from the FTIR spectrum, Hybrid support (1:8 by weight ratio of ceramic and carbon) were already prepared in aqueous 2-propanol employing sonication method on to which Pt NPs (10% by weight in all the cases) were deposited by simple chemical reduction of PtCl/sub 4/ by NaBH/sub 4/ under controlled conditions. The catalysts were subjected to various characterization techniques like TGA (for thermal stability), EDX (for chemical composition), SEM (for surface morphology) and XRD (for cell-shape and -volume, material density and average crystalline size). Catalysts efficiencies for the methanol oxidation were investigated through cyclic voltammetery (CV) by comparing electrochemical surface area, peak current, exchange current density and rate constant in the acidic and basic media. Pt/Al/sub 2/O/sub 3/-carbon exhibited better catalytic efficiencies

  8. Yarrowia lipolytica NCIM 3589, a tropical marine yeast, degrades bromoalkanes by an initial hydrolytic dehalogenation step.

    Science.gov (United States)

    Vatsal, Aakanksha; Zinjarde, Smita S; Kumar, Ameeta Ravi

    2015-04-01

    The widespread industrial use of organobromines which are known persistent organic pollutants has led to their accumulation in sediments and water bodies causing harm to animals and humans. While degradation of organochlorines by bacteria is well documented, information regarding degradation pathways of these recalcitrant organobromines is scarce. Hence, their fates and effects on the environment are of concern. The present study shows that a tropical marine yeast, Yarrowia lipolytica NCIM 3589 aerobically degrades bromoalkanes differing in carbon chain length and position of halogen substitution viz., 2-bromopropane (2-BP), 1-bromobutane (1-BB), 1,5 dibromopentane (1,5-DBP) and 1-bromodecane (1-BD) as seen by an increase in cell mass, release of bromide and concomitant decrease in concentration of brominated compound. The amount of bromoalkane degraded was 27.3, 21.9, 18.0 and 38.3 % with degradation rates of 0.076, 0.058, 0.046 and 0.117/day for 2-BP, 1-BB, 1,5-DBP and 1-BD, respectively. The initial product formed respectively were alcohols viz., 2-propanol, 1-butanol, 1-bromo, 5-pentanol and 1-decanol as detected by GC-MS. These were further metabolized to fatty acids viz., 2-propionic, 1-butyric and 1-decanoic acid eventually leading to carbon dioxide formation. Neither higher chain nor brominated fatty acids were detected. An inducible extracellular dehalogenase responsible for removal of bromide was detected with activities of 21.07, 18.82, 18.96 and 26.67 U/ml for 2-BP, 1-BB, 1,5-DBP and 1-BD, respectively. We report here for the first time the proposed aerobic pathway of bromoalkane degradation by an eukaryotic microbe Y. lipolytica 3589, involving an initial hydrolytic dehalogenation step. PMID:25708590

  9. Final Report for CRADA Agreement , AL-C-2006-01 with Microsens Biotechnologies: Detection of the Abnormal Prion Protein in Blood by Improving the Extraction of this Protein

    Energy Technology Data Exchange (ETDEWEB)

    Schmerr, Mary Jo

    2009-03-31

    Several conditions were examined to optimize the extraction protocol using Seprion beads for the abnormal prion protein. Different combinations of water, hexafluro-2-propanol and formic acid were used. The results of these extraction protocols showed that the magnetic beads coated with Seprion reagents were subject to degradation, themselves, when the extraction conditions that would solubilize the abnormal prion protein were used. These compounds caused interference in the immunoassay for the abnormal prion protein and rendered these protocols incompatible with the assay systems. In an attempt to overcome this problem, another approach was then used. The coated beads were used as an integral part of the assay platform. After washing away denaturing agents, the beads with the 'captured' abnormal prion were incubated directly in the immunoassay, followed by analysis by the capillary electrophoresis. When a capillary electrophoresis electro-kinetic separation was attempted, the beads disturbed the analysis making it impossible to interpret. A pressure separation method was then developed for capillary electrophoresis analysis. When 20 samples, 5 of which were positive were analyzed, the assay identified 4 of the 5 positives and had no false positives. When a larger number of samples were analyzed the results were not as good - there were false positives and false negatives. It was then observed that the amount of beads that were loaded was dependent upon how long the beads were allowed to settle before loading them into the capillary. This resulted in unacceptable variations in the results and explained that when large numbers of samples were evaluated the results were not consistent. Because the technical difficulties with using the Seprion beads could not be overcome at this time, another approach is underway that is outside of the scope of this CRADA. No further agreements have been developed. Because the results were not favorable, no manuscripts were

  10. Role of 5-HT(1A) and 5-HT(1B) receptors in the antidepressant-like effect of piperine in the forced swim test.

    Science.gov (United States)

    Mao, Qing-Qiu; Huang, Zhen; Ip, Siu-Po; Xian, Yan-Fang; Che, Chun-Tao

    2011-10-24

    Our previous studies have showed that treating mice with piperine significantly decreased the immobility time of the animals in the forced swim test and tail suspension test, which was related to up-regulation of serotonin (5-HT) level in the brain. The purpose of this study is to explore the contribution of 5-HT receptors in the antidepressant-like effect of piperine. The results showed that pre-treating mice with methiothepin (a non-selective 5-HT receptor antagonist, 0.1mg/kg, intraperitoneally), 4-(2'-methoxy-phenyl)-1-[2'-(n-2″-pyridinyl)-p-iodobenzamino-]ethyl-piperazine (a selective 5-HT(1A) receptor antagonist, 1mg/kg, subcutaneously) or 1-(2-(1-pyrrolyl)-phenoxy)-3-isopropylamino-2-propanol (a 5-HT(1B) receptor antagonist, 2.5mg/kg, intraperitoneally) was found to abolish the anti-immobility effect of piperine (10mg/kg, intraperitoneally) in the forced swim test. On the other hand, a sub-effective dose of piperine (1mg/kg, intraperitoneally) produced a synergistic antidepressant-like effect with (+)-8-hydroxy-2-(di-n-propylamino)tetralin (a 5-HT(1A) receptor agonist, 1mg/kg, intraperitoneally) or anpirtoline (a 5-HT(1B) receptor agonist, 0.25mg/kg, intraperitoneally). Taken together, these results suggest that the antidepressant-like effect of piperine in the mouse forced swim test may be mediated, at least in part, by the activation of 5-HT(1A) and 5-HT(1B) receptors.

  11. Classical Keggin Intercalated into Layered Double Hydroxides: Facile Preparation and Catalytic Efficiency in Knoevenagel Condensation Reactions.

    Science.gov (United States)

    Jia, Yueqing; Fang, Yanjun; Zhang, Yingkui; Miras, Haralampos N; Song, Yu-Fei

    2015-10-12

    The family of polyoxometalate (POM) intercalated layered double hydroxide (LDH) composite materials has shown great promise for the design of functional materials with numerous applications. It is known that intercalation of the classical Keggin polyoxometalate (POM) of [PW12 O40 ](3-) (PW12 ) into layered double hydroxides (LDHs) is very unlikely to take place by conventional ion exchange methods due to spatial and geometrical restrictions. In this paper, such an intercalated compound of Mg0.73 Al0.22 (OH)2 [PW12 O40 ]0.04 ⋅0.98 H2 O (Mg3 Al-PW12 ) has been successfully obtained by applying a spontaneous flocculation method. The Mg3 Al-PW12 has been fully characterized by using a wide range of methods (XRD, SEM, TEM, XPS, EDX, XPS, FT-IR, NMR, BET). XRD patterns of Mg3 Al-PW12 exhibit no impurity phase usually observed next to the (003) diffraction peak. Subsequent application of the Mg3 Al-PW12 as catalyst in Knoevenagel condensation reactions of various aldehydes and ketones with Z-CH2 -Z' type substrates (ethyl cyanoacetate and malononitrile) at 60 °C in mixed solvents (V2-propanol :Vwater =2:1) demonstrated highly efficient catalytic activity. The synergistic effect between the acidic and basic sites of the Mg3 Al-PW12 composite proved to be crucial for the efficiency of the condensation reactions. Additionally, the Mg3 Al-PW12 -catalyzed Knoevenagel condensation of benzaldehyde with ethyl cyanoacetate demonstrated the highest turnover number (TON) of 47 980 reported so far for this reaction. PMID:26337902

  12. Sonochemical degradation of the pharmaceutical fluoxetine: Effect of parameters, organic and inorganic additives and combination with a biological system

    Energy Technology Data Exchange (ETDEWEB)

    Serna-Galvis, Efraím A.; Silva-Agredo, Javier [Grupo de Investigación en Remediación Ambiental y Biocatálisis, Instituto de Química, Facultad de Ciencias Exactas y Naturales, Universidad de Antioquia UdeA, Calle 70 No. 52-21, Medellín (Colombia); Giraldo-Aguirre, Ana L. [Grupo de Diseño y Formulación de Medicamentos, Cosméticos y Afines (DYFOMECO), Facultad de Química Farmacéutica, Universidad de Antioquia UdeA, Calle 70 No. 52-21, Medellín (Colombia); Torres-Palma, Ricardo A., E-mail: ricardo.torres@udea.edu.co [Grupo de Investigación en Remediación Ambiental y Biocatálisis, Instituto de Química, Facultad de Ciencias Exactas y Naturales, Universidad de Antioquia UdeA, Calle 70 No. 52-21, Medellín (Colombia)

    2015-08-15

    Fluoxetine (FLX), one of the most widely used antidepressants in the world, is an emergent pollutant found in natural waters that causes disrupting effects on the endocrine systems of some aquatic species. This work explores the total elimination of FLX by sonochemical treatment coupled to a biological system. The biological process acting alone was shown to be unable to remove the pollutant, even under favourable conditions of pH and temperature. However, sonochemical treatment (600 kHz) was shown to be able to remove the pharmaceutical. Several parameters were evaluated for the ultrasound application: the applied power (20–60 W), dissolved gas (air, Ar and He), pH (3–11) and initial concentration of fluoxetine (2.9–162.0 μmol L{sup −1}). Additionally, the presence of organic (1-hexanol and 2-propanol) and inorganic (Fe{sup 2+}) compounds in the water matrix and the degradation of FLX in a natural mineral water were evaluated. The sonochemical treatment readily eliminates FLX following a kinetic Langmuir. After 360 min of ultrasonic irradiation, 15% mineralization was achieved. Analysis of the biodegradability provided evidence that the sonochemical process transforms the pollutant into biodegradable substances, which can then be mineralized in a subsequent biological treatment. - Highlights: • The pharmaceutical fluoxetine was effectively eliminated upon ultrasonic action. • Ultrasonic power, dissolved gas, pH and concentration of fluoxetine were evaluated. • Fe{sup 2+}, sodium nitrate or nitric acid had a positive effect on the FLX degradation. • More hydrophobic or volatile compounds than fluoxetine diminished the efficiency. • A sonochemical-biological combined process led to the total mineralization of FLX.

  13. Catalytic Hydrogenation of Acetone to Isopropanol: An Environmentally Benign Approach

    Directory of Open Access Journals (Sweden)

    Ateeq Rahman

    2011-01-01

    Full Text Available The catalytic hydrogenation of acetone is an important area of catalytic process to produce fine chemicals. Hydrogenation of acetone has important applications for heat pumps, fuel cells or in fulfilling the sizeable demand for the production of 2-propanol. Catalytic vapour phase hydrogenation of acetone has gained attention over the decades with variety of homogeneous catalysts notably Iridium, Rh, Ru complexes and heterogeneous catalysts comprising of Raney Nickel, Raney Sponge, Ni/Al2O3, Ni/SiO2, or Co-Al2O3, Pd, Rh, Ru, Re, or Fe/Al2O3 supported on SiO2 or MgO and even CoMgAl, NiMg Al layered double hydroxide, Cu metal, CuO, Cu2O. Nano catalysts are developed for actone reduction Ni maleate, cobalt oxide prepared in organic solvents. Author present a review on acetone hydrogenation under different conditions with various homogeneous and heterogeneous catalysts studied so far in literature and new strategies to develop economic and environmentally benign approach. ©2010 BCREC UNDIP. All rights reserved(Received: 16th June 2010, Revised: 18th October 2010; Accepted: 25th October 2010[How to Cite:Ateeq Rahman. (2010. Catalytic Hydrogenation of Acetone to Isopropanol: An Environmentally Benign Approach. Bulletin of Chemical Reaction Engineering and Catalysis, 5(2: 113-126. doi:10.9767/bcrec.5.2.798.113-126][DOI: http://dx.doi.org/10.9767/bcrec.5.2.798.113-126 || or local:  http://ejournal.undip.ac.id/index.php/bcrec/article/view/798

  14. Determination of thermodynamic properties of poly(cyclohexyl methacrylate)by inverse gas chromatography

    Institute of Scientific and Technical Information of China (English)

    Ismet KAYA; Cigdem Yigit PALA

    2014-01-01

    In this work,some thermodynamic properties of poly( cyclohexyl methacrylate)were studied by inverse gas chromatography( IGC). For this purpose,the polymeric substance was coated on Chromosorb W and which was filled into a glass column. The retention times(tr)of the probes were determined from the interactions of poly(cyclohexyl methacrylate)with n-pentane,n-hexane,n-heptane,n-octane,n-decane, methanol,ethanol,2-propanol,butanol,acetone,ethyl methyl ketone,benzene,toluene and o-xylene by IGC technique. Then,the specific volume(V0g)was determined for each probe molecule. By using(1/T;lnV0g) graphics,the glass transition temperature of poly( cyclohexyl methacrylate)was found to be 373 K. The adsorp-tion heat under the glass transition temperature(ΔH a ),and partial molar heat of sorption above the glass tran-sition(ΔHS1 ),partial molar free energy of sorption(ΔGS1 )and partial molar entropy of sorption(ΔSS1 )belong-ing to sorption for every probe were calculated. The partial molar heat of mixing at infinite dilution(ΔH∞1 ), partial molar free energy of mixing at infinite dilution(ΔG∞1 ),Flory-Huggins interaction parameter(χ∞12 )and weight fraction activity coefficient(a1/w1)∞ values of polymer-solute systems were calculated at different col-umn temperatures. The solubility parameters(δ2 )of the polymer were obtained by IGC technique.

  15. Relation between phase composition and photocatalytic activity of TiO{sub 2} in a sulfoxide deoxygenation reaction

    Energy Technology Data Exchange (ETDEWEB)

    Molinari, Alessandra, E-mail: alessandra.molinari@unife.it [Dipartimento di Scienze Chimiche e Farmaceutiche, Università di Ferrara, Via Fossato di Mortara 17, 44121 Ferrara (Italy); Bonino, Francesca; Magnacca, Giuliana [Dipartimento di Chimica, NIS and INSTM Reference Centre, Università di Torino, Via G. Quarello 15, I-10135 and Via P. Giuria 7, I-10125, Turin (Italy); Demaria, Francesca; Maldotti, Andrea [Dipartimento di Scienze Chimiche e Farmaceutiche, Università di Ferrara, Via Fossato di Mortara 17, 44121 Ferrara (Italy)

    2015-05-05

    In the present study we synthesize three TiO{sub 2} samples, TiO{sub 2}-500, TiO{sub 2}-750 and TiO{sub 2}-850, by a sol–gel procedure varying the rutile and anatase content by calcination at different temperatures. Characterization by XRD, NIR-Raman, UV-Raman, BET, DR-UV-Vis spectroscopy and SEM points out that TiO{sub 2}-500 consists mainly of anatase and TiO{sub 2}-850 of rutile. TiO{sub 2}-700 presents both phases on the surface that is the part of the photocatalyst interested by UV illumination. The photocatalysts are tested in the deoxygenation reaction of methyl p-tolyl sulfoxide to the corresponding sulfide using 2-propanol as hole scavenger. It is demonstrated that the presence of both anatase and rutile on the surface of TiO{sub 2}-700 is responsible of the increase of the photocatalytic activity. This is likely due to a more efficient charge separation process that increases lifetime of the charges giving availability of electrons and holes for the photocatalytic reaction. Methyl p-tolyl sulfide is formed with a selectivity of 100%. - Highlights: • TiO{sub 2} samples are synthesized via sol–gel varying the rutile and anatase composition. • TiO{sub 2}-700 (calcined at 700 °C) presents both anatase and rutile on the surface. • Efficient charges separation is allowed by the presence of anatase and rutile. • Spatial separation of charges renders TiO{sub 2}-700 the most active photocatalyst. • Methyl p-tolyl sulfoxide is transformed in sulfide with 100% selectivity.

  16. Analysis of 3-MCPD and 1,3-DCP in Various Foodstuffs Using GC-MS.

    Science.gov (United States)

    Kim, Wooseok; Jeong, Yun A; On, Jiwon; Choi, Ari; Lee, Jee-Yeon; Lee, Joon Goo; Lee, Kwang-Geun; Pyo, Heesoo

    2015-09-01

    3-Monochloro-1,2-propanediol (3-MCPD) and 1,3-dichloro-2-propanol (1,3-DCP) are not only produced in the manufacturing process of foodstuffs such as hydrolyzed vegetable proteins and soy sauce but are also formed by heat processing in the presence of fat and low water activity. 3-MCPD exists both in free and ester forms, and the ester form has been also detected in various foods. Free 3-MCPD and 1,3-DCP are classified as Group 2B by the International Agency for Research on Cancer. Although there is no data confirming the toxicity of either compound in humans, their toxicity was evidenced in animal experimentation or in vitro. Although few studies have been conducted, free 3-MCPD has been shown to have neurotoxicity, reproductive toxicity, and carcinogenicity. In contrast, 1,3-DCP only has mutagenic activity. The purpose of this study was to analyze 3-MCPD and 1,3-DCP in various foods using gas chromatography -mass spectrometry. 3-MCPD and 1,3-DCP were analyzed using phenyl boronic acid derivatization and the liquid-liquid extraction method, respectively. The analytical method for 3-MCPD and 1,3-DCP was validated in terms of linearity, limit of detection (LOD), limit of quantitation, accuracy and precision. Consequently, the LODs of 3-MCPD and 1,3-DCP in various matrices were identified to be in the ranges of 4.18~10.56 ng/g and 1.06~3.15 ng/g, respectively.

  17. Sonochemical degradation of the pharmaceutical fluoxetine: Effect of parameters, organic and inorganic additives and combination with a biological system

    International Nuclear Information System (INIS)

    Fluoxetine (FLX), one of the most widely used antidepressants in the world, is an emergent pollutant found in natural waters that causes disrupting effects on the endocrine systems of some aquatic species. This work explores the total elimination of FLX by sonochemical treatment coupled to a biological system. The biological process acting alone was shown to be unable to remove the pollutant, even under favourable conditions of pH and temperature. However, sonochemical treatment (600 kHz) was shown to be able to remove the pharmaceutical. Several parameters were evaluated for the ultrasound application: the applied power (20–60 W), dissolved gas (air, Ar and He), pH (3–11) and initial concentration of fluoxetine (2.9–162.0 μmol L−1). Additionally, the presence of organic (1-hexanol and 2-propanol) and inorganic (Fe2+) compounds in the water matrix and the degradation of FLX in a natural mineral water were evaluated. The sonochemical treatment readily eliminates FLX following a kinetic Langmuir. After 360 min of ultrasonic irradiation, 15% mineralization was achieved. Analysis of the biodegradability provided evidence that the sonochemical process transforms the pollutant into biodegradable substances, which can then be mineralized in a subsequent biological treatment. - Highlights: • The pharmaceutical fluoxetine was effectively eliminated upon ultrasonic action. • Ultrasonic power, dissolved gas, pH and concentration of fluoxetine were evaluated. • Fe2+, sodium nitrate or nitric acid had a positive effect on the FLX degradation. • More hydrophobic or volatile compounds than fluoxetine diminished the efficiency. • A sonochemical-biological combined process led to the total mineralization of FLX

  18. Toluene promotes lid 2 interfacial activation of cold active solvent tolerant lipase from Pseudomonas fluorescens strain AMS8.

    Science.gov (United States)

    Yaacob, Norhayati; Mohamad Ali, Mohd Shukuri; Salleh, Abu Bakar; Rahman, Raja Noor Zaliha Raja Abdul; Leow, Adam Thean Chor

    2016-07-01

    The utilization of cold active lipases in organic solvents proves an excellent approach for chiral synthesis and modification of fats and oil due to the inherent flexibility of lipases under low water conditions. In order to verify whether this lipase can function as a valuable synthetic catalyst, the mechanism concerning activation of the lid and interacting solvent residues in the presence of organic solvent must be well understood. A new alkaline cold-adapted lipase, AMS8, from Pseudomonas fluorescens was studied for its structural adaptation and flexibility prior to its exposure to non-polar, polar aprotic and protic solvents. Solvents such as ethanol, toluene, DMSO and 2-propanol showed to have good interactions with active sites. Asparagine (Asn) and tyrosine (Tyr) were key residues attracted to solvents because they could form hydrogen bonds. Unlike in other solvents, Phe-18, Tyr-236 and Tyr-318 were predicted to have aromatic-aromatic side-chain interactions with toluene. Non-polar solvent also was found to possess highest energy binding compared to polar solvents. Due to this circumstance, the interaction of toluene and AMS8 lipase was primarily based on hydrophobicity and molecular recognition. The molecular dynamic simulation showed that lid 2 (residues 148-167) was very flexible in toluene and Ca(2+). As a result, lid 2 moves away from the catalytic areas, leaving an opening for better substrate accessibility which promotes protein activation. Only a single lid (lid 2) showed the movement following interactions with toluene, although AMS8 lipase displayed double lids. The secondary conformation of AMS8 lipase that was affected by toluene observed a reduction of helical strands and increased coil structure. Overall, this work shows that cold active lipase, AMS8 exhibits distinguish interfacial activation and stability in the presence of polar and non-polar solvents. PMID:27474867

  19. PHOTOREDUCTIVE SEQUESTRATION OF CO2 TO FORM C1 PRODUCTS AND FUEL

    Energy Technology Data Exchange (ETDEWEB)

    Theodore Mill; Haruthai Tungudomwongsa

    2003-08-25

    Analytical methods for determining formic, acetic and oxalic acids, formaldehyde, and methanol have been evaluated and/or optimized for measuring products from photoreduction of CO{sub 2} in illuminated, aqueous suspensions of photocatalysts. An electrophoresis anion separation method (CIA) can detect aqueous formate and oxalate ions at 22 and 17 {micro}M (1 ppm), respectively. Recalibration of the Nash formaldehyde determination shows that as little as 10 {micro}M (0.3 ppm) can be detected spectrally. Several experiments using suspensions of Pt/TiO{sub 2}, SrTiO{sub 3}, and SrTiO{sub 3} with Cr and Sb were illuminated in CO{sub 2} saturated solutions. No acids were detected in most experiments using CIA; however, ion chromatography (IC) was able to detect formate and acetate at low {micro}M (sub ppm) concentrations in several experiments using Pt/TiO{sub 2} and SrTiO{sub 3} in sunlight and with xenon uv light. Analysis for methanol by gas chromatography showed that not more than 2 ppm methanol could have formed and probably less. Adding 0.6 mM 2-propanol to an irradiated CO{sub 2}/TiO{sub 2} suspension led to formation of 550 {micro}M formate, but no formaldehyde, probably because re-oxidation of formate by semiconductor holes was competitively blocked. Loss of C{sub 1} products at higher concentrations by re-oxidation may be an important process, limiting the accumulation of products. Preliminary estimates were made of the physical size of a solar CO{sub 2} photoreduction unit large enough to reduce the CO{sub 2} produced from a 1000 MW coal-fired electricity plant. A perfectly efficient system could be as small as 2 to 3 km{sup 2}.

  20. On the swelling properties of proton conducting membranes for direct methanol fuel cells

    Energy Technology Data Exchange (ETDEWEB)

    Saarinen, V.; Kreuer, K.D.; Merkle, R.; Maier, J. [Max-Planck-Institut fuer Festkoerperforschung, Heisenbergstr. 1, D-70569 Stuttgart (Germany); Schuster, M. [FuMA-Tech GmbH, Am Grubenstollen 11, D-66386 St. Ingbert (Germany)

    2007-04-15

    The swelling properties of different fluorinated (Nafion 117, poly(ethylene-alt-tetrafluoroethylene) and poly(vinylidene fluoride)-graft-poly(styrene sulfonic acid)) and hydrocarbon (sulfonated poly(phenylene sulfone)) proton conducting ionomers were investigated in alcohol (MeOH, EtOH, 2-propanol, tBuOH)-water and H{sub 2}SO{sub 4}-water mixtures. Solvent uptake and its water/alcohol selectivity were determined by thermal desorption using combined thermogravimetry (TGA) and mass spectrometry (MS). Clear trends are observed for the selectivity: preferential water uptake (alcohol rejection) correlates with high IEC (ion exchange capacity) and low solvent uptake (swelling) indicating a preferred interaction of the ionic groups (-SO{sub 3}{sup -}, H{sup +}) and the groups on the polymerbackbone carrying partial charges (e.g. sulfone units (-SO{sub 2}-) in the sulfonated poly(phenylene sulfone)) with water. The total swelling significantly decreases in the presence of H{sub 2}SO{sub 4} indicating osmosis being a major driving force in the swelling process. This is particularly low for ETFE-SA, which is highlighting its supreme mechanical properties and its high selectivity for water uptake (selectivity coefficients up to 10 for {lambda} = 7). Unlike Nafion, which shows high swelling in alcohol-water mixtures and almost no selectivity, high selectivity coefficients (up to 8) are observed for sulfonated poly(phenylene sulfone) even at medium solvent uptake ({lambda} = 12). The total solvent uptake in these highly polar ionomers even decreases with methanol mole fraction and is virtually independent of temperature (up to T = 120 C). Together with the high proton conductivity and high hydrolytic stability reported in the literature, the swelling properties presented in this work are making sulfonated poly(phenylene sulfone) interesting membrane materials for DMFC applications. (author)

  1. Combinatorial synthesis and screening of cancer cell-specific nanomedicines targeted via phage fusion proteins

    Directory of Open Access Journals (Sweden)

    James W. Gillespie

    2015-06-01

    Full Text Available Active tumor targeting of nanomedicines has recently shown significant improvements in the therapeutic activity of currently existing drug delivery systems, such as liposomal doxorubicin (Doxil/Caelyx/Lipodox. Previously, we have shown that isolated pVIII major coat proteins of the fd tet filamentous phage vector, containing cancer cell-specific peptide fusions at their N terminus, can be used as active targeting ligands in a liposomal doxorubicin delivery system in vitro and in vivo. Here, we show a novel major coat protein isolation procedure in 2-propanol that allows spontaneous incorporation of the hydrophobic protein core into preformed liposomal doxorubicin with minimal damage or drug loss while still retaining the targeting ligand exposed for cell-specific targeting. Using a panel of 12 structurally unique ligands with specificity towards breast, lung, and/or pancreatic cancer, we showed the feasibility of pVIII major coat proteins to significantly increase the throughput of targeting ligand screening in a common nanomedicine core. Phage protein-modified Lipodox samples showed an average doxorubicin recovery of 82.8% across all samples with 100% of protein incorporation in the correct orientation (N-terminus exposed. Following cytotoxicity screening in a doxorubicin-sensitive breast cancer line (MCF-7, three major groups of ligands were identified. Ligands showing the most improved cytotoxicity included: DMPGTVLP, ANGRPSMT, VNGRAEAP, and ANDVYLD showing a 25-fold improvement (p < 0.05 in toxicity. Similarly DGQYLGSQ, ETYNQPYL, and GSSEQLYL ligands with specificity towards a doxorubicin-insensitive pancreatic cancer line (PANC-1 showed significant increases in toxicity (2-fold; p < 0.05. Thus, we demonstrated proof-of-concept that pVIII major coat proteins can be screened in significantly higher throughput to identify novel ligands displaying improved therapeutic activity in a desired cancer phenotype.

  2. Chitosan and chitosan chlorhydrate based various approaches for enhancement of dissolution rate of carvedilol

    Directory of Open Access Journals (Sweden)

    Shete Amol S

    2012-12-01

    Full Text Available Abstract Background and the purpose of the study Carvedilol nonselective β-adrenoreceptor blocker, chemically (±-1-(Carbazol-4-yloxy-3-[[2-(o-methoxypHenoxy ethyl] amino]-2-propanol, slightly soluble in ethyl ether; and practically insoluble in water, gastric fluid (simulated, TS, pH 1.1, and intestinal fluid (simulated, TS without pancreatin, pH 7.5 Compounds with aqueous solubility less than 1% W/V often represents dissolution rate limited absorption. There is need to enhance the dissolution rate of carvedilol. The objective of our present investigation was to compare chitosan and chitosan chlorhydrate based various approaches for enhancement of dissolution rate of carvedilol. Methods The different formulations were prepared by different methods like solvent change approach to prepare hydrosols, solvent evaporation technique to form solid dispersions and cogrind mixtures. The prepared formulations were characterized in terms of saturation solubility, drug content, infrared spectroscopy (FTIR, differential scanning calorimetry (DSC, powder X-ray diffraction (PXRD, electron microscopy, in vitro dissolution studies and stability studies. Results The practical yield in case of hydrosols was ranged from 59.76 to 92.32%. The drug content was found to uniform among the different batches of hydrosols, cogrind mixture and solid dispersions ranged from 98.24 to 99.89%. There was significant improvement in dissolution rate of carvedilol with chitosan chlorhdyrate as compare to chitosan and explanation to this behavior was found in the differences in the wetting, solubilities and swelling capacity of the chitosan and chitosan salts, chitosan chlorhydrate rapidly wet and dissolve upon its incorporation into the dissolution medium, whereas the chitosan base, less water soluble, would take more time to dissolve. Conclusion This technique is scalable and valuable in manufacturing process in future for enhancement of dissolution of poorly water soluble

  3. Deuterium isotopic effects connected with unimolecular and concerted mechanisms. The case of 1-deutero-2-chloro alcohols; Effets isotopiques du deuterium attaches a des mecanismes unimoleculaires et concertes. Cas des deutero-1-chloro-2 alcools

    Energy Technology Data Exchange (ETDEWEB)

    Jambon, C

    1962-07-01

    After a bibliographic analysis of the probable causes of isotopic effects and their comparison, with the simplifications provided by the athermal model, a discussion of the isotopic effect of deuterium in organic molecules in terms of structural influences is presented, showing the important role of the C-D bond length which is shorter than the C-H bond length, and of the D atom's Van der Waals radius, shorter than that of the H atom. Kinetic measurements were carried out on some reactions involving the mechanisms proposed: unimolecular ionizations and halogen concentrates. The structural models chosen are: 2-chloro-cyclo-hexanols cis and trans 1-H and 2-D; 2-chloro-cyclo-pentanols cis trans 1-H and 1-D; 1-phenyl-l-chloro-2-propanol threo 2-H and 2-D. (author) [French] Apres une analyse bibliographique des causes probables d'effets isotopiques et leur comparaison, avec les simplifications qu'apporte le modele athermique, on a entrepris l'etude de la discussion isotopique du deuterium dans des molecules organiques en termes d'influences structurelles, cherchant a degager le role important de la longueur de la liaison C-D plus courte que C-H, et du rayon de Van der Waals de l'atome de D plus petit que celui de H. On a effectue des mesures cinetiques sur quelques reactions invoquant les mecanismes envisages: ionisations unimoleculaires et concentrees d'halogenes. Les modeles structuraux choisis sont: chloro 2 - cyclohexanols cis et trans H 1 et D 1; chloro 2 - cyclopentanols cis et trans H 1 et D 1; phenyl 1 - chloro 1 - propanol 2 threo H 2 et D 2. (auteur)

  4. Pharmacokinetics of mitomycin C in dogs: application of a high-performance liquid chromatographic assay.

    Science.gov (United States)

    Barbhaiya, R H; Papp, E A; Van Harken, D R; Smyth, R D

    1984-09-01

    A normal-phase high-performance liquid chromatographic (HPLC) assay was developed for the determination of mitomycin C in plasma and urine. The method involves extraction of mitomycin C from plasma or urine into ethyl acetate-2-propanol-chloroform (70:15:15) with UV detection at 365 nm. Quantitation was performed with an internal standard (porfiromycin) by the peak height ratio method. Excellent correlation was obtained between the HPLC assay and the established microbiological cup-plate bioassay. The pharmacokinetics of mitomycin C were investigated in beagle dogs following a 1-mg/kg iv (22-mg/m2) bolus dose. The plasma mitomycin C concentration versus time data were analyzed by using an open three-compartment model. The average volume of distribution was 1.90 L or 17% of body weight for the central compartment and 7.7 L or 68% of body weight for the terminal elimination phase. The volumes of distribution at steady state, calculated by model-dependent and -independent methods, compared very well with each other and were 6.5 L or 58% of body weight. Total body clearance averaged 112 mL/min, and the mean terminal plasma half-life was 53 min. The 0-24-h urinary excretion of intact mitomycin C accounted for 19% of the dose. The terminal half-life and percent urinary recovery of mitomycin C in dogs is similar to that in humans. Based on these observations, the dog appears to be a good model for studying the disposition of mitomycin C. PMID:6436466

  5. Hypoxia-dependent retinal toxicity of bioreductive anticancer prodrugs in mice.

    Science.gov (United States)

    Lee, A E; Wilson, W R

    2000-02-15

    The bioreductive anticancer prodrug CI-1010 ((2R)-1-[(2-bromoethyl)amino]-3-(2-nitro-1H-imidazol-1-yl)-2-propanol hydrobromide) is an alkylating nitroimidazole which shows selective toxicity against hypoxic cells in murine tumors, but causes extensive apoptosis in the outer retina in rodents and monkeys. This irreversible retinal toxicity has terminated preclinical development of CI-1010. We have investigated whether such toxicity is due to physiological hypoxia in the retina, and whether it is a general feature of hypoxia-selective bioreductive drugs. Retinal damage was quantified by morphometric analysis of histological sections following treatment of female C57Bl6 mice. Both CI-1010 and tirapazamine (TPZ, 1,2,4-benzotriazin-3-amine 1,4-dioxide), a bioreductive drug in Phase III clinical trial, caused a time and dose-dependent loss of photoreceptor cells of the outer retina following administration of single intraperitoneal doses. The lesion caused by TPZ was qualitatively similar to that with CI-1010, but was less severe at equivalent fractions of the maximum tolerated dose (as defined by lethality). With both bioreductive drugs, lesion severity was increased if animals breathed 10% O(2) for 3 h after drug administration, while breathing 95% O(2)/5% CO(2) was protective. Other hypoxia-selective bioreductive drugs tested (the quinone porfiromycin, the anthraquinone N-oxide AQ4N and the nitrogen mustard prodrugs SN 23816 and SN 25341) did not cause retinal damage at their maximum tolerated doses. This study suggests that the retinal toxicity of bioreductive drugs might be avoided by manipulation of tissue hypoxia using 95% O(2)/5% CO(2), although this intervention could suppress antitumor activity. The finding that not all bioreductive drugs cause retinal toxicity suggests this toxicity can be avoided through appropriate drug design. PMID:10662604

  6. Alcohol dispersions of calcium hydroxide nanoparticles for stone conservation.

    Science.gov (United States)

    Rodriguez-Navarro, Carlos; Suzuki, Amelia; Ruiz-Agudo, Encarnacion

    2013-09-10

    Alcohol dispersions of Ca(OH)2 nanoparticles, the so-called nanolimes, are emerging as an effective conservation material for the consolidation of stone, mortars, and plasters present in old masonry and/or mural paintings. To better understand how this treatment operates, to optimize its performance and broaden its applications, here we study the nano and microstructural characteristics, carbonation behavior, and consolidation efficacy of colloidal alcohol dispersions of Ca(OH)2 nanoparticles produced by both homogeneous (commercial nanolime) and heterogeneous phase synthesis (aged slaked lime and carbide lime putties). We observe that the alcohol not only provides a high colloidal stability to Ca(OH)2 particles, but also affects the kinetics of carbonation and CaCO3 polymorph selection. This is due to the pseudomorphic replacement of Ca(OH)2 particles by calcium alkoxides upon reaction with ethanol or 2-propanol. The extent of this replacement reaction depends on Ca(OH)2 size and time. Hydrolysis of alkoxides speeds up the carbonation process and increases the CaCO3 yield. The higher degree of transformation into calcium alkoxide of both the commercial nanolime and the carbide lime fosters metastable vaterite formation, while calcite precipitation is promoted upon carbonation of the aged slaked lime due its lower reactivity, which limits calcium alkoxide formation. A higher consolidation efficacy in terms of strength gain of treated porous stone is achieved in the latter case, despite the fact that the carbonation is much faster and reaches a higher yield in the former ones. Formation of alkoxides, which has been neglected in previous studies, needs to be considered when applying nanolime treatments. These results show that the use Ca(OH)2 nanoparticle dispersions prepared with either aged slaked lime or carbide lime putties is an economical and effective conservation alternative to commercial nanolimes produced by homogeneous phase synthesis. Ultimately, this

  7. Wetting transition and pretransitional thin films in binary liquids: alcohol/perfluoromethylcyclohexane mixtures studied by x-ray reflectivity

    International Nuclear Information System (INIS)

    In this study the wetting transition at the liquid-vapour interface of binary organic liquid mixtures has been investigated by x-ray reflectivity. Mixtures of various isomeric alcohols with perfluoromethylcyclohexane (PFMC) served as model systems, with alcohol carbon numbers ranging from 1 to 4. Remarkably different pretransitional behaviour of the thin films below the wetting temperature was observed, which could be classified according to the carbon number. At two-phase coexistence, no pretransitional thin films could be detected for methanol and ethanol, whereas thin-to-thick-film transitions were found for propanol and butanol and their isomers. For 1-propanol and 2-propanol, the surface of the upper, alcohol-rich phase of the gravity-separated mixture displays a wetting transition at Tw = 31.5 deg. C and 38.3 deg. C, respectively, where the thickness of a PFMC-rich film jumps from less than 25 A to values exceeding the experimental resolution of about 1200 A. For 1-butanol, 2-butanol and i-butanol, we found pretransitional film thicknesses increasing up to 100 A, with wetting transitions at Tw = 45.0 deg. C, 34.2 deg. C and 40.1 deg. C, respectively. In the single-phase region, the study of adsorption isotherms above Tw revealed novel behaviour of the adsorbed PFMC-rich film. We observed both a growing film thickness and a significantly changing composition as the coexistence line was approached. Nevertheless, the variation of the excess adsorption with distance from coexistence could still be described by a power law. (author)

  8. Evaluation of salicylic acid fatty ester prodrugs for UV protection.

    Science.gov (United States)

    Im, Jong Seob; Balakrishnan, Prabagar; Oh, Dong Hoon; Kim, Jung Sun; Jeon, Eun-Mi; Kim, Dae-Duk; Yong, Chul Soon; Choi, Han-Gon

    2011-07-01

    The purpose of this study was to investigate the physicochemical properties and in vitro evaluation of fatty ester prodrugs of salicylic acid for ultraviolet (UV) protection. The physicochemical properties such as lipophilicity, chemical stability and enzymatic hydrolysis were investigated with the following fatty ester prodrugs of salicylic acid: octanoyl (C8SA), nonanoyl (C9SA), decanoyl (C10SA), lauroyl (C12SA), myristoyl (C14SA) and palmitoyl oxysalicylate (C16SA). Furthermore, their skin permeation and accumulation were evaluated using a combination of common permeation enhancing techniques such as the use of a lipophilic receptor solution, removal of stratum corneum and delipidization of skin. Their k' values were proportional to the degree of carbon-carbon saturation in the side chain. All these fatty esters were highly stable in 2-propanol, acetonitrile and glycerin, but unstable in methanol and ethanol. They were relatively unstable in liver and skin homogenates. In particular, C16SA was mostly hydrolyzed to its parent compound in hairless mouse liver and skin homogenates, suggesting that it might be converted to salicylic acid after its topical administration. In the skin permeation and accumulation study, C16SA showed the poorest permeation in all skins, suggesting that it could not be permeated in the skin. Furthermore, C14SA and C16SA were less accumulated in delipidized skin compared with normal skin or stripped skin, suggesting that these esters had relatively strong affinities for lipids compared with the other prodrugs in the skin. C16SA showed significantly higher dermal accumulation in all skins compared with its parent salicylic acid. Thus, the palmitoyl oxysalicylate (C16SA) might be a potential candidate for UV protection due to its absence of skin permeation, smaller uptake in the lipid phase and relatively lower skin accumulation.

  9. Preparation of PtSnCu/C and PtSn/C electrocatalysts and activation by dealloying processes for ethanol electrooxidation

    International Nuclear Information System (INIS)

    PtSnCu/C (with different Pt:Sn:Cu atomic ratios) and PtSn/C (50:50) electrocatalysts were prepared by borohydride (BR) and alcohol-reduction (AR) processes using H2PtCl6.6H2O, SnCl2.2H2O and CuCl2.2H2O as metal sources, NaBH4 and ethylene glycol as reducing agents, 2-propanol and ethylene glycol/water as solvents and carbon black as support. In a further step, these electrocatalysts were activated by chemical (CD) and electrochemical (ED) dealloying processes through acid treatment and thin porous coating technique, respectively. These materials were characterized by energy dispersive X-ray, Xray diffraction, transmission electron microscopy, line scan energy dispersive Xray and cyclic voltammetry. Electrochemical studies for ethanol electro-oxidation were performed by cyclic voltammetry, chronoamperometry and in single Direct Ethanol Fuel Cell using Membrane Electrode Assembly (MEA). The anodic effluents were analysed by gas chromatography. The X-ray diffractograms of the as-synthesized electrocatalysts showed the typical face-centered cubic structure (FCC) of platinum and its alloys. After dealloying, the X-ray diffractograms showed that the Pt FCC structure was preserved. The crystallite sizes of the assynthesized electrocatalysts were in the range of PtSnCu/C (50:40:10) AR/ED > PtSnCu/C (50:10:40) BR/CD. PtSn/C (50:50) BR/CD, PtSnCu/C (50:10:40) BR/CD, PtSnCu/C (50:40:10) AR/CD electrocatalysts and Pt/C BASF, PtSn/C (75:25) BASF commercial electrocatalysts were tested in single Direct Ethanol Fuel Cell. The results showed the following performance for ethanol electro-oxidation: PtSn/C (50:50) BR/CD > PtSnCu/C (50:40:10) AR/CD > PtSnCu/C > PtSn/C (75:25) BASF > PtSnCu/C (50:10:40) BR/CD > Pt/C BASF. (author)

  10. Incipient flocculation molding: A new ceramic-forming technique

    Science.gov (United States)

    Arrasmith, Steven Reade

    Incipient Flocculation Molding (IFM) was conceived as a new near-net-shape forming technique for ceramic components. It was hypothesized that the development of a temperature-dependent deflocculant would result in a forming technique that is flexible, efficient, and capable of producing a superior microstructure with improved mechanical properties from highly reactive, submicron ceramic powders. IFM utilizes a concentrated, nonaqueous, sterically stabilized ceramic powder and/or colloidal suspension which is injected into a non-porous mold. The suspension is then flocculated by destabilizing the suspension by lowering the temperature. Flocculation is both rapid and reversible. Cooling to -20°C produces a green body with sufficient strength for removal from the mold. The solvent is removed from the green body by evaporation. The dried green body is subsequently sintered to form a dense ceramic monolith. This is the first ceramic forming method based upon the manipulation of a sterically-stabilized suspension. To demonstrate IFM, the process of grafting polyethylene glycol (PEG), with molecular weights from 600 to 8000, to alumina powders was investigated. The maximum grafted amounts were achieved by the technique of dispersing the alumina powders in molten polymer at 195°C. The ungrafted PEG was then removed by repeated centrifuging and redispersion in fresh distilled water. The rheological behavior of suspensions of the PEG-grafted powders in water, 2-propanol and 2-butanol were characterized. All of the aqueous suspensions were shear thinning. The PEG 4600-grafted alumina powder aqueous suspensions were the most fluid. Sample rods and bars were molded from 52 vol% PEG-grafted alumina suspensions in 2-butanol. The best results were obtained with a preheated aluminum mold lubricated with a fluorinated oil mold-release. The samples were dried, sintered, and their microstructure and density were compared with sintered samples dry pressed from the same alumina powder

  11. Optimization and application of methods of triacylglycerol evaluation for characterization of olive oil adulteration by soybean oil with HPLC-APCI-MS-MS.

    Science.gov (United States)

    Fasciotti, Maíra; Pereira Netto, Annibal D

    2010-05-15

    Triacylglycerols (TAGs) are the main constituents of vegetable oils where they occur in complex mixtures with characteristic distributions. Mass spectrometry using an atmospheric pressure chemical ionization interface (APCI-MS) run in positive mode and an Ion Trap mass analyser were applied in the study of olive and soybean oils and their mixtures. Direct injections of soybean and olive oil solutions allowed the identification of ions derived from the main TAGs of both oils. This procedure showed to be a simple and powerful tool to evaluate mixtures or addition of soybean to olive oil. TAG separation was optimized by high performance liquid chromatography (HPLC) using an octadecylsilica LiChrospher column (250mm x 3mm; 5microm) and a gradient composed of acetonitrile and 2-propanol allowed the separation of the main TAGs of the studied oils. APCI vaporization temperature was optimized and best signals were obtained at 370 degrees C. Multiple reaction monitoring (MRM) employing the transition of the protonated TAG molecules ([M+H](+)) to the protonated diacylglycerol fragments ([M+H-R](+)) improved the selectivity of TAG detection and was used in quantitative studies. Different strategies were developed to evaluate oil composition following TAG analysis by MRM. The external standard calibration and standard additions methods were compared for triolein quantification but the former showed to be biased. Further quantitative studies were based on the estimates of soybean and olive oil proportions in mixtures by comparison of TAG areas found in mixtures of known and unknown composition of both oils. Good agreement with expected or labeled values was found for a commercial blend containing 15% (w/w) of olive oil in soybean oil and to a 1:1 mixture of both oils, showing the potential of this method in characterizing oil mixtures and estimating oil proportions. Olive oils of different origins were also evaluated by mass spectra data obtained after direct injections of oil

  12. Is it homogeneous or heterogeneous catalysis derived from [RhCp*Cl2]2? In operando XAFS, kinetic, and crucial kinetic poisoning evidence for subnanometer Rh4 cluster-based benzene hydrogenation catalysis.

    Science.gov (United States)

    Bayram, Ercan; Linehan, John C; Fulton, John L; Roberts, John A S; Szymczak, Nathaniel K; Smurthwaite, Tricia D; Özkar, Saim; Balasubramanian, Mahalingam; Finke, Richard G

    2011-11-23

    Determining the true, kinetically dominant catalytically active species, in the classic benzene hydrogenation system pioneered by Maitlis and co-workers 34 years ago starting with [RhCp*Cl(2)](2) (Cp* = [η(5)-C(5)(CH(3))(5)]), has proven to be one of the most challenging case studies in the quest to distinguish single-metal-based "homogeneous" from polymetallic, "heterogeneous" catalysis. The reason, this study will show, is the previous failure to use the proper combination of: (i) in operando spectroscopy to determine the dominant form(s) of the precatalyst's mass under catalysis (i.e., operating) conditions, and then crucially also (ii) the previous lack of the necessary kinetic studies, catalysis being a "wholly kinetic phenomenon" as J. Halpern long ago noted. An important contribution from this study will be to reveal the power of quantitiative kinetic poisoning experiments for distinguishing single-metal, or in the present case subnanometer Rh(4) cluster-based catalysis, from larger, polymetallic Rh(0)(n) nanoparticle catalysis, at least under favorable conditions. The combined in operando X-ray absorption fine structure (XAFS) spectroscopy and kinetic evidence provide a compelling case for Rh(4)-based, with average stoichiometry "Rh(4)Cp*(2.4)Cl(4)H(c)", benzene hydrogenation catalysis in 2-propanol with added Et(3)N and at 100 °C and 50 atm initial H(2) pressure. The results also reveal, however, that if even ca. 1.4% of the total soluble Rh(0)(n) had formed nanoparticles, then those Rh(0)(n) nanoparticles would have been able to account for all the observed benzene hydrogenation catalytic rate (using commercial, ca. 2 nm, polyethyleneglycol-dodecylether hydrosol stabilized Rh(0)(n) nanoparticles as a model system). The results--especially the poisoning methodology developed and employed--are of significant, broader interest since determining the nature of the true catalyst continues to be a central, often vexing issue in any and all catalytic reactions

  13. Effects of acido-basic support properties on the catalytic hydrogenation of acetylene on gold nano-particles

    Science.gov (United States)

    Manda, Abdullah Ahmed

    Metallic gold nanoparticles supported on gamma-Al2O 3 and magnesia-alumina mixed oxide, with different magnesia content have been prepared by sol-gel method and characterized by different techniques (inductive coupled plasma-mass spectroscopy (ICP-MS), XRD, BET surface area analysis, transmission electron microscopy (TEM), CO2 and NH 3 temperature programmed desorption (TPD), H2 temperature programmed reduction (TPR) and FTIR of adsorbed CO2). Such systems were found to produce catalysts with controllable acidity, varying from catalyst possessing large density of acidic and low density of basic sites, others with acidic and basic sites of equal strength and density, and others with large basic and low acid sites densities, respectively. The catalytic assessment of the generated acidity was carried out using 2-propanol decomposition as a test reaction. The results obtained indicate that the presence of magnesia and reduced gold nanopartilces has imparted the catalysts, 1%Au/4%Mg-Al 2O3 and 1%Au/8%Mg-Al2O3, with significant base-catalytic properties. Acetylene hydrogenation and formation of coke deposits were investigated on a gold catalyst supported on gamma-Al2O3 and gold supported on alumina-magnisia mixed oxide with different gold content; 1%Au/gamma-Al 2O3, 1%Au/15%Mg-Al2O3, 2%Au/15%Mg-Al 2O3 and 4%Au/15%Mg-Al2O3. The effect of the H2/C2H2 ratio was studied over a range of values. The catalytic activity and selectivity towards ethylene and other products were investigated at different reaction temperatures. Acetylene hydrogenation was investigated in the presence and absence of ethylene in stream. It is investigated that the adsorption of the triple bond is preferred over the double bond and during selective catalytic (SCR) of C2H2 the two hydrocarbons do not compete for the same adsorption sites. The deactivation of catalysts was studied by temperature programmed oxidation (TPO). Higher content of coke over 1%Au/Al2O3 catalyst was investigated in contrast to

  14. Mechanistic Consequences of Composition in Acid Catalysis by Polyoxometalate Keggin Clusters

    Energy Technology Data Exchange (ETDEWEB)

    Macht, Josef; Janik, Michael J.; Neurock, Matthew; Iglesia, Enrique

    2008-08-06

    The research described in this product was performed in part in the Environmental Molecular Sciences Laboratory, a national scientific user facility sponsored by the Department of Energy's Office of Biological and Environmental Research and located at Pacific Northwest National Laboratory. The kinetics and mechanism of ether and alkanol cleavage reactions on Brønsted acid catalysts based on polyoxometalate (POM) clusters are described in terms of the identity and dynamics of elementary steps and the stability of the transition states involved. Measured rates and theoretical calculations show that the energies of cationic transition states and intermediates depend on the properties of reactants (proton affinity), POM clusters (deprotonation enthalpy), and ion-pairs in transition states or intermediates (stabilization energy). Rate equations and elementary steps were similar for dehydration of alkanols (2- propanol, 1- and 2-butanol, tert-butanol) and cleavage of sec-butyl-methyl ether on POM clusters with different central atoms (P, Si, Co, Al). Dehydration rates depend on the rate constant for elimination from adsorbed alkanols or ethers and on the equilibrium constant for the formation of unreactive reactant dimers. Elimination involves E1 pathways and late carbenium-ion transition states. This is consistent with small kinetic isotope effects for all deuterated alkanols, with strong effects of substituents on elimination rates, and with the similar alkene stereoselectivities measured for alkanol dehydration, ether cleavage, and alkene double-bond isomerization. n-Donor reactants (alkanols, ethers) and products (water) inhibit dehydration rates by forming stable dimers that do not undergo elimination; their stability is consistent with theoretical estimates, with the dynamics of homogeneous analogues, and with the structure and proton affinity of the n-donors. Elimination rate constants increased with increasing valence of the central POM atom, because of a

  15. Comparison of direct infusion and on-line liquid chromatography/electrospray ionization mass spectrometry for the analysis of nucleic acids.

    Science.gov (United States)

    Huber, C G; Krajete, A

    2000-07-01

    The applicability of ion-pair reversed-phase high-performance liquid chromatography/electrospray ionization mass spectrometry (IP-RP-HPLC/ESI-MS) and direct infusion/ESI-MS to the characterization of nucleic acid mixtures was evaluated by the analysis of the reaction products obtained from solid-phase synthesis of a 39-mer oligonucleotide. IP-RP-HPLC/ESI-MS was performed using 200 microm i.d. capillary columns packed with octadecylated, micropellicular poly(styrene-divinylbenzene) particles and applying gradients of acetonitrile in 50 mM triethylammonium bicarbonate (TEAB). Three different solvent systems were utilized for direct infusion/ESI-MS with removal of metal cations by on-line cation exchange: (1) 10 mM triethylamine (TEA) in 50% aqueous acetonitrile, (2) 2.2 mM TEA, 400 mM hexafluoro-2-propanol (HFIP) in 20% aqueous methanol and (3) 50 mM TEAB in 10% aqueous acetonitrile. Owing to its separation capability, the highest selectivity and specificity were achieved with IP-RP-HPLC/ESI-MS, which, apart form the 39-mer target sequence, allowed the identification of two isobutyryl-protected target sequences and a 10-mer and 20-mer failure sequence. Direct infusion/ESI-MS with TEA-acetonitrile or TEA-HFIP-methanol as solvent revealed signals for the 39-mer in the m/z range 700-1600. The presence of derivatives containing one, two, three and four isobutyryl groups indicated that the hydrolysis of the protecting groups after solid-phase synthesis was not complete. Failure sequences could not be identified by direct infusion/ESI-MS under conditions favoring multiple charging of the analytes owing to the high chemical background and coincidental overlapping of m/z signals. However, efficient charge state reduction upon addition of carbonic acid to the electrosprayed solvent shifted the signals of the 39-mer and derivatives to m/z values >2400 and allowed the detection of seven different failure sequences, ranging from the 8-mer to the 23-mer, in the mixture.

  16. Is It Homogeneous or Heterogeneous Catalysis Derived from [RhCp*Cl2]2? In Operando-XAFS, Kinetic and Crucial Kinetic Poisoning Evidence for Subnanometer Rh4 Cluster-Based Benzene Hydrogenation Catalysis

    Energy Technology Data Exchange (ETDEWEB)

    Bayram, Ercan; Linehan, John C.; Fulton, John L.; Roberts, John A.; Szymczak, Nathaniel; Smurthwaite, Tricia D.; Ozkar, Saim; Balasubramanian, Mahalingam; Finke, Richard G.

    2011-11-23

    Determining the true, kinetically dominant catalytically active species, in the classic benzene hydrogenation system pioneered by Maitlis and co-workers 34 years ago starting with [RhCp*Cl2]2 (Cp* = [{eta}5-C5(CH3)5]), has proven to be one of the most challenging case studies in the quest to distinguish single-metal-based 'homogeneous' from polymetallic, 'heterogeneous' catalysis. The reason, this study will show, is the previous failure to use the proper combination of (i) operando spectroscopy to determine the dominant form(s) of the precatalyst's mass under catalysis (i.e., operating) conditions, plus then and crucially also (ii) the previous lack of the necessary kinetic studies, catalysis being a 'wholly kinetic phenomenon' as J. Halpern long ago noted. An important contribution from this study will be to reveal the power of quantitiative kinetic poisoning experiments for distinguishing single-metal, or in this case subnanometer Rh4 cluster-based catalysis from larger, polymetallic Rh(0)n nanoparticle catalysis, at least under favorable conditions. The combined operando-XAFS (X-ray absorption fine structure) spectroscopy and kinetic evidences provide a compelling case for Rh4-based, with average stoichiometry 'Rh4Cp*2.4Cl4Hc', benzene hydrogenation catalysis in 2-propanol with added Et3N and at 100 C and 50 atm initial H2 pressure. The results also reveal, however, that if even ca. 1.4% of the total soluble Rh(0)n had formed nanoparticles, then those Rh(0)n nanoparticles would have been able to account for all the observed benzene hydrogenation catalytic rate (using commercial, ca. 2 nm, polyethyleneglycol-dodecylether hydrosol stabilized Rh(0)n nanoparticles as a model system). The results 'especially the poisoning methodology developed and employed' are of significant, broader interest since determining the nature of the true catalyst continues to be a central, often vexing issue in any and all catalytic

  17. Development of magnetic molecularly imprinted polymers for solid phase extraction of cocaine and metabolites in urine before high performance liquid chromatography - tandem mass spectrometry.

    Science.gov (United States)

    Sánchez-González, Juan; Jesús Tabernero, María; María Bermejo, Ana; Bermejo-Barrera, Pilar; Moreda-Piñeiro, Antonio

    2016-01-15

    A magnetic molecularly imprinted polymer (MMIP) has been synthesized and applied for cocaine (COC) and metabolites (benzoylecgonine, BZE; cocaethylene, CE; and ecgonine methyl ester, EME) recognition/pre-concentration in urine samples. The MMIP has been prepared using COC as a template molecule, ethylene dimethacrylate (EDMA) as a functional monomer, divinylbenzene (DVB) as a cross-linker, Fe3O4 magnetite as a magnetic component, and 2,2'-azobisisobutyronitrile (AIBN) as an initiator. The best results (MIP layer on the surface of the magnetic nanoparticles) and physical properties of the prepared MMIP were obtained when assisting the synthesis procedure with ultrasounds (325W, 37kHz, 30°C, 4h). After solid phase extraction (SPE) with the prepared adsorbent material, analytes were determined by high performance liquid chromatography - tandem mass spectrometry (HPLC-MS/MS). Variables affecting the SPE process (batch mode) were fully evaluated. Optimum retention of analytes (1.8mL of urine and 50mg of MMIP) was achieved by fixing the urine pH at 5.5 (use of a KH2PO4/NaOH, pH 5.5 buffer solution), and magnetic stirring (25°C, 700rpm) for 10min. Elution was performed by using 2mL of a dichloromethane/2-propanol/ammonium hydroxide (75:20:5) mixture under ultrasounds (325W, 35kHz, room temperature) for 5min. The method was validated according to the guidance for bioanalytical method validation of the US Department of Health and Human Services, Food and Drug Administration. The detection limits were in the range of 0.39-1.4ngL(-1). The relative standard deviations of intra- and inter-day tests ranged from 5 to 11% and from 3 to 11%, respectively. Analytical recoveries were in the range of 79-106% when spiking drug-free urine samples at three concentration levels. Good results were also obtained after analyzing an FDT +25% control material. The applicability of the method was proved for screening/quantifying COC, BZE, CE and EME in several samples from poly-drug abusers

  18. L-653,328: an ocular hypotensive agent with modest beta receptor blocking activity

    Energy Technology Data Exchange (ETDEWEB)

    Sugrue, M.F.; Gautheron, P.; Grove, J.; Mallorga, P.; Viader, M.P.; Baldwin, J.J.; Ponticello, G.S.; Varga, S.L.

    1988-05-01

    L-653,328 is the acetate ester of L-652,698 ((S)-3-tert-butylamino-1-(4-(2(hydroxy)ethyl)phenoxy)2-propanol). The penetration of L-652,698 into the albino rabbit eye was enhanced when the compound was instilled as its prodrug acetate ester. The instillation (one drop of 50 microliter) of 0.01, 0.05 and 0.1% solutions of L-653,328 significantly decreased in a dose-dependent manner the elevated intraocular pressure (IOP) of alpha-chymotrypsinized rabbits by 3.2, 4.7 and 6.1 mm Hg, respectively. A 0.01% solution of L-652,698 failed to significantly lower IOP, whereas this dose of timolol (3.8 mm Hg) and betaxolol (3.3 mm Hg) was effective. L-652,698 was active at 0.05% and 0.1%. Extraocular beta-adrenoceptor blockade was quantified in ganglion-blocked, conscious rabbits by determining effects on heart rate and blood pressure changes to i.v. isoproterenol (0.5 microgram/kg). Doses of timolol blocking isoproterenol-induced hypotension and tachycardia by 50% were 0.0065% and 0.03%, respectively. The corresponding doses for betaxolol were greater than 3% (43% inhibition) and 0.3%. Heart rate and blood pressure changes to isoproterenol were blocked by 18 and 36%, respectively, after the instillation of a 3% solution of L-653,328. The reduced propensity of L-653,328 for extraocular beta-adrenoceptor blockade stems from the modest affinity of L-652,698, its active moiety, for beta-adrenoceptors. The Ki values of L-652,698 for displacement of 125I-iodocyanopindolol binding to beta 1-(left ventricle) and beta 2-binding sites (iris + ciliary body) in the rabbit were 5.7 microM and 7.3 microM, respectively. In marked contrast, the corresponding values for timolol were 12 nM and 1.8 nM.

  19. Action of Mercaptan and Disulfide in Hydrogen Atom Exchange Reactions

    International Nuclear Information System (INIS)

    Free- radical, photochemical, and high-energy radiation-induced reactions may be catalysed or inhibited by rapid hydrogen atom exchange reactions of mercaptans and disulfides. The radical-induced, light-initiated, and benzophenone-sensitized decarbonylations of aldehydes are catalysed by mercaptans. The chain-propagating hydrogen transfer reaction, R' + RCH = O -> RH + RC = O , is made more rapid by a similar sequence of hydrogen atom transfers involving the sulfur compound: R' + C6H5CH2SH -> RH + C6H5CH2S'; C6H5CH2S + RCH = 0 -> C6H5CH2SH + RC = 0. The photoreduction of benzophenone in 2-propanol leads to benzpinacol by a non-chain reaction via the radicals (C6H5)2C-OH and (CH3)2COH. The reaction is retarded and inhibited by mercaptan and disulfide, which reconvert the radicals to the starting materials by rapid hydrogen transfer reactions and are themselves regenerated in their alternate valence states, each molecule of sulfur compound negating the chemical consequences of many quanta: (C6H5)2C-OH + AS' -> (C6H5)2C = O + ASH; (CH3)2C-OH + ASH -> (CH3)2C = 0 + AS'. Proof of the mechanism is found in: equilibration of initially present mercaptan or disulfide during inhibition; in racemization of optically active alcohol during inhibition; in deuterium exchange during inhibition. Similar inhibition is seen when only one intermediate radical is formed, as in the benzophenone- benzhydrol and acetophenone-α-methyl-benzyl alcohol systems. Inhibition by sulfur compounds, by the same mechanism, is found in the 60Co γ-ray induced conversion of benzophenone to benzpinacol; naphthalene has no protecting effect on benzophenone in the 60Co system, while quenching the photochemical reaction. The protection by sulfur compounds of solutes against radiation damage thus results from hydrogen atom transfer reactions. The photoreduction of benzophenone in an ether is also inhibited by the sulfur compounds, by hydrogen atom transfer reactions. A mechanism exists in this system

  20. Teores de retinol, beta-caroteno e alfa-tocoferol em leites bovinos comercializados na cidade de São Paulo Amounts of retinol, beta-carotene and alpha-tocopherol in cow milk comercialized in the city of São Paulo

    Directory of Open Access Journals (Sweden)

    Rute BIANCHINI

    1999-12-01

    Full Text Available Os teores de retinol, beta-caroteno e alfa-tocoferol foram determinados por cromatografia líquida de alta eficiência em leites em pó, pasteurizados e esterilizados, comercializados na Cidade de São Paulo. Após a saponificação e extração, os compostos foram determinados simultaneamente utilizando-se coluna de sílica, fase móvel constituída por hexano:isopropanol (99:1 e fluxo de 2,0mL/min. O retinol e o beta-caroteno foram determinados no detector UV/visível e o alfa-tocoferol no detector de fluorescência, ligado em série com o anterior. Os valores de vitamina A dos leites foram calculados com e sem a consideração do beta-caroteno. A maior contribuição deste nutriente no valor de vitamina A esteve entre os leites em pó, cerca de 17% em uma das marcas. Os altos teores das vitamina A e E encontrados em alguns leites, indicam que os mesmos provavelmente receberam adição destas vitaminas, não trazendo, entretanto, tal informação no rótulo. A análise de vitaminas nestes produtos indica a necessidade de maior controle de qualidade dos mesmos.The amount of retinol, beta-carotene, alpha -tocopherol in powder, pasteurized and sterilized milk, comercialized in the city of São Paulo, were analyzed by high performance liquid chromatography. After saponification and extraction, compounds were determined simultaneously through a normal-phase column, mobile phase composed by hexan:2-propanol (99:1 and 2 mL/min flow. The retinol and beta-carotene were analysed by a UV/visible detector and the alpha-tocopherol by a fluorescence detector, both linked in series. The milk vitamin A values were calculated with and without beta-carotene. The major contribution of beta-carotene in the vitamin A value was in powder milks, around 17% in one of the brands. The high amounts of vitamin A and E found in some milks indicate that they probably were enriched with these vitamins but nothing is mentioned about this in their labels. The analysis of

  1. Sustained release of bactericidal concentrations of penicillin in the pleural space via an antibiotic-eluting pigtail catheter coated with electrospun nanofibers: results from in vivo and in vitro studies

    Directory of Open Access Journals (Sweden)

    Chao YK

    2015-05-01

    Full Text Available Yin-Kai Chao,1 Cheng-Hung Lee,2 Kuo-Sheng Liu,1 Yi-Chuan Wang,3 Chih-Wei Wang,4 Shih-Jung Liu3 1Department of Thoracic and Cardiovascular Surgery, Chang Gung Memorial Hospital-Linkou, College of Medicine, Chang Gung University, Taoyuan, Taiwan; 2Division of Cardiology, Department of Internal Medicine, Chang Gung Memorial Hospital-Linkou, College of Medicine, Chang Gung University, Taoyuan, Taiwan; 3Department of Mechanical Engineering, Chang Gung University, Taoyuan, Taiwan; 4Department of Pathology, Chang Gung Memorial Hospital-Linkou, College of Medicine, Chang Gung University, Taoyuan, Taiwan Background: Inadequate intrapleural drug concentrations caused by poor penetration of systemic antibiotics into the pleural cavity is a major cause of treatment failure in empyema. Herein, we describe a novel antibiotic-eluting pigtail catheter coated with electrospun nanofibers used for the sustained release of bactericidal concentrations of penicillin in the pleural space.Methods: Electrospun nanofibers prepared using polylactide-polyglycolide copolymer and penicillin G sodium dissolved in 1,1,1,3,3,3-hexafluoro-2-propanol were used to coat the surface of an Fr6 pigtail catheter. The in vitro patterns of drug release were tested by placing the catheter in phosphate-buffered saline. In vivo studies were performed using rabbits treated with penicillin either intrapleurally (Group 1, 20 mg delivered through the catheter or systemically (Group 2, intramuscular injection, 10 mg/kg. Penicillin concentrations in the serum and pleural fluid were then measured and compared.Results: In vitro studies revealed a burst release of penicillin (10% of the total dose occurring in the first 24 hours, followed by a sustained release in the subsequent 30 days. Intrapleural drug levels were significantly higher in Group 1 than in Group 2 (P<0.001. In the former, penicillin concentrations remained above the minimum inhibitory concentration breakpoint throughout the entire

  2. 甘油合成1,3-丙二醇%Synthesis of 1,3-Propanediol from Glycerol

    Institute of Scientific and Technical Information of China (English)

    陈国辉; 孙全

    2011-01-01

    1,3-Propanediol was synthesized from glycerol by chloration,oxidation, Clemmensen reaction and hydrolysis. The structure of the target compound was determined by method of IR and MS. The molar ratio, temperature and solvent of the reaction were investigated to optimize the reaction conditions. The optimum conditions are: for chloration: 120 ℃; for oxidation: 23 ~ 27 ℃, n ( 1,3-dichloroacetone ): n ( sodium dichromate) = 1.8:1, the amount of reaction solvent: 1.4 g 1,3-dichloro-2-propanol per 1 mL water, and for Clemmensen reaction: n (1,3-dichloropropane): n ( zinc )= 1:1.2, with water as the desirable solvent, and the overall yield of 37. 1%.%以甘油为原料,经过氯代、氧化、克莱门森还原、水解4步反应,最终合成1,3-丙二醇,并用红外光谱仪和质谱仪对目标产物进行结构确定.从反应物摩尔比、反应温度、反应溶剂等优化了反应条件.最优反应条件为:氯代反应:温度120℃;氧化反应:温度23~27℃,,n(1,3-二氯-2-丙醇):n(重铬酸钠)=1.8:1,反应溶剂用量:1 mL水溶解1.4 g 1,3-二氯-2-丙醇;克莱门森还原反应:n(1,3-二氯丙酮):n(锌)=1:1.2,水作反应溶剂最佳,在该条件下,1,3-丙二醇总产率可达37.1%.

  3. Measuring acetic and formic acid by proton transfer reaction-mass spectrometry: sensitivity, humidity dependence, and quantifying interferences

    Directory of Open Access Journals (Sweden)

    M. Baasandorj

    2014-10-01

    Full Text Available We present a detailed investigation of the factors governing the quantification of formic acid (FA, acetic acid (AA and their relevant mass analogues by proton transfer reaction-mass spectrometry (PTR-MS, assess the underlying fragmentation pathways and humidity dependencies, and present a new method for separating FA and AA from their main isobaric interferences. PTR-MS sensitivities towards glycolaldehyde, ethyl acetate and peroxyacetic acid at m/z 61 are comparable to that for AA; when present, these species will interfere with ambient AA measurements by PTR-MS. Likewise, when it is present, dimethyl ether can interfere with FA measurements. On the other hand, for E/N = 125 Townsend (Td, the PTR-MS sensitivity towards ethanol at m/z 47 is 5–20× lower than for FA; ethanol will then only be an important interference when present in much higher abundance than FA. Sensitivity towards 2-propanol is m/z 79, which is also commonly used to measure benzene. However, the resulting interference for benzene is only significant when E/N is low (E/N, but decreases with humidity at high E/N due to water-driven fragmentation. Sensitivity towards FA decreases with humidity throughout the full range of E/N. For glycoaldehyde and the alcohols, the sensitivity increases with humidity due to ligand switching reactions (at low E/N and reduced fragmentation in the presence of water (at high E/N. Their role as interferences will typically be greatest at high humidity. For compounds such as AA where the humidity effect depends strongly on the collisional energy in the drift tube, simple humidity correction factors (XR will only be relevant for a specific instrumental configuration. We recommend E/N∼125 Td as an effective condition for AA and FA measurements by PTR-MS, as it optimizes between the competing E/N-dependent mechanisms controlling their sensitivities and those of the interfering species. Finally, we present the design and evaluation of an online acid

  4. 变形杆菌属脂肪酶LipK107的分离纯化、结晶及初步晶体学分析%Purification,crystallization and preliminary crystallographic analysis of a lipase from Proteus sp.K107

    Institute of Scientific and Technical Information of China (English)

    戚宝杰; 刘清海; 谢静莉; 魏东芝

    2012-01-01

    After induced by IPTG,the recombinant E.coli expressed Lipase LipK107 as HisX6 fusion protein.High purity enzyme was obtained by affinity chromatography and gel filtration chromatography.Purified lipase was analyzed by circular dichrosim(CD)in order to reveal the secondary structure composition of lipase LipK107.Then,purified lipase was crystallized by the hanging-drop vapour-diffusion method.High quality crystals were obtained using 0.1mol/L sodium citrate tribasic dihydrate pH6.2,10% v/v 2-propanol,15% w/v polyethylene glycol 4000 as precipitant.X-ray diffraction data was collected to 2.0 using synchrotron radiation.%经过异丙基-β-D-硫代吡喃半乳糖苷(IPTG)诱导,重组大肠杆菌高效表达出带有组氨酸标签的可溶性脂肪酶LipK107。通过亲和层析和凝胶层析两步法纯化,得到电泳纯的脂肪酶样品。在获得的纯酶基础上,进行了圆二色谱实验,以分析脂肪酶LipK107的二级结构组成。接着,使用悬滴气相扩散法进行了纯酶的结晶实验,经过晶体生长条件的初步筛选及优化,在0.1mol/L pH6.2柠檬酸钠,10%v/v异丙醇,15%w/v聚乙二醇4000条件下得到高质量的脂肪酶晶体,使用同步辐射光源收集了一套分辨率为2.0的X-射线衍射数据。

  5. Osmium pyme complexes for fast hydrogenation and asymmetric transfer hydrogenation of ketones.

    Science.gov (United States)

    Baratta, Walter; Ballico, Maurizio; Del Zotto, Alessandro; Siega, Katia; Magnolia, Santo; Rigo, Pierluigi

    2008-01-01

    The osmium compound trans,cis-[OsCl2(PPh3)2(Pyme)] (1) (Pyme=1-(pyridin-2-yl)methanamine), obtained from [OsCl2(PPh3)3] and Pyme, thermally isomerizes to cis,cis-[OsCl2(PPh3)(2)(Pyme)] (2) in mesitylene at 150 degrees C. Reaction of [OsCl2(PPh3)3] with Ph2P(CH2)(4)PPh2 (dppb) and Pyme in mesitylene (150 degrees C, 4 h) leads to a mixture of trans-[OsCl2(dppb)(Pyme)] (3) and cis-[OsCl2(dppb)(Pyme)] (4) in about an 1:3 molar ratio. The complex trans-[OsCl2(dppb)(Pyet)] (5) (Pyet=2-(pyridin-2-yl)ethanamine) is formed by reaction of [OsCl2(PPh3)3] with dppb and Pyet in toluene at reflux. Compounds 1, 2, 5 and the mixture of isomers 3/4 efficiently catalyze the transfer hydrogenation (TH) of different ketones in refluxing 2-propanol and in the presence of NaOiPr (2.0 mol %). Interestingly, 3/4 has been proven to reduce different ketones (even bulky) by means of TH with a remarkably high turnover frequency (TOF up to 5.7 x 10(5) h(-1)) and at very low loading (0.05-0.001 mol %). The system 3/4 also efficiently catalyzes the hydrogenation of many ketones (H2, 5.0 atm) in ethanol with KOtBu (2.0 mol %) at 70 degrees C (TOF up to 1.5 x 10(4) h(-1)). The in-situ-generated catalysts prepared by the reaction of [OsCl2(PPh3)3] with Josiphos diphosphanes and (+/-)-1-alkyl-substituted Pyme ligands, promote the enantioselective TH of different ketones with 91-96 % ee (ee=enantiomeric excess) and with a TOF of up to 1.9 x 10(4) h(-1) at 60 degrees C.

  6. Structure based protein engineering of Bacillus stearothermophilus α-amylase: toward a new substrate specificity

    International Nuclear Information System (INIS)

    Full text. Structural similarity is observed in all members of α-amylase family but different products are generated during hydrolysis of starch due to different affinities for intermediate dextrins. In order to understand the structural determinants for this property and to introduce different specificity to α-amylase of Bacillus stearothermophilus we intend to solve the three dimensional structure by X-ray crystallography of the native protein by using synchrotron radiation at Brazilian National Synchrotron Light Laboratory (LNLS). Protein was over expressed in E. coli, purified and crystallization experiments were carried out by using sparse matrix Crystal Screen and Crystal Screen II from Hampton Research (Laguna Hills, CA, USA). Several condition have produced crystals with some defined characteristic: MDP seems to be important to the crystallization: the preferential pH is around 7.5 with organic buffer (HEPES); organic solvent as 2-propanol seems to be also important for the crystallization. On those condition crystals appeared as cluster of needles or small crystals with high number of nucleation. New conditions are being prepared to improve the site and quality of crystals. Data collection of native of Bacillus stearothermophilus α-amylase will e done at Protein Crystallography Station at LNLS. Crystal structure of mutated α-amylase bu site direct mutagenesis of residues suggested by the native crystal structure will be obtained. Co-crystallization of Bacillus stearothermophilus α-amylase and oligosaccharide will be carried out to identify residues involved in the binding site to plan new mutation. In another series of mutation the putative binding site residues, once identified, will be mutated to residues observed in TAKA amylase to confer different specificity to α-amylase. Based on the available TAKA amylase structure, in the primary sequence homology and in the three dimensional model of Bacillus stearothermophilus α-amylase (using Bacillus

  7. NaBr, NaCl和KBr在几种有机溶剂中活度系数的测定%Activity Coefficient Measurement of NaBr, NaCl and KBr in Selected Organic Solvents

    Institute of Scientific and Technical Information of China (English)

    姜波; 王利生; 李弥异

    2011-01-01

    In this paper, the conductivities of NaBr in methanol, ethanol, 1-propanol, 2-propanol, NaC1 and KBr in methanol, ethanol system (solution concentration within 0. 1 mol· L-1 ) were determined at 298.15 K, 313.15 K and 323.15 K at atmosphere pressure respectively. The mean ion activity coefficients of NaBr, NaC1 and KBr in various organic solvents were calculated according to DebyeHacker limiting law and Onsager-Falkenhangen equations. The effects of concentration and temperature on activity coefficients of electrolyte solutions were discussed. The calculated results were compared with those of NaBr in ethanol, NaC1 in methanol and KBr in methanol reported in literature. The results show that the experimental data obtained by conductivity method have good agreement with data in literature.%分别测定了NaBr在甲醉、乙醇、正丙醉和异丙醇中,NaCI和KBr在甲醉和乙醉中共8个体系(溶液物质的量的浓度在0.1 mol·L(-1)范围内)在298.15,313.15和323.15 K下的电导率,利用Debye-Hiicker和Osager-Falkenhangen公式计算了以上溶液体系的平均离子活度系数,讨论了浓度和温度对电解质溶液活度系数的影响.其中NaBr在乙醇中,NaCI在甲醉中和KBr在甲醇中的平均离子活度系数的计算结果与已发表文献中的数据进行了比较.结果表明,该方法的活度系数结果与文献数据有较好的一致性.

  8. Influence of electrospinning on microstructure of regenerated Argiope bruennichi silk%静电纺再生加工对横纹金珠丝微观结构的影响

    Institute of Scientific and Technical Information of China (English)

    裔婷婷; 潘志娟

    2012-01-01

    蜘蛛丝因其优异的力学性能和良好的生物相容性引起了学者的广泛关注.为此在研究横纹金珠丝在六氟异丙醇(HFIP)中溶解性能的基础上,采用静电纺丝的方法制备再生横纹金珠丝(框丝、卵袋内层丝、卵袋外层丝),分析比较再生横纹金蛛丝和天然横纹金蛛丝在形态结构、分子构象、结晶结构以及热稳定性方面的差异.结果发现:静电纺再生框丝呈扁平带状,带宽为(751±196) nm,卵袋内层丝和卵袋外层丝直径分别为(141±46) nm和(105±37)nm.X衍射图谱和TG-DTA测定结果表明,静电纺再生加工后,横纹金珠丝结构由silkⅡ向silk Ⅰ转变,结晶度下降,主要热分解温度降低.%Spider silk has attracted wide attentions of scholars and researchers due to its excellent mechanical properties and good biocompatibility in recent years. The regenerated Argiope bruennichi silk ( scaffolding silk, egg case inner cover silk, egg case outer cover silk) was prepared by electrospinning on the basis of studying the solubility of Argiope bruennichi silk in 1,1,1,3 ,3 ,3-hexafluoro-2-propanol (HFIP). The morphology, molecular conformation, crystallinity and thermal property of the natural Argiope bruennichi silk and the electrospun Argiope bruennichi silk were compared. The results indicated the electrospun regenerated Argiope bruennichi silk was flat ribbon with the bandwidth ( 751 ± 196 ) nm and a diameter of egg case inner cover silk and egg case outer cover silk (141 ±46) nm and ( 105 ± 37) nm, respectively. The XRD and TG-DTA analysis showed that the crystal structure of electrospun Argiope bruennichi silk has changed from silk II to silk I , and the crystallinity and main thermal decomposition temperature decreased.

  9. Hydroxyl radical-related electrogenerated chemiluminescence reaction for a ruthenium tris(2,2')bipyridyl/co-reactants system at boron-doped diamond electrodes

    Energy Technology Data Exchange (ETDEWEB)

    Honda, K. [Department of Chemistry and Earth Sciences, Faculty of Science Yamaguchi University, 1677-1 Yoshida, Yamaguchi-shi, Yamaguchi 753-8512 (Japan)]. E-mail: khonda@yamaguchi-u.ac.jp; Yamaguchi, Y. [Department of Chemistry and Earth Sciences, Faculty of Science Yamaguchi University, 1677-1 Yoshida, Yamaguchi-shi, Yamaguchi 753-8512 (Japan); Yamanaka, Y. [Department of Chemistry and Earth Sciences, Faculty of Science Yamaguchi University, 1677-1 Yoshida, Yamaguchi-shi, Yamaguchi 753-8512 (Japan); Yoshimatsu, M. [Department of Chemistry and Earth Sciences, Faculty of Science Yamaguchi University, 1677-1 Yoshida, Yamaguchi-shi, Yamaguchi 753-8512 (Japan); Fukuda, Y. [Department of Chemistry and Earth Sciences, Faculty of Science Yamaguchi University, 1677-1 Yoshida, Yamaguchi-shi, Yamaguchi 753-8512 (Japan); Fujishima, A. [Kanagawa Academy of Science and Technology (KAST), 3-2-1, Sakato, Takastu-ku, Kawasaki-shi, Kanagawa 213-0012 (Japan)

    2005-11-01

    An electrogenerated chemiluminescence (ECL) reaction of the Ru(bpy){sub 3} {sup 2+} (2,2'-bipyridyl, bpy)/co-reactant system in the extremely high-potential region (over 2.6 V versus Ag/AgCl) was probed using a boron-doped diamond (BDD) electrode. At the BDD electrode, three ECL waves (1.25, 2.30 and 3.72 V) were observed in cyclic voltammograms for 20 mM ascorbic acid (AA). For the ECL peaks observed at 1.25 V corresponding to the oxidation potential for Ru(bpy){sub 3} {sup 2+} (1.15 V), the light intensities and current densities were found to depend on the square root of the AA concentration. This suggests that AA oxidation, followed by the formation of the reducing radical that is necessary for generating the excited state of Ru(bpy){sub 3} {sup 2+*} occurred through homogeneous electron-transfer between Ru(bpy){sub 3} {sup 3+} and the AA species. However, for the ECL peaks at 2.30 V, the current densities and light intensities linearly increased with increasing AA concentration, suggesting that the reducing radical was formed through the direct oxidation at the electrode surface. The ECL reaction at 3.72 V was observed only at the BDD electrode and not at other electrodes. The onset potentials for the light intensity were approximately 2.6 V, independently of the type of the co-reactants (e.g. 2-propanol and AA). The peak potentials exhibited linear relation with the co-reactant concentration. In the analysis of the ECL intensity for various co-reactants (alcohols) that show different reactivity for the hydrogen abstraction reaction, the order of the light intensities at the peaks for alcohols was found to be consistent with that for the rate constants of the hydrogen abstraction reaction. These results indicate that the co-reactant radical was formed through the hydrogen abstraction reaction with the hydroxyl radical (HO{center_dot}) generated during the oxygen evolution reaction.

  10. High Throughput Approach Applied to VOC Oxidation at Low Temperature Approche haut débit appliquée à l’oxydation basse température des COV

    Directory of Open Access Journals (Sweden)

    Jolly J.

    2013-03-01

    Full Text Available A High Throughput (HT approach is used to prepare and characterize the catalytic activity of materials for the destruction of Volatile Organic Compounds (VOC at low temperature. The interest of the Designs of Experiments (DoE in the primary screening is demonstrated through modeling catalysts composition according to the light-off temperature detected by infrared thermography. The combination of the mass spectrometry and the infrared thermography appears very useful to confirm and increase information about catalytic properties of the catalysts extracted to the primary screening stage. Finally, in situ Raman spectroscopy with infrared thermography allows to better understand the origin of the catalytic properties in the case ofAu/CeO2 catalysts. A strong interaction between gold and Ce-O bonds leading to an improvement of the cerium oxide reducibility could explain its high reactivity for 2-propanol oxidation at lower temperature. Une approche haut debit (HD est utilisée de la préparation jusqu’à la caractérisation de l’activité catalytique des matériaux pour l’élimination des Composés Organiques Volatils (COV à basse température. L’intérêt des plans d’expériences (DoE, en anglais Designs of Experiments dans le screening primaire est démontré grâce à l’identification d’une composition optimale de catalyseur prédite à l’aide des différentes températures d’ignition des catalyseurs obtenues par thermographie infrarouge. La combinaison in situ de la spectrométrie de masse et de la thermographie infrarouge s’est avérée d’une grande utilité pour confirmer et augmenter le niveau d’information concernant les propriétés catalytiques des catalyseurs provenant du screening primaire. Enfin, la spectroscopie Raman in situ couplée à la thermographie infrarouge permet de mieux comprendre l’origine des propriétés catalytiques dans le cas du catalyseur Au/CeO2. Une forte interaction entre les particules d

  11. [Determination of organic acids and inorganic anions by gradient ion chromatography].

    Science.gov (United States)

    Liu, Z; Liu, K; Shen, D; Song, Q; Mou, S; Feng, Y

    1997-07-01

    The chromatographic conditions for separation and detection of organic acids and inorganic anions by gradient ion chromatography with suppressed conductivity detection were studied. The optimized gradient programs were established. Ion chromatography were performed with a DX-100 chromatograph (DIONEX). The separation column is IonPac-AS11. Compared with NaHCO3/Na2CO3 and Na2B4O7, NaOH was the optimal eluent. The effect of organic modifier was also studied. Among methanol, 2-propanol and acetonitrile, methanol can make ion pairs such as malate and succinate, malonate and tartrate gaining baseline resolution. By using ion exchange separation, Cl-, NO3-, malate, succinate, malonate, tartrate, SO4(2-), oxalate were eluted between 5 mmol/L NaOH-16% CH3OH and 10 mmol/L NaOH-16% CH3OH in 25 min. A mobile phase composed of 30 mmol/L NaOH, 50% CH3OH and D.I. water was chosen to elute two groups of organic acids and inorganic anions: (1) quinate, formate, Cl-, malate, malonate, oxalate, citrate, isocitrate, aconitate; (2) lactate, Cl-, SO4(2-), tartrate, PO4(3-), citrate, isocitrate, aconitate. The detection limits (S/N = 3) were 0.1625 (quinate), 0.0691 (formate), 0.0115 (Cl-), 0.0886 (malate), 0.0591 (malonate), 0.0263 (oxalate), 0.1147 (citrate), 0.2017 (isocitrate), 0.3656 (cis-aconitate), 0.1045 (trans-aconitate), 0.1950 (lactate), 0.0729 (tartrate), 0.0224 (SO4(2-)) and 0.0692 (PO4(3-)) mg/L. The relative standard deviations were lower than 11.9% (n = 7) and the correlation coefficients ranged from 0.9212 for Cl- to 0.9999 for formate. The method was applied to determine the organic acids and inorganic anions of beverages and citric acids fermenting-medium. The results were satisfactory.

  12. Control of fibroin conformation: Toward the development of a biomimetic spinning process for silk fibers

    Science.gov (United States)

    Carlson, Kimberly Ann Trabbic

    1999-09-01

    Nature has shown that silks are sophisticated structural materials with remarkable mechanical properties; however, they are produced using far milder conditions than high-performance synthetic polymer fibers. While recent advances in molecular biotechnology have taken great strides toward the production of proteinaceous biopolymers, little is known about the processing conditions needed to spin fibers with the correct microstructures and mechanical properties. It is the purpose of this research to gain a fundamental understanding about how processing conditions affect the molecular structure of a model protein biopolymer, Bombyx mori silkworm fibroin, the structural protein of cocoon silk. Fibers of B. mori fibroin were wet spun from 1,1,1,3,3,3-hexafluoro-2-propanol (HFIP) into a methanol coagulation bath. X-ray fiber diffraction and quantitative Raman spectroscopy were used to determine that both naturally- and synthetically-spun fibers contain a high degree of beta-sheet (~50%). Fibers subjected to a post-spinning draw exhibited a preferential molecular alignment parallel to the fiber axis resulting in increased strength, stiffness, and extensibility. Fibers with microstructures and mechanical properties most similar to those of naturally-spun fibers were reproduced in synthetically-spun fibers with a draw ratio of 3.5. The transformation of helical fibroin in HFIP to beta-sheet sheet fibroin in synthetically-spun fibers was determined to be caused by the methanol coagulation bath. The kinetics beta-sheet fibroin crystallization from aqueous solution was investigated by monitoring the sigmoidal progression of gel formation using turbidity and Raman spectroscopy. Gelation kinetics were evaluated by measuring lag time, maximum gelation rate, and optical density to determine the effects of protein concentration, detergent concentration (nucleating agent), headgroup chemistry, ionic strength, pH, and temperature. An optimal molar ratio between SDS and fibroin (100

  13. Local sustained delivery of acetylsalicylic acid via hybrid stent with biodegradable nanofibers reduces adhesion of blood cells and promotes reendothelialization of the denuded artery

    Directory of Open Access Journals (Sweden)

    Lee CH

    2014-01-01

    Full Text Available Cheng-Hung Lee,1,2 Yu-Huang Lin,3 Shang-Hung Chang,1 Chun-Der Tai,3 Shih-Jung Liu,2 Yen Chu,4 Chao-Jan Wang,5 Ming-Yi Hsu,5 Hung Chang,6 Gwo-Jyh Chang,7 Kuo-Chun Hung,1 Ming-Jer Hsieh,1 Fen-Chiung Lin,1 I-Chang Hsieh,1 Ming-Shien Wen,1 Yenlin Huang81Division of Cardiology, Department of Internal Medicine, Chang Gung Memorial Hospital, Chang Gung University College of Medicine, Linkou, 2Department of Mechanical Engineering, 3Graduate Institute of Medical Mechatronics, Chang Gung University, 4Laboratory of Cardiovascular Physiology, Division of Thoracic and Cardiovascular Surgery, 5Department of Medical Imaging and Intervention, 6Hematology-Oncology Division, Department of Internal Medicine, Chang Gung Memorial Hospital, Linkou, 7Graduate Institute of Clinical Medicinal Sciences, Chang Gung University College of Medicine, Linkou, 8Department of Anatomical Pathology, Chang Gung Memorial Hospital, Linkou, Tao-Yuan, TaiwanAbstract: Incomplete endothelialization, blood cell adhesion to vascular stents, and inflammation of arteries can result in acute stent thromboses. The systemic administration of acetylsalicylic acid decreases endothelial dysfunction, potentially reducing thrombus, enhancing vasodilatation, and inhibiting the progression of atherosclerosis; but, this is weakened by upper gastrointestinal bleeding. This study proposes a hybrid stent with biodegradable nanofibers, for the local, sustained delivery of acetylsalicylic acid to injured artery walls. Biodegradable nanofibers are prepared by first dissolving poly(D,L-lactide-co-glycolide and acetylsalicylic acid in 1,1,1,3,3,3-hexafluoro-2-propanol. The solution is then electrospun into nanofibrous tubes, which are then mounted onto commercially available bare-metal stents. In vitro release rates of pharmaceuticals from nanofibers are characterized using an elution method, and a high-performance liquid chromatography assay. The experimental results suggest that biodegradable nanofibers

  14. Application of physiologically based pharmacokinetic modeling in predicting drug–drug interactions for sarpogrelate hydrochloride in humans

    Directory of Open Access Journals (Sweden)

    Min JS

    2016-09-01

    Full Text Available Jee Sun Min,1 Doyun Kim,1 Jung Bae Park,1 Hyunjin Heo,1 Soo Hyeon Bae,2 Jae Hong Seo,1 Euichaul Oh,1 Soo Kyung Bae1 1Integrated Research Institute of Pharmaceutical Sciences, College of Pharmacy, The Catholic University of Korea, Bucheon, 2Department of Pharmacology, College of Medicine, The Catholic University of Korea, Seocho-gu, Seoul, South Korea Background: Evaluating the potential risk of metabolic drug–drug interactions (DDIs is clinically important. Objective: To develop a physiologically based pharmacokinetic (PBPK model for sarpogrelate hydrochloride and its active metabolite, (R,S-1-{2-[2-(3-methoxyphenylethyl]-phenoxy}-3-(dimethylamino-2-propanol (M-1, in order to predict DDIs between sarpogrelate and the clinically relevant cytochrome P450 (CYP 2D6 substrates, metoprolol, desipramine, dextromethorphan, imipramine, and tolterodine. Methods: The PBPK model was developed, incorporating the physicochemical and pharmacokinetic properties of sarpogrelate hydrochloride, and M-1 based on the findings from in vitro and in vivo studies. Subsequently, the model was verified by comparing the predicted concentration-time profiles and pharmacokinetic parameters of sarpogrelate and M-1 to the observed clinical data. Finally, the verified model was used to simulate clinical DDIs between sarpogrelate hydrochloride and sensitive CYP2D6 substrates. The predictive performance of the model was assessed by comparing predicted results to observed data after coadministering sarpogrelate hydrochloride and metoprolol. Results: The developed PBPK model accurately predicted sarpogrelate and M-1 plasma concentration profiles after single or multiple doses of sarpogrelate hydrochloride. The simulated ratios of area under the curve and maximum plasma concentration of metoprolol in the presence of sarpogrelate hydrochloride to baseline were in good agreement with the observed ratios. The predicted fold-increases in the area under the curve ratios of metoprolol

  15. 'Click' generated 1,2,3-triazole based organosulfur/selenium ligands and their Pd(ii) and Ru(ii) complexes: their synthesis, structure and catalytic applications.

    Science.gov (United States)

    Kumar, Satyendra; Saleem, Fariha; Singh, Ajai K

    2016-07-28

    1-(2,6-Diisopropylphenyl)-4-(phenylthio/selenomethyl)-1H-1,2,3-triazole (L1/L2) was synthesized by a 'Click' reaction and treated with [Pd(CH3CN)2Cl2] for 5 h or [(η(6)-C6H6)RuCl(μ-Cl)]2 for 8 h (followed by reaction with NH4PF6) at room temperature, resulting in complexes [Pd(L)Cl2] (1 and 2) or [(η(6)-C6H6)Ru(L)Cl]PF6 (3 and 4) (L = L1 or L2), respectively. The four complexes (1-4) and ligands (L1 and L2) were characterized with (1)H, (13)C{(1)H} and (77)Se{(1)H} NMR spectroscopy and high resolution mass spectrometry. The single crystal structures of 1-4 were solved. The geometry of Pd in 1 and 2 is distorted square planar. The Pd-S and Pd-Se bond distances in 1 and 2 are 2.277(3) and 2.384(6) Å respectively. In 3 and 4, there is a pseudo-octahedral "piano-stool" type disposition of donor atoms around Ru. The Ru-S and Ru-Se bond lengths in 3 and 4 are 2.3728(12) and 2.4741(6) Å respectively. The catalytic activity of complexes 1 and 2 was explored for Suzuki-Miyaura coupling (SMC) in water and the Sonogashira coupling reaction. For various aryl bromides, including deactivated ones, complexes 1 and 2 were found to be efficient catalysts for both couplings. The optimum loading of 1 and 2 required to catalyze both coupling reactions is of the order of 0.001-2 mol% of Pd. For SMC, no additive or phase transfer catalyst was added. For catalysis of the transfer hydrogenation (TH) of aldehydes and ketones, the half-sandwich Ru(ii) complexes 3 and 4 were explored. Their optimum catalytic loading was found to be 0.1-0.4 mol% of Ru. For TH, both the water solvent and the glycerol hydrogen source are environmentally friendly. The catalytic efficiencies of 3 and 4 are comparable with those reported for other catalysts for TH carried out with 2-propanol or glycerol as a H-source. 1, with a sulfur ligand, is more efficient than 2 (Se analog) for both SMC and the Sonogashira coupling. The activities of 3 and 4 for TH are in the order Se > S. PMID:27338234

  16. Enantiomeric separation and simulation studies of pheniramine, oxybutynin, cetirizine, and brinzolamide chiral drugs on amylose-based columns.

    Science.gov (United States)

    Ali, Imran; Al-Othman, Zeid A; Al-Warthan, Abdulrahman; Alam, Syed Dilshad; Farooqi, Javed A

    2014-03-01

    Solid phase extraction (SPE)-chiral separation of the important drugs pheniramine, oxybutynin, cetirizine, and brinzolamide was achieved on the C18 cartridge and AmyCoat (150 x 46 mm) and Chiralpak AD (25 cm x 0.46 cm id) chiral columns in human plasma. Pheniramine, oxybutynin, cetirizine, and brinzolamide were resolved using n-hexane-2-PrOH-DEA (85:15:0.1, v/v), n-hexane-2-PrOH-DEA (80:20:0.1, v/v), n-hexane-2-PrOH-DEA (70:30:0.2, v/v), and n-hexane-2-propanol (90:10, v/v) as mobile phases. The separation was carried out at 25 ± 1 ºC temperature with detection at 225 nm for cetirizine and oxybutynin and 220 nm for pheniramine and brinzolamide. The flow rates of the mobile phases were 0.5 mL min(-1). The retention factors of pheniramine, oxybutynin, cetirizine and brinzolamide were 3.25 and 4.34, 4.76 and 5.64, 6.10 and 6.60, and 1.64 and 2.01, respectively. The separation factors of these drugs were 1.33, 1.18, 1.09 and 1.20 while their resolutions factors were 1.09, 1.45, 1.63 and 1.25, and 1.15, respectively. The absolute configurations of the eluted enantiomers of the reported drugs were determined by simulation studies. It was observed that the order of enantiomers elution of the reported drugs was S-pheniramine > R-pheniramine; R-oxybutynin > S-oxybutynin; S-cetirizine > R-cetirizine; and S-brinzolamide > R-brinzolamide. The mechanism of separation was also determined at the supramolecular level by considering interactions and modeling results. The reported SPE-chiral high-performance liquid chromatography (HPLC) methods are suitable for the enantiomeric analyses of these drugs in any biological sample. In addition, simulation studies may be used to determine the absolute configuration of the first and second eluted enantiomers. PMID:24464520

  17. PHOTOREDUCTIVE SEQUESTRATION OF CO2 TO FORM C1 PRODUCTS AND FUEL

    Energy Technology Data Exchange (ETDEWEB)

    Theodore Mill; Haruthai Tungudomwongsa

    2004-02-24

    We have investigated the photochemical reduction of CO{sub 2} in aqueous solution to form C{sub 1} products using a variety of oxide semiconductors and near UV light. Conventional oxide photosemiconductors including TiO{sub 2} and SrTiO{sub 3}, as well as modified oxide semiconductors including Pt/TiO{sub 2} and SrTiO{sub 3}/Cr-Sb, TiO{sub 2}/Fe{sub 3}O{sub 4} or TiO{sub 2}/Fe(CN){sub 6}{sup 3-} were used. Analysis for formate, acetate, formaldehyde, methanol and methane were conducted by a variety of analytical methods. Despite extensive published data on the facile reduction of CO{sub 2} by these semiconductors, we found only trace quantities of formate and acetate (typically less than 1 ppm) and no unequivocal evidence for formation of the other products. The quantum efficiencies of TiO{sub 2} and SrTiO{sub 3} for forming formate and acetate from CO{sub 2} are estimated to be 0.1-0.2% or less. The spectral properties of the unmodified oxides (TiO{sub 2}, SrTiO{sub 3}) restricts their use of solar irradiation to about 10% of the available near UV and visible spectrum, thereby giving an overall quantum and spectral efficiency of less than 0.01%. Semiconductor oxides modified with, Cr and Sb, Fe{sub 3}O{sub 4} or Fe(CN){sub 6}{sup 3-} exhibited no enhanced efficiency. However, Pt/TiO{sub 2} does produce more formate and acetate than TiO{sub 2} alone by about a factor of two. Addition of 0.6 mM 2-propanol to an irradiated CO{sub 2}/TiO{sub 2} suspension led to formation of larger amounts (0.55 mM, 25 ppm) of formate, but no formaldehyde. The higher yield is probably because re-oxidation of formate by semiconductor holes was competitively blocked by propanol acting as a sacrificial electron donor. Reoxidation of formate by TiO{sub 2} under argon is 80 times faster than reduction. Thus, reoxidation could be an important process limiting the accumulation of products and will require new design strategies for reducing accumulation of products in the photocatalytic zone

  18. Nickel(II) complexes of pentadentate N5 ligands as catalysts for alkane hydroxylation by using m-CPBA as oxidant: a combined experimental and computational study.

    Science.gov (United States)

    Sankaralingam, Muniyandi; Balamurugan, Mani; Palaniandavar, Mallayan; Vadivelu, Prabha; Suresh, Cherumuttathu H

    2014-09-01

    energy to the high-spin state. The lower catalytic activity of complex 5 is mainly due to the formation of thermodynamically less accessible m-CPBA-coordinated precursor of [Ni(II) (L5)(OOCOC(6)H(4)Cl)](+) (5 a). Adamantane is oxidized to 1-adamantanol, 2-adamantanol, and 2-adamantanone (3°/2°, 10.6-11.5), and cumene is selectively oxidized to 2-phenyl-2-propanol. The incorporation of sterically hindering pyridylmethyl and quinolylmethyl donor ligands around the Ni(II) leads to a high 3°/2° bond selectivity for adamantane oxidation, which is in contrast to the lower cyclohexane oxidation activities of the complexes. PMID:25100547

  19. I Situ Laser Interferometry and Fluorescence Quenching Measurements of Poly(methyl Methacrylate) Thin Film Dissolution.

    Science.gov (United States)

    Wang, Fei

    The dissolution mechanisms of poly(methyl methacrylate) (PMMA) thin films in selected organic solvents was investigated. The dissolution was monitored using an in situ laser interferometry and fluorescence quenching (LIFQ) technique. Phenanthrene -labeled PMMA (Phe-PMMA) was used as a probe. Solutions of PMMA in toluene were spin-coated onto sapphire substrate to form films approximately 1 μm thick. The LIFQ results show that for PMMA film dissolution the transition layer thickness increases until the dissolution reaches its steady state. Then this final transition layer thickness (FTL) does not change until solvent vanguard molecules reach the surface of the substrate. Thermal history effects on PMMA film dissolution were examined. The dissolution rate decreases with increasing baking temperature and reaches a constant value for annealing at 150^circC. The results show that the thermal history has negligible effect on the factor of reduction f obtained from interferometry measurements. Fluorescence quenching measurements, by contrast, suggest that transition layer thickness decreases with increasing baking temperature. This suggests that the fluorescence quenching part of the LIFQ experiment is sensitive to the Fickian precursor portion of the solvent concentration profile in the film. The dissolution of PMMA films in acetone, 2-butanone, and 2-pentanone was studied. The results show that the dissolution rate decreases significantly with increasing solvent molecular size. Significant differences are found for FTL values calculated from LIFQ experiments and those calculated from f obtained by laser interferometry. Values of f are essentially identical in three solvents used. The effect of non-solvent on PMMA dissolution was studied by using 2-propanol and 2-butanone mixtures as solvents. The dissolution rate decreases with increasing non-solvent content. This indicates a strong thermodynamic effect, especially at high concentration of non-solvent. Molecular weight

  20. Dissolution detection of testosterone undecanoate capsule in vitro%十一酸睾酮胶囊体外溶出度的测定

    Institute of Scientific and Technical Information of China (English)

    程周; 安仁波; 张慧; 李迎; 孙建绪; 郑爱萍

    2016-01-01

    Objective To determin the dissolution of testosterone undecanoate capsule in vitro with an established HPLC method. Methods The dissolution was determined by the second method described in China(ChP)2015,Pharmacopoeia. Totally 900 ml of 0.25%sodium lauryl sulfate solution with pH 6.8 phosphate buffer were used as dissolution media,and the rotation speed was 75 r/min. The dissolution time was 120 min and the dissolution was determined by HPLC. The HPLC column was phenomenex@C18 column(250 mm×4.6 mm,5μm). The mobile phase was 2-propanol-acetonitrile-water(45∶45∶10,V/V/V)with a flow rate of 1.0 ml/min and the detection wavelength of 240 nm. The column temperature was 40℃and the injection volume was 20μl. Results The average recovery of the method was about 100.55%(n=9). The calibration curves showed good linearity(r2=0.9999,n=7)within ranges of 1-50μg/ml. Conclusion The method is convenient and sensitive in the dissolution determination of testosterone undecanoate capsule.%目的: HPLC法测定十一酸睾酮胶囊的体外溶出。方法采用《中国药典》2015年版溶出度测定第二法,以pH6.8的磷酸缓冲液(含0.25%十二烷基硫酸钠)900 ml为溶出介质,转速75 r/min,溶出时间为120 min。使用HPLC法对溶出样品检测,采用phenomenex@C18色谱柱(4.6 mm×250 mm,5μm);流动相:异丙醇-乙腈-水(45∶45∶10,V/V/V);流速:1.0 ml/min;检测波长:240 nm;柱温:40℃;进样量:20μl。结果本法平均回收率为100.55%(n=9);在1~50μg/ml范围内线性关系良好(R2=0.9999,n=3)。结论方法简便、灵敏、准确、专属性强;可用于十一酸睾酮胶囊溶出度的检测。

  1. Polyelectrolyte-assisted preparation and characterization of nanostructured ZnO thin films

    Energy Technology Data Exchange (ETDEWEB)

    Jia, Shijun

    2005-05-15

    The present work focuses on the synthesis and characterization of nanostructured ZnO thin films onto silicon wafers modified by self-assembled-monolayers via chemical bath deposition. Two precursor solutions were designed and used for the film deposition, in which two different polymers were introduced respectively to control the growth of the ZnO colloidal particles in solution. ZnO films were deposited from an aqueous solution containing zinc salt and hexamethylenetetramine (HMTA) in the presence of a graft-copolymer (P (MAA{sub 0.50}-co(MAA-EO{sub 20}){sub 0.50}){sub 70}). A film-formation-diagram was established based on the results obtained by scanning electron microscopy (SEM) and atomic force microscopy (AFM), which describes the influence of the concentration of HMTA and copolymer on the ZnO film formation. According to the film morphology, film formation can be classified into three categories: (a) island-like films, (b) uniform films and (c) canyon-like films. The ZnO films annealed at temperatures of 450 C, 500 C, 600 C and 700 C were examined by X-ray diffraction (XRD) and transmission electron microscopy (TEM). After annealing, the films are polycrystalline ZnO with wurtzite structure. XRD measurements indicate that with increasing annealing temperature, the average grain size increases accordingly and the crystallinity of the films is improved. Upon heating to 600 C, the ZnO films exhibit preferred orientation with c-axis normal to substrate, whereas the films annealed at 700 C even show a more explicit texture. By annealing at temperatures above 600 C the ZnO film reacts with the substrate to form an interfacial layer of Zn{sub 2}SiO{sub 4}, which grows thicker at elevated annealing temperatures. The ZnO films annealed at 600 C and 700 C show strong UV emission. Another non-aqueous solution system for ZnO thin film deposition was established, in which 2- propanol was used as a solvent and Zn(CH3COO){sub 2}.2H{sub 2}O as well as NaOH as reactants

  2. A research on the performance of SF/COL/PLCL electrospun three-dimensiona nanofiber scaffold%SF/COL/PLCL静电纺丝三维纳米纤维支架材料的性能研究

    Institute of Scientific and Technical Information of China (English)

    殷丽华; 王红; 张忠芮; 黄嵩涛; 王家奎; 秦子顺; 孙琪; 余占海

    2014-01-01

    The aim of this study was tostructure a kind of three-dimensiona nanofiber scaffold composed of SF, collagenⅠand PLCL by using electrospinning technique and to evaluate its performance.We took 1,1,1,3,3,3-hexafluoro-2-propanol (HFIP)as solvent to prepare different mass ratios of SF/collagenⅠ/PLCL scaffolds (0∶100,30∶70,50∶50,70∶30,100∶0)and the properties of these scaffolds were studied before and after they were crosslinked by 25% glutaraldehyde vapor for 48 hours.The results were described as follow:scan-ning electron microscopy(SEM)and the contact water angle meter analysis showed that the uniformity of com-posite nanofibers was improved and with the existence of PLCL,the hydrophilic property decreased.XRD anal-ysis indicates that the nanofibers scaffolds had higher crystallinity after crosslinked.The thermal stability of the scaffold material was also increased.With rising levels of PLCL,the properties of the scaffolds were increased significantly after crosslinking.When the human periodontal ligament stem cells(hPDLSCs)were seeded on SF/collagenⅠ/PLCL scaffolds,they grew well and showed better ability of adhesion and proliferation.Among the scaffolds,PLCL content of 70% did best with significant differences.Our study indicated that this kind of electrospun three-dimensiona nanofiber scaffold might be a potential candidate for restoration of periodontal de-fect and the periodontal tissue engineering.%采用静电纺丝法以六氟异丙醇(HFIP)为溶剂,将质量比为70∶30的 SF/COL (丝素/胶原)和PLLC(聚左旋乳酸己内酯)共混制备质量比为0∶100,30∶70,50∶50,70∶30,100∶0的8% SF/COL/PLCL的三维纳米纤维支架,25%戊二醛蒸汽交联48 h后检测各组比例支架材料的理化性能及生物性能。扫描电镜显示纳米纤维形貌良好,均为纳米级别;X射线衍射结果显示交联后材料结晶度增强,Silk Ⅰ构象由α-折叠形成稳定的β-折叠;材料交联后为疏水性, PLCL的加入

  3. SF/COL/PLLA静电纺丝三维纳米纤维支架材料的性能研究*%A research on the performance of SF/COL/PLLA electrospun three-dimensiona nanofiber scaffold

    Institute of Scientific and Technical Information of China (English)

    张忠芮; 王红; 高维岳; 王家奎; 黄嵩涛; 殷丽华; 王琳; 余占海

    2014-01-01

    The aim of this study was to prepare a kind of nanofiber scaffolds composed of different mass ratios of silkfi-broin(SF)/collagen/PLLA by using electrospinning technique and to evaluate its properties.1 ,1 ,1 ,3 ,3 ,3-hexafluoro-2-propanol (HFIP)was taken as solvent to prepare the nanofiber scaffolds and the mass ratios of SF/collagen/PLLA were set as 0∶100,30∶70,50∶50,70∶30,100∶0.And then the preoperties of the as-prepared samples were tested before and after crosslinked by 25% glutaraldehyde vapor for 48 h.The scaffolds were characterized by scanning electron mi-croscopy (SEM),X-ray diffraction (XRD),thermo gravimetric (TG)analysis and the hydrophily was analysed by water contact angle (WCA)analysis.The results of SEM revealed that the uniformity of the blending nanofibers had im-proved.The thermal stability of the scaffold material increased with the increase of the blend ratios of PLLA.The XRD results indicated that stableβ-folding conformation of silk has formed and the crystallization of materials has increased. The contact water angle meter analysis suggested that the hydrophilic property of the blending composite nanofibers de-creased with the existence of PLLA.The periodontal ligament stem cells (PDLSCs)were seeded on the blending com-posite nanofibers in vitro.The cells grew well on the surface of materials,and had great adhesion and proliferation abili-ties.The cytocompatibility and physicochemical properties of the scaffold with content of 70% PLLA are superior to other groups,which suggest the as-prepared sampleis expected to become a new type of scaffold forperiodontal tissue en-gineering.%基于PLLA(左旋聚乳酸)的优异性能,以六氟异丙醇(HFIP)为溶剂采用静电纺丝法制备质量比为0∶100,30∶70,50∶50,70∶30和100∶0的8%SF/COL/PLLA共混纳米纤维支架,并用浓度为25%戊二醛蒸汽交联48 h,通过扫描电镜、X 射线衍射、热重分析仪、接触角检测仪对共混材料交联前后的理化性

  4. 胶原/丝素电纺纳米纤维膜体外培养肝细胞的研究%In vitro Study of Collagen/Silk Nanofiber Scaffold on Hepatocytes

    Institute of Scientific and Technical Information of China (English)

    胡玮; 崔新爱; 刘欣; 顾汉卿

    2012-01-01

    In this work a collagen/silk nanofibrous scaffold was fabricated via electrospinning technique. Human hepatoma cell line HepG2 were seeded on the scaffold. The cell morphology, viability and other functions were investigated. In the scaffold preparation, 1,1,1,3,3,3- hexafluoro- 2-propanol (HFIP) was used as solvent to prepare the collagen/silk nanofiber scaffold in the electrospinning, and the mass ratio of collagen/silk fibroin was 100:0, 70:30, 50:50, 30:70, 0:100. The Scanning electron microscopy (SEM) images showed that the average diameter of the fibers ranged from 550 nm to 1100 nm, which was proportionally correlated with SF content. Cell culture results showed that HepG2 cells grew well on the surface of the scaffolds and integrated with the scaffold fibers. The collagen/silk nanofiber scaffold supported the cells growing in a steady state whitin 4-9 days. The urea synthesis and protein secretion have significant differences with the ones of control group. Cells growing in the nanofibrous scaffold with SF content of 50% displayed better status and functions than those in the other groups. Compared with cells in the control group, HepG2 cell grows well in the collagen/silk nanofiber scaffold and maintained the functions in longer time.%本实验采用静电纺丝技术制备胶原/丝素纳米纤维支架,对支架上培养的人肿瘤肝细胞HepG2进行形态学观察、细胞功能和代谢功能检测.胶原/丝素纳米纤维支架以六氟异丙醇(HFIP)为溶剂通过静电纺丝技术制备,5种支架材料胶原和丝素配比分别为10∶0、7∶3、5∶5、3∶7、0∶10.扫描电镜结果显示制备的纤维平均直径在550 ~1100 nm之间,随着丝素含量的增加纤维平均直径增加.细胞培养结果显示HepG2细胞在材料表面生长状态良好并与支架材料紧密结合.随培养时间延长,常规培养组细胞在第5d后逐渐死亡,失去细胞功能,胶原/丝素纳米纤维支架组细胞在4~9d内能够维持稳

  5. Preparation of PtSnCu/C and PtSn/C electrocatalysts and activation by dealloying processes for ethanol electrooxidation; Preparacao de eletrocatalisadores PtSnCu/C e PtSn/C e ativacao por processos de dealloying para aplicacao na oxidacao eletroquuimica do etanol

    Energy Technology Data Exchange (ETDEWEB)

    Crisafulli, Rudy

    2013-06-01

    PtSnCu/C (with different Pt:Sn:Cu atomic ratios) and PtSn/C (50:50) electrocatalysts were prepared by borohydride (BR) and alcohol-reduction (AR) processes using H{sub 2}PtCl{sub 6}.6H{sub 2}O, SnCl{sub 2}.2H{sub 2}O and CuCl{sub 2}.2H{sub 2}O as metal sources, NaBH{sub 4} and ethylene glycol as reducing agents, 2-propanol and ethylene glycol/water as solvents and carbon black as support. In a further step, these electrocatalysts were activated by chemical (CD) and electrochemical (ED) dealloying processes through acid treatment and thin porous coating technique, respectively. These materials were characterized by energy dispersive X-ray, Xray diffraction, transmission electron microscopy, line scan energy dispersive Xray and cyclic voltammetry. Electrochemical studies for ethanol electro-oxidation were performed by cyclic voltammetry, chronoamperometry and in single Direct Ethanol Fuel Cell using Membrane Electrode Assembly (MEA). The anodic effluents were analysed by gas chromatography. The X-ray diffractograms of the as-synthesized electrocatalysts showed the typical face-centered cubic structure (FCC) of platinum and its alloys. After dealloying, the X-ray diffractograms showed that the Pt FCC structure was preserved. The crystallite sizes of the assynthesized electrocatalysts were in the range of <=2 nm to 3 nm and after dealloying there were no significant variations in sizes. The energy dispersive Xray analysis of the as-synthesized electrocatalysts showed a Pt:Sn and Pt:Sn:Cu atomic ratios similar to the nominal values. After chemical and electrochemical dealloying of the electrocatalysts the ranged Pt:Sn and Pt:Sn:Cu atomic ratios showed that Cu and Sn atoms were removed. However, chemical dealloying process proved to be more efficient for removing Cu and electrochemical dealloying for removing Sn. The line scan energy dispersive X-ray analysis showed that acid and electrochemical treatments were efficient to dealloying Cu and/or Sn superficial atoms of

  6. Photoreduction of 99Tc Pertechnetate by Nanometer-Sized Metal Oxides: New Strategies for Formation and Sequestration of Low-Valent Technetium

    Energy Technology Data Exchange (ETDEWEB)

    Burton-Pye, Benjamin P. [Hunter College of the City Univ. of New York, NY (United States); Radivojevic, Ivana [Hunter College of the City Univ. of New York, NY (United States); McGregor, Donna [Hunter College of the City Univ. of New York, NY (United States). Graduate Center; Mbomekalle, Israel M. [Hunter College of the City Univ. of New York, NY (United States); Lukens, Wayne W. [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States); Francesconi, Lynn C. [Hunter College of the City Univ. of New York, NY (United States). Graduate Center

    2011-11-23

    Technetium-99 (99Tc)(β-max: 293.7 keV; t1/2: 2.1 x 105 years) is a byproduct of uranium-235 fission and comprises a large component of radioactive waste. Under aerobic conditions and in a neutral- basic environment, the pertechnetate anion (99TcO4-) is stable. 99TcO4- is very soluble, migrates easily through the environment and does not sorb well onto mineral surfaces, soils or sediments. This study moves forward a new strategy for the reduction of TcO4- and chemical incorporation of the reduced 99Tc into a metal oxide material. This strategy employs a single material, a polyoxometalate (POM), α2-[P2W17O61]10-, that can be photoactivated in the presence of 2-propanol to transfer electrons to TcO4- and incorporate the reduced 99Tc covalently into the α2- framework to form the TcVO species, TcVO(α2-P2W17O61)7-. This occurs via the formation of an intermediate species that slowly converts to TcVO(α2-P2W17O61)7-. EXAFS and XANES analysis and preliminary EPR analysis, suggests that the intermediate consists of a Tc(IV) α2- species where the 99Tc is likely bound to only 2 of the 4 W-O oxygen atoms in the α2-[P2W17O61]10- defect. This intermediate then oxidizes and converts to the 99TcVO(α2-P2W17O61)7- product. The reduction and incorporation of 99TcO4- was accomplished in a ''one pot'' reaction using both sunlight and UV irradiation, and monitored as a function of time

  7. A simple and specific high performance liquid chromatography method for the assay of a series of novel dermal penetration enhancers.

    Science.gov (United States)

    Michniak, B B; Seyda, K L

    1993-02-01

    Synopsis A series of clofibric acid amides has been synthesized and previously reported by the authors as possessing enhancer activity in vitro in athymic nude mouse skin against model drugs, hydrocortisone-21-acetate and beta-methasone-17-valerate. An assay was required for each of these enhancers however, which would be specific for each compound and would also separate model drugs and their metabolite peaks. This study reports reverse phase high performance liquid chromatography assays for clofibric acid amide and seven derivatives (Ia-Ig). All enhancers showed maximum absorption at 232 nm, betamethasone (BM) and its valerate (BMV) at 238 nm, and hydrocortisone (HC) and its acetate (HCA) at 242 nm. Practical units of detection for the amides were 0.46-2.8 mug ml(-1) and peaks were sharp and well-separated from steroid peaks in three vehicles - methanol alone. Franz diffusion cell receptor phase samples (isotonic phosphate buffer), and full-thickness athymic nude mouse skin extracts in methanol. Mobile phases consisted of various proportions of acetonitrile and water, some with 2-propanol. The octyl amide for example, with mobile phase CH(3)CN: H(2)O (85:15) at 1 ml min(-1) had a retention time (t(R)) of 7.9 mins. Under the same conditions, retention times for the steroids were HC, t(R)= 3.3 mins; HCA, t(R)= 4.3 mins; BM, t(R)= 3.4 mins; BMV, t(R)= 4.6 mins. Résumé Les auteurs avaient démontré dans un article précédent le pouvoir accélérateur de pénétration dermique in vitro d'une gamme d'amides d'acide clofibrique sur la peau de souris sans poils, et sans thymus avec des médicaments types tels que l'acetate 21 d'hydrocortisone et le valerate 17 de beta-metasone. Il a cependant été requis, pour chacun de ces accélérateurs, un test spécifique pour chaque composition, permettant de séparer chaque médicament et les pics des métabolites. Cette étude décrit des tests par chromatographie liquide à haute performance en phase inverse pour l

  8. Pharmacokinetic study of inosiplex tablet in healthy volunteers%异丙肌苷片在健康人体内的药动学

    Institute of Scientific and Technical Information of China (English)

    宋薇; 杨静; 李雪晴; 贾艳艳; 杨林; 周伦; 鹿成韬; 文爱东

    2012-01-01

    OBJECTIVE To study the pharmacokinetics of inosiplex in healthy subjects following multiple dosing of inosiplex tablet. METHODS 10 healthy volunteers (5 females and 5 males) were assigned to receive 1000 mg inosiplex tablet at morning, noon, and evening for consecutive 7 days. The plasma concentrations of N,N-dimethylamino-2 propanol(Dip) and p-acet-aminobenzoic acid (PACBA) were measured by fully validated LC-MS/MS and HPLC method, respectively The pharmacoki-netic parameters were calculated by DAS software. RESULTS The main pharmacokinetic parameters of single dosing of inosiplex tablet were as follows: for Dip, t max and Cmax were (1. 55 ± 0. 16)h and (2. 24 ± 0. 18)μg·mL-1 , respectively;t1/2 was (4. 42 ± 0. 81)h;AUC,-24 was(12.93 ± 2. 1)μg·h·mL-1 ; respectively. In the case of PACBA, t max and Cmax were(1.03 ±0. 51) h and (5. 18 ± 1.80 )μg·mL-1 , respectively; t 1/2 was(0. 95 ± 0. 13)h; AUC0-24 was (7. 69 ± 1. 13)μg·h·mL-1;The main pharmacokinetic parameters of multiple dosing of inosiplex tablet were as follows: for Dip, t max and C ss max were (1. 00 ± 0. 46)h and (2.49 ± 0. 11)μg·mL-1, respectively; t 1/2 was (5. 74 ± 1. 24) h; AUd-24 was (16. 06 ±2. 80) μg· h·mL-1,C ss av was (1. 36 ± 0. 19)μg·mL-1 ;DF was 1. 29 ± 0. 31 , respectively. In the case of PACBA, t max and C ss max were (0. 50 ± 0. 00) h and (7. 37 ± 0.94) μg·mL-1 , respectively; t1/2 was (1.04±0. 17) h; AUC0-24 was (7.90 ± 1. 16) μg·h·mL-1 ;C ss av was (0.99±0. 14)μg· mL-1 ;DF was 7. 44 ± 0. 90. CONCLUSION The method which we developed is sensitive, accurate and simple. And the Dip and PACBA have been accumulated after multi-dosing of inosiplex administration.%目的:探讨健康受试者多次口服异丙肌苷片1000 mg后体内药动学特点.方法:10例健康受试者,男女各半,每次口服1 000 mg异丙肌苷片,tid,连续7d,采用液相色谱-串联质谱法(LC-MS/MS)和高效液相色谱法(HPLC)分别测定血浆中N,N-二甲氨基2

  9. On the interaction of uranium with the bioligands citric acid and glucose; Zur Wechselwirkung von Uran mit den Bioliganden Citronensaeure und Glucose

    Energy Technology Data Exchange (ETDEWEB)

    Steudtner, Robin

    2011-10-26

    For a better understanding of the actinide behaviour in human (in term of metabolism, retention, excretion) and in geological and biological systems, it is of prime importance to have a good knowledge of the relevant speciation. In model systems the chemical behaviour of uranium regarding complex formation and redox reaction were investigated. On this basis determinates thermodynamics constants and redox behaviour are used to prognoses a safety assessment for the respective system. The pentavalent uranium(V) is a metastable intermediate in natural redox system between uranium(IV) and uranium(VI). In this study the uranium(V) fluorescence was detected by laser spectroscopic methods ({lambda}{sub ex} = 255 nm) for the first time. The peak maxima ({lambda}{sub ex} = 255 nm) of luminescence spectrum of the photo reduced U(V) in aqueous perchlorate/2-propanol solution was detected at 440 nm and a fluorescence lifetime of 1.1 {+-} 0.02 {mu}s was calculated. The stable aqueous uranyl(V)-tricarbonate complex was characterized by fluorescence spectroscopy ({lambda}{sub ex} = 255 nm and 408 nm). The known quench effects of carbonate could be minimized by coupling the laser fluorescence system with the low temperature technique. The resulting U(V) fluorescence emission bands were detected between 375 nm and 445 nm. The peak maxima were identified at 401.5 nm ({lambda}{sub ex} = 255 nm) and 413.0 nm ({lambda}{sub ex} = 408 nm). The fluorescence lifetime of the uranyl(V)-carbonate species was determined at 153 K as 120 {+-} 0.1 {mu}s ({lambda}{sub ex} = 255 nm). In addition the fluorescence of uranium(V) was verifies by confocal laser scanning microscopy. The oxidation process from uranium(IV) to uranium(VI) was investigated on solid uraninite (UO{sub 2}) and uranium(IV) tetra chloride (UCl{sub 4}) and a 1 x 10{sup -2} M uranium(IV) sulphate (U{sup IV}SO{sub 4}) solution. By continuous oxygen transfer the uranium(IV) was oxidized slowly to uranium(VI). The temporal process was

  10. On the interaction of uranium with the bioligands citric acid and glucose; Zur Wechselwirkung von Uran mit den Bioliganden Citronensaeure und Glucose

    Energy Technology Data Exchange (ETDEWEB)

    Steudtner, Robin

    2011-10-26

    For a better understanding of the actinide behaviour in human (in term of metabolism, retention, excretion) and in geological and biological systems, it is of prime importance to have a good knowledge of the relevant speciation. In model systems the chemical behaviour of uranium regarding complex formation and redox reaction were investigated. On this basis determinates thermodynamics constants and redox behaviour are used to prognoses a safety assessment for the respective system. The pentavalent uranium(V) is a metastable intermediate in natural redox system between uranium(IV) and uranium(VI). In this study the uranium(V) fluorescence was detected by laser spectroscopic methods ({lambda}{sub ex} = 255 nm) for the first time. The peak maxima ({lambda}{sub ex} = 255 nm) of luminescence spectrum of the photo reduced U(V) in aqueous perchlorate/2-propanol solution was detected at 440 nm and a fluorescence lifetime of 1.1 {+-} 0.02 {mu}s was calculated. The stable aqueous uranyl(V)-tricarbonate complex was characterized by fluorescence spectroscopy ({lambda}{sub ex} = 255 nm and 408 nm). The known quench effects of carbonate could be minimized by coupling the laser fluorescence system with the low temperature technique. The resulting U(V) fluorescence emission bands were detected between 375 nm and 445 nm. The peak maxima were identified at 401.5 nm ({lambda}{sub ex} = 255 nm) and 413.0 nm ({lambda}{sub ex} = 408 nm). The fluorescence lifetime of the uranyl(V)-carbonate species was determined at 153 K as 120 {+-} 0.1 {mu}s ({lambda}{sub ex} = 255 nm). In addition the fluorescence of uranium(V) was verifies by confocal laser scanning microscopy. The oxidation process from uranium(IV) to uranium(VI) was investigated on solid uraninite (UO{sub 2}) and uranium(IV) tetra chloride (UCl{sub 4}) and a 1 x 10{sup -2} M uranium(IV) sulphate (U{sup IV}SO{sub 4}) solution. By continuous oxygen transfer the uranium(IV) was oxidized slowly to uranium(VI). The temporal process was