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Sample records for surface stationary phase

  1. Preparation and evaluation of surface-bonded tricationic ionic liquid silica as stationary phases for high-performance liquid chromatography.

    Science.gov (United States)

    Qiao, Lizhen; Shi, Xianzhe; Lu, Xin; Xu, Guowang

    2015-05-29

    Two tricationic ionic liquids were prepared and then bonded onto the surface of supporting silica materials through "thiol-ene" click chemistry as new stationary phases for high-performance liquid chromatography. The obtained columns of tricationic ionic liquids were evaluated respectively in the reversed-phase liquid chromatography (RPLC) mode and hydrophilic interaction liquid chromatography (HILIC) mode, and possess ideal column efficiency of 80,000 plates/m in the RPLC mode with naphthalene as the test solute. The tricationic ionic liquid stationary phases exhibit good hydrophobic and shape selectivity to hydrophobic compounds, and RPLC retention behavior with multiple interactions. In the HILIC mode, the retention and selectivity were evaluated through the efficient separation of nucleosides and bases as well as flavonoids, and the typical HILIC retention behavior was demonstrated by investigating retention changes of hydrophilic solutes with water volume fraction in mobile phase. The results show that the tricationic ionic liquid columns possess great prospect for applications in analysis of hydrophobic and hydrophilic samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  2. Optimising reversed-phase liquid chromatographic separation of an acidic mixture on a monolithic stationary phase with the aid of response surface methodology and experimental design.

    Science.gov (United States)

    Wang, Y; Harrison, M; Clark, B J

    2006-02-10

    An optimization strategy for the separation of an acidic mixture by employing a monolithic stationary phase is presented, with the aid of experimental design and response surface methodology (RSM). An orthogonal array design (OAD) OA(16) (2(15)) was used to choose the significant parameters for the optimization. The significant factors were optimized by using a central composite design (CCD) and the quadratic models between the dependent and the independent parameters were built. The mathematical models were tested on a number of simulated data set and had a coefficient of R(2) > 0.97 (n = 16). On applying the optimization strategy, the factor effects were visualized as three-dimensional (3D) response surfaces and contour plots. The optimal condition was achieved in less than 40 min by using the monolithic packing with the mobile phase of methanol/20 mM phosphate buffer pH 2.7 (25.5/74.5, v/v). The method showed good agreement between the experimental data and predictive value throughout the studied parameter space and were suitable for optimization studies on the monolithic stationary phase for acidic compounds.

  3. Carbon nanotube stationary phases for microchip electrochromatography

    DEFF Research Database (Denmark)

    Mogensen, Klaus Bo; Bøggild, Peter; Kutter, Jörg Peter

    The use of nanomaterials in separation science has increased rapidly in the last decade. The reason for this is to take advantage of the unique properties of these materials, such as a very high surface-to-volume ratio and favourable sorbent behaviour. Carbon nanostructures, such as carbon...... surface can furthermore be used directly as a stationary phase in reverse-phase separations, thereby avoiding subsequent functionalization of the nanostructures. This significantly reduces the fabrication time and possibly also increases the reproducibility of the column performance. In this presentation......, microfluidic devices with microfabricated carbon nanotube columns for electrochromatographic separations will be presented. The electrically conductive carbon nanotube layer has been patterned into hexoganol micropillars in order to support electroosmotic flow without forming gas bubbles from electrolysis...

  4. Response surface methodology for the determination of the design space of enantiomeric separations on cinchona-based zwitterionic chiral stationary phases by high performance liquid chromatography.

    Science.gov (United States)

    Hanafi, Rasha Sayed; Lämmerhofer, Michael

    2018-01-26

    Quality-by-Design approach for enantioselective HPLC method development surpasses Quality-by-Testing in offering the optimal separation conditions with the least number of experiments and in its ability to describe the method's Design Space visually which helps to determine enantiorecognition to a significant extent. Although some schemes exist for enantiomeric separations on Cinchona-based zwitterionic stationary phases, the exact design space and the weights by which each of the chromatographic parameters influences the separation have not yet been statistically studied. In the current work, a screening design followed by a Response Surface Methodology optimization design were adopted for enantioseparation optimization of 3 model drugs namely the acidic Fmoc leucine, the amphoteric tryptophan and the basic salbutamol. The screening design proved that the acid/base additives are of utmost importance for the 3 chiral drugs, and that among 3 different pairs of acids and bases, acetic acid and diethylamine is the couple able to provide acceptable resolution at variable conditions. Visualization of the response surface of the retention factor, separation factor and resolution helped describe accurately the magnitude by which each chromatographic factor (% MeOH, concentration and ratio of acid base modifiers) affects the separation while interacting with other parameters. The global optima compromising highest enantioresolution with the least run time for the 3 chiral model drugs varied extremely, where it was best to set low % methanol with equal ratio of acid-base modifiers for the acidic drug, very high % methanol and 10-fold higher concentration of the acid for the amphoteric drug while 20 folds of the base modifier with moderate %methanol were needed for the basic drug. Considering the selected drugs as models for many series of structurally related compounds, the design space defined and the optimum conditions computed are the key for method development on

  5. Stationary phases for superheated water chromatography

    CERN Document Server

    Saha, S

    2002-01-01

    This project focused on the comparison of conventional liquid chromatography and superheated water chromatography. It examined the differences in efficiency and retention of a range of different stationary phases. Alkyl aryl ketones and eight aromatic compounds were separated on PBD-zirconia, Xterra RP 18, Luna C sub 1 sub 8 (2) and Oasis HLB columns using conventional LC and superheated water chromatography system. The retention indices were determined in the different eluents. On changing the organic component of the eluent from methanol to acetonitrile to superheated water considerable improvements were found in the peak shapes and column efficiencies on the PBD-zirconia and Oasis HLB columns. PS-DVB, PBD-zirconia and Xterra RP 18 columns have been used in efficiency studies. It was found that simply elevating the column temperature did not increase the efficiency of a separation in superheated water chromatography. The efficiency depended on flow rate, injection volume and also mobile phase preheating sys...

  6. Liquid Crystals as Stationary Phases in Chromatography.

    Science.gov (United States)

    Grajek, H; Witkiewicz, Z; Purchała, M; Drzewiński, W

    2016-01-01

    The most correct analysis of the compositions of diverse analytes mixtures is significant for analytical studies in different fields; however, many prevalent analytes cannot be identified employing traditional partition gas chromatographic methods. Thus, the increasing requirements on analytes of isomeric compounds and the problems encountered in their separation demand a study of more diverse analytical systems which are characterised by higher selectivity. Therefore, the selectivity and polarities of various liquid crystals (rod-like, banana-shape, biforked, oxygen, sulphur, nitrogen, and metal containing molecules, Schiff-base, and polymeric dendrimers) employed as liquid crystalline stationary phases (LCSPs) have been discussed from both points of views, namely, their analytical applications and thermodynamic characteristics of infinitely diluted probes with different acceptor-donor properties. Extreme particular effort has been paid to the different interdependencies between the bound up chemical structures of liquid crystal molecules with their different acceptor-donor properties and the connected resolution capabilities in the interpretation of the probe-LCSP systems, on the basis of the [Formula: see text] and [Formula: see text] dependencies, with regard to the LCSP compositions, which have been controlled by the counterbalancing of the enthalpy and entropy factors. The properties of binary systems composed of liquid crystalline poly(propyleneimine) dendrimers-rod-like molecules of liquid crystals and effects of the dendrimer structure, the chemical nature, and molecular size of the non-mesogens on the ability to dissolve in the liquid crystalline phases, have been interpreted. Practical applications of metallomesogenes and chiral stationary phases for analytical separation of different organic substances have also been taken into consideration.

  7. Tentacle-type zwitterionic stationary phase prepared by surface-initiated graft polymerization of 3-[N,N-dimethyl-N-(methacryloyloxyethyl)-ammonium] propanesulfonate through peroxide groups tethered on porous silica.

    Science.gov (United States)

    Jiang, Wen; Irgum, Knut

    2002-09-15

    A novel stationary phase with tentacle-type zwitterionic interaction layer was synthesized by free radical graft polymerization of 3-[N,N-dimethyl-N-(methacryloyloxyethyl)ammonium]propanesulfonate (SPE) from the surface of Kromasil porous silica particles. The polymerization was initiated by thermal cleavage of tert-butylperoxy groups covalently attached to the particle surface, and the material therefore carries a tentacle-type polymeric interaction layer with 3-sulfopropylbetaine functional moieties. The composition of the surface graft was determined by elemental analysis, and the surface charge was measured using photon correlation spectroscopy. The measured zeta-potentials were close to 0 and nearly independent of pH, and the tentacle character of the interactive layers were evident from the lack of colloidal stability in the absence of salt (antipolyelectrolytic behavior) and a marked increase in column back-pressure when the concentration of perchloric acid or perchlorate salt was increased. The chromatographic properties were evaluated on columns packed with the functionalized material, and it was shown that this zwitterionic stationary phase could simultaneously and independently separate inorganic anions and cations using aqueous solutions of perchloric acid or perchlorate salts as eluents. The material was also capable of separating two acidic and three basic proteins in a single run, using gradient salt elution at constant pH.

  8. Novel open tubular CEC with tentacle-type polymer stationary phase functionalized by phenylalanine.

    Science.gov (United States)

    Xu, Liang; Sun, Yan

    2008-02-01

    A novel stationary phase with tentacle-type polymer chains with epoxy groups was fabricated for open tubular CEC. The fabrication procedure of the stationary phase included pretreatment of capillary inner wall, silanization, and glycidyl methacrylate (GMA)-grafted polymerization. The influence of initiator concentration and polymerization time on the resulting polymer stationary phase was studied by measuring EOF mobility and hydrophobicity of the prepared capillary column. SEM showed that the capillary inner wall was evenly coated with a polymer film showing a wrinkly surface. The prepared GMA-grafted stationary phase could be easily modified with different chromatographic ligands by the ring-opening reaction of the epoxy groups. In this study, phenylalanine (Phe) was selected as the ligand. Benzene derivatives and three amino acids were then separated, respectively, using the Phe modified tentacle-type capillary column. As a control, separations were also performed on a monolayer Phe-modified capillary. The tentacle-type polymer stationary phase was found affording stronger retention and better resolution in the separation of benzene derivatives and tryptophan, tyrosine, and Phe mixtures compared with the monolayer stationary phase.

  9. Recent development of ionic liquid stationary phases for liquid chromatography.

    Science.gov (United States)

    Shi, Xianzhe; Qiao, Lizhen; Xu, Guowang

    2015-11-13

    Based on their particular physicochemical characteristics, ionic liquids have been widely applied in many fields of analytical chemistry. Many types of ionic liquids were immobilized on a support like silica or monolith as stationary phases for liquid chromatography. Moreover, different approaches were developed to bond covalently ionic liquids onto the supporting materials. The obtained ionic liquid stationary phases show multi-mode mechanism including hydrophobic, hydrophilic, hydrogen bond, anion exchange, π-π, and dipole-dipole interactions. Therefore, they could be used in different chromatographic modes including ion-exchange, RPLC, NPLC and HILIC to separate various classes of compounds. This review mainly summarizes the immobilized patterns and types of ionic liquid stationary phases, their retention mechanisms and applications in the recent five years. Copyright © 2015 Elsevier B.V. All rights reserved.

  10. Immobilized strychnine as a new chiral stationary phase for HPLC.

    Science.gov (United States)

    Sýkora, David; Vozka, Jiří; Tesařová, Eva; Kalíková, Květa; Havlík, Martin; Matějka, Pavel; Král, Vladimír

    2017-08-01

    A new ion-exchanger type chiral stationary phase for high-performance liquid chromatography was prepared. The synthetic protocol is based on derivatization of silica with (3-iodopropyl)trimethoxysilane in the first step followed by immobilization of strychnine via quaternization of nitrogen atom of the alkaloid strychnine. The synthesized chiral stationary phase was chromatographically characterized. The main effort was headed towards the evaluation of the enantioselectivity of the novel sorbent. For that purpose a set of suitable chiral probes, specifically, binaphthyl derivatives, was employed. The influence of methanol content, concentration of aqueous ammonium acetate buffer, and its pH on retention factors, separation selectivity, and resolution of the atropoisomers of the mentioned chiral solutes was studied in detail. It was demonstrated that the new chiral stationary phase was capable to separate atropoisomers of four out of seven testing compounds. Despite the strong influence of the above mentioned variables on retention, their impact on selectivity and resolution was rather moderate. Concerning retention mechanism, it seems that electrostatic interaction between the positively charged quaternary nitrogen of the chiral stationary phase and anionic solute participates significantly in the retention process. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Accumulation of hns mutations specifically in stationary phase in an ...

    Indian Academy of Sciences (India)

    + mutation profile in another control strain. These results suggest a positive selection for hns muta- tions when rpoS function is compromised and occurs specif- ically in the stationary phase. The strains used were iso- genic and differed only at the rpoS and tnaA loci that carried the transposon Tn10. No interaction between ...

  12. Accumulation of hns mutations specifically in stationary phase in an ...

    Indian Academy of Sciences (India)

    Accumulation of hns mutations specifically in stationary phase in an. E. coli strain carrying an impaired rpoS locus. STUTI K. DESAI and S. MAHADEVAN∗. Department of Molecular Reproduction, Development and Genetics, Indian Institute of Science,. Bangalore 560 012, India. Introduction. Interplay between regulators in ...

  13. Evaluation of hydrophilic interaction liquid chromatography stationary phases for analysis of opium alkaloids.

    Science.gov (United States)

    Bagheri, Mohsen; Taheri, Mohammadreza; Farhadpour, Mohsen; Rezadoost, Hassan; Ghassempour, Alireza; Aboul-Enein, Hassan Y

    2017-08-18

    The separation of a mixture containing five major opium alkaloids, namely morphine, codeine, thebaine, noscapine and papaverine has been investigated in hydrophilic interaction liquid chromatography (HILIC) mode using five different stationary phases: bare silica, zwitterion, aminopropyl, diol and cyanopropyl. In order to propose the appropriate column for separation and purification, retention behaviors of the five natural opioids have been studied on mentioned HILIC stationary phases. The mechanism of separation in diverse HILIC media, based on the formation of water-rich layer on surface of the HILIC stationary phases and the physicochemical properties of opium alkaloids, such as pKa (acidic pK) and the octanol-water distribution coefficient (log Do/w) are discussed. Chromatographic responses including modified limit of detection LOD m , signal to noise ratio (S/N) m , and defined modified R Sm have considered for suggestion of the suitable column for quantitative/qualitative and preparative purposes. According to the obtained results, diol stationary phase is best suited for analytical chromatography, whereas bare silica and zwitterionic stationary phases are appropriate for preparative applications. Copyright © 2017 Elsevier B.V. All rights reserved.

  14. Separation of flavonoids on different phenyl-bonded stationary phases-the influence of polar groups in stationary phase structure.

    Science.gov (United States)

    Janas, Petr; Bocian, Szymon; Jandera, Pavel; Kowalkowski, Tomasz; Buszewski, Bogusław

    2016-01-15

    Four phenyl-bonded stationary phases, differing in polar embedded group between spacer and phenyl ring, were used for the separation of flavonoids in reversed-phase conditions. In addition, the work was focused on the comparison of these stationary phases in terms of retention and nature of interactions between flavonoid solutes and both, mobile and stationary phases. The differences and similarities between the columns and between individual flavonoids were evaluated by a statistical analysis. The retention over the wider range of mobile phase composition was described using well known model suggested for partition chromatographic systems. Due to differences in polarity of flavonoids, gradient elution had to be applied to achieve appropriate conditions for the successful separation. A chromatographic optimization software was employed for establish the appropriate profiles of gradient separations using UV detection at 275 nm. The most appropriate conditions for the separation of flavonoids were apparent on the phenyl and phenoxy columns. Copyright © 2015 Elsevier B.V. All rights reserved.

  15. Adsorption behaviors of neutral and ionizable compounds on hybrid stationary phases in the absence (BEH-C18) and the presence (CSH-C18) of immobile surface charges.

    Science.gov (United States)

    Gritti, Fabrice; Guiochon, Georges

    2013-03-22

    The adsorption behaviors of a neutral (caffeine) and a positively charged compound (nortriptylinium) are investigated on two RPLC/hybrid stationary phases, eluted with a low ionic strength buffer (phosphate buffer, W(S)pH 2.63, I=10mM). The first phase, bridge ethylene hybrid (BEH), is neutral at all pHs whereas the second, charged surface hybrid (CSH), contains a protonated ligand at W(W)pH C18 at 20mV and by the subsequent decrease of the equilibrium constant of weak adsorption sites (C18 environment) and removal of the strong adsorption sites (accessible silanols). At the highest sample loadings (5 and 20μL, C=30g/L), the EML and the bi-EML isotherms failed because some adsorbate-adsorbate interactions take place when bulk concentrations exceed 0.2g/L. The experimental data were then successively fitted to an empirical heterogeneous Langmuir-Moreau (LM) explicit isotherm. The best saturation capacities of the empirical heterogeneous LM isotherm is consistent with the manufacturer's estimate of the surface concentration of residual silanols onto the BEH- and CSH-C18 endcapped adsorbent (<0.1μmol/m(2)). Copyright © 2013 Elsevier B.V. All rights reserved.

  16. Axially symmetric, stationary gravitational field equations and pseudospherical surfaces

    International Nuclear Information System (INIS)

    Tomimatsu, Akira.

    1981-04-01

    For axially symmetric, stationary gravitational field equations, a new Lax pair of the inverse scattering method is presented from a geometrical point of view. The metric coefficient e sup(2γ) (= -g sub(rho rho)g sub(tt)sup(-1)) is taken as the basic field variable, which satisfies an equation describing pseudospherical surfaces, i.e., surfaces of constant negative Gaussian curvature. The equations for other metric coefficients are also discussed. (author)

  17. Effects of the surface concentration of fixed charges in C18-bonded stationary phases on the adsorption process and on the preparative chromatography of small ionizable compounds.

    Science.gov (United States)

    Gritti, Fabrice; Guiochon, Georges

    2014-11-06

    The effects of the surface concentration of positive charges attached to the surface of research BEH-C 18 hybrid particles on the overloaded band profiles and the adsorption isotherms of a neutral (caffeine) and a positively charged (nortryptilinium hydrochloride) compounds were measured and investigated. The inverse method (IM) of chromatography was used to determine the isotherm parameters. Three columns were packed with endcapped BEH-C 18 particles doped with three different charge densities on their surfaces (LOW, MEDIUM and HIGH). Two other columns packed with unbonded, non-endcapped, and endcapped BEH-C 18 particles served as standard reference materials. Minor disturbance method (MDM) experiments were conducted with acetonitrile/water mixtures in order to assess qualitatively the surface densities of the fixed positive charges. A more quantitative approach based on the solution of the linearized Poisson-Boltzmann equation and the decrease of the experimental Henry constant was also applied. The results show that the surface concentrations of the fixed charges in the LOW, MEDIUM and HIGH columns were 0.029, 0.050, and 0.064μmol/m 2 , e.g., close to two orders of magnitude smaller than the surface density of bonded C 18 chains (2.1μmol/m 2 ). The adsorption isotherm of the ionizable compound nortryptilinium onto the BEH-C 18 columns is consistent with a two-sites adsorption model. The density of the high energy sites correlates directly to the total amount of the fixed charges and isolated silanols amidst the C 18 -bonded chains. The amount of low energy sites reflects the specific surface area of the adsorbent. The binding constants on the high- and low-energy adsorption sites are respectively ten and two times lower on the HIGH column than on the reference endcapped column. The active sites are closer to the adsorbent surface than the weak adsorption sites. Finally, a higher production rate of ionizable compounds can be achieved in preparative

  18. Kinetic performance of stationary phases for gas chromatography based on poly(oligoethyleneglycoldiacrylate).

    Science.gov (United States)

    Korolev, A; Shyrayeva, V; Popova, T; Kanateva, A; Kurganov, A

    2016-08-19

    Open capillary columns with polymeric stationary phases based on poly(oligoethyleneglycoldiacrylate) were prepared and tested on their kinetic performance. Stationary phases prepared with low molar mass monomers were inferior to stationary phases based on high molar mass monomers. Structure of these stationary phases appeared to be favorable for solute diffusion in the stationary phase. These columns were also characterized by improved kinetic performance limit. Stationary phase based on poly(ethylenglycol) and prepared according to the traditional procedure, demonstrated average kinetic performance. Optimal kinetic performance limit curves characterizing the prepared stationary phases were evaluated in this work using new simple procedure based on extraction of optimal values from the corresponding matrix. This technique makes it possible to evaluate optimal kinetic performance limit curves without any additional simplifications and cumbersome calculations. Copyright © 2016 Elsevier B.V. All rights reserved.

  19. Experimental comparison of chiral metal-organic framework used as stationary phase in chromatography.

    Science.gov (United States)

    Xie, Sheng-Ming; Zhang, Mei; Fei, Zhi-Xin; Yuan, Li-Ming

    2014-10-10

    Chiral metal-organic frameworks (MOFs) are a new class of multifunctional material, which possess diverse structures and unusual properties such as high surface area, uniform and permanent cavities, as well as good chemical and thermal stability. Their chiral functionality makes them attractive as novel enantioselective adsorbents and stationary phases in separation science. In this paper, the experimental comparison of a chiral MOF [In₃O(obb)₃(HCO₂)(H₂O)] solvent used as a stationary phase was investigated in gas chromatography (GC), high-performance liquid chromatography (HPLC) and capillary electrochromatography (CEC). The potential relationship between the structure and components of chiral MOFs with their chiral recognition ability and selectivity are presented. Copyright © 2014 Elsevier B.V. All rights reserved.

  20. Study of Stationary Phase Metabolism Via Isotopomer Analysis of Amino Acids from an Isolated Protein

    Energy Technology Data Exchange (ETDEWEB)

    Shaikh, AfshanS.; Tang, YinjieJ.; Mukhopadhyay, Aindrila; Martin, Hector Garcia; Gin, Jennifer; Benke, Peter; Keasling, Jay D.

    2009-09-14

    Microbial production of many commercially important secondary metabolites occurs during stationary phase, and methods to measure metabolic flux during this growth phase would be valuable. Metabolic flux analysis is often based on isotopomer information from proteinogenic amino acids. As such, flux analysis primarily reflects the metabolism pertinent to the growth phase during which most proteins are synthesized. To investigate central metabolism and amino acids synthesis activity during stationary phase, addition of fully 13C-labeled glucose followed by induction of green fluorescent protein (GFP) expression during stationary phase was used. Our results indicate that Escherichia coli was able to produce new proteins (i.e., GFP) in the stationary phase, and the amino acids in GFP were mostly from degraded proteins synthesized during the exponential growth phase. Among amino acid biosynthetic pathways, only those for serine, alanine, glutamate/glutamine, and aspartate/asparagine had significant activity during the stationary phase.

  1. Escherichia coli adhesive coating as a chiral stationary phase for open tubular capillary electrochromatography enantioseparation

    International Nuclear Information System (INIS)

    Fu, Qifeng; Zhang, Kailian; Gao, Die; Wang, Lujun; Yang, Fengqing; Liu, Yao; Xia, Zhining

    2017-01-01

    Bacteria, the microorganism with intrinsic chirality, have numerous fascinating chiral phenomena such as various chirality-triggered biological processes and behaviors. Herein, bacteria were firstly explored as novel chiral stationary phases in open-tubular capillary electrochromatography (OT-CEC) for enantioseparation of fluoroquinolone enantiomers and simultaneous separation of six fluoroquinolone antibiotics. The model strain, i.e. non-pathogenic Escherichia coli (E. coli) DH5α, was adhered onto the inner surface of positively charged polyethyleneimine (PEI) modified capillaries based on the bacterial adhesion characteristics and strong electrostatic interaction. The morphology and thickness of the bacteria adhesive coatings in the capillary were characterized by field emission scanning electron microscopy (FESEM) and atomic force microscopy (AFM). Baseline separation of ofloxacin and partial separation of lomefloxacin enantiomers could be achieved by the E. coli coated columns. The preparation parameters including the coating time and concentration of bacteria that affecting the chiral resolution were intensively investigated. The electrophoretic parameters, including pH, buffer concentration and applied voltage, were also optimized. The developed method was validated (linearity, LOD, LOQ, intra-day, inter-day and column-to-column repeatability and recovery) and successfully utilized for the quantitative analysis of ofloxacin enantiomers in the ofloxacin tablets. Moreover, only a slight decrease in the separation efficiency was observed after 90 consecutive runs on the E. coli@capillary. These results demonstrated that bacteria are promising stationary phases for chiral separation in CEC. - Highlights: • Bacteria were firstly introduced in OT-CEC as a chiral stationary phase for chiral separation. • Enantioseparation of ofloxacin enantiomers was achieved on E. coli coated open tubular capillary column. • Bacterial stationary phases may be used to

  2. Escherichia coli adhesive coating as a chiral stationary phase for open tubular capillary electrochromatography enantioseparation

    Energy Technology Data Exchange (ETDEWEB)

    Fu, Qifeng, E-mail: fuqifeng1990@163.com [Department of Medicinal Chemistry, Southwest Medical University, Luzhou 646000 (China); Zhang, Kailian; Gao, Die; Wang, Lujun [Department of Medicinal Chemistry, Southwest Medical University, Luzhou 646000 (China); Yang, Fengqing; Liu, Yao [School of Chemistry and Chemical Engineering, Chongqing University, Chongqing 400030 (China); Xia, Zhining, E-mail: tcm_anal_cqu@163.com [Innovative Drug Research Centre and School of Pharmaceutical Sciences, Chongqing University, Chongqing 400030 (China); School of Chemistry and Chemical Engineering, Chongqing University, Chongqing 400030 (China)

    2017-05-29

    Bacteria, the microorganism with intrinsic chirality, have numerous fascinating chiral phenomena such as various chirality-triggered biological processes and behaviors. Herein, bacteria were firstly explored as novel chiral stationary phases in open-tubular capillary electrochromatography (OT-CEC) for enantioseparation of fluoroquinolone enantiomers and simultaneous separation of six fluoroquinolone antibiotics. The model strain, i.e. non-pathogenic Escherichia coli (E. coli) DH5α, was adhered onto the inner surface of positively charged polyethyleneimine (PEI) modified capillaries based on the bacterial adhesion characteristics and strong electrostatic interaction. The morphology and thickness of the bacteria adhesive coatings in the capillary were characterized by field emission scanning electron microscopy (FESEM) and atomic force microscopy (AFM). Baseline separation of ofloxacin and partial separation of lomefloxacin enantiomers could be achieved by the E. coli coated columns. The preparation parameters including the coating time and concentration of bacteria that affecting the chiral resolution were intensively investigated. The electrophoretic parameters, including pH, buffer concentration and applied voltage, were also optimized. The developed method was validated (linearity, LOD, LOQ, intra-day, inter-day and column-to-column repeatability and recovery) and successfully utilized for the quantitative analysis of ofloxacin enantiomers in the ofloxacin tablets. Moreover, only a slight decrease in the separation efficiency was observed after 90 consecutive runs on the E. coli@capillary. These results demonstrated that bacteria are promising stationary phases for chiral separation in CEC. - Highlights: • Bacteria were firstly introduced in OT-CEC as a chiral stationary phase for chiral separation. • Enantioseparation of ofloxacin enantiomers was achieved on E. coli coated open tubular capillary column. • Bacterial stationary phases may be used to

  3. Population Dynamics of the Stationary Phase Utilizing the ARGOS Method

    Science.gov (United States)

    Algarni, S.; Charest, A. J.; Iannacchione, G. S.

    2015-03-01

    The Area Recorded Generalized Optical Scattering (ARGOS) approach to light scattering employs large image capture array allowing for a well-defined geometry in which images may be manipulated to extract structure with intensity at a specific scattering wave vector (I(q)) and dynamics with intensity at a specific scattering wave vector over time (I (q,t)). The ARGOS method provides morphological dynamics noninvasively over a long time period and allows for a variety of aqueous conditions. This is important because traditional growth models do not provide for conditions similar to the natural environment. The present study found that the population dynamics of bacteria do not follow a traditional growth model and that the ARGOS method allowed for the observation of bacterial changes in terms of individual particles and population dynamics in real time. The observations of relative total intensity suggest that there is no stationary phase and that the bacterial population demonstrates sinusoidal type patterns consistently subsequent to the log phase growth. These observation were compared to shape changes by modeling fractal dimension and size changes by modeling effective radius.

  4. A new methodology to determine the isoeluotropic conditions on ultra-performance flash purification stationary phases from analytical reversed liquid chromatography stationary phase.

    Science.gov (United States)

    Héron, Sylvie; Charbonneau, Didier; Albisson, Pauline; Estievenart, Guillaume; Groni, Sihem; Tchapla, Alain

    2015-06-05

    Nowadays, the determination of the experimental chromatographic conditions to be used in Reversed Phase Liquid Ultra-Performance Flash Purification is still challenging. This is due to four different items. In most cases, flash purification stationary phases are not available with geometry of column used in analytical chromatography. The flash purification columns are single-use only. From the point of view of selectivity and retention, few RPLC phases exist with properties of separation identical for analytical and flash purification supports. Characterization methods and databases used for comparing analytical RPLC columns do not include stationary phases for RP flash purification columns. The goal of this work is to develop a new method development strategy which permits the determination of the experimental chromatographic conditions on RP ultra-performance flash purification columns. It relies on the knowledge of any isocratic conditions obtained on any given initial reversed stationary phase. The final conditions to implement on the RP ultra-performance flash purification phase enable either to keep the retention range of a selected solute constant, or to set it around a previously chosen value. The rules of transfer in linear gradient mode are also described. The methodology was valid, whatever the initial RP stationary and mobile phases, for different chemical classes, whatever the bonding, particle diameter, porous or core shell particle, towards different RP alkyl and analogues stationary and mobile phases. Copyright © 2015 Elsevier B.V. All rights reserved.

  5. An integrated fritless column for on-chip capillary electrochromatography with conventional stationary phases

    NARCIS (Netherlands)

    Ceriotti, Laura; De Rooij, Nico F.; Verpoorte, Elisabeth

    2002-01-01

    A new polymer device for use with conventional particulate stationary phases for on-chip, fritless, capillary electrochromatography (CEC) has been realized. The structure includes an injector and a tapered column in which the particles of the stationary phase are retained and stabilized. The chips

  6. The method of stationary phase and the method of Fresnel zones

    NARCIS (Netherlands)

    Kampen, N.G. van

    1958-01-01

    The method of stationary phase is discussed and reasons are given why it is often preferable to the method of steepest descent, in spite of the mathematicians' partiality to the latter. The method of Fresnel zones is compared with the method of stationary phase and is shown to be a primitive version

  7. Thermal and Hydrothermal Treatment of Silica Gels as Solid Stationary Phases in Gas Chromatography

    Directory of Open Access Journals (Sweden)

    Ashraf Yehia El-Naggar

    2013-01-01

    Full Text Available Silica gel was prepared and treated thermally and hydrothermally and was characterized as solid stationary phase in gas chromatography. The characteristics have been evaluated in terms of polarity, selectivity, and separation efficiencies. These parameters were used to assess the outer silica surface contributions and the degree of surface deactivation brought about by different treatment techniques. The parent silica elutes the paraffinic hydrocarbons with high efficiency of separation and elutes aromatic hydrocarbons with nearly good separation and has bad separation of alcohols. The calcined silica at 500°C and 1000°C has a pronounced effect on the separation of aromatic hydrocarbons compared with the parent silica and hydrothermal treatment of silica. With respect to alcohols separation, the obtained bad separations using treated and untreated silica reflect the little effect of the thermal and hydrothermal treatment on the silica surface deactivation.

  8. Ceramic stationary gas turbine development. Final report, Phase 1

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    1994-09-01

    This report summarizes work performed by Solar Turbines Inc. and its subcontractors during the period September 25, 1992 through April 30, 1993. The objective of the work is to improve the performance of stationary gas turbines in cogeneration through implementation of selected ceramic components.

  9. Detection of hidden stationary deformations of vibrating surfaces by use of time-averaged digital holographic interferometry.

    Science.gov (United States)

    Demoli, Nazif; Vukicevic, Dalibor

    2004-10-15

    A method of detecting displacements of a surface from its steady-state position to its equilibrium position while it is vibrating has been developed by use of time-average digital holographic interferometry. This method permits extraction of such a hidden deformation by creating two separated systems of interferogram fringes: one corresponding to a time-varying resonantly oscillating optical phase, the other to the stationary phase modification. A mathematical description of the method and illustrative results of experimental verification are presented.

  10. The proteomics of quiescent and nonquiescent cell differentiation in yeast stationary-phase cultures.

    Science.gov (United States)

    Davidson, George S; Joe, Ray M; Roy, Sushmita; Meirelles, Osorio; Allen, Chris P; Wilson, Melissa R; Tapia, Phillip H; Manzanilla, Elaine E; Dodson, Anne E; Chakraborty, Swagata; Carter, Mark; Young, Susan; Edwards, Bruce; Sklar, Larry; Werner-Washburne, Margaret

    2011-04-01

    As yeast cultures enter stationary phase in rich, glucose-based medium, differentiation of two major subpopulations of cells, termed quiescent and nonquiescent, is observed. Differences in mRNA abundance between exponentially growing and stationary-phase cultures and quiescent and nonquiescent cells are known, but little was known about protein abundance in these cells. To measure protein abundance in exponential and stationary-phase cultures, the yeast GFP-fusion library (4159 strains) was examined during exponential and stationary phases, using high-throughput flow cytometry (HyperCyt). Approximately 5% of proteins in the library showed twofold or greater changes in median fluorescence intensity (abundance) between the two conditions. We examined 38 strains exhibiting two distinct fluorescence-intensity peaks in stationary phase and determined that the two fluorescence peaks distinguished quiescent and nonquiescent cells, the two major subpopulations of cells in stationary-phase cultures. GFP-fusion proteins in this group were more abundant in quiescent cells, and half were involved in mitochondrial function, consistent with the sixfold increase in respiration observed in quiescent cells and the relative absence of Cit1p:GFP in nonquiescent cells. Finally, examination of quiescent cell-specific GFP-fusion proteins revealed symmetry in protein accumulation in dividing quiescent and nonquiescent cells after glucose exhaustion, leading to a new model for the differentiation of these cells.

  11. Synthesis and characterization of mesoporous silica modified with chiral auxiliaries for their potential application as chiral stationary phase.

    Science.gov (United States)

    Mayani, Vishal J; Abdi, S H R; Kureshy, R I; Khan, N H; Agrawal, Santosh; Jasra, R V

    2008-05-16

    Novel chiral stationary phase (CSP) based on chiral aminoalcohol immobilized on ordered mesoporous silica SBA-15 1a and standard silica 1b and their copper complexes 1a' and 1b', respectively, was synthesized as potential material for chiral ligand exchange chromatography (CLEC). Microanalysis, inductively coupled plasma spectroscopy (ICP), thermo-gravimetric analysis (TGA), cross polarized magic angle spinning (CP-MAS) (13)C NMR, Powder X-ray diffraction (PXRD), FTIR, N(2) adsorption isotherm, scanning electron microscopy (SEM), transmitted electron microscope (TEM) and solid reflectance UV-vis spectroscopy were used to characterize these materials. All the chiral stationary phases thus synthesized were used for the separation of different racemic compounds such as mandelic acid, 2,2'-dihydroxy-1,1'-binaphthalene BINOL) and diethyl tartrate by simple medium-pressure column chromatography. Successful enantio-separation of racemic mandelic acid was achieved with all the stationary phases but 1a and 1b gave slightly better resolution than their copper complexes 1a' and 1b'. Remarkably these materials are stable under the given experimental conditions and can be used repeatedly for several cycles of enantioresolution. It was observed that the porosity and surface area of the stationary phase play an important role in the chiral separation.

  12. Recombinant Staphylococcal protein A with cysteine residue for preparation of affinity chromatography stationary phase and immunosensor applications

    Directory of Open Access Journals (Sweden)

    Gorbatiuk O. B.

    2015-04-01

    Full Text Available Aim. Engineering of recombinant Staphylococcal protein A with cysteine residue (SPA-Cys for preparation of affinity chromatography stationary phase and formation of bioselective element of immunosensor. Methods. DNA sequences encoding IgG-binding region of SPA, His-tag and cysteine were genetically fused and expressed in E. coli. SPA-Cys was immobilized on maleimide-functionalized silica beads for affinity chromatography stationary phase preparation and on a gold sensor surface as a bioselective element of immunosensor. Results. SPA-Cys was expressed at a high-level in a soluble form. The target protein was purified and showed a high IgG-binding activity. The capacity of the obtained SPA-Cys-based affinity chromatography stationary phase was 10–12 mg of IgG /ml. The purity of eluted IgG was more than 95 % in one-step purification procedure. The developed SPA-Cys-based bioselective element of immunosensor selectively interacted with human IgG and did not interact with the control proteins. Conclusions. The recombinant Staphylococcal protein A with cysteine residue was successfully used for the preparation of affinity chromatography stationary phase and formation of the bioselective element of immunosensor.

  13. Carbon nanotube based stationary phases for microchip chromatography

    DEFF Research Database (Denmark)

    Mogensen, Klaus Bo; Kutter, Jörg Peter

    2012-01-01

    already been demonstrated in more classical formats, for improved separation performance in gas and liquid chromatography, and for unique applications in solid phase extraction. Carbon nanotubes are now also entering the field of microfluidics, where there is a large potential to be able to provide......The objective of this article is to provide an overview and critical evaluation of the use of carbon nanotubes and related carbon-based nanomaterials for microchip chromatography. The unique properties of carbon nanotubes, such as a very high surface area and intriguing adsorptive behaviour, have...... integrated, tailor-made nanotube columns by means of catalytic growth of the nanotubes inside the fluidic channels. An evaluation of the different implementations of carbon nanotubes and related carbon-based nanomaterials for microfluidic chromatography devices is given in terms of separation performance...

  14. Alkali Metal Modification of Silica Gel-Based Stationary Phase in Gas Chromatography

    Directory of Open Access Journals (Sweden)

    Ashraf Yehia El-Naggar

    2013-01-01

    Full Text Available Modification of the precipitated silica gel was done by treatment with alkali metal (NaCl before and after calcination. The silica surfaces before and after modification were confirmed by infrared spectroscopy in order to observe the strength and abundance of the acidic surface OH group bands which play an important role in the adsorption properties of polar and nonpolar solutes. The surface-modified silica gels were tested as GC solid stationary phases in terms of the separation efficiency for various groups of non-polar and polar solutes. Also, thermodynamic parameters (ΔH, ΔG, and ΔS were determined using n-hexane as a probe in order to show the adsorbate-adsorbent interaction. It was observed that the non-polar solutes could be separated Independent on the reactivity and porosity of the silica surfaces. The efficiency of the surface-modified silica gels to separate the aromatic hydrocarbons seemed to be strongly influenced by the density of the surface hydroxyls.

  15. Evaluating the robustness of the enantioselective stationary phases on the Rosetta mission against space vacuum vaporization

    Science.gov (United States)

    Meierhenrich, Uwe J.; Cason, Julie R. L.; Szopa, Cyril; Sternberg, Robert; Raulin, François; Thiemann, Wolfram H.-P.; Goesmann, Fred

    2013-12-01

    The European Space Agency's Rosetta mission was launched in March 2004 in order to reach comet 67P/Churyumov-Gerasimenko by August 2014. The Cometary Sampling and Composition experiment (COSAC) onboard the Rosetta mission's lander "Philae" has been designed for the cometary in situ detection and quantification of organic molecules using gas chromatography coupled to mass spectrometry (GC-MS). The GC unit of COSAC is equipped with eight capillary columns that will each provide a specific stationary phase for molecular separation. Three of these stationary phases will be used to chromatographically resolve enantiomers, as they are composed of liquid polymers of polydimethylsiloxane (PDMS) to which chiral valine or cyclodextrin units are attached. Throughout the ten years of Rosetta's journey through space to reach comet 67P, these liquid stationary phases have been exposed to space vacuum, as the capillary columns within the COSAC unit were not sealed or filled with carrier gas. Long term exposures to space vacuum can cause damage to such liquid stationary phases as key monomers, volatiles, and chiral selectors can be vaporized and lost in transit. We have therefore exposed identical spare units of COSAC's chiral stationary phases over eight years to vacuum conditions mimicking those experienced in space and we have now investigated their resolution capabilities towards different enantiomers both before and after exposure to space vacuum environments. We have observed that enantiomeric resolution capabilities of these chiral liquid enantioselective stationary phases has not been affected by exposure to space vacuum conditions. Thus we conclude that the three chiral stationary phases of the COSAC experiment onboard the Rosetta mission lander "Philae" can be considered to have maintained their resolution capacities throughout their journey prior to cometary landing in November 2014.

  16. Application of the zeta potential for stationary phase characterization in ion chromatography.

    Science.gov (United States)

    Buszewski, Bogusław; Jaćkowska, Magdalena; Bocian, Szymon; Dziubakiewicz, Ewelina

    2013-01-01

    Two series of homemade stationary bonded phases for ion chromatography were investigated according to their zeta potential. One set of dendrimer anion exchanger was synthesized on the polymer support whereas the second material was prepared on the silica gel. The zeta potential data in water environment as well as buffered water solution were obtained. The influence of the length of anion-exchanger chains, the type of the support of the modified surface, and charge distribution on these data was investigated. Additionally, the zeta potential was correlated with retention factor of inorganic ions to describe their influence on the retention mechanism in ion chromatography. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. A new 14-membered tetraazamacrocycle-bonded silica stationary phase for reversed-phase high-performance liquid chromatography.

    Science.gov (United States)

    He, Lijun; Zhang, Mingliang; Zhao, Wenjie; Liu, Jie; Jiang, Xiuming; Zhang, Shusheng; Qu, Lingbo

    2012-01-30

    A new high-performance liquid chromatography stationary phase has been prepared by covalently bonding 14-membered tetraazamacrocycle to silica gel using γ-chloropropyltrimethoxylsilane as coupling agent. The structure of the new material was characterized by infrared spectroscopy and elemental analysis. With 32 solutes including aromatic and aliphatic compounds, the linear solvation energy relationship method was successfully used to chromatographically evaluate the new phase in reversed phase mode. The retention property of the new phase shows evident similarity with that of ODS stationary phase, as well as distinctive, unique retention characteristics. The separations of n-alkylbenzene, carbamate and organophosphorus pesticides with diversified functional groups as well as phenolic compounds demonstrate that in addition to hydrophobic interaction, dipole-dipole interaction and hydrogen bonding interaction plus acid-base equilibrium could also be simultaneously offered by this new stationary phase, as a result excellent chromatographic performances are guaranteed. Copyright © 2011 Elsevier B.V. All rights reserved.

  18. Evaluation of gamma radiation effects on stationary phases using gas chromatografy

    International Nuclear Information System (INIS)

    Basso, M.A.; Collins, K.E.; Collins, C.H.

    1988-01-01

    The overall objetive of this project is a thorough study of the effect of gamma radiation on supported stationary phases used in packed-column gas chromatography. The phases studied were SP-2100 on Supelcoport and SE-30 on Chromsorb W. The fases were irradiated with cobalt-60 gamma rays to various doses and subsequently subjected to tests of extractability, termal stability and efficiency as a chromatographic column packing. Extraction tests indicate that low doses of radiation are sufficient to produce significant immobilization of these polymethylsilicones; that is, to produce chemical bonds between different polymer chains or between the stationary phase and the support. Thermal stability is also increased. The values calculated for the number of theoretical plates (n) and resolution (Rsub (s)) after analysis of four synthetic mixtures of organic compounds also increase, in most cases, indicating that the gamma irradiation has positively altered the behavior of these stationary phases. (author) [pt

  19. Comparison of GC stationary phases for the separation of fatty acid methyl esters in biodiesel fuels.

    Science.gov (United States)

    Goding, Julian C; Ragon, Dorisanne Y; O'Connor, Jack B; Boehm, Sarah J; Hupp, Amber M

    2013-07-01

    The fatty acid methyl ester (FAME) content of biodiesel fuels has traditionally been determined using gas chromatography with a polar stationary phase. In this study, a direct comparison of the separation of FAMEs present in various biodiesel samples on three polar stationary phases and one moderately polar stationary phase (with comparable column dimensions) was performed. Retention on each column was based on solubility in and polarity of the phase. Quantitative metrics describing the resolution of important FAME pairs indicate high resolution on all polar columns, yet the best resolution, particularly of geometric isomers, is achieved on the cyanopropyl column. In addition, the separation of four C18 monounsaturated isomers was optimized and the elution order determined on each column. FAME composition of various biodiesel fuel types was determined on each column to illustrate (1) chemical differences in biodiesels produced from different feedstocks and (2) chemical similarities in biodiesels of the same feedstock type produced in different locations and harvest seasons.

  20. Enantiomeric Resolution of Drugs and Metabolites in Polysaccharide- and Protein-Based Chiral Stationary Phases

    Directory of Open Access Journals (Sweden)

    Bonato Pierina S.

    2002-01-01

    Full Text Available Several chiral stationary phases based on polysaccharide derivatives and proteins were evaluated for the resolution of some chiral drugs and their metabolites. The polysaccharide-based stationary phases CHIRALCEL OD-H, CHIRALCEL OB-H, CHIRALCEL OJ, CHIRALPAK AD and CHIRALPAK AS were evaluated under normal phase conditions, using hexane:2-propanol or hexane:ethanol as mobile phase. Diethylamine and trifluoracetic acid were also added to improve peak shape. The CHIRALCEL OJ-R, CHIRALCEL OD-R and CHIRALCEL OD-H columns were evaluated under reversed-phase conditions, using acetonitrile:H2O or acetonitrile:NaClO4 solution. The protein- based stationary phases, CHIRAL AGP and ULTRON ES-OVM columns were used with mobile phases consisting of a buffer solution supplemented with an organic modifier. Among the polysaccharide-based stationary phases, CHIRALPAK AD provided better resolution for almost all drugs and metabolites studied. The ULTRON ES-OVM column was particularly suitable for the resolution of the four enantiomers of thioridazine-2-sulfoxide.

  1. The upper surface of an Escherichia coli swarm is stationary.

    Science.gov (United States)

    Zhang, Rongjing; Turner, Linda; Berg, Howard C

    2010-01-05

    When grown in a rich medium on agar, many bacteria elongate, produce more flagella, and swim in a thin film of fluid over the agar surface in swirling packs. Cells that spread in this way are said to swarm. The agar is a solid gel, with pores smaller than the bacteria, so the swarm/agar interface is fixed. Here we show, in experiments with Escherichia coli, that the swarm/air interface also is fixed. We deposited MgO smoke particles on the top surface of an E. coli swarm near its advancing edge, where cells move in a single layer, and then followed the motion of the particles by dark-field microscopy and the motion of the underlying cells by phase-contrast microscopy. Remarkably, the smoke particles remained fixed (diffusing only a few micrometers) while the swarming cells streamed past underneath. The diffusion coefficients of the smoke particles were smaller over the virgin agar ahead of the swarm than over the swarm itself. Changes between these two modes of behavior were evident within 10-20 microm of the swarm edge, indicating an increase in depth of the fluid in advance of the swarm. The only plausible way that the swarm/air interface can be fixed is that it is covered by a surfactant monolayer pinned at its edges. When a swarm is exposed to air, such a monolayer can markedly reduce water loss. When cells invade tissue, the ability to move rapidly between closely opposed fixed surfaces is a useful trait.

  2. Metal-Organic Framework Thin Films as Stationary Phases in Microfabricated Gas-Chromatography Columns.

    Energy Technology Data Exchange (ETDEWEB)

    Read, Douglas [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States); Sillerud, Colin Halliday [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)

    2016-01-01

    The overarching goal of this project is to integrate Sandia's microfabricated gas-chromatography ( GC) columns with a stationary phase material that is capable of retaining high-volatility chemicals and permanent gases. The successful integration of such a material with GCs would dramatically expand the repertoire of detectable compounds for Sandia's various microanalysis systems. One such promising class of candidate materials is metal-organic frameworks (MOFs). In this report we detail our methods for controlled deposition of HKUST-1 MOF stationary phases within GC columns. We demonstrate: the chromatographic separation of natural gas; a method for determining MOF film thickness from chromatography alone; and the first-reported GC x GC separation of natural gas -- in general -- let alone for two disparate MOF stationary phases. In addition we determine the fundamental thermodynamic constant for mass sorption, the partition coefficient, for HKUST-1 and several light hydrocarbons and select toxic industrial chemicals.

  3. NHEJ enzymes LigD and Ku participate in stationary-phase mutagenesis in Pseudomonas putida.

    Science.gov (United States)

    Paris, Ülvi; Mikkel, Katren; Tavita, Kairi; Saumaa, Signe; Teras, Riho; Kivisaar, Maia

    2015-07-01

    Under growth-restricting conditions bacterial populations can rapidly evolve by a process known as stationary-phase mutagenesis. Bacterial nonhomologous end-joining (NHEJ) system which consists of the DNA-end-binding enzyme Ku and the multifunctional DNA ligase LigD has been shown to be important for survival of bacteria especially during quiescent states, such as late stationary-phase populations or sporulation. In this study we provide genetic evidence that NHEJ enzymes participate in stationary-phase mutagenesis in a population of carbon-starved Pseudomonas putida. Both the absence of LigD or Ku resulted in characteristic spectra of stationary-phase mutations that differed from each other and also from the wild-type spectrum. This indicates that LigD and Ku may participate also in mutagenic pathways that are independent from each other. Our results also imply that both phosphoesterase (PE) and polymerase (POL) domains of the LigD protein are involved in the occurrence of mutations in starving P. putida. The participation of both Ku and LigD in the occurrence of stationary-phase mutations was further supported by the results of the analysis of mutation spectra in stationary-phase sigma factor RpoS-minus background. The spectra of mutations identified in the RpoS-minus background were also distinct if LigD or Ku was absent. Interestingly, the effects of the presence of these enzymes on the frequency of occurrence of certain types of mutations were different or even opposite in the RpoS-proficient and deficient backgrounds. These results imply that RpoS affects performance of mutagenic pathways in starving P. putida that utilize LigD and/or Ku. Copyright © 2015. Published by Elsevier B.V.

  4. Nanocellulose Derivative/Silica Hybrid Core-Shell Chiral Stationary Phase: Preparation and Enantioseparation Performance

    Directory of Open Access Journals (Sweden)

    Xiaoli Zhang

    2016-05-01

    Full Text Available Core-shell silica microspheres with a nanocellulose derivative in the hybrid shell were successfully prepared as a chiral stationary phase by a layer-by-layer self-assembly method. The hybrid shell assembled on the silica core was formed using a surfactant as template by the copolymerization reaction of tetraethyl orthosilicate and the nanocellulose derivative bearing triethoxysilyl and 3,5-dimethylphenyl groups. The resulting nanocellulose hybrid core-shell chiral packing materials (CPMs were characterized and packed into columns, and their enantioseparation performance was evaluated by high performance liquid chromatography. The results showed that CPMs exhibited uniform surface morphology and core-shell structures. Various types of chiral compounds were efficiently separated under normal and reversed phase mode. Moreover, chloroform and tetrahydrofuran as mobile phase additives could obviously improve the resolution during the chiral separation processes. CPMs still have good chiral separation property when eluted with solvent systems with a high content of tetrahydrofuran and chloroform, which proved the high solvent resistance of this new material.

  5. Photochemically Immobilized 4-Methylbenzoyl Cellulose as a Powerful Chiral Stationary Phase for Enantioselective Chromatography

    Directory of Open Access Journals (Sweden)

    Eric Francotte

    2016-12-01

    Full Text Available A process to immobilize para-methylbenzoyl cellulose (PMBC on silica gel has been developed and applied to prepare chiral stationary phases (CSPs for enantioselective chromatography. The immobilization was achieved by simple irradiation of the polysaccharide derivative with ultraviolet light after coating on a silica gel support. The influence of parameters such as irradiation time and solvent on immobilization effectiveness were investigated. The performance of the prepared immobilized phases were evaluated by injection of a series of racemic compounds onto the packed columns and determination of their chiral recognition ability. By contrast to the classical coated phase, the immobilized CSP can be used under various chromatographic conditions without limitation of organic solvent types as the mobile phase. This extended applicability permits to improve selectivity and to resolve chiral compounds which are not or only poorly soluble in the mobile phases which are compatible with the non-immobilized PMBC stationary phase.

  6. Preparation of a ribonucleic acid-(polyamidoamine)-(zirconia-urea-formaldehyde resin) high-performance liquid affinity chromatographic stationary phase.

    Science.gov (United States)

    Lei, S; Yu, S; Zhao, C

    2001-07-01

    A preparative method for a high-performance liquid affinity chromatographic (HPLAC) stationary phase is described. The 3- to 5-microm nonporous composite spherical microparticles of zirconia and urea-formaldehyde (UF) resin are synthesized through the reaction of zirconyl chloride with hexamethylene tetra-amine and urea, and then it is used as the matrix of the HPLAC stationary phase of which the diameter and structure are determined by scanning electron microscopy. In a methanol medium, the polyamidoamine (PAMAM) starburst dentritic spacer arms are linked with the imido-groups on the surface of the matrix by the Michael addition reaction with methyl acrylate and the amination reaction with ethylene diamine. After repeating these steps in triplets, amine-terminated dentritic spacer arms with a generation of 3 are obtained. The topological structure of the spacer arms is examined by solid-state 13C NMR. The Br-substituted ribonucleic acid (RNA) ligand is obtained by the reaction of liquid bromine with RNA and bonded to the dendritic spacer arms of the matrix in a solution of NaOH (pH 9-11). The binding capacity of RNA is measured by UV spectrophotometry. A new type of stationary phase--RNA-(PAMAM)-(zirconia-UF resin--for HPLAC, which possesses starburst dendritic spacer arms, is synthesized and used for the separation of biological macromolecules.

  7. Profiling of Campylobacter jejuni Proteome in Exponential and Stationary Phase of Growth

    Directory of Open Access Journals (Sweden)

    Hana Turonova

    2017-05-01

    Full Text Available Campylobacter jejuni has been reported as a major cause of bacterial food-borne enteritides in developed countries during the last decade. Despite its fastidious growth requirements, including low level of oxygen and high level of CO2, this pathogen is able to persist in the environment without permanent loss of its viability and virulence. As C. jejuni is not able to multiply outside a host, the cells spend significant amount of time in stationary phase of growth. The entry into the stationary phase is often correlated to resistance to various stresses in bacteria. The switching between exponential and stationary phases is frequently mediated by the regulator sigma S (RpoS. However, this factor is absent in C. jejuni and molecular mechanisms responsible for transition of cells to the stationary phase remain elusive. In this work, proteomic profiles of cells from exponential and stationary phases were compared using 2-D electrophoresis (2DE fingerprinting combined with mass spectrometry analysis and qRT-PCR. The identified proteins, whose expression differed between the two phases, are mostly involved in protein biosynthesis, carbon metabolism, stress response and motility. Altered expression was observed also in the pleiotropic regulator CosR that was over-expressed during stationary phase. A shift between transcript and protein level evolution of CosR throughout the growth of C. jejuni was observed using qRT-PCR and (2DE. From these data, we hypothesized that CosR could undergo a negative autoregulation in stationary phase. A consensus sequence resulting from promoter sequence alignment of genes potentially regulated by CosR, including its own upstream region, among C. jejuni strains is proposed. To verify experimentally the potential autoregulation of CosR at the DNA level, electrophoretic mobility shift assay was performed with DNA fragments of CosR promoter region and rCosR. Different migration pattern of the promoter fragments indicates

  8. [Using barium fluoride fine particles as stationary phase for TLC/FTIR analysis].

    Science.gov (United States)

    Liu, Xi; Pan, Qing-hua; Ding, Jie; Zhu, Qing; He, An-qi; Yue, Shi-juan; Li, Xiao-pei; Hu, Li-ping; Xia, Jin-ming; Liu, Cui-ge; Wei, Yong-ju; Yu, Jiang; Yang, Zhan-lan; Zhu, Xi; Xu, Yi-zhuang; Wu, Jin-guang

    2011-07-01

    In situ TLC/FTIR technique has tremendous potential in the analysis of complex mixtures. However, the progress in this technique was quite slow. The reason is that conventional stationary phase such as silica gel etc. has strong absorption in FTIR spectrum and thus brings about severe interference in the detection of samples. To solve the problem, the authors propose to use barium fluoride fine particles as stationary phase of TLC plate. The reasons are as follows: Barium fluoride wafer has been extensively used as infrared window in FTIR experiments and it has no absorbance in an IR region between 4 000 and 800 cm'. As a matter of fact, the atomic mass of barium and fluoride is quite large, thus the normal vibration of BaF2 lattice is limited in far-IR region and low frequency part of mid-IR region. Therefore, the interference caused by IR absorption of stationary phase can be resolved if BaF2 is used as stationary phase of TLC plate. Moreover, BaF2 is quite stable and insolvable in water and most organic solvents and it will not be dissolved by mobile phase or react with samples in TLC separation. Additionally, decreasing the particle size of BaF2 is very important in TLC/FTIR analysis technique. The reason is two-fold: First, decreasing the particle size of stationary phase is helpful to improving the efficiency of separation by TLC plate; second, decreasing the size of BaFz particle can improve the quality of FTIR spectra by alleviating the problem of light scattering. By optimizing the synthetic conditions, fine particles of barium fluoride were obtained. SEM results indicate that the size of the BaF2 particles is around 500 nm. FTIR spectrum of the BaF2 particles shows that no absorption of impurity was observed. Moreover, the elevation of baseline caused by light scattering is insignificant. The authors have developed a new technique named "settlement volatilization method" to prepare TLC plate without polymeric adhesive that may bring about significant

  9. Convergence to stationary solutions for a parabolic-hyperbolic phase-field system

    Czech Academy of Sciences Publication Activity Database

    Grasselli, M.; Petzeltová, Hana; Schimperna, G.

    2006-01-01

    Roč. 5, č. 4 (2006), s. 827-838 ISSN 1534-0392 R&D Projects: GA AV ČR(CZ) IAA1019302 Institutional research plan: CEZ:AV0Z10190503 Keywords : phase-field models * convergence to stationary solutions * Łojasiewicz-Simon inequality Subject RIV: BA - General Mathematics Impact factor: 0.857, year: 2006

  10. Silica, alumina and aluminosilicates as solid stationary phases in gas chromatography

    Directory of Open Access Journals (Sweden)

    S. Faramawy

    2016-09-01

    Full Text Available Silica, alumina and Aluminosilicates of different Si/Al ratios were prepared by conventional precipitation or co-precipitation methods and then subjected to thermal treatment at 800 °C. The parent and thermally treated materials were characterized by means of FTIR, SEM and thermal analysis (DTA and TGA in order to elucidate the main structural properties. Surface textural characteristics were investigated by means of nitrogen adsorption–desorption isotherms at −196 °C. Pore size distribution curves indicated the presence of mesopores (10–150 Å exhibiting maxima at 35 Å. The maxima were shifted toward higher values by increasing the alumina content. Thermodynamic parameters, ΔH, ΔG and ΔS, were determined by means of inverse gas chromatography using n-hexane as a probe. The untreated and thermally treated materials were tested as solid stationary phases in gas chromatography. The separation efficiency of various non polar and polar compounds was explained in terms of surface texture and thermodynamic parameters.

  11. Carbon nanotube based stationary phases for microchip chromatography

    DEFF Research Database (Denmark)

    Mogensen, Klaus Bo; Kutter, Jörg Peter

    2012-01-01

    The objective of this article is to provide an overview and critical evaluation of the use of carbon nanotubes and related carbon-based nanomaterials for microchip chromatography. The unique properties of carbon nanotubes, such as a very high surface area and intriguing adsorptive behaviour, have...... integrated, tailor-made nanotube columns by means of catalytic growth of the nanotubes inside the fluidic channels. An evaluation of the different implementations of carbon nanotubes and related carbon-based nanomaterials for microfluidic chromatography devices is given in terms of separation performance...

  12. Nanomaterials as stationary phases and supports in liquid chromatography.

    Science.gov (United States)

    Beeram, Sandya R; Rodriguez, Elliott; Doddavenkatanna, Suresh; Li, Zhao; Pekarek, Allegra; Peev, Darin; Goerl, Kathryn; Trovato, Gianfranco; Hofmann, Tino; Hage, David S

    2017-10-01

    The development of various nanomaterials over the last few decades has led to many applications for these materials in liquid chromatography (LC). This review will look at the types of nanomaterials that have been incorporated into LC systems and the applications that have been explored for such systems. A number of carbon-based nanomaterials and inorganic nanomaterials have been considered for use in LC, ranging from carbon nanotubes, fullerenes and nanodiamonds to metal nanoparticles and nanostructures based on silica, alumina, zirconia and titanium dioxide. Many ways have been described for incorporating these nanomaterials into LC systems. These methods have included covalent immobilization, adsorption, entrapment, and the synthesis or direct development of nanomaterials as part of a chromatographic support. Nanomaterials have been used in many types of LC. These applications have included the reversed-phase, normal-phase, ion-exchange, and affinity modes of LC, as well as related methods such as chiral separations, ion-pair chromatography and hydrophilic interaction liquid chromatography. Both small and large analytes (e.g., dyes, drugs, amino acids, peptides and proteins) have been used to evaluate possible applications for these nanomaterial-based methods. The use of nanomaterials in columns, capillaries and planar chromatography has been considered as part of these efforts. Potential advantages of nanomaterials in these applications have included their good chemical and physical stabilities, the variety of interactions many nanomaterials can have with analytes, and their unique retention properties in some separation formats. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Exploitation of a microporous organic polymer as a stationary phase for capillary gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Lu, Cuiming; Liu, Shuqin; Xu, Jianqiao; Ding, Yajuan; Ouyang, Gangfeng, E-mail: cesoygf@mail.sysu.edu.cn

    2016-01-01

    Microporous organic polymers (MOPs) have emerged as a new class of functional porous materials with unique characteristics and potential uses in diverse areas. However, the field of MOPs for gas chromatographic (GC) separations has not been well explored. Herein, a MOP namely KAPs-1 was dynamic coated onto a capillary column for the first time. The fabricated column exhibited a nonpolar nature and the column efficiency for n-dodecane was up to 7769 plates m{sup −1}. The KAPs-1 coated column showed high GC separation performance for a series of volatile organic compounds (VOCs) including the challenging ethylbenzene and xylene isomers, which could not be resolved at baseline on the commercial 5% phenyl polysiloxane stationary phase. Moreover, the relative standard deviations for five replicate determinations of the studied analytes were 0.0–0.6%, 0.9–3.2%, 1.1–5.9%, 0.8–3.7% for retention time, peak area, peak height and peak width, respectively. To investigate the interaction between some analytes and the stationary phase, thermodynamic and kinetic parameters were also evaluated. The results of this study show it is very promising to utilize MOPs as stationary phases for capillary GC. - Highlights: • A microporous organic polymer was explored as a novel stationary phase for capillary GC. • The column showed high separation performance for VOCs including the challenging ethylbenzene and xylene isomers. • Thermodynamic and kinetic parameters for BTEXs were determined to study the analyte-stationary phase interaction.

  14. Exploitation of a microporous organic polymer as a stationary phase for capillary gas chromatography

    International Nuclear Information System (INIS)

    Lu, Cuiming; Liu, Shuqin; Xu, Jianqiao; Ding, Yajuan; Ouyang, Gangfeng

    2016-01-01

    Microporous organic polymers (MOPs) have emerged as a new class of functional porous materials with unique characteristics and potential uses in diverse areas. However, the field of MOPs for gas chromatographic (GC) separations has not been well explored. Herein, a MOP namely KAPs-1 was dynamic coated onto a capillary column for the first time. The fabricated column exhibited a nonpolar nature and the column efficiency for n-dodecane was up to 7769 plates m −1 . The KAPs-1 coated column showed high GC separation performance for a series of volatile organic compounds (VOCs) including the challenging ethylbenzene and xylene isomers, which could not be resolved at baseline on the commercial 5% phenyl polysiloxane stationary phase. Moreover, the relative standard deviations for five replicate determinations of the studied analytes were 0.0–0.6%, 0.9–3.2%, 1.1–5.9%, 0.8–3.7% for retention time, peak area, peak height and peak width, respectively. To investigate the interaction between some analytes and the stationary phase, thermodynamic and kinetic parameters were also evaluated. The results of this study show it is very promising to utilize MOPs as stationary phases for capillary GC. - Highlights: • A microporous organic polymer was explored as a novel stationary phase for capillary GC. • The column showed high separation performance for VOCs including the challenging ethylbenzene and xylene isomers. • Thermodynamic and kinetic parameters for BTEXs were determined to study the analyte-stationary phase interaction.

  15. Preparation and chromatographic evaluation of a newly designed steviol glycoside modified-silica stationary phase in hydrophilic interaction liquid chromatography and reversed phase liquid chromatography.

    Science.gov (United States)

    Liang, Tu; Fu, Qing; Shen, Aijin; Wang, Hui; Jin, Yu; Xin, Huaxia; Ke, Yanxiong; Guo, Zhimou; Liang, Xinmiao

    2015-04-03

    A diterpene glycoside compound, rebaudioside A (commonly abbreviated as RA), was immobilized onto porous silica surface through "thiol-ene" click chemistry strategy. The successful immobilization of the RA on the silica support was confirmed by FT-IR and elemental analysis. Chromatographic characteristics of the new stationary phase, named Click TE-RA, were evaluated by a set of diverse analytes such as carbohydrates, nucleosides, and organic acids in hydrophilic interaction liquid chromatography (HILIC) mode. The effects of water content, buffer pH and concentration were investigated and a typical HILIC retention feature of Click TE-RA was observed at high organic modifier content. The Click TE-RA stationary phase was further studied by a series of glycoside compounds. Tunable retention mechanisms from hydrophilic to hydrophobic interactions were observed. Separation of very polar compounds including oligosaccharides, nucleic acid bases and nucleosides using Click TE-RA in HILIC mode was successfully accomplished. In addition, separation of saponins both in HILIC and reversed-phase liquid chromatography (RPLC) modes was performed, demonstrating the presence of orthogonality between two different modes on Click TE-RA column. The multiple interactions induced by polar sugar group and hydrophobic aglycone group allowed this Click TE-RA to serve as a multi-mode stationary phase in two-dimensional liquid chromatography. Copyright © 2015 Elsevier B.V. All rights reserved.

  16. Advances in enantiomeric resolution on monolithic chiral stationary phases in liquid chromatography and electrochromatography.

    Science.gov (United States)

    Al-Othman, Zeid A; Al-Warthan, Abdulrahman; Ali, Imran

    2014-05-01

    During the last decade, chiral monolithic stationary phases have been prepared and used for rapid enantioseparations in CEC and HPLC. Various chiral selectors are used to prepare these CSPs. The preparation, properties, and applications of these CSPs are discussed in this paper. Attempts have been made to describe optimization strategies and the chiral recognition mechanisms. A comparison of chiral separations in CEC and HPLC is described. Efforts have also been made to predict the future perspectives and challenges of chiral monolithic stationary phases. The most effective chiral selectors include polysaccharides, cyclodextrins, and macrocyclic glycopeptide antibiotics. These chiral phases produced acceptable analytical enantiomeric separation of a variety of racemates. However, the development of these CSPs for preparative-scale separations is needed. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. HPLC Enantioseparation of Phenylcarbamic Acid Derivatives by Using Macrocyclic Chiral Stationary Phases

    Directory of Open Access Journals (Sweden)

    Hroboňová Katarína

    2016-06-01

    Full Text Available The HPLC by using chiral stationary phases based on macrocyclic antibiotics, dimethylphenyl carbamate cyklofructan 7 and β-cyclodextrin in terms of polar-organic separation mode (mobile phase methanol/acetonitrile/acetic acid/triethylamine were used for enantioseparation of alkoxy derivatives of phenylcarbamic acid. The effect of the analyte structures on the efficiency of enantioseparation was investigated. The most suitable stationary phase was teicoplanin aglycone, where the separations of the enantiomers were obtained (the resolution value from 0.65 to 2.90, depending on the structure of the analyte. Significant effect on the resolution of the enantiomers has position of alkoxy substituent in the hydrophobic part of the molecule. The enantiorecognition was achieved for 3-alkoxysubstituted derivatives.

  18. A comparison of the radiosensitivity of stationary, exponential and G1 phase wild type and repair deficient yeast cultures: supporting evidence for stationary phase yeast cells being in G0

    International Nuclear Information System (INIS)

    Tippins, R.S.; Parry, J.M.

    1982-01-01

    The main points to emerge from this comparison of the radiosensitivity of stationary, exponential and G 1 phase yeast cultures were: (1) In wild type yeast cultures, G 1 cells were the most sensitive to the lethal effects of X-rays, exponential phase cells were the most resistant and stationary phase cells were intermediate in sensitivity. (2) With the excision-repair-defective strain D61-3 (rad 3) stationary phase cells were more resistant than exponential cells with G 1 cells again being most sensitive. (3) The rad 50 gene present in JD50 had a marked effect on the X-ray inactivation response of this strain. In the presence of the defective rad 50 allele, exponential phase cells were as sensitive as G 1 phase cells, with stationary phase cells being more resistant than either. (4) There were marked differences in sensitivity between stationary phase and G 1 phase cells. These differences, along with other physiological differences reported by other workers, lead the authors to suggest that stationary phase cells can be better described as being in G 0 phase, i.e. a stage which is outside the normal mitotic cell cycle of an exponential culture. (author)

  19. The extracellular proteome of Rhizobium etli CE3 in exponential and stationary growth phase

    Directory of Open Access Journals (Sweden)

    Mendoza-Hernández Guillermo

    2010-10-01

    Full Text Available Abstract Background The extracellular proteome or secretome of symbiotic bacteria like Rhizobium etli is presumed to be a key element of their infection strategy and survival. Rhizobia infect the roots of leguminous plants and establish a mutually beneficial symbiosis. To find out the possible role of secreted proteins we analyzed the extracellular proteome of R. etli CE3 in the exponential and stationary growth phases in minimal medium, supplemented with succinate-ammonium. Results The extracellular proteins were obtained by phenol extraction and identified by LC-ESI MS/MS. We identified 192 and 191 proteins for the exponential and stationary phases respectively. Using the software Signal P, we predicted signal peptides for 12.95% and 35.60% of the proteins identified in the exponential and stationary phases, respectively, which could therefore be secreted by the Sec pathway. For the exponential growth phase, we found in abundance proteins like the ribosomal proteins, toxins and proteins belonging to the group "defence mechanisms". For the stationary growth phase, we found that the most abundant proteins were those with unknown function, and in many of these we identified characteristic domains of proteases and peptidases. Conclusions Our study provided the first dataset of the secretome of R. etli and its modifications, which may lead to novel insights into the adaptive response of different stages of growth. In addition, we found a high number of proteins with unknown function; these proteins could be analyzed in future research to elucidate their role in the extracellular proteome of R. etli.

  20. Separation of piracetam derivatives on polysaccharide-based chiral stationary phases.

    Science.gov (United States)

    Kažoka, H; Koliškina, O; Veinberg, G; Vorona, M

    2013-03-15

    High-performance liquid chromatography was used for the enantiomeric separation of two chiral piracetam derivatives. The suitability of six commercially available polysaccharide-based chiral stationary phases (CSPs) under normal phase mode for direct enantioseparation has been investigated. The influence of the CSPs as well the nature and content of an alcoholic modifier in the mobile phase on separation and elution order was studied. It was established that CSP Lux Amylose-2 shows high chiral recognition ability towards 4-phenylsubstituted piracetam derivatives. Copyright © 2013 Elsevier B.V. All rights reserved.

  1. Selectivity differences of water-soluble vitamins separated on hydrophilic interaction stationary phases.

    Science.gov (United States)

    Yang, Yuanzhong; Boysen, Reinhard I; Hearn, Milton T W

    2013-06-01

    In this study, the retention behavior and selectivity differences of water-soluble vitamins were evaluated with three types of polar stationary phases (i.e. an underivatized silica phase, an amide phase, and an amino phase) operated in the hydrophilic interaction chromatographic mode with ESI mass spectrometric detection. The effects of mobile phase composition, including buffer pH and concentration, on the retention and selectivity of the vitamins were investigated. In all stationary phases, the neutral or weakly charged vitamins exhibited very weak retention under each of the pH conditions, while the acidic and more basic vitamins showed diverse retention behaviors. With the underivatized silica phase, increasing the salt concentration of the mobile phase resulted in enhanced retention of the acidic vitamins, but decreased retention of the basic vitamins. These observations thus signify the involvement of secondary mechanisms, such as electrostatic interaction in the retention of these analytes. Under optimized conditions, a baseline separation of all vitamins was achieved with excellent peak efficiency. In addition, the effects of water content in the sample on retention and peak efficiency were examined, with sample stacking effects observed when the injected sample contained a high amount of water. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. Speckle phase near random surfaces

    Science.gov (United States)

    Chen, Xiaoyi; Cheng, Chuanfu; An, Guoqiang; Han, Yujing; Rong, Zhenyu; Zhang, Li; Zhang, Meina

    2018-03-01

    Based on Kirchhoff approximation theory, the speckle phase near random surfaces with different roughness is numerically simulated. As expected, the properties of the speckle phase near the random surfaces are different from that in far field. In addition, as scattering distances and roughness increase, the average fluctuations of the speckle phase become larger. Unusually, the speckle phase is somewhat similar to the corresponding surface topography. We have performed experiments to verify the theoretical simulation results. Studies in this paper contribute to understanding the evolution of speckle phase near a random surface and provide a possible way to identify a random surface structure based on its speckle phase.

  3. Strengthening of the DNA-protein complex during stationary phase aging of cell cultures

    International Nuclear Information System (INIS)

    Khokhlov, A.N.; Chirkova, E.Yu.; Gorin, A.I.

    1986-01-01

    The possibility of accumulation of cross-linkages in the DNA-protein complex was studied during stationary phase aging of cells in culture. Chinese hamster cells were used in the experiments, along with human fibroblasts. 3 H-thymidine, 14 C-valine, and 14 C-leucine were added to the medium. The quantity of protein firmly bound with DNA was judged from the value of the coefficient 14 C/ 3 H determined with allowance for penetration of counting from the 14 C-channel into the 3 H-channel. The authors maintain that the results presented in this paper provide further evidence of the value of stationary phase cell cultures for the study of the mechanisms of aging and also of some of the general principles underlying hereditary pathology

  4. Preparative separation of the polar part from the rhizomes of Anemarrhena asphodeloides using a hydrophilic C18 stationary phase.

    Science.gov (United States)

    Cai, Jianfeng; Xin, Huaxia; Cheng, Lingping; Fu, YanHui; Jiang, Dasen; Feng, Jiatao; Fu, Qing; Jin, Yu; Liang, Xinmiao

    2017-09-15

    The goal of this study was to develop a method that utilized a hydrophilic C18 stationary phase in the preparative high performance liquid chromatography to isolate the polar part from the rhizomes of Anemarrhena asphodeloides. The results showed that an initial mobile phase of pure water for the separation could greatly increase the retention and solubility of the polar compounds at the preparative scale. Introducing polar groups on the surface of the hydrophilic C18 column together with the use of optimized mobile phase compositions improved the column separation selectivity for polar compounds. Eleven previously undescribed compounds in Anemarrhena asphodeloides were obtained, indicating that the method developed in this study would facilitate the purification and separation of the polar part of traditional Chinese medicines. Copyright © 2017 Elsevier B.V. All rights reserved.

  5. Temporal transcriptomic analysis of Desulfovibrio vulgaris Hildenborough transition into stationary phase growth during electrondonor depletion

    Energy Technology Data Exchange (ETDEWEB)

    Clark, M.E.; He, Q.; He, Z.; Huang, K.H.; Alm, E.J.; Wan, X.-F.; Hazen, T.C.; Arkin, A.P.; Wall, J.D.; Zhou, J.-Z.; Fields, M.W.

    2006-08-01

    Desulfovibrio vulgaris was cultivated in a defined medium, and biomass was sampled for approximately 70 h to characterize the shifts in gene expression as cells transitioned from the exponential to the stationary phase during electron donor depletion. In addition to temporal transcriptomics, total protein, carbohydrate, lactate, acetate, and sulfate levels were measured. The microarray data were examined for statistically significant expression changes, hierarchical cluster analysis, and promoter element prediction and were validated by quantitative PCR. As the cells transitioned from the exponential phase to the stationary phase, a majority of the down-expressed genes were involved in translation and transcription, and this trend continued at the remaining times. There were general increases in relative expression for intracellular trafficking and secretion, ion transport, and coenzyme metabolism as the cells entered the stationary phase. As expected, the DNA replication machinery was down-expressed, and the expression of genes involved in DNA repair increased during the stationary phase. Genes involved in amino acid acquisition, carbohydrate metabolism, energy production, and cell envelope biogenesis did not exhibit uniform transcriptional responses. Interestingly, most phage-related genes were up-expressed at the onset of the stationary phase. This result suggested that nutrient depletion may affect community dynamics and DNA transfer mechanisms of sulfate-reducing bacteria via the phage cycle. The putative feoAB system (in addition to other presumptive iron metabolism genes) was significantly up-expressed, and this suggested the possible importance of Fe{sup 2+} acquisition under metal-reducing conditions. The expression of a large subset of carbohydrate-related genes was altered, and the total cellular carbohydrate levels declined during the growth phase transition. Interestingly, the D. vulgaris genome does not contain a putative rpoS gene, a common attribute

  6. Stationary phase selection and comprehensive two-dimensional gas chromatographic analysis of trace biodiesel in petroleum-based fuel.

    Science.gov (United States)

    Seeley, John V; Bates, Carly T; McCurry, James D; Seeley, Stacy K

    2012-02-24

    The GC×GC solvation parameter model has been used to identify effective stationary phases for the separation of fatty acid methyl esters (FAMEs) from petroleum hydrocarbons. This simple mathematical model was used to screen the 1225 different combinations of 50 stationary phases. The most promising pairs combined a poly(methyltrifluoropropylsiloxane) stationary phase with a poly(dimethyldiphenylsiloxane) stationary phase. The theoretical results were experimentally tested by equipping a GC×GC instrument with a DB-210 primary stationary phase and an HP-50+ secondary stationary phase. This instrument was used to analyze trace levels of FAMEs in kerosene. The FAMEs were fully separated from the petroleum hydrocarbons on the secondary dimension of the 2-D chromatogram. The resulting GC×GC method was shown to be capable of accurately quantifying FAME levels as low as 2 ppm (w/w). These results demonstrate the utility of the solvation parameter model for identifying optimal stationary phases for high resolution GC×GC separations. Furthermore, this work presents an effective method for determining the level of biodiesel contamination in aviation fuel and other petroleum-based fuels. Copyright © 2011 Elsevier B.V. All rights reserved.

  7. Surface Stress with Non-stationary Weak Winds and Stable Stratification

    Science.gov (United States)

    Mahrt, L.; Thomas, Christoph K.

    2016-04-01

    The behaviour of turbulent transport in the weak-wind, stably-stratified, boundary layer over land is examined in terms of the non-stationarity of the wind field using measurements from three field programs. These field programs include towers ranging from 12 to 20 m in height and an extensive horizontal network of sonic anemometers. The relationship of the friction velocity to the stratification and non-stationary submeso motions is investigated from several points of view and nominally quantified. The relationship of the turbulence to the stratification is less systematic than expected partly due to enhancement of the turbulence by submeso motions. Cause and effect relationships are difficult to isolate because the non-stationary momentum flux significantly modifies the profile of the non-stationary mean flow. The link between the turbulence and accelerations at the surface is examined in terms of the changing vertical structure of the wind profile and sudden increases in the downward transport of momentum.

  8. Exploitation of a microporous organic polymer as a stationary phase for capillary gas chromatography.

    Science.gov (United States)

    Lu, Cuiming; Liu, Shuqin; Xu, Jianqiao; Ding, Yajuan; Ouyang, Gangfeng

    2016-01-01

    Microporous organic polymers (MOPs) have emerged as a new class of functional porous materials with unique characteristics and potential uses in diverse areas. However, the field of MOPs for gas chromatographic (GC) separations has not been well explored. Herein, a MOP namely KAPs-1 was dynamic coated onto a capillary column for the first time. The fabricated column exhibited a nonpolar nature and the column efficiency for n-dodecane was up to 7769 plates m(-1). The KAPs-1 coated column showed high GC separation performance for a series of volatile organic compounds (VOCs) including the challenging ethylbenzene and xylene isomers, which could not be resolved at baseline on the commercial 5% phenyl polysiloxane stationary phase. Moreover, the relative standard deviations for five replicate determinations of the studied analytes were 0.0-0.6%, 0.9-3.2%, 1.1-5.9%, 0.8-3.7% for retention time, peak area, peak height and peak width, respectively. To investigate the interaction between some analytes and the stationary phase, thermodynamic and kinetic parameters were also evaluated. The results of this study show it is very promising to utilize MOPs as stationary phases for capillary GC. Copyright © 2015 Elsevier B.V. All rights reserved.

  9. Enhanced dipicolinic acid production during the stationary phase in Bacillus subtilis by blocking acetoin synthesis.

    Science.gov (United States)

    Toya, Yoshihiro; Hirasawa, Takashi; Ishikawa, Shu; Chumsakul, Onuma; Morimoto, Takuya; Liu, Shenghao; Masuda, Kenta; Kageyama, Yasushi; Ozaki, Katsuya; Ogasawara, Naotake; Shimizu, Hiroshi

    2015-01-01

    Bacterial bio-production during the stationary phase is expected to lead to a high target yield because the cells do not consume the substrate for growth. Bacillus subtilis is widely used for bio-production, but little is known about the metabolism during the stationary phase. In this study, we focused on the dipicolinic acid (DPA) production by B. subtilis and investigated the metabolism. We found that DPA production competes with acetoin synthesis and that acetoin synthesis genes (alsSD) deletion increases DPA productivity by 1.4-fold. The mutant showed interesting features where the glucose uptake was inhibited, whereas the cell density increased by approximately 50%, resulting in similar volumetric glucose consumption to that of the parental strain. The metabolic profiles revealed accumulation of pyruvate, acetyl-CoA, and the TCA cycle intermediates in the alsSD mutant. Our results indicate that alsSD-deleted B. subtilis has potential as an effective host for stationary-phase production of compounds synthesized from these intermediates.

  10. Eukaryotic initiation factor 5A dephosphorylation is required for translational arrest in stationary phase cells.

    Science.gov (United States)

    Chung, Janete; Rocha, Antonio A; Tonelli, Renata R; Castilho, Beatriz A; Schenkman, Sergio

    2013-04-15

    The protein known as eIF5A (eukaryotic initiation factor 5A) has an elusive role in translation. It has a unique and essential hypusine modification at a conserved lysine residue in most eukaryotes. In addition, this protein is modified by phosphorylation with unknown functions. In the present study we show that a phosphorylated state of eIF5A predominates in exponentially growing Trypanosoma cruzi cells, and extensive dephosphorylation occurs in cells in stationary phase. Phosphorylation occurs mainly at Ser(2), as shown in yeast eIF5A. In addition, a novel phosphorylation site was identified at Tyr(21). In exponential cells, T. cruzi eIF5A is partially associated with polysomes, compatible with a proposed function as an elongation factor, and becomes relatively enriched in polysomal fractions in stationary phase. Overexpression of the wild-type eIF5A, or eIF5A with Ser(2) replaced by an aspartate residue, but not by alanine, increases the rate of cell proliferation and protein synthesis. However, the presence of an aspartate residue instead of Ser(2) is toxic for cells reaching the stationary phase, which show a less-pronounced protein synthesis arrest and a decreased amount of eIF5A in dense fractions of sucrose gradients. We conclude that eIF5A phosphorylation and dephosphorylation cycles regulate translation according to the growth conditions.

  11. Graphitic carbon nitride as high-resolution stationary phase for gas chromatographic separations.

    Science.gov (United States)

    Zheng, Yunzhong; Qi, Meiling; Fu, Ruonong

    2016-07-08

    This work presents the first example of utilization of graphitic carbon nitride (g-C3N4) as stationary phase for capillary gas chromatographic (GC) separations. The statically coated g-C3N4 column showed the column efficiencies of 3760 plates/m and weak polarity. Its resolving capability and retention behaviours were investigated by using the Grob test mixture, and mixtures of diverse types of analytes, and structural and positional isomers. The results showed superior separation performance of the g-C3N4 stationary phase for some critical analytes and preferential retention for aromatic analytes. Specifically, it exhibited high-resolution capability for aromatic and aliphatic isomers such as methylnaphthalenes and dimethylnaphthalenes, phenanthrene and anthracene and alkane isomers. In addition, g-C3N4 column showed excellent thermal stability up to 280°C and good repeatability with relative standard deviation (RSD) values less than 0.09% for intra-day, below 0.23% for inter-day and in the range of 1.9-8.4% for between-column, respectively. The advantageous separation performance shows the potential of g-C3N4 and related materials as stationary phase in GC and other separation technologies. Copyright © 2016 Elsevier B.V. All rights reserved.

  12. Hierarchical CaCO3 chromatography: a stationary phase based on biominerals.

    Science.gov (United States)

    Sato, Kosuke; Oaki, Yuya; Takahashi, Daisuke; Toshima, Kazunobu; Imai, Hiroaki

    2015-03-23

    In biomineralization, acidic macromolecules play important roles for the growth control of crystals through a specific interaction. Inspired by this interaction, we report on an application of the hierarchical structures in CaCO3 biominerals to a stationary phase of chromatography. The separation and purification of acidic small organic molecules are achieved by thin-layer chromatography and flash chromatography using the powder of biominerals as the stationary phase. The unit nanocrystals and their oriented assembly, the hierarchical structure, are suitable for the adsorption site of the target organic molecules and the flow path of the elution solvents, respectively. The separation mode is ascribed to the specific adsorption of the acidic molecules on the crystal face and the coordination of the functional groups to the calcium ions. The results imply that a new family of stationary phase of chromatography can be developed by the fine tuning of hierarchical structures in CaCO3 materials. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Silanol suppressing potency of alkyl-imidazolium ionic liquids on C18 stationary phases.

    Science.gov (United States)

    Fernández-Navarro, J J; Torres-Lapasió, J R; Ruiz-Ángel, M J; García-Álvarez-Coque, M C

    2012-04-06

    Residual silanols on C18 columns yield undesirable slow-kinetics ion-exchange interactions with positively charged basic compounds that result in asymmetrical peaks, low efficiencies and long retention times. The purity of the silica employed as supporting material, and the technique used to form the bonded phase, which varies with the brand and manufacturer, give rise to different amounts of residual silanols in the packings, and consequently, different chromatographic performance. One of the most efficient and widespread strategies to reduce or even eliminate the different performance among columns is the addition of a reagent to the mobile phase to block the silanol sites. However, the intrinsic nature of both stationary phase and additive leads to particular results. In this work, a group of basic compounds were analysed using six C18 stationary phases (Zorbax SB-C18, X-Terra MS C18, Kromasil, Lichrospher, Nucleosil, and Spherisorb) and acetonitrile-water mixtures. Two ionic liquids (ILs), 1-butyl- and 1-hexyl-3-methyl-imidazolium tetrafluoroborates, were added to the mobile phases to evaluate their silanol suppressing potency, based on the decreased retention of the basic compounds when the silanols are blocked (described by the Horváth equation), and the improvement in peak profile (described by the plots of the peak half-widths at diverse retention times). The suppressing potency based on the retention can be misleading when the adsorption of the IL anion is not negligible, since the anion attracts the cationic basic compounds increasing the retention. However, the accessibility of basic compounds to the silanols is prevented by both IL cation and anion, improving the peak profiles for all stationary phases. This was especially remarkable for Spherisorb, which in the absence of additive yielded by far the worst performance. 1-Hexyl-3-methyl-imidazolium tetrafluoroborate was the best additive in terms of retention and peak profile (width and asymmetry

  14. Enantioseparation of Six Antihistamines with Immobilized Cellulose Chiral Stationary Phase by HPLC.

    Science.gov (United States)

    Zhou, Jie; Luo, Pei; Chen, Shanshan; Meng, Lingchang; Sun, Chong; Du, Qiuzheng; Sun, Fang

    2016-04-01

    A stereoselective high performance liquid chromatography method has been developed for the chiral separation of the enantiomers of six antihistamines, doxylamine, carbinoxamine, dioxopromethazine, oxomemazine, cetirizine and hydroxyzine. The effects of mobile phase additive, column temperature and flow rate on the retention time and resolution were studied. Enantiomeric separation of cetirizine, doxylamine and hydroxyzine were achieved on cellulose tris-(3,5-dichlorophenylcarbamate) immobilized on silica gel chiral stationary phase known as Chiralpak IC (RS = 3.74, RS = 1.85 and RS = 1.74, respectively). © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  15. Radiation stimulation during the early stationary growth phase in Synechococcus lividus and its correlation with photooxidative stress occurring before the stationary phase

    International Nuclear Information System (INIS)

    Conter, A.; Dupouy, D.; Vincent, C.; Planel, H.

    1987-01-01

    The effects of chronic gamma radiation at dose rates ranging from 0.058 mGy d-1 on growth rate calculated during the early stationary phase were studied. A stimulatory effect occurred for all doses and for all phases of the cells selected for use in the inoculation of the medium. During the same period, the rate of nucleic acid synthesis was increased in irradiated cultures compared to control cultures. The stimulating effect always occurred in cultures irradiated from the inoculation to the eighteenth day only. This result led us to conclude that the stimulation mechanism depended upon the events occurring at the end of the exponential phase in the deceleration period. Studies on cell metabolism showed that cells presented features of photooxidative stress in this period. Increases in superoxide dismutase, glutathione reductase and glucose-6-phosphate dehydrogenase were observed in irradiated cultures. It was assumed that irradiation at very low doses could help cells to better defend against photooxidative stress by increasing oxidants that activate the glucose metabolism and C5-sugars production and nucleic acid synthesis

  16. Search for improved fluorinated stationary phases for separation of fluorine-containing pharmaceuticals from their desfluoro analogs.

    Science.gov (United States)

    Regalado, Erik L; Makarov, Alexey A; McClain, Ray; Przybyciel, Matthew; Welch, Christopher J

    2015-02-06

    Evaluation of a several fluorine-containing stationary phases for the chromatographic separation of fluorine-containing pharmaceuticals from their corresponding desfluoro analogs revealed a number of perfluoroaryl and perfluoroalky stationary phases that afford good separations. These fluorous stationary phases exhibit greater retention for the fluorine-containing compounds relative to the H-containing analogs, consistent with a fluorophilic retention mechanism. While both perfluoroalkyl and perfluoroaryl stationary phases afford adequate resolution, the perfluoroaryl columns generally exhibit superior separation factor (α) and peak efficiency (N), resulting in faster baseline separations, with the Hypersil Gold PFP and Poroshell 120 PFP columns providing the best overall performance for the test group studied. Copyright © 2014 Elsevier B.V. All rights reserved.

  17. Argentation gas chromatography revisited: Separation of light olefin/paraffin mixtures using silver-based ionic liquid stationary phases.

    Science.gov (United States)

    Nan, He; Zhang, Cheng; Venkatesh, Amrit; Rossini, Aaron J; Anderson, Jared L

    2017-11-10

    Silver ion or argentation chromatography utilizes stationary phases containing silver ions for the separation of unsaturated compounds. In this study, a mixed-ligand silver-based ionic liquid (IL) was evaluated for the first time as a gas chromatographic (GC) stationary phase for the separation of light olefin/paraffin mixtures. The selectivity of the stationary phase toward olefins can be tuned by adjusting the ratio of silver ion and the mixed ligands. The maximum allowable operating temperature of these stationary phases was determined to be between 125°C and 150°C. Nuclear magnetic resonance (NMR) spectroscopy was used to characterize the coordination behavior of the silver-based IL as well as provide an understanding into the retention mechanism of light olefins. Copyright © 2017 Elsevier B.V. All rights reserved.

  18. Theory for Transitions Between Exponential and Stationary Phases: Universal Laws for Lag Time

    Science.gov (United States)

    Himeoka, Yusuke; Kaneko, Kunihiko

    2017-04-01

    The quantitative characterization of bacterial growth has attracted substantial attention since Monod's pioneering study. Theoretical and experimental works have uncovered several laws for describing the exponential growth phase, in which the number of cells grows exponentially. However, microorganism growth also exhibits lag, stationary, and death phases under starvation conditions, in which cell growth is highly suppressed, for which quantitative laws or theories are markedly underdeveloped. In fact, the models commonly adopted for the exponential phase that consist of autocatalytic chemical components, including ribosomes, can only show exponential growth or decay in a population; thus, phases that halt growth are not realized. Here, we propose a simple, coarse-grained cell model that includes an extra class of macromolecular components in addition to the autocatalytic active components that facilitate cellular growth. These extra components form a complex with the active components to inhibit the catalytic process. Depending on the nutrient condition, the model exhibits typical transitions among the lag, exponential, stationary, and death phases. Furthermore, the lag time needed for growth recovery after starvation follows the square root of the starvation time and is inversely related to the maximal growth rate. This is in agreement with experimental observations, in which the length of time of cell starvation is memorized in the slow accumulation of molecules. Moreover, the lag time distributed among cells is skewed with a long time tail. If the starvation time is longer, an exponential tail appears, which is also consistent with experimental data. Our theory further predicts a strong dependence of lag time on the speed of substrate depletion, which can be tested experimentally. The present model and theoretical analysis provide universal growth laws beyond the exponential phase, offering insight into how cells halt growth without entering the death phase.

  19. Proteomic Analysis of Stationary Phase in the Marine Bacterium "Candidatus Pelagibacter ubique"

    Energy Technology Data Exchange (ETDEWEB)

    Sowell, S. M.; Norbeck, A. D.; Lipton, M. S.; Nicora, C. D.; Callister, S. J.; Smith, R. D.; Barofsky, D. F.; Giovannoni, S. J.

    2008-05-09

    The α-proteobacterium ‘Candidatus Pelagibacter ubique’ str. HTCC1062, and most other members of the SAR11 clade, lack genes for assimilatory sulfate reduction, making them dependent on organosulfur compounds that occur naturally in seawater. To investigate how these cells adapt to sulfur limitation, batch cultures were grown in defined media containing either limiting or non-limiting amounts of dimethylsulfoniopropionate (DMSP) as the sole sulfur source. Protein and mRNA expression were measured during exponential growth, immediately prior to stationary phase, and in late stationary phase. Two distinct responses were observed: one as DMSP became exhausted, and another as cells acclimated to a sulfur-limited environment. The first response was characterized by increased transcription and translation of all Ca. P. ubique genes downstream of previously confirmed S-adenosyl methionine (SAM) riboswitches: bhmT, mmuM, and metY. Proteins encoded by these genes were up to 33 times more abundant as DMSP became limiting. Their predicted function is to shunt all available sulfur to methionine. The secondary response, observed during sulfur-depleted stationary phase, was a 6-10 fold increase in transcription of the heme c shuttle ccmC and two small genes of unknown function (SAR11_1163 and SAR11_1164). This bacterium's strategy for coping with sulfur stress appears to be intracellular redistribution to support methionine biosynthesis, rather than increasing organosulfur import. Many of the genes and SAM riboswitches involved in this response are located in a hypervariable genome region (HVR). One of these HVR genes, ordL, is located downstream of a conserved motif that evidence suggests is a novel riboswitch.

  20. Stationary phase expression of the arginine biosynthetic operon argCBH in Escherichia coli

    Directory of Open Access Journals (Sweden)

    Sun Yuan

    2006-02-01

    Full Text Available Abstract Background Arginine biosynthesis in Escherichia coli is elevated in response to nutrient limitation, stress or arginine restriction. Though control of the pathway in response to arginine limitation is largely modulated by the ArgR repressor, other factors may be involved in increased stationary phase and stress expression. Results In this study, we report that expression of the argCBH operon is induced in stationary phase cultures and is reduced in strains possessing a mutation in rpoS, which encodes an alternative sigma factor. Using strains carrying defined argR, and rpoS mutations, we evaluated the relative contributions of these two regulators to the expression of argH using operon-lacZ fusions. While ArgR was the main factor responsible for modulating expression of argCBH, RpoS was also required for full expression of this biosynthetic operon at low arginine concentrations (below 60 μM L-arginine, a level at which growth of an arginine auxotroph was limited by arginine. When the argCBH operon was fully de-repressed (arginine limited, levels of expression were only one third of those observed in ΔargR mutants, indicating that the argCBH operon is partially repressed by ArgR even in the absence of arginine. In addition, argCBH expression was 30-fold higher in ΔargR mutants relative to levels found in wild type, fully-repressed strains, and this expression was independent of RpoS. Conclusion The results of this study indicate that both derepression and positive control by RpoS are required for full control of arginine biosynthesis in stationary phase cultures of E. coli.

  1. Bacteriophage T4 Infection of Stationary Phase E. coli: Life after Log from a Phage Perspective.

    Science.gov (United States)

    Bryan, Daniel; El-Shibiny, Ayman; Hobbs, Zack; Porter, Jillian; Kutter, Elizabeth M

    2016-01-01

    Virtually all studies of phage infections investigate bacteria growing exponentially in rich media. In nature, however, phages largely encounter non-growing cells. Bacteria entering stationary phase often activate well-studied stress defense mechanisms that drastically alter the cell, facilitating its long-term survival. An understanding of phage-host interactions in such conditions is of major importance from both an ecological and therapeutic standpoint. Here, we show that bacteriophage T4 can efficiently bind to, infect and kill E. coli in stationary phase, both in the presence and absence of a functional stationary-phase sigma factor, and explore the response of T4-infected stationary phase cells to the addition of fresh nutrients 5 or 24 h after that infection. An unexpected new mode of response has been identified. "Hibernation" mode is a persistent but reversible dormant state in which the infected cells make at least some phage enzymes, but halt phage development until appropriate nutrients become available before producing phage particles. Our evidence indicates that the block in hibernation mode occurs after the middle-mode stage of phage development; host DNA breakdown and the incorporation of the released nucleotides into phage DNA indicate that the enzymes of the nucleotide synthesizing complex, under middle-mode control, have been made and assembled into a functional state. Once fresh glucose and amino acids become available, the standard lytic infection process rapidly resumes and concentrations of up to 10(11) progeny phage (an average of about 40 phage per initially present cell) are produced. All evidence is consistent with the hibernation-mode control point lying between middle mode and late mode T4 gene expression. We have also observed a "scavenger" response, where the infecting phage takes advantage of whatever few nutrients are available to produce small quantities of progeny within 2 to 5 h after infection. The scavenger response seems able

  2. Bacteriophage T4 Infection of Stationary Phase E. coli: Life after Log from a Phage Perspective

    Directory of Open Access Journals (Sweden)

    Elizabeth Martin Kutter

    2016-09-01

    Full Text Available Virtually all studies of phage infections investigate bacteria growing exponentially in rich media. In nature, however, phages largely encounter non-growing cells. Bacteria entering stationary phase often activate well-studied stress defense mechanisms that drastically alter the cell, facilitating its long-term survival. An understanding of phage-host interactions in such conditions is of major importance from both an ecological and therapeutic standpoint. Here, we show that bacteriophage T4 can efficiently bind to, infect and kill E. coli in stationary phase, both in the presence and absence of a functional stationary-phase sigma factor, and explore the response of T4-infected stationary phase cells to the addition of fresh nutrients 5 or 24 hours after that infection. An unexpected new mode of response has been identified. Hibernation mode is a persistent but reversible dormant state in which the infected cells make at least some phage enzymes, but halt phage development until appropriate nutrients become available before producing phage particles. Our evidence indicates that the block in hibernation mode occurs after the middle-mode stage of phage development; host DNA breakdown and the incorporation of the released nucleotides into phage DNA indicate that the enzymes of the nucleotide synthesizing complex, under middle-mode control, have been made and assembled into a functional state. Once fresh glucose and amino acids become available, the standard lytic infection process rapidly resumes and concentrations of up to 1011 progeny phage (an average of about 40 phage per initially-present cell are produced. All evidence is consistent with the hibernation-mode control point lying between middle mode and late mode T4 gene expression. We have also observed a scavenger response, where the infecting phage takes advantage of whatever few nutrients are available to produce small quantities of progeny within 2 to 5 hours after infection. The scavenger

  3. Homochiral metal-organic framework used as a stationary phase for high-performance liquid chromatography.

    Science.gov (United States)

    Kong, Jiao; Zhang, Mei; Duan, Ai-Hong; Zhang, Jun-Hui; Yang, Rui; Yuan, Li-Ming

    2015-02-01

    Metal-organic frameworks are promising porous materials. Chiral metal-organic frameworks have attracted considerable attention in controlling enantioselectivity. In this study, a homochiral metal-organic framework [Co(2) (D-cam)(2) (TMDPy)] (D-cam = D-camphorates, TMDPy = 4,4'-trimethylenedipyridine) with a non-interpenetrating primitive cubic net has been used as a chiral stationary phase in high-performance liquid chromatography. It has allowed the successful separation of six positional isomers and six chiral compounds. The good selectivity and baseline separation, or at least 60% valley separation, confirmed its excellent molecular recognition characteristics. The relative standard deviations for the retention time of run-to-run and column-to-column were less than 1.8 and 3.1%, respectively. These results demonstrate that [Co(2) (D-cam)(2) (TMDPy)] may represent a promising chiral stationary phase for use in high-performance liquid chromatography. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Accelerating the quality control of pharmaceuticals using monolithic stationary phases: a review of recent HPLC applications.

    Science.gov (United States)

    Zacharis, Constantinos K

    2009-07-01

    High-performance liquid chromatography (HPLC) is the predominant technique in the quality control of pharmaceutical formulations. HPLC offers highly sensitive and selective analytical methods with increased robustness and separation efficiency. The majority of HPLC-based methodologies are based on the usage of particulate-based columns and cannot be applied at elevated flow rates (> 2 mL/min) due to excessive back-pressure. Therefore, the typical duration of separation cycles is in the range of 5-30 min, making most assays time-consuming, especially when a lot of samples have to be analyzed in a minimum amount of time. Monolithic stationary phases for HPLC offer a very interesting alternative to conventional particulate-based columns. The size of the skeleton and the distribution of the pores of monolithic materials offer the possibility of developing efficient separation protocols at higher flow-rates due to the low pressure-drop across the column. The present review intends to cover the applications of monolithic based HPLC stationary phases in the quality control of pharmaceutical formulations, including identification of active pharmaceutical ingredient, assay, purity, dissolution, blending, and dosage uniformity, etc.

  5. Battle of the Bacteria: Characterizing the Evolutionary Advantage of Stationary Phase Growth

    Directory of Open Access Journals (Sweden)

    Karin E. Kram

    2016-05-01

    Full Text Available Providing students with authentic research opportunities has been shown to enhance learning and increase retention in STEM majors. Accordingly, we have developed a novel microbiology lab module, which focuses on the molecular mechanisms of evolution in E. coli, by examining the growth advantage in stationary phase (GASP phenotype. The GASP phenotype is demonstrated by growing cells into long-term stationary phase (LTSP and then competing them against un-aged cells in a fresh culture. This module includes learning goals related to strengthening practical laboratory skills and improving student understanding of evolution. In addition, the students generate novel data regarding the effects of different environmental stresses on GASP and the relationship between evolution, genotypic change, mutation frequency, and cell stress. Pairs of students are provided with the experimental background, select a specific aspect of the growth medium to modify, and generate a hypothesis regarding how this alteration will impact the GASP phenotype. From this module, we have demonstrated that students are able to achieve the established learning goals and have produced data that has furthered our understanding of the GASP phenotype.

  6. The Trypanosoma cruzi nucleolus: a morphometrical analysis of cultured epimastigotes in the exponential and stationary phases.

    Science.gov (United States)

    Nepomuceno-Mejía, Tomás; Lara-Martínez, Reyna; Cevallos, Ana María; López-Villaseñor, Imelda; Jiménez-García, Luis Felipe; Hernández, Roberto

    2010-12-01

    Our group is interested in rRNA and ribosome biogenesis in the parasitic protozoan Trypanosoma cruzi. Epimastigotes represent an extracellular replicative stage of T. cruzi and can be cultured in axenic media. The growth curve of epimastigotes allows assessment of potential differences in the nucleoli of cells undergoing growth-rate transitions. To establish cellular parameters for studying ribosome biogenesis in T. cruzi, a morphometric analysis of the nucleoli of cultured cells in the exponential and stationary phases was conducted. Electron micrograph-based measurements of nuclear sections from independent cells demonstrated that the nucleolar area is over twofold higher in exponentially growing cells, as compared with epimastigotes in the stationary phase. The granular component of the nucleoli of actively growing cells was the main structural element. Cycloheximide moderately reduced the apparent size of the nucleoli without an apparent disruption of their architecture. Our results provide a firm basis for the establishment of an experimental model to study the organization of the nucleolus during the growth and development of T. cruzi. © 2010 Federation of European Microbiological Societies Published by Blackwell Publishing Ltd. All rights reserved.

  7. Retention behavior of resorcinarene-based cavitands on C8 and C18 stationary phases.

    Science.gov (United States)

    Bartó, Endre; Prauda, Ibolya; Kilár, Ferenc; Kiss, Ibolya; Felinger, Attila

    2015-09-01

    The understanding of the retention behavior of large molecules is an area of interest in liquid chromatography. Resorcinarene-based cavitands are cavity-shaped cyclic oligomers that can create host-guest interactions. We have investigated the chromatographic behavior of two types of cyclic tetramers as analytes in high-performance liquid chromatography. The experiments were performed at four different temperatures (15, 25, 35, 45°C) on two types of reversed stationary phases (C8 and C18 ) from two different manufacturers. We have found a huge difference between the retention of resorcinarenes and cavitands. In some cases, the retention factor of cavitands was even a hundred times larger than the retention factor of resorcinarenes. The retention of methylated derivates was two to four times larger compared to that of demethylated compounds on every column. The opposite retention behavior of the resorcinarenes and cavitands on the two types of stationary phases showed well the difference of the selectivity of the XTerra and BDS Hypersil columns. The retention mechanism was studied by the thermodynamic parameters calculated from the van't Hoff equation. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Genomewide Dam Methylation in Escherichia coli during Long-Term Stationary Phase.

    Science.gov (United States)

    Westphal, Lacey L; Sauvey, Peter; Champion, Matthew M; Ehrenreich, Ian M; Finkel, Steven E

    2016-01-01

    DNA methylation in prokaryotes is widespread. The most common modification of the genome is the methylation of adenine at the N-6 position. In Escherichia coli K-12 and many gammaproteobacteria, this modification is catalyzed by DNA adenine methyltransferase (Dam) at the GATC consensus sequence and is known to modulate cellular processes including transcriptional regulation of gene expression, initiation of chromosomal replication, and DNA mismatch repair. While studies thus far have focused on the motifs associated with methylated adenine (meA), the frequency of meA across the genome, and temporal dynamics during early periods of incubation, here we conduct the first study on the temporal dynamics of adenine methylation in E. coli by Dam throughout all five phases of the bacterial life cycle in the laboratory. Using single-molecule real-time sequencing, we show that virtually all GATC sites are significantly methylated over time; nearly complete methylation of the chromosome was confirmed by mass spectroscopy analysis. However, we also detect 66 sites whose methylation patterns change significantly over time within a population, including three sites associated with sialic acid transport and catabolism, suggesting a potential role for Dam regulation of these genes; differential expression of this subset of genes was confirmed by quantitative real-time PCR. Further, we show significant growth defects of the dam mutant during long-term stationary phase (LTSP). Together these data suggest that the cell places a high premium on fully methylating the chromosome and that alterations in methylation patterns may have significant impact on patterns of transcription, maintenance of genetic fidelity, and cell survival. IMPORTANCE While it has been shown that methylation remains relatively constant into early stationary phase of E. coli , this study goes further through death phase and long-term stationary phase, a unique time in the bacterial life cycle due to nutrient

  9. Planar spatial correlations, anisotropy, and specific surface area of stationary random porous media

    International Nuclear Information System (INIS)

    Berryman, J.G.

    1998-01-01

    An earlier result of the author showed that an anisotropic spatial correlation function of a random porous medium could be used to compute the specific surface area when it is stationary as well as anisotropic by first performing a three-dimensional radial average and then taking the first derivative with respect to lag at the origin. This result generalized the earlier result for isotropic porous media of Debye et al. [J. Appl. Phys. 28, 679 (1957)]. The present article provides more detailed information about the use of spatial correlation functions for anisotropic porous media and in particular shows that, for stationary anisotropic media, the specific surface area can be related to the derivative of the two-dimensional radial average of the correlation function measured from cross sections taken through the anisotropic medium. The main concept is first illustrated using a simple pedagogical example for an anisotropic distribution of spherical voids. Then, a general derivation of formulas relating the derivative of the planar correlation functions to surface integrals is presented. When the surface normal is uniformly distributed (as is the case for any distribution of spherical voids), our formulas can be used to relate a specific surface area to easily measurable quantities from any single cross section. When the surface normal is not distributed uniformly (as would be the case for an oriented distribution of ellipsoidal voids), our results show how to obtain valid estimates of specific surface area by averaging measurements on three orthogonal cross sections. One important general observation for porous media is that the surface area from nearly flat cracks may be underestimated from measurements on orthogonal cross sections if any of the cross sections happen to lie in the plane of the cracks. This result is illustrated by taking the very small aspect ratio (penny-shaped crack) limit of an oblate spheroid, but holds for other types of flat surfaces as well

  10. Phase diagrams for surface alloys

    DEFF Research Database (Denmark)

    Christensen, Asbjørn; Ruban, Andrei; Stoltze, Per

    1997-01-01

    We discuss surface alloy phases and their stability based on surface phase diagrams constructed from the surface energy as a function of the surface composition. We show that in the simplest cases of pseudomorphic overlayers there are four generic classes of systems, characterized by the sign...... is based on density-functional calculations using the coherent-potential approximation and on effective-medium theory. We give self-consistent density-functional results for the segregation energy and surface mixing energy for all combinations of the transition and noble metals. Finally we discuss...

  11. Integrated Time and Phase Synchronization Strategy for a Multichannel Spaceborne-Stationary Bistatic SAR System

    Directory of Open Access Journals (Sweden)

    Feng Hong

    2016-07-01

    Full Text Available The spatial separation of the transmitter and receiver in Bistatic Synthetic Aperture Radar (BiSAR makes it a promising and useful supplement to a classical Monostatic SAR system (MonoSAR. This paper proposes a novel integrated time and phase synchronization strategy for a multichannel spaceborne-stationary BiSAR system. Firstly, the time synchronization strategy is proposed, which includes Pulse Repetition Frequency (PRF generation under noisy conditions, multichannel calibration and the alignment of the recorded data with the orbital data. Furthermore, the phase synchronization strategy, which fully considers the deteriorative factors in the BiSAR configuration, is well studied. The contribution of the phase synchronization strategy includes two aspects: it not only compensates the phase error, but also improves the Signal to Noise Ratio (SNR of the obtained signals. Specifically, all direct signals on different PRF time can be reconstructed with the shift and phase compensation operation using a reference signal. Besides, since the parameters of the reference signal can be estimated only once using the selected practical direct signal and a priori information, the processing complexity is well reduced. Final imaging results with and without compensation for real data are presented to validate the proposed synchronization strategy.

  12. Dependence of Arctic climate on the latitudinal position of stationary waves and to high-latitudes surface warming

    Science.gov (United States)

    Shin, Yechul; Kang, Sarah M.; Watanabe, Masahiro

    2017-12-01

    Previous studies suggest large uncertainties in the stationary wave response under global warming. Here, we investigate how the Arctic climate responds to changes in the latitudinal position of stationary waves, and to high-latitudes surface warming that mimics the effect of Arctic sea ice loss under global warming. To generate stationary waves in an atmospheric model coupled to slab ocean, a series of experiments is performed where the thermal forcing with a zonal wavenumber-2 (with zero zonal-mean) is prescribed at the surface at different latitude bands in the Northern Hemisphere. When the stationary waves are generated in the subtropics, the cooling response dominates over the warming response in the lower troposphere due to cloud radiative effects. Then, the low-level baroclinicity is reduced in the subtropics, which gives rise to a poleward shift of the eddy driven jet, thereby inducing substantial cooling in the northern high latitudes. As the stationary waves are progressively generated at higher latitudes, the zonal-mean climate state gradually becomes more similar to the integration with no stationary waves. These differences in the mean climate affect the Arctic climate response to high-latitudes surface warming. Additional surface heating over the Arctic is imposed to the reference climates in which the stationary waves are located at different latitude bands. When the stationary waves are positioned at lower latitudes, the eddy driven jet is located at higher latitude, closer to the prescribed Arctic heating. As baroclinicity is more effectively perturbed, the jet shifts more equatorward that accompanies a larger reduction in the poleward eddy transport of heat and momentum. A stronger eddy-induced descending motion creates greater warming over the Arctic. Our study calls for a more accurate simulation of the present-day stationary wave pattern to enhance the predictability of the Arctic warming response in a changing climate.

  13. Novel RpoS-Dependent Mechanisms Strengthen the Envelope Permeability Barrier during Stationary Phase.

    Science.gov (United States)

    Mitchell, Angela M; Wang, Wei; Silhavy, Thomas J

    2017-01-15

    Gram-negative bacteria have effective methods of excluding toxic compounds, including a largely impermeable outer membrane (OM) and a range of efflux pumps. Furthermore, when cells become nutrient limited, RpoS enacts a global expression change providing cross-protection against many stresses. Here, we utilized sensitivity to an anionic detergent (sodium dodecyl sulfate [SDS]) to probe changes occurring to the cell's permeability barrier during nutrient limitation. Escherichia coli is resistant to SDS whether cells are actively growing, carbon limited, or nitrogen limited. In actively growing cells, this resistance depends on the AcrAB-TolC efflux pump; however, this pump is not necessary for protection under either carbon-limiting or nitrogen-limiting conditions, suggesting an alternative mechanism(s) of SDS resistance. In carbon-limited cells, RpoS-dependent pathways lessen the permeability of the OM, preventing the necessity for efflux. In nitrogen-limited but not carbon-limited cells, the loss of rpoS can be completely compensated for by the AcrAB-TolC efflux pump. We suggest that this difference simply reflects the fact that nitrogen-limited cells have access to a metabolizable energy (carbon) source that can efficiently power the efflux pump. Using a transposon mutant pool sequencing (Tn-Seq) approach, we identified three genes, sanA, dacA, and yhdP, that are necessary for RpoS-dependent SDS resistance in carbon-limited stationary phase. Using genetic analysis, we determined that these genes are involved in two different envelope-strengthening pathways. These genes have not previously been implicated in stationary-phase stress responses. A third novel RpoS-dependent pathway appears to strengthen the cell's permeability barrier in nitrogen-limited cells. Thus, though cells remain phenotypically SDS resistant, SDS resistance mechanisms differ significantly between growth states. Gram-negative bacteria are intrinsically resistant to detergents and many

  14. New poly(styrene/divinylbenzene) based stationary phases for the solid phase extraction of pesticides and the chromatography of carbohydrates

    International Nuclear Information System (INIS)

    Wartusch, I.

    2002-02-01

    The introduced sorbents based on poly(styrene/divinylbenzene) are studied regarding their extraction behavior of pesticides out of water. The sorbents are prepared with different porogens like n-octanol, n-decanol, n-dodecanol and acetone. The comparison of the extraction properties of these substances shows that the use of n-octanol as a porogen leads to the best recoveries. Furthermore this sorbent is compared to a stationary phase prepared via ring opening metathesis polymerization (ROMP) and to commercially available silica-C18. It is shown that the poly(styrene/divinylbenzene) based material on average yields higher recoveries as the other materials. Only the extraction of relatively polar pesticides works better with the ROMP based sorbent. For the chromatography of carbohydrates nonporous particles with diameters of about 3 μm were synthesized via poly(styrene/divinylbenzene) using the activated swelling method. Quaternary ammonia functional groups were introduced into the poly(styrene/divinylbenzene) particles via their nitration, reduction and quaternization. The applicability of these stationary phases for anion exchange chromatography is shown by separation of different kinds of sugars using a pulsed amperometric detection system. Monosaccharides are isocratically separated using an eluent containing sodium hydroxide, separations of disaccharides and oligosaccharides are performed using sodium acetate gradients. Linearity, detection limits and reproducibility of the system are investigated by the analysis of glucose, sucrose and fructose out of the real samples Coca Cola and apple juice. (author)

  15. Branched polyethyleneimine-bonded tentacle-type polymer stationary phase for peptides and proteins separations by open-tubular capillary electrochromatography.

    Science.gov (United States)

    Zhang, Xiaowei; Yang, Juan; Liu, Shaofeng; Lin, Xucong; Xie, Zenghong

    2011-12-01

    A novel tentacle-type polymer stationary phase covalently modified with branched polyethyleneimine (PEI) was developed for peptides and proteins separations by open-tubular CEC (OT-CEC). The preparation procedure included the silanization of capillary inner wall, in situ graft polymerization and PEI functionalization. A wrinkly polymer surface of multitudinous steric amine groups was evenly formed on the capillary inner wall, and anodic EOF could be gained within a wide pH range of 2.5-7.5. The electroosmotic mobility was examined for its dependence on pH as well as PEI concentrations. Good repeatability was gained with RSD for the migration time of EOF marker within 4.8% and satisfactory chemical stability was validated. Due to the existence of amine groups on the surface of tentacle-type polymer stationary phase, the silanol effect that occurs between the positively charged biomolecules and the silanols of the capillary column was greatly suppressed. Compared with a monolayer-coating capillary, seven enkephalin-related peptides were well resolved on the PEI-bonded column with high efficiencies. Favorable separations of peptides and proteins with high column efficiencies were obtained in 144,000-189,000 and 97,000-170,000 plates/m. Branched PEI-bonded tentacle-type polymer stationary phase has been proven to afford satisfactory retention and resolution of peptides and proteins. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Two Synthetic Methods for Preparation of Chiral Stationary Phases Using Crystalline Degradation Products of Vancomycin: Column Performance for Enantioseparation of Acidic and Basic Drugs.

    Science.gov (United States)

    Abdollahpour, Assem; Heydari, Rouhollah; Shamsipur, Mojtaba

    2017-07-01

    Two chiral stationary phases (CSPs) based on crystalline degradation products (CDPs) of vancomycin by using different synthetic methods were prepared and compared. Crystalline degradation products of vancomycin were produced by hydrolytic loss of ammonia from vancomycin molecules. Performances of two chiral columns prepared with these degradation products were investigated using several acidic and basic drugs as model analytes. Retention and resolution of these analytes on the prepared columns, as two main parameters, in enantioseparation were studied. The results demonstrated that the stationary phase preparation procedure has a significant effect on the column performance. The resolving powers of prepared columns for enantiomers resolution were changed with the variation in vancomycin-CDP coverage on the silica support. Elemental analysis was used to monitor the surface coverage of silica support by vancomycin-CDP. The results showed that both columns can be successfully applied to chiral separation studies.

  17. Second-Phase Sampling Designs for Non-Stationary Spatial Variables.

    Science.gov (United States)

    Delmelle, Eric M; Goovaerts, Pierre

    2009-10-15

    In spatial sampling, once initial samples of the primary variable have been collected, it is possible to take additional measurements, an approach known as second-phase sampling. Additional samples are usually collected away from observation locations, or where the kriging variance is maximum. However, the kriging variance (also known as prediction error variance) is independent of data values and computed under the assumption of stationary spatial process, which is often violated in practice. In this paper, we weight the kriging variance with another criterion, giving greater sampling importance to locations exhibiting significant spatial roughness that is computed by a spatial moving average window. Additional samples are allocated using a simulated annealing procedure since the weighted objective function is non-linear. A case study using an exhaustive remote sensing image illustrates the procedure. Combinations of first-phase systematic and nested sampling designs (or patterns) of varying densities are generated, while the location of additional observations is guided in a way which optimizes the proposed objective function. The true pixel value at the new points is extracted, the semivariogram model updated, and the image reconstructed. Second-phase sampling patterns optimizing the proposed criterion lead to predictions closer to the true image than when using the kriging variance as the main criterion. This improvement is stronger when there is a low density of first-phase samples, and decreases however as the initial density increases.

  18. Formation of aromatics in thermally induced reactions of chemically bonded RP-C18 stationary phase.

    Science.gov (United States)

    Prus, Wojciech

    2014-10-01

    In continuation of the research on the thermally induced chemical transformation of the silica-based chemically bonded stationary phases (C18), the oxidative cleavage of the silicon-carbon bonds with hydrogen peroxide and potassium fluoride was utilized, followed by the gas chromatography coupled with mass spectrometry (GC-MS) study of the resulting products. These investigations allowed determination of the probable structures of certain thermal modification products as the various different alkyl derivatives of the phenylsilane ligands. Apart from aromatic compounds, the products with unsaturated bonds and carbonyl functionalities were found in the analyzed extracts. The analysis of the GC-MS chromatograms reveals that under the applied working conditions, the investigated process runs with relatively low yields. © The Author [2013]. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  19. Conventional and fast gas chromatography analysis of biodiesel blends using an ionic liquid stationary phase.

    Science.gov (United States)

    Ragonese, Carla; Tranchida, Peter Quinto; Sciarrone, Danilo; Mondello, Luigi

    2009-12-18

    The present research is focused on the GC-FID determination of fatty acid methyl esters (FAMEs) in diesel blends, by means of an ionic liquid stationary phase, characterized by a dicationic 1,9-di(3-vinyl-imidazolium)nonane bis(trifluoromethyl)sulfonylimidate structure (SLB-IL100). The high polarity of the ionic liquid stationary phase allowed the separation of the FAMEs, from the less-retained hydrocarbons, thus avoiding the requirement of a hydrocarbon LC pre-separation. The results derived from the analyses of a soybean FAMEs B20 sample, carried out on an SLB-IL100 conventional column (30 m x 0.25 mm i.d. x 0.20 mm d(f)), were compared with those attained on a polyethylene glycol column, of equivalent dimensions. Conventional and fast GC methods, for the analysis of FAMEs in diesel blends, were developed on an SLB-IL100 30 m x 0.25 mm i.d. x 0.20 microm d(f) and on an SLB-IL100 12 m x 0.10 mm i.d. x 0.08 microm d(f) column, respectively. The optimized IL methods were subjected to validation: retention time and peak area intra-day precision (n=5) were good, with CV % values lower than 0.08% and 4.9%, respectively. With regards to the quantitation of FAMEs in biodiesel blends, a five points calibration curve was constructed, using C(17:0) as internal standard.

  20. Procedure 5 Quality Assurance Requirements For Vapor Phase Mercury Continuous Emissions Monitoring Systems And Sorbent Trap Monitoring Systems Used For Compliance Determination At Stationary Sources

    Science.gov (United States)

    Promulgated quality assurance Procedure 5 Quality Assurance Requirements For Vapor Phase Mercury Continuous Emissions Monitoring Systems And Sorbent Trap Monitoring Systems Used For Compliance Determination At Stationary Sources

  1. Enantioseparation and chiral recognition mechanism of new chiral derivatives of xanthones on macrocyclic antibiotic stationary phases.

    Science.gov (United States)

    Fernandes, Carla; Tiritan, Maria Elizabeth; Cass, Quezia; Kairys, Visvaldas; Fernandes, Miguel Xavier; Pinto, Madalena

    2012-06-08

    A chiral HPLC method using four macrocyclic antibiotic chiral stationary phases (CSPs) has been investigated for determination of the enantiomeric purity of fourteen new chiral derivatives of xanthones (CDXs). The separations were performed with the CSPs Chirobiotic T, Chirobiotic TAG, Chirobiotic V and Chirobiotic R under multimodal elution conditions (normal-phase, reversed-phase and polar ionic mode). The analyses were performed at room temperature in isocratic mode and UV and CD detection at a wavelength of 254 nm. The best enantioselectivity and resolution were achieved on Chirobiotic R and Chirobiotic T CSPs, under normal elution conditions, with R(S) ranging from 1.25 to 2.50 and from 0.78 to 2.06, respectively. The optimized chromatographic conditions allowed the determination of the enantiomeric ratio of eight CDXs, always higher than 99%. In order to better understand the chromatographic behavior at a molecular level, and the structural features associated with the chiral recognition mechanism, computational studies by molecular docking were carried out using VDock. These studies shed light on the mechanisms involved in the enantioseparation for this important class of chiral compounds. Copyright © 2012 Elsevier B.V. All rights reserved.

  2. Peptidoglycan Recycling in Gram-Positive Bacteria Is Crucial for Survival in Stationary Phase

    Science.gov (United States)

    Borisova, Marina; Gaupp, Rosmarie; Duckworth, Amanda; Schneider, Alexander; Dalügge, Désirée; Mühleck, Maraike; Deubel, Denise; Unsleber, Sandra; Yu, Wenqi; Muth, Günther; Bischoff, Markus; Götz, Friedrich

    2016-01-01

    ABSTRACT Peptidoglycan recycling is a metabolic process by which Gram-negative bacteria reutilize up to half of their cell wall within one generation during vegetative growth. Whether peptidoglycan recycling also occurs in Gram-positive bacteria has so far remained unclear. We show here that three Gram-positive model organisms, Staphylococcus aureus, Bacillus subtilis, and Streptomyces coelicolor, all recycle the sugar N-acetylmuramic acid (MurNAc) of their peptidoglycan during growth in rich medium. They possess MurNAc-6-phosphate (MurNAc-6P) etherase (MurQ in E. coli) enzymes, which are responsible for the intracellular conversion of MurNAc-6P to N-acetylglucosamine-6-phosphate and d-lactate. By applying mass spectrometry, we observed accumulation of MurNAc-6P in MurNAc-6P etherase deletion mutants but not in either the isogenic parental strains or complemented strains, suggesting that MurQ orthologs are required for the recycling of cell wall-derived MurNAc in these bacteria. Quantification of MurNAc-6P in ΔmurQ cells of S. aureus and B. subtilis revealed small amounts during exponential growth phase (0.19 nmol and 0.03 nmol, respectively, per ml of cells at an optical density at 600 nm [OD600] of 1) but large amounts during transition (0.56 nmol and 0.52 nmol) and stationary (0.53 nmol and 1.36 nmol) phases. The addition of MurNAc to ΔmurQ cultures greatly increased the levels of intracellular MurNAc-6P in all growth phases. The ΔmurQ mutants of S. aureus and B. subtilis showed no growth deficiency in rich medium compared to the growth of the respective parental strains, but intriguingly, they had a severe survival disadvantage in late stationary phase. Thus, although peptidoglycan recycling is apparently not essential for the growth of Gram-positive bacteria, it provides a benefit for long-term survival. PMID:27729505

  3. Effect of benzalkonium chloride on viability and energy metabolism in exponential- and stationary-growth-phase cells of Listeria monocytogenes

    NARCIS (Netherlands)

    Luppens, S.B.I.; Abee, T.; Oosterom, J.

    2001-01-01

    The difference in killing exponential- and stationary-phase cells of Listeria monocytogenes by benzalkonium chloride (BAC) was investigated by plate counting and linked to relevant bioenergetic parameters. At a low concentration of BAC (8 mg liter-1), a similar reduction in viable cell numbers was

  4. A polyacrylamide-based silica stationary phase for the separation of carbohydrates using alcohols as the weak eluent in hydrophilic interaction liquid chromatography.

    Science.gov (United States)

    Cai, Jianfeng; Cheng, Lingping; Zhao, Jianchao; Fu, Qing; Jin, Yu; Ke, Yanxiong; Liang, Xinmiao

    2017-11-17

    A hydrophilic interaction liquid chromatography (HILIC) stationary phase was prepared by a two-step synthesis method, immobilizing polyacrylamide on silica sphere particles. The stationary phase (named PA, 5μm dia) was evaluated using a mixture of carbohydrates in HILIC mode and the column efficiency reached 121,000Nm -1 . The retention behavior of carbohydrates on PA stationary phase was investigated with three different organic solvents (acetonitrile, ethanol and methanol) employed as the weak eluent. The strongest hydrophilicity of PA stationary phase was observed in both acetonitrile and methanol as the weak eluent, when compared with another two amide stationary phases. Attributing to its high hydrophilicity, three oligosaccharides (xylooligosaccharide, fructooligosaccharide and chitooligosaccharides) presented good retention on PA stationary phase using alcohols/water as mobile phase. Finally, PA stationary phase was successfully applied for the purification of galactooligosaccharides and saponins of Paris polyphylla. It is feasible to use safer and cheaper alcohols to replace acetonitrile as the weak eluent for green analysis and purification of polar compounds on PA stationary phase. Copyright © 2017. Published by Elsevier B.V.

  5. Evaluation of mesoporous silicas functionalized with C18 groups as stationary phases for the solid-phase extraction of steroid hormones in milk.

    Science.gov (United States)

    Pérez-Fernández, Virginia; Morante-Zarcero, Sonia; Pérez-Quintanilla, Damián; García, María Ángeles; Marina, María Luisa; Alonso, Isabel Sierra

    2014-06-01

    In this work, two mesoporous silicas functionalized with C18 groups (SM-C18 and SBA-15-C18) have been synthesized for their evaluation as stationary phases in SPE for the extraction and preconcentration of seven steroid hormones (estrone, estradiol, estriol, ethinyl estradiol, diethylstilbestrol, testosterone, and progesterone ) from milk. The characterization of both materials by diverse techniques such as transmission electron microscopy, SEM, thermogravimetric analysis, X-ray diffraction, and adsorption-desorption isotherms showed that the mesoporous silicas had a high surface area, high pore volume, and a homogeneous distribution of the pores and that both silicas presented a similar degree of functionalization. An analytical methodology for the simultaneous separation of the seven selected steroids by HPLC-DAD was developed. Both silicas were evaluated as stationary phases in SPE for the extraction of the steroid hormones from milk. This HPLC-DAD method was applied to the analysis of all extracts obtained in the SPE experiments, showing that from the two synthesized mesoporus silicas, SBA-15-C18 silica enabled the extraction of the seven compounds with recoveries between 88 and 108% for all except for estriol, for which a recovery of 62% was obtained. The analytical characteristics of this methodology were evaluated, showing good precision and linearity (R2 > 0.994) for all analytes. The comparison of the results obtained with this silica and those obtained with commercial C18 particles and with some other commercial cartridges usually employed in the extraction of steroids showed that SBA-15-C18 silica was able to extract the seven steroids with higher recovery values. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Impact of column and stationary phase properties on the productivity in chiral preparative LC.

    Science.gov (United States)

    Forssén, Patrik; Fornstedt, Torgny

    2018-03-01

    By generating 1500 random chiral separation systems, assuming two-site Langmuir interactions, we investigated numerically how the maximal productivity (P R,max ) was affected by changes in stationary phase adsorption properties. The relative change in P R,max , when one adsorption property changed 10%, was determined for each system and for each studied parameter the corresponding productivity change distribution of the systems was analyzed. We could conclude that there is no reason to have columns with more than 500 theoretical plates and larger selectivity than 3. More specifically, we found that changes in selectivity have a major impact on P R,max if it is below ∼2 and, interestingly, increasing selectivity when it is above ∼3 decreases P R,max . Increase in relative saturation capacity will have a major impact on P R,max if it is below ∼40%, but only modest above this percent. Increasing total monolayer saturation capacity, or decreasing the first eluting enantiomer's retention factor, will have a modest effect on P R,max and increased efficiency will have almost no effect at all on P R,max unless it is below ∼500 theoretical plates. Finally, we showed that chiral columns with superior analytic performance might have inferior preparative performance, or vice versa. It is, therefore, not possible to assess columns based on their analytical performance alone. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Proteomic analysis of lactose-starved Lactobacillus casei during stationary growth phase.

    Science.gov (United States)

    Hussain, M A; Knight, M I; Britz, M L

    2009-03-01

    Starvation stress is a condition that nonstarter lactic acid bacteria (NSLAB) normally encounter. This study was aimed to investigate starvation-induced proteins in Lactobacillus casei during stationary growth phase. The impact of carbohydrate starvation on L. casei GCRL163 was investigated using two different media (a modified de Man, Rogosa and Sharpe broth and a semi-defined medium). Cells were grown in the presence of excess lactose (1%) or starvation (0%) and differences in the patterns of one-dimensional sodium dodecyl sulfate-polyacrylamide gel electrophoresis and two-dimensional electrophoresis of the cytosolic protein fractions were investigated. Differentially regulated proteins were identified by MALDI-TOF/TOF mass spectrometry. Many differentially regulated proteins were enzymes of various metabolic pathways involved in carbohydrate metabolism to yield energy. Differences in protein expression were also observed in the two culture conditions tested in this experiment. Numerous glycolytic enzymes were differentially regulated under lactose starvation. The differential expression of these glycolytic enzymes suggests a potential survival strategy under harsh growth conditions (i.e. lactose starvation). This paper reports improved understanding of stress responses and survival mechanism of NSLAB under lactose-depleted cheese-ripening condition. This knowledge of how NSLAB bacteria adapt to lactose starvation could be applied to predict the performances of bacteria in other industrial applications.

  8. Site-Specific Ser/Thr/Tyr Phosphoproteome of Sinorhizobium meliloti at Stationary Phase.

    Directory of Open Access Journals (Sweden)

    Tao Liu

    Full Text Available Sinorhizobium meliloti, a facultative microsymbiont of alfalfa, should fine-tune its cellular processes to live saprophytically in soils characterized with limited nutrients and diverse stresses. In this study, TiO2 enrichment and LC-MS/MS were used to uncover the site-specific Ser/Thr/Tyr phosphoproteome of S. meliloti in minimum medium at stationary phase. There are a total of 96 unique phosphorylated sites, with a Ser/Thr/Tyr distribution of 63:28:5, in 77 proteins. Phosphoproteins identified in S. meliloti showed a wide distribution pattern regarding to functional categories, such as replication, transcription, translation, posttranslational modification, transport and metabolism of amino acids, carbohydrate, inorganic ion, succinoglycan etc. Ser/Thr/Tyr phosphosites identified within the conserved motif in proteins of key cellular function indicate a crucial role of phosphorylation in modulating cellular physiology. Moreover, phosphorylation in proteins involved in processes related to rhizobial adaptation was also discussed, such as those identified in SMa0114 and PhaP2 (polyhydroxybutyrate synthesis, ActR (pH stress and microaerobic adaption, SupA (potassium stress, chaperonin GroEL2 (viability and potentially symbiosis, and ExoP (succinoglycan synthesis and secretion. These Ser/Thr/Tyr phosphosites identified herein would be helpful for our further investigation and understanding of the role of phosphorylation in rhizobial physiology.

  9. A comparison of protein A chromatographic stationary phases: performance characteristics for monoclonal antibody purification.

    Science.gov (United States)

    Liu, Zhuo; Mostafa, Sigma S; Shukla, Abhinav A

    2015-01-01

    Protein A chromatography remains the dominant capture step used during the downstream purification of monoclonal antibodies (mAbs). With the recent expiry of the Repligen patent on recombinant Protein A, a variety of new Protein A resins have been introduced in the market. Given productivity limitations during downstream processing that have come into sharper focus with the recent increase in cell culture titers for mAbs, the selection of an appropriate Protein A resin has direct implications on the overall process economics of mAb production. The performance of seven different Protein A chromatographic resins was compared with respect to static binding capacity and dynamic binding capacity as a function of flow rate. This data was translated into a comparison of productivity (g mAb purified per unit resin volume per unit time) for the seven stationary phases. In addition, elution pH and host cell protein impurity levels after product capture on each of these resins were determined. The current article provides an effective methodology and dataset for the selection of the optimal Protein A chromatographic resin. © 2014 International Union of Biochemistry and Molecular Biology, Inc.

  10. Chiral separation of helical chromenes with chloromethyl phenylcarbamate polysaccharide-based stationary phases.

    Science.gov (United States)

    Ianni, Federica; Scorzoni, Stefania; Gentili, Pier Luigi; Di Michele, Alessandro; Frigoli, Michel; Camaioni, Emidio; Ortica, Fausto; Sardella, Roccaldo

    2017-12-12

    Two chloromethyl phenylcarbamate-based chiral stationary phases, one containing an amylose-type chiral selector (Lux Amylose 2, from Phenomenex) and the other a cellulose-type one (Lux Cellulose-4, from Phenomenex), were successfully used for the chiral resolution of three helical chromenes featuring a helicene-like structure. The compound bearing a phenyl substituent on the helicene-like structure was enantioresolved at 25°C with Lux Cellulose-4 and a n-hexane/1-propanol 99:1 v/v eluent. With a n-hexane/2-propanol 99.8:0.2 v/v mobile phase, the same column (operated at 35°C) provided the separation of the four isomers of the compound having a hexyl residue on the helicene-like motif and an additional asymmetric carbon. Lux Amylose-2 was necessary for the enantioseparation of the compound having the sole hexyl residue on the helical scaffold. For the last compound a n-hexane/2-propanol 99.8:0.2 v/v eluent was used, and the column temperature was fixed at 5°C. The enantiomer elution order was appraised by using electronic circular dichroism and theoretical calculations. Notably, different thermodynamics of retention and enantioseparation were observed for molecules with pronounced structural similarity, that is, the enantiomer pairs of the compound containing the additional asymmetric carbon atom. Indeed, both entropically and enthalpically controlled adsorption and separation processes were observed. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Enantioselective determination of arotinolol in human plasma by HPLC using teicoplanin chiral stationary phase.

    Science.gov (United States)

    Aboul-Enein, Hassan Y; Hefnawy, Mohamed M

    2003-10-01

    A sensitive enantioselective high-performance liquid chromatography (HPLC) method was developed and validated to determine S-(+)- and R-(-)-arotinolol in human plasma. Baseline resolution was achieved by using teicoplanin macrocyclic antibiotic chiral stationary phase (CSP) known as Chirobiotic T with a polar organic mobile phase consisting of methanol:glacial acetic acid:triethylamine, 100:0.1:0.1, (v/v/v) at a fl ow rate of 0.8 mL/min and UV detection set at 317 nm. Human plasma was spiked with stock solution of arotinolol enantiomers and labetalol as the internal standard. The assay involved the use of liquid-liquid extraction procedure with ethyl ether under alkaline condition for human plasma sample prior to HPLC analysis. Recoveries for S-(+)- and R-(-)-arotinolol enantiomers were in the range 93-103% at 200-1400 ng/mL level. Intra-day and inter-day precision calculated as %RSD was in the ranges 1.3-3.4 and 1.9-4.5% for both enantiomers, respectively. Intra-day and inter-day accuracies calculated as percentage error were in the ranges 1.2-3.5 and 1.5-6.2% for both enantiomers, respectively. Linear calibration curves in the concentration range 100-1500 ng/mL for each enantiomer showed a correlation coefficient (r) of 0.9998. The limit of quantitation (LOQ) and limit of detection (LOD) for each enantiomer in human plasma were 100 and 50 ng/mL (S/N = 3), respectively. Copyright 2003 John Wiley & Sons, Ltd.

  12. Synthesis of a mixed-model stationary phase derived from glutamine for HPLC separation of structurally different biologically active compounds: HILIC and reversed-phase applications.

    Science.gov (United States)

    Aral, Tarık; Aral, Hayriye; Ziyadanoğulları, Berrin; Ziyadanoğulları, Recep

    2015-01-01

    A novel mixed-mode stationary phase was synthesised starting from N-Boc-glutamine, aniline and spherical silica gel (4 µm, 60 Å). The prepared stationary phase was characterized by IR and elemental analysis. The new stationary phase bears an embedded amide group into phenyl ring, highly polar a terminal amide group and non-polar groups (phenyl and alkyl groups). At first, this new mixed-mode stationary phase was used for HILIC separation of four nucleotides and five nucleosides. The effects of different separation conditions, such as pH value, mobile phase and temperature, on the separation process were investigated. The optimum separation for nucleotides was achieved using HILIC isocratic elution with aqueous mobile phase and acetonitrile with 20°C column temperature. Under these conditions, the four nucleotides could be separated and detected at 265 nm within 14 min. Five nucleosides were separated under HILIC isocratic elution with aqueous mobile phase containing pH=3.25 phosphate buffer (10mM) and acetonitrile with 20°C column temperature and detected at 265 nm within 14 min. Chromatographic parameters as retention factor, selectivity, theoretical plate number and peak asymmetry factor were calculated for the effect of temperature and water content in mobile phase on the separation process. The new column was also tested for nucleotides and nucleosides mixture and six analytes were separated in 10min. The chromatographic behaviours of these polar analytes on the new mixed-model stationary phase were compared with those of HILIC columns under similar conditions. Further, phytohormones and phenolic compounds were separated in order to see influence of the new stationary phase in reverse phase conditions. Eleven plant phytohormones were separated within 13 min using RP-HPLC gradient elution with aqueous mobile phase containing pH=2.5 phosphate buffer (10mM) and acetonitrile with 20°C column temperature and detected at 230 or 278 nm. The best separation

  13. Preparation of chitosan-graft-(β-cyclodextrin) based sol-gel stationary phase for open-tubular capillary electrochromatography.

    Science.gov (United States)

    Lü, Haixia; Li, Qingyin; Yu, Xiaowei; Yi, Jiaojiao; Xie, Zenghong

    2013-07-01

    A novel open-tubular CEC column coated with chitosan-graft-(β-CD) (CDCS) was prepared using sol-gel technique. In the sol-gel approach, owing to the 3D network of sol-gel and the strong chemical bond between the stationary phase and the surface of capillary columns, good chromatographic characteristics and unique selectivity in separating isomers were shown. The column efficiencies of 55,000∼163,000 plates/m for the isomeric xanthopterin and phenoxy acid herbicides using the sol-gel-derived CDCS columns were achieved. Good stabilities were demonstrated that the RSD values for the retention time of thiourea and isoxanthopterin were 1.3 and 1.4% (run to run, n = 5), 1.6 and 2.0% (day to day, n = 3), 2.9 and 3.1% (column to column, n = 3), respectively. The sol-gel-coated CDCS columns have shown improved separations of isomeric xanthopterin in comparison with CDCS-bonded capillary column. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Microstructure-based analysis and simulation of flow and mass transfer in chromatographic stationary phases

    Science.gov (United States)

    Koku, Harun

    Limitations of mass transfer in chromatographic bioseparations employing traditional packed particles have fuelled the inception and development of alternative stationary phases with improved performance characteristics. This work investigates case studies in two categories of these alternative media, namely polymer-modified packed particles and continuous monolithic phases, for insight into their enhanced properties. Specifically, high-resolution microscopy techniques and image-based analysis algorithms were implemented to extract morphology information for these materials, in an attempt to elucidate the relation between microstructure and performance. For the monolith, mesoscopic simulation methods were also employed for a more rigorous analysis of the flow and dispersion behavior. Scanning and transmission electron microscopy images of the commercial polymer-modified, agarose-based particle Sepharose XL were compared to those for its unmodified counterpart, Sepharose FF. Local regions in the composite dextran-agarose Sepharose XL particles were noted to exhibit a denser network of fibers and smaller pore sizes overall, compared to those in the traditional Sepharose FF particles. Images of particles equilibrated with high concentrations of protein revealed a significant difference in protein localization patterns, with the stained protein in XL occupying a markedly higher area fraction of the images. This suggests a higher volume available for adsorption and provides visual clues into how the consistently higher static capacity of these polymer-modified particles is manifested. Treatment of the XL particles with dextranase, an enzyme that breaks down dextran, resulted in a reduction of protein coverage, providing evidence that it is indeed the dextran that is responsible for the improved static capacity in this polymer-modified stationary phase. Imaging and image analysis techniques were also used to analyze the commercial CIM(TM) disk monolith. Two- and three

  15. Contaminants migration in the soil: the influence of transfer between the mobile and stationary phases

    International Nuclear Information System (INIS)

    Moreira, R.M.; Sabino, C.S.V.; Macedo, W.A.

    1996-01-01

    Three transport mechanisms control the contaminant migration in saturated soils: advection, diffusion and interchanges between liquid and solid phases. These interchanges define the retention by the soil and the contaminant delay related to the liquid phase flow. Therefore, the knowledge of the adsorption/desorption characteristics of the solute in solid surfaces is fundamental for the evaluation of toxic agent releases to the compartment soil. This communication reports the study which is being performed by the Centro de Desenvolvimento da Tecnologia Nuclear (CDTN) in this area, particularly with cesium and mercury by using X-ray absorption spectroscopy for contaminants migration

  16. Regenerated silica gel as stationary phase on vacuum column chromatography to purify temulawak's extracts

    Science.gov (United States)

    Cahyono, Bambang; Maduwu, Ratna Dewi; Widayat, Suzery, Meiny

    2015-12-01

    Commercial silica gel only used once by many researchers and affected high cost for purification process, also less support the green chemistry program. This research focused in regeneration silica gel that used purification of temulawak's extracts (Curcuma xanthorrhiza Roxb) by vacuum column chromatography. Sample extracts (contains 10.1195±0.5971% of curcuminoids) was purified by vacuum column chromatography (pressure: 45 kPa, column: 100mm on length and 16mm on diameter). Ethanol 96% and acetone were compared as eluent. The amount of solvent and yield of curcuminoids used as indicator purification. The silica gel was regenerated with heating in 600°C for 8 hours The silica gels were analyzed by IR spectroscopy and X-ray diffraction. Furthermore, regenerated silica gel was used as the stationary phase in vacuum column chromatography under the same conditions with the previous purification. All the purification experiments were performed in three repetitions. Based on regression equation, y=0.132x+0.0011 (r2=0.9997) the yield of curcuminoids on purified products using ethanol as the eluent was improved 4.26% (to 14.3724±0.5749%) and by acetone was improved 3,03% (to 13.1450 ±0.6318%). The IR spectrum of both silica gel showed the same vibration profile and also there were three crystallinity peaks missing on its X-ray diffraction. Regenerated silica gel has the same performance with new silica gel in purification of temulawak's extract: by ethanol has increased 4.08% (14.1947±0.7415%) and 2.93% (13.0447±0.4822) by acetone. In addition, all purification products showed similar TLC profiles. Purification using regenerated silica gel as the adsorbent on vacuum column chromatography has exactly same potential with the new silica gel.

  17. Enantiodifferentiation of whisky and cognac lactones using gas chromatography with different cyclodextrin chiral stationary phases.

    Science.gov (United States)

    Schmarr, Hans-Georg; Mathes, Maximilian; Wall, Kristina; Metzner, Frank; Fraefel, Marius

    2017-09-22

    The chiral lactone 5-butyl-4-methyloxolan-2-one or 5-butyl-4-methyldihydro-2(3H)-furanone, often named whisky lactone, is found in oak wood, then contributing to the appreciated flavor of beverages stored in such wooden barrels. Its next higher homologue is named cognac lactone (5-pentyl-4-methyloxolan-2-one or 5-pentyl-4-methyldihydro-2(3H)-furanone), however is much less known, probably due to its minor concentration level. In order to study the direct enantioseparation of both lactones by gas chromatography on chiral stationary phases, individual enantiomers, particularly for cognac lactone were made available. This was achieved by baker's yeast reduction of synthesized ethyl 3-methyl-4-oxononanoate or, after hydrolysis, of the corresponding 4-ketoacid, that gave access to individual enantiomers of cognac lactone. Good enantioseparation was achieved for both whisky and cognac lactone with high values for the chiral resolution with 6-O-tert. butyl dimethylsilyl-2,3-dialkylated or 6-O-tert. butyl dimethylsilyl-2,3-diacylated cyclodextrin derivatives as chiral selectors. The influence of the nature and position of derivatization of the cyclodextrin moiety revealed a strong impact on the chiral recognition mechanism, as the investigated alkylated derivatives heptakis-(2,6-di-O-iso-pentyl-3-O-allyl)-β-cyclodextrin and octakis-(2,3-di-O-pentyl-6-O-methyl)-γ-cyclodextrin did not provide any or only minor chiral selectivity for the two lactones. Copyright © 2017 Elsevier B.V. All rights reserved.

  18. Enantiomeric separation of iridium (III) complexes using HPLC chiral stationary phases based on amylose derivatives

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Hee Eun; Seo, Na Hyeon; Hyun, Myung Ho [Dept. of Chemistry and Chemistry Institute for Functional Materials, Pusan National University, Busan (Korea, Republic of)

    2016-12-15

    Cyclometalated iridium (III) complexes formed with three identical cyclometalating (C-N) ligands (homoleptic) or formed with two cyclometalating (C-N) ligands and one ancillary (LX) ligand (heteroleptic) have been known as highly phosphorescent materials and, thus, they have been utilized as efficient phosphorescent dopants in organic light emitting diodes (OLEDs) 1–3 or as effective phosphorescent chemosensors. 4–7 Cylometalated iridium (III) complexes are chiral compounds consisting of lambda (Λ, left-handed) and delta (Δ, right-handed) isomers. Racemic cyclometa- lated iridium (III) complexes emit light with no net polarization, but optically active cyclometalated iridium (III) complexes emit circularly polarized light. 8,9 Circularly polarized light can be used in various fields including highly efficient three dimensional electronic devices, photo nic devices for optical data storage, biological assays, and others. 8,9 In order to obtain optically active cylometalated iridium (III) complexes and to determine the enantiomeric composition of optically active cylometalated iridium (III) complexes, liquid chromatogr aphic enantiomer separation method on chiral stationary phases (CSPs) has been used. For example, Okamoto and coworkers first reported the high performance liquid chromatographic (HPLC) direct enantiomeric separation of two homoleptic cylometalated iridium (III) complexes on immobilized amylose tris(3,5- dimethylphenylcarbamate) (Chiralpak IA), coated cellulose tris(3,5-dimethylphenylcarbamate) (Chiralc el OD), and coated cellulose tris(4-methylbenzoate) (Chiralce l OJ). 10 Supercritical fluid chromatography (SFC) was also used by Bernhard and coworkers for the enantiomeric separation of cylometalated iridium (III) complexes on coated amylose tris(3,5-dimethylphenylcarbamate) (Chiralpak AD-H). 8 However, the general use of the HPLC method for the direct enantiomeric separation of homoleptic.

  19. Regenerated silica gel as stationary phase on vacuum column chromatography to purify temulawak’s extracts

    International Nuclear Information System (INIS)

    Cahyono, Bambang; Maduwu, Ratna Dewi; Widayat,; Suzery, Meiny

    2015-01-01

    Commercial silica gel only used once by many researchers and affected high cost for purification process, also less support the green chemistry program. This research focused in regeneration silica gel that used purification of temulawak’s extracts (Curcuma xanthorrhiza Roxb) by vacuum column chromatography. Sample extracts (contains 10.1195±0.5971% of curcuminoids) was purified by vacuum column chromatography (pressure: 45 kPa, column: 100mm on length and 16mm on diameter). Ethanol 96% and acetone were compared as eluent. The amount of solvent and yield of curcuminoids used as indicator purification. The silica gel was regenerated with heating in 600°C for 8 hours The silica gels were analyzed by IR spectroscopy and X-ray diffraction. Furthermore, regenerated silica gel was used as the stationary phase in vacuum column chromatography under the same conditions with the previous purification. All the purification experiments were performed in three repetitions. Based on regression equation, y=0.132x+0.0011 (r 2 =0.9997) the yield of curcuminoids on purified products using ethanol as the eluent was improved 4.26% (to 14.3724±0.5749%) and by acetone was improved 3,03% (to 13.1450 ±0.6318%). The IR spectrum of both silica gel showed the same vibration profile and also there were three crystallinity peaks missing on its X-ray diffraction. Regenerated silica gel has the same performance with new silica gel in purification of temulawak’s extract: by ethanol has increased 4.08% (14.1947±0.7415%) and 2.93% (13.0447±0.4822) by acetone. In addition, all purification products showed similar TLC profiles. Purification using regenerated silica gel as the adsorbent on vacuum column chromatography has exactly same potential with the new silica gel

  20. Regenerated silica gel as stationary phase on vacuum column chromatography to purify temulawak’s extracts

    Energy Technology Data Exchange (ETDEWEB)

    Cahyono, Bambang; Maduwu, Ratna Dewi; Widayat,; Suzery, Meiny [Organic Chemistry Laboratory, Departement of Chemistry, Diponegoro University Jln Prof. Soedharto SH, Tembalang, Semarang 50275, Indonesia Tel / Fax: (024) 7460058 (Indonesia)

    2015-12-29

    Commercial silica gel only used once by many researchers and affected high cost for purification process, also less support the green chemistry program. This research focused in regeneration silica gel that used purification of temulawak’s extracts (Curcuma xanthorrhiza Roxb) by vacuum column chromatography. Sample extracts (contains 10.1195±0.5971% of curcuminoids) was purified by vacuum column chromatography (pressure: 45 kPa, column: 100mm on length and 16mm on diameter). Ethanol 96% and acetone were compared as eluent. The amount of solvent and yield of curcuminoids used as indicator purification. The silica gel was regenerated with heating in 600°C for 8 hours The silica gels were analyzed by IR spectroscopy and X-ray diffraction. Furthermore, regenerated silica gel was used as the stationary phase in vacuum column chromatography under the same conditions with the previous purification. All the purification experiments were performed in three repetitions. Based on regression equation, y=0.132x+0.0011 (r{sup 2}=0.9997) the yield of curcuminoids on purified products using ethanol as the eluent was improved 4.26% (to 14.3724±0.5749%) and by acetone was improved 3,03% (to 13.1450 ±0.6318%). The IR spectrum of both silica gel showed the same vibration profile and also there were three crystallinity peaks missing on its X-ray diffraction. Regenerated silica gel has the same performance with new silica gel in purification of temulawak’s extract: by ethanol has increased 4.08% (14.1947±0.7415%) and 2.93% (13.0447±0.4822) by acetone. In addition, all purification products showed similar TLC profiles. Purification using regenerated silica gel as the adsorbent on vacuum column chromatography has exactly same potential with the new silica gel.

  1. Enantiomeric separation of iridium (III) complexes using HPLC chiral stationary phases based on amylose derivatives

    International Nuclear Information System (INIS)

    Kim, Hee Eun; Seo, Na Hyeon; Hyun, Myung Ho

    2016-01-01

    Cyclometalated iridium (III) complexes formed with three identical cyclometalating (C-N) ligands (homoleptic) or formed with two cyclometalating (C-N) ligands and one ancillary (LX) ligand (heteroleptic) have been known as highly phosphorescent materials and, thus, they have been utilized as efficient phosphorescent dopants in organic light emitting diodes (OLEDs) 1–3 or as effective phosphorescent chemosensors. 4–7 Cylometalated iridium (III) complexes are chiral compounds consisting of lambda (Λ, left-handed) and delta (Δ, right-handed) isomers. Racemic cyclometa- lated iridium (III) complexes emit light with no net polarization, but optically active cyclometalated iridium (III) complexes emit circularly polarized light. 8,9 Circularly polarized light can be used in various fields including highly efficient three dimensional electronic devices, photo nic devices for optical data storage, biological assays, and others. 8,9 In order to obtain optically active cylometalated iridium (III) complexes and to determine the enantiomeric composition of optically active cylometalated iridium (III) complexes, liquid chromatogr aphic enantiomer separation method on chiral stationary phases (CSPs) has been used. For example, Okamoto and coworkers first reported the high performance liquid chromatographic (HPLC) direct enantiomeric separation of two homoleptic cylometalated iridium (III) complexes on immobilized amylose tris(3,5- dimethylphenylcarbamate) (Chiralpak IA), coated cellulose tris(3,5-dimethylphenylcarbamate) (Chiralc el OD), and coated cellulose tris(4-methylbenzoate) (Chiralce l OJ). 10 Supercritical fluid chromatography (SFC) was also used by Bernhard and coworkers for the enantiomeric separation of cylometalated iridium (III) complexes on coated amylose tris(3,5-dimethylphenylcarbamate) (Chiralpak AD-H). 8 However, the general use of the HPLC method for the direct enantiomeric separation of homoleptic

  2. Capillary electrochromatography of inorganic cations in open tubular columns with a controllable capacity multilayered stationary phase architecture

    Czech Academy of Sciences Publication Activity Database

    Kubáň, Pavel; Kubáň, P.; Kubáň, V.; Hauser, P.C.; Boček, Petr

    2008-01-01

    Roč. 1190, 1-2 (2008), s. 377-382 ISSN 0021-9673 R&D Projects: GA ČR GA203/08/1536; GA AV ČR IAA400310703; GA AV ČR IAA400310609 Institutional research plan: CEZ:AV0Z40310501 Keywords : contactless conductivity detection * open- tubular columns * stationary phases Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.756, year: 2008

  3. Role of nutrient limitation and stationary-phase existence in Klebsiella pneumoniae biofilm resistance to ampicillin and ciprofloxacin.

    Science.gov (United States)

    Anderl, Jeff N; Zahller, Jeff; Roe, Frank; Stewart, Philip S

    2003-04-01

    Biofilms formed by Klebsiella pneumoniae resisted killing during prolonged exposure to ampicillin or ciprofloxacin even though these agents have been shown to penetrate bacterial aggregates. Bacteria dispersed from biofilms into medium quickly regained most of their susceptibility. Experiments with free-floating bacteria showed that stationary-phase bacteria were protected from killing by either antibiotic, especially when the test was performed in medium lacking carbon and nitrogen sources. These results suggested that the antibiotic tolerance of biofilm bacteria could be explained by nutrient limitation in the biofilm leading to stationary-phase existence of at least some of the cells in the biofilm. This mechanism was supported by experimental characterization of nutrient availability and growth status in biofilms. The average specific growth rate of bacteria in biofilms was only 0.032 h(-1) compared to the specific growth rate of planktonic bacteria of 0.59 h(-1) measured in the same medium. Glucose did not penetrate all the way through the biofilm, and oxygen was shown to penetrate only into the upper 100 micro m. The specific catalase activity was elevated in biofilm bacteria to a level similar to that of stationary-phase planktonic cells. Transmission electron microscopy revealed that bacteria were affected by ampicillin near the periphery of the biofilm but were not affected in the interior. Taken together, these results indicate that K. pneumoniae in this system experience nutrient limitation locally within the biofilm, leading to zones in which the bacteria enter stationary phase and are growing slowly or not at all. In these inactive regions, bacteria are less susceptible to killing by antibiotics.

  4. Micro-fabricated semi-packed column for gas chromatography by using functionalized parylene as a stationary phase

    International Nuclear Information System (INIS)

    Nakai, T; Nishiyama, S; Shuzo, M; Delaunay, J-J; Yamada, I

    2009-01-01

    The conformal coating of effective stationary phases onto micro-fabricated columns having complex geometries such as semi-packed columns poses a real challenge. Here, we report for the first time the conformal coating of a semi-packed column with amino-functionalized parylene diX-AM (poly-aminomethyl-[2,2]-paracyclophane), which was found to be an effective stationary-phase material for the chromatography of short-retention-time compounds. A semi-packed column (consisting of a zigzag array of 30 µm square micro-pillars in a 1.0 m long, 180 µm wide and 230 µm deep channel) and an open tubular column (1.0 m long, 160 µm wide and 230 µm deep channel) used for comparison purposes were micro-fabricated on silicon that was subsequently coated with diX-AM parylene and thermally bonded. The chromatograms recorded on a commercial gas chromatograph demonstrated the usefulness of the conformal diX-AM coating as a stationary phase for semi-packed columns. The separation efficiency of the semi-packed column was found to be more than ten times that of the open tubular column

  5. A stationary phase solution for mountain waves with application to mesospheric mountain waves generated by Auckland Island

    Science.gov (United States)

    Broutman, Dave; Eckermann, Stephen D.; Knight, Harold; Ma, Jun

    2017-01-01

    A relatively general stationary phase solution is derived for mountain waves from localized topography. It applies to hydrostatic, nonhydrostatic, or anelastic dispersion relations, to arbitrary localized topography, and to arbitrary smooth vertically varying background temperature and vector wind profiles. A simple method is introduced to compute the ray Jacobian that quantifies the effects of horizontal geometrical spreading in the stationary phase solution. The stationary phase solution is applied to mesospheric mountain waves generated by Auckland Island during the Deep Propagating Gravity Wave Experiment. The results are compared to a Fourier solution. The emphasis is on interpretations involving horizontal geometrical spreading. The results show larger horizontal geometrical spreading for nonhydrostatic waves than for hydrostatic waves in the region directly above the island; the dominant effect of horizontal geometrical spreading in the lower ˜30 km of the atmosphere, compared to the effects of refraction and background density variation; and the enhanced geometrical spreading due to directional wind in the approach to a critical layer in the mesosphere.

  6. Damage identification from uniform load surface using continuous and stationary wavelet transforms

    Directory of Open Access Journals (Sweden)

    M. Masoumi

    Full Text Available Derived from flexibility matrix, Uniform Load Surface (ULS is used to identify damages in beam-type structures. This method is beneficial in terms of more participating the lower order modes and having less prone to noise and irregularities in the measured data in comparison with the original flexibility matrix technique. Therefore, these characteristics make this approach a practical tool in the field of damage identification. This paper presents a procedure to employ stationary wavelet transform multi-resolution analysis (SWT-MRA to refine ULS obtained from the damaged structure and then using continuous wavelet transform (CWT for localizing the discontinuity of improved ULS as a sign of damage site. Evaluation of the proposed method is carried out by examining a cantilever beam as a numerical case, where the ULS is formed by using mode shapes of damaged beam and two kinds of wavelets (i.e. symmetrical 4 and bior 6.8 is applied for discerning the induced crack. Moreover, a laboratory test is conducted on a free-free beam to experimentally evaluate the practicability of the technique.

  7. Characterization of polyaniline-coated stationary phases by using the linear solvation energy relationship in the hydrophilic interaction liquid chromatography mode using capillary liquid chromatography.

    Science.gov (United States)

    Taraba, Lukáš; Křížek, Tomáš; Hodek, Ondřej; Kalíková, Květa; Coufal, Pavel

    2017-02-01

    A polyaniline coating was used to modify the surface of bare silica gel and octadecyl silica stationary phases to characterize the properties of altered materials. It was assumed that the mixed-mode retention was established on the basis of the polyaniline chemical structure and its combination with the original sorbents. Polyaniline was deposited onto the original surfaces during the chemical polymerization of aniline hydrochloride. The prepared materials were slurry packed into capillary columns and systematic chromatographic characterization was performed using the linear solvation energy relationship, also employing descriptors that allow inclusion of ionic interactions in the proposed retention mechanism. The retention times of 80 solutes with various chemical structures were measured in the hydrophilic interaction liquid chromatography mode. The obtained results demonstrated the significant contribution of the polyaniline coating to the retention mechanism under the given conditions; the assumed mixed-mode retention was confirmed. The dominant retention interaction for both modified stationary phases was based on the protonation of nitrogen atoms in the polyaniline structure, leading to suitable retention and selectivity for the hydrophilic analytes, especially anionic and zwitterionic species. Thus, especially, the polyaniline-coated bare silica gel sorbent seems to be promising for potential applications related to the separation of polar compounds. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. A 2H nuclear magnetic resonance study of the state of water in neat silica and zwitterionic stationary phases and its influence on the chromatographic retention characteristics in hydrophilic interaction high-performance liquid chromatography.

    Science.gov (United States)

    Wikberg, Erika; Sparrman, Tobias; Viklund, Camilla; Jonsson, Tobias; Irgum, Knut

    2011-09-23

    2H NMR has been used as a tool for probing the state of water in hydrophilic stationary phases for liquid chromatography at temperatures between -80 and +4 °C. The fraction of water that remained unfrozen in four different neat silicas with nominal pore sizes between 60 and 300 Å, and in silicas with polymeric sulfobetaine zwitterionic functionalities prepared in different ways, could be determined by measurements of the line widths and temperature-corrected integrals of the 2H signals. The phase transitions detected during thawing made it possible to estimate the amount of non-freezable water in each phase. A distinct difference was seen between the neat and modified silicas tested. For the neat silicas, the relationship between the freezing point depression and their pore size followed the expected Gibbs-Thomson relationship. The polymeric stationary phases were found to contain considerably higher amounts of non-freezable water compared to the neat silica, which is attributed to the structural effect that the sulfobetaine polymers have on the water layer close to the stationary phase surface. The sulfobetaine stationary phases were used alongside the 100 Å silica to separate a number of polar compounds in hydrophilic interaction (HILIC) mode, and the retention characteristics could be explained in terms of the surface water structure, as well as by the porous properties of the stationary phases. This provides solid evidence supporting a partitioning mechanism, or at least of the existence of an immobilized layer of water into which partitioning could be occurring. Copyright © 2011 Elsevier B.V. All rights reserved.

  9. Preparation, characterization and application of a reversed phase liquid chromatography/hydrophilic interaction chromatography mixed-mode C18-DTT stationary phase.

    Science.gov (United States)

    Wang, Qing; Long, Yao; Yao, Lin; Xu, Li; Shi, Zhi-Guo; Xu, Lanying

    2016-01-01

    A mixed-mode chromatographic stationary phase, C18-DTT (dithiothreitol) silica (SiO2) was prepared through "thiol-ene" click chemistry. The obtained material was characterized by fourier transform infrared spectroscope, nitrogen adsorption analysis and contact angle analysis. Chromatographic performance of the C18-DTT was systemically evaluated by studying the effect of acetonitrile content, pH, buffer concentration of the mobile phase and column temperature. It was demonstrated that the novel stationary phase possessed reversed phase liquid chromatography (RPLC)/hydrophilic interaction liquid chromatography (HILIC) mixed-mode property. The stop-flow test revealed that C18-DTT exhibited excellent compatibility with 100% aqueous mobile phase. Additionally, the stability and column-to-column reproducibility of the C18-DTT material were satisfactory, with relative standard deviations of retention factor of the tested analytes (verapamil, fenbufen, guanine, tetrandrine and nicotinic acid) in the range of 1.82-3.72% and 0.85-1.93%, respectively. Finally, the application of C18-DTT column was demonstrated in the separation of non-steroidal anti-inflammatory drugs, aromatic carboxylic acids, alkaloids, nucleo-analytes and polycyclic aromatic hydrocarbons. It had great resolving power in the analysis of various compounds in HILIC and RPLC chromatographic conditions and was a promising RPLC/HILIC mixed-mode stationary phase. Copyright © 2015 Elsevier B.V. All rights reserved.

  10. High performance liquid chromatographic separation of eight drugs collected in Chinese Pharmacopoeia 2010 on amylose ramification chiral stationary phase

    Directory of Open Access Journals (Sweden)

    Yan Wang

    2012-10-01

    Full Text Available The enantiomers separation of eight pharmaceutical racemates collected in Chinese Pharmacopoeia 2010 (Ch.P2010, including nitrendipine, felodipine, omeprazole, praziquantel, sulpiride, clenbuterol hydrochloride, verapamil hydrochloride and chlorphenamine maleate, was performed on chiral stationary phase of amylose ramification by high performance liquid chromatography (HPLC on Chiralpak AD-H column and Chiralpak AS-H column with the mobile phase consisted of isopropanol and n-hexane. The detection wavelength and the flow rate were set at 254 nm and 0.7 mL/min, respectively. The effects of proportion of organic additives, alcohol displacer and temperature on the separation were investigated. The results indicated that eight chiral drugs were separated on chiral stationary phase of amylase ramification in normal phase chromatographic system. The chromatographic retention and resolution of enantiomers were adjusted by factors, including the changes of the concentration of alcohol displacer in mobile phase, organic alkaline modifier and column temperature. It was shown that the resolution was improved with reducing concentration of alcohol displacer. When the concentration of organic alkaline modifier was 0.2%, the resolution and the peak shape were fairly good. Most racemates mentioned above had the best resolution at column temperature of 25 °C. The best temperature should be kept unchanged in the process of separation so as to obtain stable separation results.

  11. A phase angle based diagnostic scheme to planetary gear faults diagnostics under non-stationary operational conditions

    Science.gov (United States)

    Feng, Ke; Wang, Kesheng; Ni, Qing; Zuo, Ming J.; Wei, Dongdong

    2017-11-01

    Planetary gearbox is a critical component for rotating machinery. It is widely used in wind turbines, aerospace and transmission systems in heavy industry. Thus, it is important to monitor planetary gearboxes, especially for fault diagnostics, during its operational conditions. However, in practice, operational conditions of planetary gearbox are often characterized by variations of rotational speeds and loads, which may bring difficulties for fault diagnosis through the measured vibrations. In this paper, phase angle data extracted from measured planetary gearbox vibrations is used for fault detection under non-stationary operational conditions. Together with sample entropy, fault diagnosis on planetary gearbox is implemented. The proposed scheme is explained and demonstrated in both simulation and experimental studies. The scheme proves to be effective and features advantages on fault diagnosis of planetary gearboxes under non-stationary operational conditions.

  12. Two dimensional reversed-phase-reversed-phase separations isomeric separations incorporating C18 and carbon clad zirconia stationary phases.

    Science.gov (United States)

    Gray, Michael; Dennis, Gary R; Wormell, Paul; Shalliker, R Andrew; Slonecker, Patrick

    2002-11-01

    Informational theory and a geometric approach to factor analysis were employed to evaluate the degree of orthogonality of a two-dimensional reversed-phase-reversed-phase chromatographic system. The system incorporated a C18 column as one dimension and a carbon clad zirconia column as the second dimension. In order to study the resolving power of this system, the separation of a sample matrix containing an artificial mix of 32 isomers (structural and diastereoisomers) was evaluated. Using this system, between 25 and 28 of the 32 isomers could be separated, depending on the mobile phase combinations--with resolution that could not possibly be achieved in a single one dimensional separation. The results from this study indicate that in order to fully evaluate the resolving power of a 2D system multiple methods of analysis are most appropriate. This becomes increasingly important when the sample contains components that are very closely related and the retention of solutes is clustered in one quadrant of the 2D space. Ultimately, the usefulness of the 2D separation is determined by the goals of analyst.

  13. Increased lignocellulosic inhibitor tolerance of Saccharomyces cerevisiae cell populations in early stationary phase.

    Science.gov (United States)

    Narayanan, Venkatachalam; Schelin, Jenny; Gorwa-Grauslund, Marie; van Niel, Ed Wj; Carlquist, Magnus

    2017-01-01

    Production of second-generation bioethanol and other bulk chemicals by yeast fermentation requires cells that tolerate inhibitory lignocellulosic compounds at low pH. Saccharomyces cerevisiae displays high plasticity with regard to inhibitor tolerance, and adaptation of cell populations to process conditions is essential for reaching efficient and robust fermentations. In this study, we assessed responses of isogenic yeast cell populations in different physiological states to combinations of acetic acid, vanillin and furfural at low pH. We found that cells in early stationary phase (ESP) exhibited significantly increased tolerance compared to cells in logarithmic phase, and had a similar ability to initiate growth in the presence of inhibitors as pre-adapted cells. The ESP cultures consisted of subpopulations with different buoyant cell densities which were isolated with flotation and analysed separately. These so-called quiescent (Q) and non-quiescent (NQ) cells were found to possess similar abilities to initiate growth in the presence of lignocellulosic inhibitors at pH 3.7, and had similar viabilities under static conditions. Therefore, differentiation into Q-cells was not the cause for increased tolerance of ESP cultures. Flow cytometry analysis of cell viability, intracellular pH and reactive oxygen species levels revealed that tolerant cell populations had a characteristic response upon inhibitor perturbations. Growth in the presence of a combination of inhibitors at low pH correlated with pre-cultures having a high frequency of cells with low pH i and low ROS levels. Furthermore, only a subpopulation of ESP cultures was able to tolerate lignocellulosic inhibitors at low pH, while pre-adapted cell populations displayed an almost uniform high tolerance to the adverse condition. This was in stark contrast to cell populations growing exponentially in non-inhibitory medium that were uniformly sensitive to the inhibitors at low pH. ESP cultures of S. cerevisiae

  14. [Preparation of 1 µm non-porous C18 silica gel stationary phase for chiral-pressurized capillary electrochromatography].

    Science.gov (United States)

    Lu, Yangfang; Wang, Hui; Wang, Guiming; Wang, Yan; Gu, Xue; Yan, Chao

    2015-03-01

    Non-porous C18 silica gel stationary phase (1 µm) was prepared and applied to chiral separation in pressurized capillary electrochromatography (pCEC) for the enantioseparation of various basic compounds. The non-porous silica particles (1 µm) were synthesized using modified St6ber method. C18 stationary phase (1 µm) was prepared by immobilization of chloro-dimethyl-octadecylsilane. Using carboxymethyl-β-cyclodextrin (CM-β-CD) as the chiral additive, the pCEC conditions including the content of acetonitrile (ACN), concentration of buffer, pH, the concentration of chiral additive and flow rate as well as applied voltage were investigated to obtain the optimal pCEC conditions for the separation of four basic chiral compounds. The column provided an efficiency of up to 190,000 plates/m. Bupropion hydrochloride, clenbuterol hydrochloride, metoprolol tartrate, and esmolol hydrochloride were baseline separated under the conditions of 5 mmol/L ammonium acetate buffer at pH 4. 0 with 20% (v/ v) acetonitrile, and 15 mmol/L CM-β-CD as the chiral additive. The applied voltage was 2 kV and flow rate was 0.03 mL/min with splitting ratio of 300:1. The resolution were 1.55, 2.82, 1. 69, 1. 70 for bupropion hydrochloride, clenbuterol hydrochloride, metoprolol tartrate, esmolol hydrochloride, respectively. The C18 coverage was improved by repeating silylation method. The synthesized 1 µm C18 packings have better mechanical strength and longer service life because of the special, non-porous structure. The column used in pCEC mode showed better separation of the racemates and a higher rate compared with those used in the capillary liquid chromatography (cLC) mode. This study provided an alternative way for the method of pCEC enantioseparation with chiral additives in the mobile phase and demonstrated the feasibility of micron particle stationary phase in chiral separation.

  15. Exploring the enantiorecognition mechanism of Cinchona alkaloid-based zwitterionic chiral stationary phases and the basic trans-paroxetine enantiomers.

    Science.gov (United States)

    Sardella, Roccaldo; Macchiarulo, Antonio; Urbinati, Fabrizio; Ianni, Federica; Carotti, Andrea; Kohout, Michal; Lindner, Wolfgang; Péter, Antal; Ilisz, István

    2017-11-21

    The enantiomers of trans-paroxetine (the selectand) were separated on four chiral stationary phases incorporating either quinine [ZWIX(+), ZWIX(+A)] or quinidine [ZWIX(-), ZWIX(-A)] and (R,R)-aminocyclohexanesulfonic acid [in ZWIX(-), and ZWIX(+A)] or (S,S)-aminocyclohexanesulfonic acid [in ZWIX(+), and ZWIX(-A)] chiral selectors. The zwitterion nature of the phases is due to the presence of either (R,R)- or (S,S)-aminocyclohexanesulfonic acid in the selector structure bearing the quinuclidine moiety. ZWIX(+) and ZWIX(-) phases are available on the market with the commercial names CHIRALPAK ZWIX(+) and CHIRALPAK ZWIX(-), respectively. With the aim of rationalizing the enantiomer elution order with the above chiral stationary phases, a molecular dynamic protocol was applied and two energetic parameters were initially measured: selectand conformational energy and selectand interaction energy. In the search for other descriptors allowing a better fitting with the experimental evidences, in the present work we consider an energetic parameter, defined as the selector conformational energy, which resulted to be relevant in the explanation of the experimental elution order in most of the cases. Very importantly, the computational data produced by the present study strongly support the outstanding role of the conformational energy of the chiral selector as it interacts with the analytes. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Preparation and characterization of mesoporous silicas modified with chiral selectors as stationary phase for high-performance liquid chromatography.

    Science.gov (United States)

    Pérez-Quintanilla, Damián; Morante-Zarcero, Sonia; Sierra, Isabel

    2014-01-15

    New hybrid materials were prepared as novel chiral stationary phases (CSPs) for high-performance liquid chromatography (HPLC). Pure mesoporous silica (SM) and ethylene-bridged periodic mesostructured organosilica (PMO) were functionalized, by a post-synthesis method, with derivates of erythromycin and vancomycin. N2 adsorption-desorption measurements, XRD, FT-IR, MAS NMR, SEM, TEM and elemental analysis were used to characterize the physico-chemical properties of these mesostructured materials, before and after the modification process. The synthesized particles had non-symmetrical 3-D wormhole-like mesostructure, spherical morphology, and a mean pore diameter between 53 and 59 Å. CSPs prepared were tested for the separation of four chiral β-blockers (atenolol, metoprolol, pindolol and propranolol) in normal phase (NP) and polar organic phase (PO) elution modes. Much stronger chiral interaction was observed in vancomycin-modified silicas. Results obtained in these preliminary studies will permit in future works to improve the synthesis route in order to design mesoporous materials with better performance as a chiral stationary phase for HPLC. Copyright © 2013 Elsevier Inc. All rights reserved.

  17. Two-surface Monte Carlo with basin hopping: quantum mechanical trajectory and multiple stationary points of water cluster.

    Science.gov (United States)

    Bandyopadhyay, Pradipta

    2008-04-07

    The efficiency of the two-surface monte carlo (TSMC) method depends on the closeness of the actual potential and the biasing potential used to propagate the system of interest. In this work, it is shown that by combining the basin hopping method with TSMC, the efficiency of the method can be increased by several folds. TSMC with basin hopping is used to generate quantum mechanical trajectory and large number of stationary points of water clusters.

  18. Existence of quasi-stationary neutron and x-ray states near the surface of a deformed single crystal

    CERN Document Server

    Iolin, E

    1999-01-01

    The problem of x-ray or neutron multiply internally reflected inside a bent single crystal plate (Bragg geometry) is considered. It is found that such multiple reflections lead to the existence of quasi-stationary (QS) states. QS states are discrete and correspond to the resonance of motion of the tie point between the front surface and a 'turning place' inside a single crystal. (author)

  19. Selective Essential Oils from Spice or Culinary Herbs Have High Activity against Stationary Phase and Biofilm Borrelia burgdorferi.

    Science.gov (United States)

    Feng, Jie; Zhang, Shuo; Shi, Wanliang; Zubcevik, Nevena; Miklossy, Judith; Zhang, Ying

    2017-01-01

    Although the majority of patients with acute Lyme disease can be cured with the standard 2-4 week antibiotic treatment, about 10-20% of patients continue suffering from chronic symptoms described as posttreatment Lyme disease syndrome. While the cause for this is debated, one possibility is that persister bacteria are not killed by the current Lyme antibiotics and remain active in the system. It has been reported that essential oils have antimicrobial activities and some have been used by patients with persisting Lyme disease symptoms. However, the activity of essential oils against the causative agent Borrelia burgdorferi ( B. burgdorferi ) has not been well studied. Here, we evaluated the activity of 34 essential oils against B. burgdorferi stationary phase culture as a model for persister bacteria. We found that not all essential oils had activity against the B. burgdorferi stationary phase culture, with top five essential oils (oregano, cinnamon bark, clove bud, citronella, and wintergreen) at a low concentration of 0.25% showing high anti-persister activity that is more active than the known persister drug daptomycin. Interestingly, some highly active essential oils were found to have excellent anti-biofilm ability as shown by their ability to dissolve the aggregated biofilm-like structures. The top three hits, oregano, cinnamon bark, and clove bud completely eradicated all viable cells without any regrowth in subculture in fresh medium, whereas but not citronella and wintergreen did not have this effect. Carvacrol was found to be the most active ingredient of oregano oil showing excellent activity against B. burgdorferi stationary phase cells, while other ingredients of oregano oil p-cymene and α-terpinene had no apparent activity. Future studies are needed to characterize and optimize the active essential oils in drug combination studies in vitro and in vivo and to address their safety and pharmacokinetic properties before they can be considered as a

  20. Selective Essential Oils from Spice or Culinary Herbs Have High Activity against Stationary Phase and Biofilm Borrelia burgdorferi

    Science.gov (United States)

    Feng, Jie; Zhang, Shuo; Shi, Wanliang; Zubcevik, Nevena; Miklossy, Judith; Zhang, Ying

    2017-01-01

    Although the majority of patients with acute Lyme disease can be cured with the standard 2–4 week antibiotic treatment, about 10–20% of patients continue suffering from chronic symptoms described as posttreatment Lyme disease syndrome. While the cause for this is debated, one possibility is that persister bacteria are not killed by the current Lyme antibiotics and remain active in the system. It has been reported that essential oils have antimicrobial activities and some have been used by patients with persisting Lyme disease symptoms. However, the activity of essential oils against the causative agent Borrelia burgdorferi (B. burgdorferi) has not been well studied. Here, we evaluated the activity of 34 essential oils against B. burgdorferi stationary phase culture as a model for persister bacteria. We found that not all essential oils had activity against the B. burgdorferi stationary phase culture, with top five essential oils (oregano, cinnamon bark, clove bud, citronella, and wintergreen) at a low concentration of 0.25% showing high anti-persister activity that is more active than the known persister drug daptomycin. Interestingly, some highly active essential oils were found to have excellent anti-biofilm ability as shown by their ability to dissolve the aggregated biofilm-like structures. The top three hits, oregano, cinnamon bark, and clove bud completely eradicated all viable cells without any regrowth in subculture in fresh medium, whereas but not citronella and wintergreen did not have this effect. Carvacrol was found to be the most active ingredient of oregano oil showing excellent activity against B. burgdorferi stationary phase cells, while other ingredients of oregano oil p-cymene and α-terpinene had no apparent activity. Future studies are needed to characterize and optimize the active essential oils in drug combination studies in vitro and in vivo and to address their safety and pharmacokinetic properties before they can be considered as a

  1. Ionic liquids as water-compatible GC stationary phases for the analysis of fragrances and essential oils.

    Science.gov (United States)

    Cagliero, Cecilia; Bicchi, Carlo; Cordero, Chiara; Liberto, Erica; Rubiolo, Patrizia; Sgorbini, Barbara

    2018-02-13

    Fragrances and products deriving from essential oils are often formulated or diluted in aqueous media, usually ethanol/water. Gas chromatography (GC) is the technique of choice to analyze volatiles. However, when using columns coated with conventional stationary phases, its application to aqueous samples often requires time-consuming and/or discriminative sample preparation techniques to extract the target analytes from the aqueous medium, so as to avoid its direct injection. In GC with conventional columns, water produces peak asymmetry, poor sensitivity and efficiency, strong adsorption, stationary phase degradation, and, last but not least, it is not easy to detect reliably when present in high amounts. In 2012, Armstrong's group introduced new fully water-compatible ionic-liquid (IL)-based GC capillary columns based on phosphonium and imidazolium derivative cations combined with trifluoromethanesulphonate. These columns were recently made available commercially by Supelco, under the trade name Watercol™. These derivatives maintain IL's unique selectivity and chromatographic properties, and enable water to be used as injection solvent, thus avoiding the sample preparation procedures required by conventional columns. This study reports and critically discusses the results of commercially available water-compatible IL columns for direct analysis of aqueous samples in the fragrance and essential oil fields by GC with thermal conductivity (TCD) and/or flame ionization detectors (FID). The results showed that water-compatible IL-based stationary phases can successfully be adopted for qualitative and quantitative analysis of fragrances and essential oils directly diluted in aqueous solvents. On the other hand, the study also shows that their inertness needs to be further increased and (possibly) the range of operative temperature extended when water is the main solvent of the sample.

  2. Selective Essential Oils from Spice or Culinary Herbs Have High Activity against Stationary Phase and Biofilm Borrelia burgdorferi

    Directory of Open Access Journals (Sweden)

    Jie Feng

    2017-10-01

    Full Text Available Although the majority of patients with acute Lyme disease can be cured with the standard 2–4 week antibiotic treatment, about 10–20% of patients continue suffering from chronic symptoms described as posttreatment Lyme disease syndrome. While the cause for this is debated, one possibility is that persister bacteria are not killed by the current Lyme antibiotics and remain active in the system. It has been reported that essential oils have antimicrobial activities and some have been used by patients with persisting Lyme disease symptoms. However, the activity of essential oils against the causative agent Borrelia burgdorferi (B. burgdorferi has not been well studied. Here, we evaluated the activity of 34 essential oils against B. burgdorferi stationary phase culture as a model for persister bacteria. We found that not all essential oils had activity against the B. burgdorferi stationary phase culture, with top five essential oils (oregano, cinnamon bark, clove bud, citronella, and wintergreen at a low concentration of 0.25% showing high anti-persister activity that is more active than the known persister drug daptomycin. Interestingly, some highly active essential oils were found to have excellent anti-biofilm ability as shown by their ability to dissolve the aggregated biofilm-like structures. The top three hits, oregano, cinnamon bark, and clove bud completely eradicated all viable cells without any regrowth in subculture in fresh medium, whereas but not citronella and wintergreen did not have this effect. Carvacrol was found to be the most active ingredient of oregano oil showing excellent activity against B. burgdorferi stationary phase cells, while other ingredients of oregano oil p-cymene and α-terpinene had no apparent activity. Future studies are needed to characterize and optimize the active essential oils in drug combination studies in vitro and in vivo and to address their safety and pharmacokinetic properties before they can be

  3. Modeling, analysis, and design of stationary reference frame droop controlled parallel three-phase voltage source inverters

    DEFF Research Database (Denmark)

    Vasquez, Juan Carlos; Guerrero, Josep M.; Savaghebi, Mehdi

    2011-01-01

    Power electronics based microgrids consist of a number of voltage source inverters (VSIs) operating in parallel. In this paper, the modeling, control design, and stability analysis of three-phase VSIs are derived. The proposed voltage and current inner control loops and the mathematical models...... of the VSIs were based on the stationary reference frame. A hierarchical control for the paralleled VSI system was developed based on three levels. The primary control includes the droop method and the virtual impedance loops, in order to share active and reactive power. The secondary control restores...

  4. Resolution and determination of enantiomeric purity of new chiral derivatives of xanthones using polysaccharide-based stationary phases.

    Science.gov (United States)

    Fernandes, Carla; Brandão, Pedro; Santos, Alexandre; Tiritan, Maria Elizabeth; Afonso, Carlos; Cass, Quezia B; Pinto, Madalena M

    2012-12-21

    The enantioresolution and determination of the enantiomeric purity of 24 new chiral derivatives of xanthones (CDXs) were investigated on polysaccharide-based chiral stationary phases (CSPs). The tris-3,5-dimethylphenylcarbamates of cellulose and amylose and tris-3,5-dimethoxyphenylcarbamate of amylose were selected as CSPs for this work. The separation of enantiomeric mixtures of CDXs was explored under multimodal elution conditions. All the enantiomeric mixtures of CDXs were enantioseparated with very high enantioselectivity and resolution with α and R(S) ranging from 1.43 to 12.41 and from 1.48 to 10.29, respectively. The best performances were achieved on amylose tris-3,5-dimethylphenylcarbamate stationary phase under polar organic elution conditions. Furthermore the enantiomeric purity for all the CDXs was measured, achieving values higher than 99%. Based on the obtained results, the influence of the mobile phases and structural features of the CSPs and CDXs on chiral discrimination are also discussed. Copyright © 2012 Elsevier B.V. All rights reserved.

  5. Effects of supercritical fluid chromatography conditions on enantioselectivity and performance of polyproline-derived chiral stationary phases.

    Science.gov (United States)

    Novell, Arnau; Méndez, Alberto; Minguillón, Cristina

    2015-07-17

    The chromatographic behaviour and performance of four polyproline-derived chiral stationary phases (CSPs) were tested using supercritical fluid chromatography (SFC). A series of structurally related racemic compounds, whose enantioseparation was proved to be sensitive to the type of mobile phase used in NP-HPLC, were chosen to be tested in the SFC conditions. Good enantioselection ability was shown by the CSPs for the analytes tested in the new conditions. Resolution, efficiency and analysis time, were considerably improved with respect to NP-HPLC when CO2/alcohol mobile phases were used. Monolithic columns clearly show enhanced chromatographic parameters and improved performance respect to their bead-based counterparts. Copyright © 2015 Elsevier B.V. All rights reserved.

  6. Determination of nitrosamines and caffeine metabolites in wastewaters using gas chromatography mass spectrometry and ionic liquid stationary phases.

    Science.gov (United States)

    Reyes-Contreras, Carolina; Domínguez, Carmen; Bayona, Josep M

    2012-10-26

    Recently, the interest to assess the environmental and human health effects of a wide group of emerging contaminants is growing worldwide. However, one of the main problems associated to their exposure is their determination in environmental matrices. It is hindered by the high polarity of most of these analytes, the poor selectivity obtained with low polarity stationary phases and the high background obtained with polar columns commonly used in GC-MS. Accordingly, this study examines the suitability of ionic liquid (IL) (e.g. SLB-IL59, SLB-IL61, SLB-IL82 and SLB-IL111) as stationary phases for GC-MS and their application to the determination of nitrosamines and caffeine metabolites in wastewater samples. Different chromatographic conditions were evaluated and results discussed in terms of resolution and peak symmetry. The SLB-IL111 column enabled the baseline separation and quantification of 7 nitrosamines in a shorter analysis time compared with cyanopropylphenyl polysiloxane commonly used. On the other hand, the SLB-IL59 column provided the best results for caffeine metabolites. Copyright © 2012 Elsevier B.V. All rights reserved.

  7. Quantitative analysis of molecular interaction potentials of ionic liquid anions using multi-functionalized stationary phases in HPLC.

    Science.gov (United States)

    Cho, Chul-Woong; Stolte, Stefan; Ranke, Johannes; Preiss, Ulrich; Krossing, Ingo; Thöming, Jorg

    2014-08-04

    The molecular interaction potentials, including S (dipolarity/polarizability), A (hydrogen bonding acidity), and B (hydrogen bonding basicity), of anions are experimentally determined using multi-functionalized stationary phases in high-performance liquid chromatography (HPLC) systems. We employ three different multi-functionalized stationary phase columns (Obelisc R, Obelisc N, and Acclaim Trinity-P1) combined with two ingredients, namely, acetonitrile (ACN) and methanol (MeOH). These conditions can cause neutral, cationic, and anionic compounds to be retained. By using the retention characteristics of calibration compounds, including cations, anions, and neutral compounds, system parameters including the ionic interaction terms (zc Zc , za Za ) are evaluated using multiple linear regression, resulting in a standard deviation (SD) of 0.090-0.158 log units. Based on the system parameters and retention characteristics of the anions of interest, their molecular interaction potentials are characterized on the same scale for neutral and cationic molecules. Furthermore, to verify the determined molecular interaction potentials, we predict anion hydrophobicity. The results show that the determined S, A, and B, together with the computable descriptors E (excess molar refraction) and V (McGowan volume), can predict anion hydrophobicity with R(2) =0.982 and SD=0.167 (dimensionless). © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Purification of Monoclonal Antibodies Using a Fiber Based Cation-Exchange Stationary Phase: Parameter Determination and Modeling

    Directory of Open Access Journals (Sweden)

    Jan Schwellenbach

    2016-10-01

    Full Text Available Monoclonal antibodies (mAb currently dominate the market for protein therapeutics. Because chromatography unit operations are critical for the purification of therapeutic proteins, the process integration of novel chromatographic stationary phases, driven by the demand for more economic process schemes, is a field of ongoing research. Within this study it was demonstrated that the description and prediction of mAb purification on a novel fiber based cation-exchange stationary phase can be achieved using a physico-chemical model. All relevant mass-transport phenomena during a bind and elute chromatographic cycle, namely convection, axial dispersion, boundary layer mass-transfer, and the salt dependent binding behavior in the fiber bed were described. This work highlights the combination of model adaption, simulation, and experimental parameter determination through separate measurements, correlations, or geometric considerations, independent from the chromatographic cycle. The salt dependent binding behavior of a purified mAb was determined by the measurement of adsorption isotherms using batch adsorption experiments. Utilizing a combination of size exclusion and protein A chromatography as analytic techniques, this approach can be extended to a cell culture broth, describing the salt dependent binding behavior of multiple components. Model testing and validation was performed with experimental bind and elute cycles using purified mAb as well as a clarified cell culture broth. A comparison between model calculations and experimental data showed a good agreement. The influence of the model parameters is discussed in detail.

  9. Quinine-Based Zwitterionic Chiral Stationary Phase as a Complementary Tool for Peptide Analysis: Mobile Phase Effects on Enantio- and Stereoselectivity of Underivatized Oligopeptides.

    Science.gov (United States)

    Ianni, Federica; Sardella, Roccaldo; Carotti, Andrea; Natalini, Benedetto; Lindner, Wolfgang; Lämmerhofer, Michael

    2016-01-01

    Peptide stereoisomer analysis is of importance for quality control of therapeutic peptides, the analysis of stereochemical integrity of bioactive peptides in food, and the elucidation of the stereochemistry of peptides from a natural chiral pool which often contains one or more D-amino acid residues. In this work, a series of model peptide stereoisomers (enantiomers and diastereomers) were analyzed on a zwitterionic ion-exchanger chiral stationary phase (Chiralpak ZWIX(+) 5 µm), in order to investigate the retention and separation performance for such compounds on this chiral stationary phase and elucidate its utility for this purpose. The goal of the study focused on 1) investigations of the effects of the sample matrix used to dissolve the peptide samples; 2) optimization of the mobile phase (enabling deriving information on factors of relevance for retention and separation); and 3) derivation of structure-selectivity relationships. It turned out that small di- and tripeptides can be well resolved under optimized conditions, typically with resolutions larger than 1.5. The optimized mobile phase often consisted of methanol-tetrahydrofuran-water (49:49:2; v/v/v) with 25 mM formic acid and 12.5 mM diethylamine. This work proposes some guidance on which mobile phases can be most efficiently used for peptide stereoisomer separations on Chiralpak ZWIX. Chirality 28:5-16, 2016. © 2015 Wiley Periodicals, Inc. © 2015 Wiley Periodicals, Inc.

  10. Effect of Secondary Equilibria on the Adsorption of Ibuprofen Enantiomers on a Chiral Stationary Phase with a Grafted Antibiotic Eremomycin

    Science.gov (United States)

    Reshetova, E. N.; Asnin, L. D.; Kachmarsky, K.

    2018-02-01

    The chromatographic separation of ibuprofen enantiomers on a Nautilus-E chiral stationary phase with a grafted eremomycin antibiotic at high column loading is accompanied by distortion of the shape of chromatographic peaks. A model is proposed to explain this phenomenon. A number of factors are considered in the model: the ionization of ibuprofen in the mobile phase, the pH change in the mass transfer zone caused by ionization, and competitive adsorption involving buffer components. Simulations performed using this model within the theory of nonequilibrium chromatography allow the shape of chromatograms for large amounts of S- and R-ibuprofen samples to be predicted. The adsorption mechanism is found to be mainly ion-exchange. The contribution from the molecular adsorption of ibuprofen to the total retention is shown to be several percent.

  11. Characterizing the selectivity of stationary phases and organic modifiers in reversed-phase high-performance liquid chromatographic systems by a general solvation equation using gradient elution.

    Science.gov (United States)

    Du, C M; Valko, K; Bevan, C; Reynolds, D; Abraham, M H

    2000-11-01

    Retention data for a set of 69 compounds using rapid gradient elution are obtained on a wide range of reversed-phase stationary phases and organic modifiers. The chromatographic stationary phases studied are Inertsil (IN)-ODS, pentafluorophenyl, fluoro-octyl, n-propylcyano, Polymer (PLRP-S 100), and hexylphenyl. The organic solvent modifiers are 2,2,2-trifluoroethanol (TFE); 1,1,1,3,3,3-hexafluoropropan-2-ol (HFIP); isopropanol; methanol (MeOH); acetonitrile (AcN); tetrahydrofuran; 1,4-dioxane; N,N-dimethylformamide; and mixed solvents of dimethylsulfoxide (DMSO) with AcN and DMSO with MeOH (1:1). A total of 25 chromatographic systems are analyzed using a solvation equation. In general, most of the systems give reasonable statistics. The selectivity of the reversed phase-high-performance liquid chromatographic (HPLC) systems with respect to the solute's dipolarity-polarity, hydrogen-bond acidity, and basicity are reflected in correspondingly large coefficients in the solvation equation. We wanted to find the most orthogonal HPLC systems, showing the highest possible selectivity difference in order to derive molecular descriptors using the gradient retention times of a compound. We selected eight chromatographic systems that have a large range of coefficients of interest (s, a, and b) similar to those found in water-solvent partitions used previously to derive molecular descriptors. The systems selected are IN-ODS phases with AcN, MeOH, TFE, and HFIP as mobile phase, PLRP-S 100 phase with AcN, propylcyano phase with AcN and MeOH, and fluorooctyl phase with TFE. Using the retention data obtained for a compound in the selected chromatographic systems, we can estimate the molecular descriptors with the faster and simpler gradient elution method.

  12. A Model for Solving the Maxwell Quasi Stationary Equations in a 3-Phase Electric Reduction Furnace

    Directory of Open Access Journals (Sweden)

    S. Ekrann

    1982-10-01

    Full Text Available A computer code has been developed for the approximate computation of electric and magnetic fields within an electric reduction furnace. The paper describes the numerical methods used to solve Maxwell's quasi-stationary equations, which are the governing equations for this problem. The equations are discretized by a staggered grid finite difference technique. The resulting algebraic equations are solved by iterating between computations of electric and magnetic quantities. This 'outer' iteration converges only when the skin depth is larger or of about the same magnitude as the linear dimensions of the computational domain. In solving for electric quantities with magnetic quantities being regarded as known, and vice versa, the central computational task is the solution of a Poisson equation for a scalar potential. These equations are solved by line successive overrelaxation combined with a rebalancing technique.

  13. The impact of non-stationary flows on the surface stress in the weak-wind stable boundary layer

    Science.gov (United States)

    Thomas, Christoph; Mahrt, Larry

    2016-04-01

    The behaviour of turbulent transport in the weak-wind stably stratified boundary layer is examined in terms of the non-stationarity of the wind field based upon field observations. Extensive sonic anemometer measurements from horizontal networks and vertical towers ranging from 12 to 20 m height and innovative fiber-optic distributed temperature sensing observations were collected from three field programs in moderately sloped terrain with a varying degree of surface heterogeneity, namely the Shallow Cold Pool (SCP) and the Flow Over Snow Surfaces (FLOSS) II experiments in Colorado (USA), and the Advanced Canopy Resolution Experiment (ARCFLO) in Oregon (USA). The relationship of the friction velocity to the stratification and small non-stationary submeso motions is studied from several points of view and nominally quantified. The relationship of the turbulence to the stratification is less systematic than expected due to the important submeso-scale motions. Consequently, the roles of the wind speed and stratification are not adequately accommodated by a single non-dimensional combination, such as the bulk Richardson number. However, cause and effect relationships are difficult to isolate because the non-stationary momentum flux significantly modifies the profile of the non-stationary mean flow. The link between the turbulence and accelerations at the surface is examined in terms of the changing vertical structure of the wind profile and sudden increases of downward transport of momentum. The latter may be significant in explaining the small-scale weak turbulence during stable stratification and deviations from conventional flux-profile relationships. Contrary to expectations, the vertical coherence was strongest for weakest winds and declined fast with increasing velocities, which suggests that submeso-scale motions are much deeper than previously thought.

  14. A weak cation-exchange monolith as stationary phase for the separation of peptide diastereomers by CEC.

    Science.gov (United States)

    Ludewig, Ronny; Nietzsche, Sandor; Scriba, Gerhard K E

    2011-01-01

    A CEC weak cation-exchange monolith has been prepared by in situ polymerization of acrylamide, methylenebisacrylamide and 4-acrylamidobutyric acid in a decanol-dimethylsulfoxide mixture as porogen. The columns were evaluated by SEM and characterized with regard to the separation of diastereomers and α/β-isomers of aspartyl peptides. Column preparation was reproducible as evidenced by comparison of the analyte retention times of several columns prepared simultaneously. Analyte separation was achieved using mobile phases consisting of acidic phosphate buffer and ACN. Under these conditions the peptides migrated due to their electrophoretic mobility but the EOF also contributed as driving force as a function of the pH of the mobile phase due to increasing dissociation of the carboxyl groups of the polymer. Raising the pH of the mobile phase also resulted in deprotonation of the peptides reducing analyte mobility. Due to these mechanisms each pair of diastereomeric peptides displayed the highest resolution at a different pH of the buffer component of the mobile phase. Comparing the weak-cation exchange monolith to an RP monolith and a strong cation-exchange monolith different elution order of some peptide diastereomers was observed, clearly illustrating that interactions with the stationary phase contribute to the CEC separations. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Direct enantioseparation of underivatized aliphatic 3-hydroxyalkanoic acids with a quinine-based zwitterionic chiral stationary phase.

    Science.gov (United States)

    Ianni, Federica; Pataj, Zoltán; Gross, Harald; Sardella, Roccaldo; Natalini, Benedetto; Lindner, Wolfgang; Lämmerhofer, Michael

    2014-10-10

    While aliphatic 2-hydroxyalkanoic acids have been more or less successfully enantioseparated with various chiral stationary phases by HPLC and GC, analogous applications on underivatized aliphatic 3-hydroxyalkanoic acids are completely absent in the scientific literature. With the aim of closing this gap, the enantioseparation of 3-hydroxybutyric acid, 3-hydroxydecanoic acid and 3-hydroxymyristic acid has been performed with two ion-exchange type chiral stationary phases (CSPs): one containing the anion-exchange type tert-butyl carbamoyl quinine chiral selector motif (Chiralpak QN-AX), and the other carrying the new zwitterionic variant based on trans-(S,S)-2-aminocyclohexanesulfonic acid-derivatized quinine carbamate (Chiralpak ZWIX(+)) as the chiral selector and enantiodiscriminating element, respectively. The zwitterionic enantiorecognition material provided better results in terms of enantioselectivity and resolution compared to the anion-exchanger CSP at reduced retention times due to the intramolecular counterion effect imposed by the sulfonic acid moiety and its competition with the 3-hydroxyalkanoic acid analyte for ionic interaction at the quininium-anion exchanger site. It is thus recommended as the CSP of first choice for enantioseparations of the class of aliphatic 3-hydroxyalkanoic acids. With use of polar organic eluent composed of ACN/MeOH/AcOH - 95/5/0.05 (v/v/v), a good compromise in terms of analysis time and enantioresolution quality was accomplished. The major experimental variables have been investigated for optimization of the resolution and allowed to derive information on the enantiorecognition mechanism. Corresponding Chiralpak ZWIX(-), based on pseudo-enantiomeric selector derived from quinidine and trans-(R,R)-2-aminocyclohexanesulfonic acid with opposite configurations provided reversed enantiomer elution orders. It has further to be stressed that these separations can be obtained with mass spectrometry compatible mobile phases

  16. Preparation, characterization and application of N-methylene phosphonic acid chitosan grafted magnesia–zirconia stationary phase

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Qing; Chen, Jie; Huang, Kun; Zhang, Xin; Xu, Li [Tongji School of Pharmacy, Huazhong University of Science and Technology, Wuhan 430030 (China); Shi, Zhi-guo, E-mail: shizg@whu.edu.cn [Department of Chemistry, Wuhan University, Wuhan 430072 (China)

    2015-01-07

    Highlights: • N-methylene phosphonic acid chitosan grafted MgO–ZrO{sub 2} was prepared. • It exhibited superior HILIC chromatographic performance to the bare MgO–ZrO{sub 2}. • Monosaccharides, phospholipids and peptides were successfully separated. • It was a promising HILIC stationary phase. - Abstract: A hydrophilic stationary phase (SP) was prepared through grafting N-methylene phosphonic acid chitosan on magnesia–zirconia particles (P-CTS-MgO–ZrO{sub 2}) via Lewis acid–base interaction. The resulting material was characterized by thermogravimetric analysis, Fourier transform infrared spectroscopy, scanning electron microscope and nitrogen adsorption analysis. The chromatographic performance of P-CTS-MgO–ZrO{sub 2} was systemically evaluated by studying effect of acetonitrile content, pH and buffer concentration in the mobile phase. The results demonstrated that the novel SP provided hydrophilic, electrostatic-repulsion and ion-exchange interactions. Compared to the bare MgO–ZrO{sub 2}, P-CTS-MgO–ZrO{sub 2} exhibited superior peak shape, reasonable resolution and reduced analysis time in separation of basic analytes. Besides, remarkable resolving power of acids, i.e. six non-steroidal anti-inflammatory drugs which failed to be eluted from the bare MgO–ZrO{sub 2}, was obtained with the theoretical plate number (N/m) of 4653–31313, asymmetry factor <1.21 and the resolution of 1.6–3.4. Finally, P-CTS-MgO–ZrO{sub 2} SP was applied to separate monosaccharides, phospholipids and peptides. P-CTS-MgO–ZrO{sub 2} was a promising hydrophilic SP for wide applications.

  17. Kinetic modeling of sporulation and product formation in stationary phase by Bacillus coagulans RK-02 vis-à-vis other Bacilli.

    Science.gov (United States)

    Das, Subhasish; Sen, Ramkrishna

    2011-10-01

    A logistic kinetic model was derived and validated to characterize the dynamics of a sporogenous bacterium in stationary phase with respect to sporulation and product formation. The kinetic constants as determined using this model are particularly important for describing intrinsic properties of a sporogenous bacterial culture in stationary phase. Non-linear curve fitting of the experimental data into the mathematical model showed very good correlation with the predicted values for sporulation and lipase production by Bacillus coagulans RK-02 culture in minimal media. Model fitting of literature data of sporulation and product (protease and amylase) formation in the stationary phase by some other Bacilli and comparison of the results of model fitting with those of Bacillus coagulans helped validate the significance and robustness of the developed kinetic model. Copyright © 2011 Elsevier Ltd. All rights reserved.

  18. Two-dimensional high-performance thin-layer chromatography of tryptic bovine albumin digest using normal- and reverse-phase systems with silanized silica stationary phase.

    Science.gov (United States)

    Gwarda, Radosław Łukasz; Dzido, Tadeusz Henryk

    2013-10-18

    Among many advantages of planar techniques, two-dimensional (2D) separation seems to be the most important for analysis of complex samples. Here we present quick, simple and efficient two-dimensional high-performance thin-layer chromatography (2D HPTLC) of bovine albumin digest using commercial HPTLC RP-18W plates (silica based stationary phase with chemically bonded octadecyl ligands of coverage density 0.5μmol/m(2) from Merck, Darmstadt). We show, that at low or high concentration of water in the mobile phase comprised methanol and some additives the chromatographic systems with the plates mentioned demonstrate normal- or reversed-phase liquid chromatography properties, respectively, for separation of peptides obtained. These two systems show quite different separation selectivity and their combination into 2D HPTLC process provides excellent separation of peptides of the bovine albumin digest. Copyright © 2013 Elsevier B.V. All rights reserved.

  19. Clean synthesis of molecular recognition polymeric materials with chiral sensing capability using supercritical fluid technology. Application as HPLC stationary phases.

    Science.gov (United States)

    da Silva, Mara Soares; Vão, Eva R; Temtem, Márcio; Mafra, Luís; Caldeira, Jorge; Aguiar-Ricardo, Ana; Casimiro, Teresa

    2010-03-15

    Molecularly imprinted polymers (MIPs) of poly(ethylene glycol dimethacrylate) and poly(N-isopropylacrylamide-co-ethylene glycol dimethacrylate) were synthesized for the first time in supercritical carbon dioxide (scCO(2)), using Boc-L-tryptophan as template. Supercritical fluid technology provides a clean and one-step synthetic route for the preparation of affinity polymeric materials with sensing capability for specific molecules. The polymeric materials were tested as stationary HPLC phases for the enantiomeric separation of L- and D-tryptophan. HPLC results prove that the synthesized MIPs are able to recognize the template molecule towards its enantiomer which opens up potential applications in chromatographic chiral separation. (c) 2009 Elsevier B.V. All rights reserved.

  20. A Nutrient-Regulated Cyclic Diguanylate Phosphodiesterase Controls Clostridium difficile Biofilm and Toxin Production during Stationary Phase.

    Science.gov (United States)

    Purcell, Erin B; McKee, Robert W; Courson, David S; Garrett, Elizabeth M; McBride, Shonna M; Cheney, Richard E; Tamayo, Rita

    2017-09-01

    The signaling molecule cyclic diguanylate (c-di-GMP) mediates physiological adaptation to extracellular stimuli in a wide range of bacteria. The complex metabolic pathways governing c-di-GMP synthesis and degradation are highly regulated, but the specific cues that impact c-di-GMP signaling are largely unknown. In the intestinal pathogen Clostridium difficile , c-di-GMP inhibits flagellar motility and toxin production and promotes pilus-dependent biofilm formation, but no specific biological functions have been ascribed to any of the individual c-di-GMP synthases or phosphodiesterases (PDEs). Here, we report the functional and biochemical characterization of a c-di-GMP PDE, PdcA, 1 of 37 confirmed or putative c-di-GMP metabolism proteins in C. difficile 630. Our studies reveal that pdcA transcription is controlled by the nutrient-regulated transcriptional regulator CodY and accordingly increases during stationary phase. In addition, PdcA PDE activity is allosterically regulated by GTP, further linking c-di-GMP levels to nutrient availability. Mutation of pdcA increased biofilm formation and reduced toxin biosynthesis without affecting swimming motility or global intracellular c-di-GMP. Analysis of the transcriptional response to pdcA mutation indicates that PdcA-dependent phenotypes manifest during stationary phase, consistent with regulation by CodY. These results demonstrate that inactivation of this single PDE gene is sufficient to impact multiple c-di-GMP-dependent phenotypes, including the production of major virulence factors, and suggest a link between c-di-GMP signaling and nutrient availability. Copyright © 2017 American Society for Microbiology.

  1. Membrane chromatography: protein purification from E. coli lysate using newly designed and commercial anion-exchange stationary phases.

    Science.gov (United States)

    Bhut, Bharat V; Christensen, Kenneth A; Husson, Scott M

    2010-07-23

    This contribution describes the purification of anthrax protective antigen (PA) protein from Escherichia coli lysate using bind-and-elute chromatography with newly designed weak anion-exchange membranes. Protein separation performance of the new AEX membrane adsorber was compared with the commercial Sartobind D membrane adsorber and HiTrap DEAE FF resin column under preparative scale conditions. Dynamic protein binding capacities of all three stationary phases were determined using breakthrough curve analysis. The AEX membrane showed higher binding capacities than the Sartobind D membrane at equivalent volumetric throughput and higher capacities than the HiTrap DEAE FF resin column at 15 times higher volumetric throughput. Anion-exchange chromatography was performed using all three stationary phases to purify PA protein. Quantitative SDS-PAGE analysis of effluent fractions showed that the purity of PA protein was higher for membrane adsorbers than the HiTrap DEAE FF resin column and was the same for the new AEX membrane and Sartobind D membrane adsorbers. The effects of E. coli lysate load volume and volumetric flow rate on PA protein separation resolution using the membrane adsorbers were minor, and the peak elution profile remained un-changed even under conditions where >75% of the total protein dynamic binding capacity of the membranes had been utilized. PA protein peak resolution was higher using pH-gradient elution than with ionic strength gradient elution. Overall, the results clearly demonstrate that membrane chromatography is a high-capacity, high-throughput, high-resolution separation technique, and that resolution in membrane chromatography can be higher than resin column chromatography under preparative conditions and at much higher volumetric throughput. Copyright (c) 2010 Elsevier B.V. All rights reserved.

  2. Proline accumulation protects Saccharomyces cerevisiae cells in stationary phase from ethanol stress by reducing reactive oxygen species levels.

    Science.gov (United States)

    Takagi, Hiroshi; Taguchi, Junpei; Kaino, Tomohiro

    2016-08-01

    During fermentation processes, Saccharomyces cerevisiae cells are exposed to multiple stresses, including a high concentration of ethanol that represents toxicity through intracellular reactive oxygen species (ROS) generation. We previously reported that proline protected yeast cells from damage caused by various stresses, such as freezing and ethanol. As an anti-oxidant, proline is suggested to scavenge intracellular ROS. In this study, we examined the role of intracellular proline during ethanol treatment in S. cerevisiae strains that accumulate different concentrations of proline. When cultured in YPD medium, there was a significant accumulation of proline in the put1 mutant strain, which is deficient in proline oxidase, in the stationary phase. Expression of the mutant PRO1 gene, which encodes the γ-glutamyl kinase variant (Asp154Asn or Ile150Thr) with desensitization to feedback inhibition by proline in the put1 mutant strain, showed a prominent increase in proline content as compared with that of the wild-type strain. The oxidation level was clearly increased in wild-type cells after exposure to ethanol, indicating that the generation of ROS occurred. Interestingly, proline accumulation significantly reduces the ROS level and increases the survival rate of yeast cells in the stationary phase under ethanol stress conditions. However, there was not a clear correlation between proline content and survival rate in yeast cells. An appropriate level of intracellular proline in yeast might be important for its stress-protective effect. Hence, the engineering of proline metabolism could be promising for breeding stress-tolerant industrial yeast strains. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  3. HIGH PERFORMANCE LIQUID CHROMATOGRAPHIC SEPARATION OF THE ENANTIOMERS OF ORGANOPHOSPHORUS PESTICIDES ON POLYSACCHARIDE CHIRAL STATIONARY PHASES

    Science.gov (United States)

    High-performance liquid chromatographic separation of the individual enantiomers of 12 organophosphorus pesticides (OPs) was obtained on polysaccharide enantioselective HPLC columns using alkane-alcohol mobile phase. The OP pesticides were crotoxyphos, dialifor, fonofos, fenamiph...

  4. HPLC SEPARATION OF CHIRAL ORGANOPHOSPHORUS PESTICIDES ON POLYSACCHARIDE CHIRAL STATIONARY PHASES

    Science.gov (United States)

    High-performance liquid chromatographic separation of the individual enantiomers of 12 organophosphorus pesticides (OPs) were obtained on polysaccharide chiral HPLC columns using an alkane-alcohol mobile phase. The OP pesticides were crotoxyphos, dialifor, dyfonate, fenamiphos, ...

  5. Lunar Surface Navigation, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — To support extended lunar operations, precision localization and route mapping is required for planetary EVA, manned rovers and lunar surface mobility units. A...

  6. Preparation of a silica stationary phase co-functionalized with Wulff-type phenylboronate and C12 for mixed-mode liquid chromatography.

    Science.gov (United States)

    Li, Hengye; Zhang, Xuemeng; Zhang, Lin; Wang, Xiaojin; Kong, Fenying; Fan, Dahe; Li, Lei; Wang, Wei

    2017-04-15

    A silica stationary phase was designed and synthesized through the co-functionalization of silica with Wulff-type phenylboronate and C12 for mixed-mode liquid chromatography applications. The as-synthesized stationary phase was characterized by elemental analysis and Fourier Transform-InfraRed Spectroscopy (FT-IR). Retention mechanisms, including boronate affinity (BA), reversed-phase (RP) and anion-exchange (AE), were involved. Retention mechanism switching was easily realized by adjustment of the mobile phase constitution. Cis-diol compounds could be selectively captured under neutral conditions in BA mode and off-line separated in RP mode. Neutral, basic, acidic and amphiprotic compounds were chromatographed on the column in RP chromatography, while inorganic anions were chromatographed in AE chromatography to characterize the mixed-mode nature of the prepared stationary phase. In addition, the RP performance was compared with an octadecyl silica column in terms of column efficiency (N/m), asymmetry factor (A f ), retention factor (k) and resolution (Rs). The prepared stationary phase offered multiple interactions with analytes in addition to hydrophobic interactions under RP elution conditions. Based on the mixed-mode properties, off-line 2D-LC, for selective capture and separation of urinary nucleosides, was successfully realized on a single column, demonstrating its powerful application potential for complex samples. Copyright © 2017 Elsevier B.V. All rights reserved.

  7. Development and Comparison of Air Pollution Exposure Surfaces Derived from On-Road Mobile Monitoring and Short-Term Stationary Sidewalk Measurements.

    Science.gov (United States)

    Minet, Laura; Liu, Rick; Valois, Marie-France; Xu, Junshi; Weichenthal, Scott; Hatzopoulou, Marianne

    2018-03-06

    Land-use regression (LUR) models of air pollutants are frequently developed on the basis of short-term stationary or mobile monitoring approaches, which raises the question of whether these two data collection protocols lead to similar exposure surfaces. In this study, we measured ultrafine particles (UFP) and black carbon (BC) concentrations in Toronto during summer 2016, using two short-term data collection approaches: mobile, involving 3023 road segments sampled on bicycles, and stationary, involving 92 sidewalk locations. We developed four LUR models and exposure surfaces, for the two pollutants and measurement protocols. Coefficients of determination ( R 2 ) varied from 0.434 to 0.525. Various small-scale traffic variables were included in the mobile LUR. Pearson correlation coefficients between the mobile and stationary surfaces were 0.23 for UFP and 0.49 for BC. We also compared the two surfaces using personal exposures from a panel study in Toronto conducted during the same period. The personal exposures differed from the outdoor exposures derived from the combination of GPS information and exposure surfaces. For UFP, the median for personal outdoor exposure was 26 344 part/cm 3 , while the cycling and stationary surfaces predicted medians of 31 201 and 19 057 part/cm 3 . Similar trends were observed for BC, with median exposures of 1764 (personal), 1799 (cycling), and 1469 ng/m 3 (stationary).

  8. Antimicrobial efficacy of chlorine dioxide against Candida albicans in stationary and starvation phases in human root canal: An in-vitro study

    Directory of Open Access Journals (Sweden)

    Shirur Krishnaraj Somayaji

    2014-01-01

    Full Text Available Introduction: Candida albicans (C. albicans is the most commonly isolated fungal pathogen from dental root canal. C. albicans forms biofilm and develops resistance against root canal irrigants . This study determines the fungicidal efficacy of 13.8% chlorine dioxide in extracted human teeth at stationary and starvation phases of C. albicans. Materials and Methods: Teeth were decoronated and coronal portion of the roots were prepared into blocks, which were incubated at 37°C with C. albicans for five days. The samples were treated with chlorine dioxide for 12 and 20 minutes. Total of fifty blocks were taken in the study. Colony-forming units were counted in Sabourauds dextrose agar and scanning electron microscopic observation was done. Data were analyzed by one-way ANOVA and Bonferoni′s post hoc test. Results: Teeth at stationary phase (12 min showed mean colony count of 28,000 ± 1814 which is significantly (P < 0.001 less than control group. Teeth at starvation phase (12 min showed colony count of 65,600 ± 1912 which is also significantly (P < 0.001 less than control group. Teeth irrigated at stationary phase (20 min showed mean colony count of 23,400 ± 1776 (P < 0.001. Teeth irrigated at starvation phase (20 min showed mean colony count of 48,100 ± 1663 which is also significantly (P < 0.001 less than that of control group. Conclusion: Treatment of chlorine dioxide reduces the C. albicans count in root canals of extracted human teeth at stationary and starvation phases. Efficacy of chlorine dioxide against C. albicans is relatively higher in stationary phase than that of starvation phase.

  9. Growth potential of exponential- and stationary-phase Salmonella Typhimurium during sausage fermentation

    DEFF Research Database (Denmark)

    Birk, Tina; Henriksen, Sidsel; Müller, K.

    2016-01-01

    Raw meat for sausage production can be contaminated with Salmonella. For technical reasons, meat is often frozen prior to mincing but it is unknown how growth of Salmonella in meat prior to freezing affects its growth potential during sausage fermentation. We investigated survival of exponential-...... fermentation, sporadic growth of exponential-phase cells of S. Typhimurium was observed drawing attention to the handling and storage of sausage meat.......Raw meat for sausage production can be contaminated with Salmonella. For technical reasons, meat is often frozen prior to mincing but it is unknown how growth of Salmonella in meat prior to freezing affects its growth potential during sausage fermentation. We investigated survival of exponential...... starter culture. With no starter culture, both strains grew in both growth phases. In general, a functional starter culture abolished S. Typhimurium growth independent of growth phase and we concluded that ensuring correct fermentation is important for sausage safety. However, despite efficient...

  10. Laboratory-Scale Preparative Enantioseparations of Pharmaceutically Relevant Compounds on Commercially Available Chiral Stationary Phases for HPLC.

    Science.gov (United States)

    Sardella, Roccaldo; Ianni, Federica; Marinozzi, Maura; Macchiarulo, Antonio; Natalini, Benedetto

    2017-01-01

    In response to the outburst of research in the field of synthetic medicinal chemistry, enantioselective chromatography methods based on the use of chiral stationary phases (CSPs) found immediate acceptance as the elective choice for the analytical determinations of the enantiomeric purity of synthetic compounds. In contrast to an initial scepticism, also the preparative-scale applications are gaining increasing recognition as a powerful alternative to enantioselective synthesis for the supply of pure enantiomers of bioactive compounds. The increasing success of liquid chromatography methods has been made possible thanks to the development of highly efficient CSPs allowing the enantioresolution of practically all the chemical classes of chiral compounds. However, only few CSPs are really suitable for preparative- scale applications, being the loading capacity is the major concern for preparativescale enantioseparations. The cellulose- and amylose-based CSPs present the highest loading capacity and enantiodiscrimination power, which makes these CSPs the most versatile and applicable for preparative-scale applications in all the applicable elution modes (reversedphase, normal-phase, and with polar-organic or polar-ionic eluents). However, also other types of CSPs have been successfully employed at this regard (brush-type phases, polyacrylamide and cross-linked di-allyltartardiamide phases as well as cyclodextrin, and glycopeptide containing phases). Several instrumental methods exist for the determination of the absolute configuration of organic compounds in absence of known enantiopure reference standards. The most widely known are X-ray crystallography, followed by chirooptical methods [e.g., electronic and vibrational circular dichroism (ECD and VCD, respectively)] and nuclear magnetic resonance (NMR) spectroscopy. All these aspects will be treated in the review. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

  11. The chiral separation of triazole pesticides enantiomers by amylose-tris (3,5-dimethylphenylcarbamate) chiral stationary phase.

    Science.gov (United States)

    Wang, Peng; Liu, Donghui; Jiang, Shuren; Xu, Yangguang; Zhou, Zhiqiang

    2008-10-01

    The amylose-tris(3,5-dimethylphenylcarbamate) chiral stationary phase was synthesized and used to separate the enantiomers of triazole pesticides by high-performance liquid chromatography. The mobile phase was n-hexane-isopropanol applying a flow rate of 1.0 mL/min. Six triazole pesticides were enantioselectively separated. Myclobutanil, paclobutrazol, tebuconazole, and uniconazole obtained complete separation with the resolution factors of 5.73, 2.99, 1.72, and 2.07, respectively, and imazalil and diniconazole obtained partial separation with the resolution factors of 0.79 and 0.77 under the optimized conditions. The effect of the content of isopropanol as well as column temperature on the separation was investigated. A circular dichroism detector was used to identify the enantiomers and determine the elution orders. The results showed the low temperature was good for the chiral separation except for diniconazole. The thermodynamic parameters calculated based on linear Van't Hoff plots showed the chiral separations were controlled by enthalpy.

  12. Separation of adrenergic amines in Citrus aurantium L. var. amara by capillary electrochromatography using a novel monolithic stationary phase.

    Science.gov (United States)

    Chizzali, Evelyn; Nischang, Ivo; Ganzera, Markus

    2011-08-01

    This manuscript reports on the use of capillary electrochromatography for the determination of tyramine, (±) synephrine, and (±) octopamine, the major alkaloids in bitter orange peel. A novel methacrylate-based monolithic stationary phase was prepared by UV-photopolymerization in 100 μm id fused-silica capillaries. It facilitated the quantitative assessment of alkaloids with a mobile phase comprising aqueous 10 mM ammonium acetate in ACN and isopropanol. Applied voltage and temperature were 25 kV and 25°C, and samples were injected in electrokinetic mode. The method reported herein revealed adequate sensitivity (LOD ≤0.6 μg/mL), repeatability (σrel ≤4.1%), accuracy (recovery rates between 95.2 and 102.2%), and precision (intra-day variation ≤5.7%, inter-day variation ≤4.1%). The application of the CEC assay on C. aurantium var. amara plant material and dietary supplements, which usually are advertised for slimming properties, indicated that synephrine (0.17-0.82%) is the dominant alkaloid. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Ion chromatography of transition metals: specific alteration of retention by complexation reactions in the mobile and on the stationary phase

    International Nuclear Information System (INIS)

    Baumgartner, S.

    1992-05-01

    Ion chromatography of mono- and bivalent cations was performed on a conventional cation exchanger. The pH influence of an ethylene-diamine/citrate eluent was significant for the retention of alkaline earth and transition metals, but negligible for alkali ions. This was dealt with from a mechanistic point of view. Mobile phase optimization allowed fast isocratic analysis of mono- and bivalent cations and the separation of the radionuclides Cs-137 and Sr-90. A newly synthesized stationary phase containing iminodiacetate (IDA) function was investigated for cation chromatography using ethylenediamine/citrate eluents, polyhydroxy acid and dipicolinic acid. The column's high selectivity for transition metal ions in comparison to alkali and alkaline earth metals may be governed by the choice of complexing ability and pH of the eluent. Applications verified by atomic absorption spectroscopy include alkaline earth metals in beverages and the determination of Co, Cd and Zn in solutions containing more than 10 14 -fold excess of Na and Mg, such as sea water

  14. Use of serially coupled capillary columns with different polarity of stationary phases for the separation of the natural complex volatile mixture of the marine red alga Corallina elongata.

    Science.gov (United States)

    Dembitsky, V M; Srebnik, M

    2002-09-01

    Separation of a complex of natural volatile compounds using serially coupled capillary columns with different polarity of stationary phases by gas chromatography-mass spectrometry from the medicinal marine red alga Corallina elongata is reported. Nearly 200 hydrocarbons, halogen compounds, fatty acids, and other metabolites were found. Using this gas chromatography procedure we demonstrate the successful separation of different volatile organic compounds.

  15. Increments to chiral recognition facilitating enantiomer separations of chiral acids, bases, and ampholytes using Cinchona-based zwitterion exchanger chiral stationary phases.

    Science.gov (United States)

    Wernisch, Stefanie; Pell, Reinhard; Lindner, Wolfgang

    2012-07-01

    The intramolecular distances of anion and cation exchanger sites of zwitterionic chiral stationary phases represent potential tuning sites for enantiomer selectivity. In this contribution, we investigate the influence of alkanesulfonic acid chain length and flexibility on enantiomer separations of chiral acids, bases, and amphoteric molecules for six Cinchona alkaloid-based chiral stationary phases in comparison with structurally related anion and cation exchangers. Employing polar-organic elution conditions, we observed an intramolecular counterion effect for acidic analytes which led to reduced retention times but did not impair enantiomer selectivities. Retention of amphoteric analytes is based on simultaneous double ion pairing of their charged functional groups with the acidic and basic sites of the zwitterionic selectors. A chiral center in the vicinity of the strong cation exchanger site is vital for chiral separations of bases. Sterically demanding side chains are beneficial for separations of free amino acids. Enantioseparations of free (un-derivatized) peptides were particularly successful in stationary phases with straight-chain alkanesulfonic acid sites, pointing to a beneficial influence of more flexible moieties. In addition, we observed pseudo-enantiomeric behavior of quinine and quinidine-derived chiral stationary phases facilitating reversal of elution orders for all analytes. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. An inverse voter model for co-evolutionary networks: Stationary efficiency and phase transitions

    International Nuclear Information System (INIS)

    Zhu Chenping; Kong Hui; Li Li; Gu Zhiming; Xiong Shijie

    2011-01-01

    In some co-evolutionary networks, the nodes always flip their states between two opposite ones, changing the types of the links to others correspondingly. Meanwhile, the link-rewiring and state-flipping processes feed back each other, and only the links between the nodes in the opposite states are productive in generating flow for the network. We propose an inverse voter model to depict the basic features of them. New phase transitions from full efficiency to deficiency state are found by both the analysis and simulations starting from the random graphs and small-world networks. We suggest a new way to measure the efficiency of networks.

  17. Non-stationary filtration mode during chemical reactions with the gas phase

    Science.gov (United States)

    Zavialov, Ivan; Konyukhov, Andrey; Negodyaev, Sergey

    2015-04-01

    An experimental and numerical study of filtration accompanied by chemical reactions between displacing fluid and solid skeleton is considered. Glass balls (400-500 μm in diameter) were placed in 1 cm gap between two glass sheets and were used as model porous medium. The baking soda was added to the glass balls. The 70% solution of acetic acid was used as the displacer. The modeling porous medium was saturated with a mineral oil, and then 70% solution of colored acetic acid was pumped through the medium. The glass balls and a mineral oil have a similar refractive index, so the model porous medium was optically transparent. During the filtration, the gas phase was generated by the chemical reactions between the baking soda and acetic acid, and time-dependent displacement of the chemical reaction front was observed. The front of the chemical reaction was associated with the most intensive gas separation. The front moved, stopped, and then moved again to the area where it had been already. We called this process a secondary oxidation wave. To describe this effect, we added to the balance equations a term associated with the formation and disappearance of phases due to chemical reactions. The equations were supplemented by Darcy's law for multiphase filtration. Nonstationarity front propagation of the chemical reaction in the numerical experiment was observed at Damköhler numbers greater than 100. The mathematical modelling was agreed well with the experimental results.

  18. Inhomogeneous Stripe Phase Revisited for Surface Superconductivity

    Science.gov (United States)

    Barzykin, Victor; Gor'kov, Lev P.

    2002-11-01

    We consider 2D surface superconductivity in high magnetic fields parallel to the surface. We demonstrate that the spin-orbit interaction at the surface changes the properties of the inhomogeneous superconducting Larkin-Ovchinnikov-Fulde-Ferrell (LOFF) state that develops above fields given by the paramagnetic criterion. Strong spin-orbit interaction significantly broadens the range of existence of the LOFF phase, which takes the form of periodic superconducting stripes running along the field direction on the surface, leading to the anisotropy of its properties. Our results provide a tool for studying surface superconductivity as a function of doping.

  19. Sinorhizobium meliloti sigma factors RpoE1 and RpoE4 are activated in stationary phase in response to sulfite.

    Directory of Open Access Journals (Sweden)

    Bénédicte Bastiat

    Full Text Available Rhizobia are soil bacteria able to establish a nitrogen-fixing symbiosis with legume plants. Both in soil and in planta, rhizobia spend non-growing periods resembling the stationary phase of in vitro-cultured bacteria. The primary objective of this work was to better characterize gene regulation in this biologically relevant growth stage in Sinorhizobium meliloti. By a tap-tag/mass spectrometry approach, we identified five sigma factors co-purifying with the RNA polymerase in stationary phase: the general stress response regulator RpoE2, the heat shock sigma factor RpoH2, and three extra-cytoplasmic function sigma factors (RpoE1, RpoE3 and RpoE4 belonging to the poorly characterized ECF26 subgroup. We then showed that RpoE1 and RpoE4 i are activated upon metabolism of sulfite-generating compounds (thiosulfate and taurine, ii display overlapping regulatory activities, iii govern a dedicated sulfite response by controlling expression of the sulfite dehydrogenase SorT, iv are activated in stationary phase, likely as a result of endogenous sulfite generation during bacterial growth. We showed that SorT is required for optimal growth of S. meliloti in the presence of sulfite, suggesting that the response governed by RpoE1 and RpoE4 may be advantageous for bacteria in stationary phase either by providing a sulfite detoxification function or by contributing to energy production through sulfite respiration. This paper therefore reports the first characterization of ECF26 sigma factors, the first description of sigma factors involved in control of sulphur metabolism, and the first indication that endogenous sulfite may act as a signal for regulation of gene expression upon entry of bacteria in stationary phase.

  20. Nano-electrospray tandem mass spectrometric analysis of the acetylation state of histones H3 and H4 in stationary phase in Saccharomyces cerevisiae

    Directory of Open Access Journals (Sweden)

    Patterton Hugh G

    2011-07-01

    Full Text Available Abstract Background The involvement of histone acetylation in facilitating gene expression is well-established, particularly in the case of histones H3 and H4. It was previously shown in Saccharomyces cerevisiae that gene expression was significantly down-regulated and chromatin more condensed in stationary phase compared to exponential phase. We were therefore interested in establishing the acetylation state of histone H3 and H4 in stationary and in exponential phase, since the regulation of this modification could contribute to transcriptional shut-down and chromatin compaction during semi-quiescence. Results We made use of nano-spray tandem mass spectrometry to perform a precursor ion scan to detect an m/z 126 immonium ion, diagnostic of an Nε-acetylated lysine residue that allowed unambiguous identification of acetylated as opposed to tri-methylated lysine. The fragmentation spectra of peptides thus identified were searched with Mascot against the Swiss-Prot database, and the y-ion and b-ion fragmentation series subsequently analyzed for mass shifts compatible with acetylated lysine residues. We found that K9, K14 and K36 of histone H3 and K12 and K16 of histone H4 were acetylated in exponential phase (bulk histones, but could not detect these modifications in histones isolated from stationary phase cells at the sensitivity level of the mass spectrometer. The corresponding un-acetylated peptides were, however, observed. A significantly higher level of acetylation of these residues in exponential phase was confirmed by immuno-blotting. Conclusion H4K16 acetylation was previously shown to disrupt formation of condensed chromatin in vitro. We propose that de-acetylation of H4K16 allowed formation of condensed chromatin in stationary phase, and that acetylation of H3K9, H3K14, H3K36, and H4K12 reflected the active transcriptional state of the yeast genome in exponential phase.

  1. Synthesis and characterization of nanometric zinc oxide for a stationary phase in liquid chromatography

    Science.gov (United States)

    Gordillo-Delgado, F.; Soto-Barrera, C. C.; Plazas-Saldaña, J.

    2017-01-01

    The increasing demand for equipment to remove organic compounds in industry and research activity has led to evaluate nanometric zinc oxide (ZnO). In this work, we present the ZnO nanoparticles synthesis for reusing of discarded columns, as a low-cost alternative. The compound was obtained by sol-gel technique using zinc chloride and sodium hydroxide as precursors and a drying temperature of 169°C. An X-ray diffractometer was used to estimate the average particle size at 20.3±0.2nm the adsorption capacity was 0.0144L/g and the chemical resistance was tested with HCl and NaOH. The ZnO nanopowder was packed with 100psi pressure in an empty C-18 column cavity. The column packing resolution was evaluated using a high performance liquid chromatographer (HPLC-Thermo Scientific Dionex UltiMate 3000); using a caffeine standard, the following parameters were established: solvent flow: 1.2mL/min, average column temperature: 40°C, running time: 10 minutes, mobile phase acetonitrile-water composition (9:1). These results validate the potential of ZnO nanopowder as a column packing material in HPLC technique.

  2. Electrochromatographic performance of conventional and polar-embedded C16 silica monolithic stationary phases.

    Science.gov (United States)

    Ye, Fanggui; Huang, Baojun; Wang, Shun; Zhao, Shulin

    2010-11-01

    A novel monolithic silica column that has a polar-embedded amide-secondary amine group linking with C16 functionality for RP-CEC is described. The amide-secondary aminealkyloxysilane was synthesized by the reaction of 3-(2-aminoethylamino) propyltrimethoxysilane with hexadecanoyl chloride. Then, the silylant agent was bonded to the silica monolith matrix to produce hexadecanamide-secondary amine bonded silica (HDAIS) monolithic column. The electrochromatographic performance of HDAIS monolithic column for the separation of neutral, basic and polar solutes was studied, which was compared to that using the hexadecyl bonded silica monolithic column. The HDAIS monolithic column displayed reduced hydrophobic retention characteristics in the separation of five hydrophobic n-alkylbenzenes and four polar phenols when compared to the hexadecyl bonded silica monolithic column. A very much reduced silanol activity of HDAIS monolithic column was observed in the separation of test basic mixture including four aromatic amines, atenolol and metoprolol with 10 mM borate buffer (pH 7.5) containing 30% v/v ACN as the mobile phase. The comparison results indicate good performance for both polar and basic mixtures on HDAIS monolithic column in RP-CEC, and also show promising results for further applications.

  3. Preparation and evaluation of bonded linear polymethacrylate stationary phases for open tubular capillary electrokinetic chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Tan, Z.J.; Remcho, V.T. [West Virginia Univ., Morgantown, WV (United States)

    1997-02-15

    A new procedure for the preparation of thick polymethacrylate films bonded in 25 {mu}m i.d. fused-silica capillaries is developed. The etched silica surface is first modified with an unsaturated organosilane, which is later incorporated into the polymer film. The capillary is then filled with a monomer solution, and polymerization is initiated by incubation at elevated temperature. This thermoinitiation method enables the use of ordinary polyimide-jacketed capillaries in preparing the columns. The effect of monomer concentration on the resulting polymer film was studied by open tubular capillary electrokinetic chromatography using p-hydroxybenzoates (parabens) as test solutes. Good separations were achieved using short capillaries. Run-to-run retention time reproducibility was excellent, with RSDs of 2% (n = 50) being representative. For the linear polymer films produced, retention of analytes increased as the monomer concentration increased to a certain value, at which point the capacity factors level off with further increases in monomer concentration. The electroosmotic flow velocity decreases with increasing monomer concentration. The efficiency for an unretained test probe (acetone) reaches 270 000 plates/m. 13 refs., 10 figs., 1 tab.

  4. A reversed-phase/hydrophilic interaction mixed-mode C18-Diol stationary phase for multiple applications.

    Science.gov (United States)

    Wang, Qing; Ye, Mao; Xu, Li; Shi, Zhi-guo

    2015-08-12

    A mixed-mode chromatographic packing material, C18 and diol groups modified silica (C18-Diol), was prepared with controllable hydrophobicity and hydrophilicity. It demonstrated excellent aqueous compatibility and stability in aqueous mobile phase; compared to the traditional C18 column, improved peak shape of basic analytes was also obtained. Additionally, it exhibited both reversed-phase liquid chromatographic (RPLC) and hydrophilic interaction chromatographic (HILIC) performance; the analyte separation scope was thus enlarged, demonstrated by simultaneous separation of twenty acids, bases and neutrals. More interestingly, a novel on-line two-dimensional liquid chromatography on the single column (2D-LC-1C) was established by modifying the high performance liquid chromatographic instrument only with the addition of an extra six-port two-position valve. The early co-eluted components of the extract of Lonicera japonica on the 1st-dimension (RPLC) were collected for the online re-injection to the 2nd-dimension (HILIC) by conveniently varying the mobile phase components. Six more peaks were obtained. The established system was simple, easy operation and low cost, which had advantages in analyzing complicated samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  5. Enantiomeric Separation of 1-(Benzofuran-2-yl)alkylamines on Chiral Stationary Phases Based on Chiral Crown Ethers

    Energy Technology Data Exchange (ETDEWEB)

    Park, Soohyun; Kim, Sang Jun; Hyun, Myung Ho [Pusan National Univ., Busan (Korea, Republic of)

    2012-10-15

    Optically active chiral amines are important as building blocks for pharmaceuticals and as scaffolds for chiral ligands and, consequently, many efforts have been devoted to the development of efficient methods for their preparation. For example, reduction of amine precursors with chiral catalysts, enzymatic kinetic resolution or dynamic kinetic resolution of racemic amines and the direct amination of ketones with transaminases have been developed as the efficient methods for the preparation of optically active chiral amines. During the process of developing or utilizing optically active chiral amines, the methods for the determination of their enantiomeric composition are essential. Among various methods, liquid chromatographic resolution of enantiomers on chiral stationary phases (CSPs) have been known to be one of the most accurate and economic means for the determination of the enantiomeric composition of optically active chiral compounds. Especially, CSPs based on chiral crown ethers have been successfully used for the resolution of racemic primary amines. For example, CSPs based on (+)-(18-crown-6)-2,3,11,12-tetracarboxylic acid (CSP 1, Figure 1) or (3,3'-diphenyl-1,1'-binaphthyl)-20-crown-6 (CSP 2 and CSP 3, Figure 1) have been known to be quite effective for the resolution of cyclic and non-cyclic amines, various fluoroquinolone antibacterials containing a primary amino group, tocainide (antiarrhythmic agent) and its analogues, aryl-a-amino ketones and 3-amino-1,4-benzodiazepin-2-ones.

  6. Preparation and characterization of tentacle-type polymer stationary phase modified with graphene oxide for open-tubular capillary electrochromatography.

    Science.gov (United States)

    Gao, Xing; Mo, Rongzhen; Ji, Yibing

    2015-06-26

    In this research, a novel organic polymer coated stationary phase modified with inorganic nanomaterial was prepared for open-tubular capillary electrochromatography (OT-CEC). The capillary was developed by covalent attaching graphene oxide (GO) onto the tentacle-type polymer chains grafted capillary which was derivatized with ammonium hydroxide. Scanning electron microscopy (SEM) and Raman spectroscopy provided evidences that the tentacle-type polymer and GO were coated to the capillary inner wall. This novel GO-polymer modified capillary column generated a strong and stable electroosmotic flow (EOF) from anode to cathode with the running electrolytes of pH ranging from 4.0 to 9.0, and showed excellent separation ability toward neutral small molecules, amino acids and ephedrine-pseudoephedrine isomers with resolution higher than 2.30 and column efficiency up to over 170,000 plates/m. The repeatabilities of the GO-GMA@capillary were satisfying with relative standard deviations for intra-day and inter-day runs less than 3.27%, and column-to-column runs less than 7.49%. Additionally, the separation performance of GO-polymer modified capillary was compared with that of the polymer coated capillary and GO coated capillary. Copyright © 2015 Elsevier B.V. All rights reserved.

  7. Synergistic effects on enantioselectivity of zwitterionic chiral stationary phases for separations of chiral acids, bases, and amino acids by HPLC.

    Science.gov (United States)

    Hoffmann, Christian V; Pell, Reinhard; Lämmerhofer, Michael; Lindner, Wolfgang

    2008-11-15

    In an attempt to overcome the limited applicability scope of earlier proposed Cinchona alkaloid-based chiral weak anion exchangers (WAX) and recently reported aminosulfonic acid-based chiral strong cation exchangers (SCX), which are conceptionally restricted to oppositely charged solutes, their individual chiral selector (SO) subunits have been fused in a combinatorial synthesis approach into single, now zwitterionic, chiral SO motifs. The corresponding zwitterionic ion-exchange-type chiral stationary phases (CSPs) in fact combined the applicability spectra of the parent chiral ion exchangers allowing for enantioseparations of chiral acids and amine-type solutes in liquid chromatography using polar organic mode with largely rivaling separation factors as compared to the parent WAX and SCX CSPs. Furthermore, the application spectrum could be remarkably expanded to various zwitterionic analytes such as alpha- and beta-amino acids and peptides. A set of structurally related yet different CSPs consisting of either a quinine or quinidine alkaloid moiety as anion-exchange subunit and various chiral or achiral amino acids as cation-exchange subunits enabled us to derive structure-enantioselectivity relationships, which clearly provided strong unequivocal evidence for synergistic effects of the two oppositely charged ion-exchange subunits being involved in molecular recognition of zwitterionic analytes by zwitterionic SOs driven by double ionic coordination.

  8. Synthesis and characterization of a novel stationary phase, Si-Zr/Ti(PMTDS), based upon ternary oxide support for high performance liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Amparo, Maura R.; Marques, Fabiana A.; Faria, Anizio M., E-mail: anizio@pontal.ufu.br [Universidade Federal de Uberlandia (FACIP/UFU), Ituiutaba, MG (Brazil). Faculdade de Ciencias Integradas do Pontal

    2013-09-15

    A new stationary phase based on the thermal immobilization of poly(methyltetradecylsiloxane) (PMTDS) on silica particles coated with a mixture of zirconia and titania was prepared and evaluated for the chromatographic separation of test mixtures. The spherical particles were characterized by elemental analysis, SEM, FTIR and {sup 29}Si NMR. The physicochemical properties of PMTDS phase supported on Si-Zr/Ti were intermediate between PMTDS phases supported on titanized silica and zirconized silica. The chromatographic performance of Si-Zr/Ti(PMTDS) phase was similar to PMTDS phases based on metal oxide coated silica having only one metal oxide and the preparation of a Si-Zr/Ti(PMTDS) phase allowed evaluation of the effect of each oxide, zirconia and titania, on the separation process and on the stability of the immobilized polymer phase. The hydrolytic stability of Si-Zr/Ti(PMTDS) stationary phase was similar to the Si-Ti(PMTDS) phase, improving the chemical stability of the silica-based PMTDS phase by about 100%. (author)

  9. An innovative monolithic zwitterionic stationary phase for the separation of phenolic acids in coffee bean extracts by capillary electrochromatography.

    Science.gov (United States)

    Murauer, Adele; Bakry, Rania; Schottenberger, Herwig; Huck, Christian; Ganzera, Markus

    2017-04-22

    A methacrylate based monolith, containing the innovative zwitterionic monomer (3-allyl-1-imidazol)propane sulfonate, was prepared in 100 μm I.D. silica capillaries by UV initiated photo-polymerization. Composition of the porogen, i.e. a mixture of 1-propanol, 1,4 butanediol and water, was of great importance to obtain a homogeneous monolith with satisfactory permeability and good electrochromatographic performance. Morphology of the stationary phase was studied in Scanning Electron Microscopy and IR experiments, which revealed a good attachment to the capillary wall, flowthrough-pores in the range of 0.5-2 μm, and a continuous monolithic structure. The developed material was well suited for the analysis of six common phenolic acids (salicylic, cinnamic, syringic, rosmarinic, caffeic and chlorogenic acid) by CEC. Their separation was possible in less than 8 min with a mobile phase comprising a 12 mM aqueous ammonium acetate solution with pH 8.5 and acetonitrile, at an applied voltage of - 20 kV. The developed method was validated (R 2  ≥ 0.995; LOD ≤ 3.9 μg mL -1 , except for salicylic acid; recovery rates from 94 to 104%) and successfully used for the determination of phenolic acids in Coffea arabica samples. All of them contained cinnamic, syringic and caffeic acid, however only in unroasted coffee beans chlorogenic acid (0.06%) was found. The quantitative results were in good agreement to reported literature data. Copyright © 2017 The Author(s). Published by Elsevier B.V. All rights reserved.

  10. Inhomogeneous LOFF phase revisited for surface superconductivity

    Science.gov (United States)

    Barzykin, Victor; Gor'kov, Lev P.

    2003-03-01

    We consider 2D surface superconductivity in high magnetic fields parallel to the surface. We demonstrate that the spin-orbit interaction at the surface changes the properties of the inhomogeneous superconducting Larkin-Ovchinnikov-Fulde-Ferrell state that develops above fields given by the paramagnetic criterion. Strong spin-orbit interaction significantly broadens the range of existence of the LOFF phase, which takes the form of periodic superconducting stripes running along the field direction on the surface, leading to the anisotropy of its properties. We also discuss this problem for the d-wave pairing to indicate the possibility of a re-orientation transition as the magnetic field direction is rotated in the plane parallel to the surface. Our results provide a tool for studying surface superconductivity This work was supported in part by NHMFL through the NSF Cooperative agreement No. DMR-9521035 and the State of Florida, in part (VB) by the University of Tennessee.

  11. Numerical analysis of non-stationary free surface flow in a Pelton bucket

    Energy Technology Data Exchange (ETDEWEB)

    Hana, Morten

    1999-07-01

    Computation and analysis of flow in Pelton buckets have been carried out. First a graphical method is investigated and partially improved. In order to decide whether to improve the method further or disregard it in favour of commercial computational fluid dynamics (CFD) codes, a study on numerical methods for free surface flow was carried out. This part of this work concentrates on the theoretical background for different numerical methods, and describes some practical considerations. Although small programs were created based on the literature survey, but only one reported herein, it was soon found that commonly available numerical codes were favourable in use. A code, RIPPLE, was acquired to study the Volume of Fluid (VOF) method in detail. The commercial codes used were Flow-3D and CFX-4. These programs were used in three different cases. First, a simplified 2-dimensional case was verified experimentally. Next, a 3-dimensional fixed jet calculation was carried out. Finally, numerical calculations with relative motion between the jet and buckets were carried out with CFX-4. The conclusion is that commercial CFD codes can replace the graphical method. But careful implementation is needed in order to resolve the special features of Pelton turbines, which are the free surface, the complex geometry and the relative motion between the jet and the bucket.

  12. Amorphous Phases on the Surface of Mars

    Science.gov (United States)

    Rampe, E. B.; Morris, R. V.; Ruff, S. W.; Horgan, B.; Dehouck, E.; Achilles, C. N.; Ming, D. W.; Bish, D. L.; Chipera, S. J.

    2014-01-01

    Both primary (volcanic/impact glasses) and secondary (opal/silica, allophane, hisingerite, npOx, S-bearing) amorphous phases appear to be major components of martian surface materials based on orbital and in-situ measurements. A key observation is that whereas regional/global scale amorphous components include altered glass and npOx, local scale amorphous phases include hydrated silica/opal. This suggests widespread alteration at low water-to-rock ratios, perhaps due to snow/ice melt with variable pH, and localized alteration at high water-to-rock ratios. Orbital and in-situ measurements of the regional/global amorphous component on Mars suggests that it is made up of at least three phases: npOx, amorphous silicate (likely altered glass), and an amorphous S-bearing phase. Fundamental questions regarding the composition and the formation of the regional/global amorphous component(s) still remain: Do the phases form locally or have they been homogenized through aeolian activity and derived from the global dust? Is the parent glass volcanic, impact, or both? Are the phases separate or intimately mixed (e.g., as in palagonite)? When did the amorphous phases form? To address the question of source (local and/or global), we need to look for variations in the different phases within the amorphous component through continued modeling of the chemical composition of the amorphous phases in samples from Gale using CheMin and APXS data. If we find variations (e.g., a lack of or enrichment in amorphous silicate in some samples), this may imply a local source for some phases. Furthermore, the chemical composition of the weathering products may give insight into the formation mechanisms of the parent glass (e.g., impact glasses contain higher Al and lower Si [30], so we might expect allophane as a weathering product of impact glass). To address the question of whether these phases are separate or intimately mixed, we need to do laboratory studies of naturally altered samples made

  13. Construction of a hydrazone-linked chiral covalent organic framework-silica composite as the stationary phase for high performance liquid chromatography.

    Science.gov (United States)

    Zhang, Kai; Cai, Song-Liang; Yan, Yi-Lun; He, Zi-Hao; Lin, Hui-Mei; Huang, Xiao-Ling; Zheng, Sheng-Run; Fan, Jun; Zhang, Wei-Guang

    2017-10-13

    Covalent organic frameworks (COFs), as an emerging class of crystalline porous organic polymers, have great potential for applications in chromatographic separation owning to their fascinating crystalline structures and outstanding properties. However, development of COF materials as novel stationary phases in high performance liquid chromatography (HPLC) is just in its infancy. Herein, we report the design and construction of a new hydrazone-linked chiral COF, termed BtaMth COF, from a chiral hydrazide building block (Mth) and present a one-pot synthetic method for the fabrication of BtaMth@SiO 2 composite for HPLC separation of isomers. The as-synthesized BtaMth chiral COF displays good crystallinity, high porosity, as well as excellent chemical stability. Meanwhile, the fabricated HPLC column by using BtaMth@SiO 2 composite as the new stationary phase exhibits high resolution performances for the separation of positional isomers including nitrotoluene and nitrochlorobenzene, as well as cis-trans isomers including beta-cypermethrin and metconazole. Additionally, some effects such as the composition of the mobile phase and column temperature for HPLC separations on the BtaMth@SiO 2 packed column also have been studied in detail. The successful applications indicate the great potentials of hydrazone-linked chiral COF-silica composite as novel stationary phase for the efficient HPLC separation. Copyright © 2017 Elsevier B.V. All rights reserved.

  14. The rye mutants identify a role for Ssn/Srb proteins of the RNA polymerase II holoenzyme during stationary phase entry in Saccharomyces cerevisiae.

    Science.gov (United States)

    Chang, Y W; Howard, S C; Budovskaya, Y V; Rine, J; Herman, P K

    2001-01-01

    Saccharomyces cerevisiae cells enter into a distinct resting state, known as stationary phase, in response to specific types of nutrient deprivation. We have identified a collection of mutants that exhibited a defective transcriptional response to nutrient limitation and failed to enter into a normal stationary phase. These rye mutants were isolated on the basis of defects in the regulation of YGP1 expression. In wild-type cells, YGP1 levels increased during the growth arrest caused by nutrient deprivation or inactivation of the Ras signaling pathway. In contrast, the levels of YGP1 and related genes were significantly elevated in the rye mutants during log phase growth. The rye defects were not specific to this YGP1 response as these mutants also exhibited multiple defects in stationary phase properties, including an inability to survive periods of prolonged starvation. These data indicated that the RYE genes might encode important regulators of yeast cell growth. Interestingly, three of the RYE genes encoded the Ssn/Srb proteins, Srb9p, Srb10p, and Srb11p, which are associated with the RNA polymerase II holoenzyme. Thus, the RNA polymerase II holoenzyme may be a target of the signaling pathways responsible for coordinating yeast cell growth with nutrient availability.

  15. Continuous beds (monoliths): stationary phases for liquid chromatography formed using the hydrophobic interaction-based phase separation mechanism.

    Science.gov (United States)

    Maruska, Audrius; Kornysova, Olga

    2004-04-30

    The pioneering research work published by Hjertén et al. [J. Chromatogr. 473 (1989) 273] in 1989 dealing with development and application of the continuous bed (monolithic) technique as an attractive alternative for the classical packed columns in chromatography, stimulated further investigations in this direction. The research data published since that time on the development and application of the continuous beds formed using hydrophobic interaction-based phase separation mechanism are reviewed. Some innovative species of the beds, such as polyrotaxane beds or nonparticulate restricted-access materials for direct analysis of the biological fluids in the capillary format are also discussed. Characteristic features and practical details of the continuous bed technique are revealed. Due to many advantages, the continuous bed technique became a competitor with the traditional packings in capillary or chip-based microanalysis. The importance of the continuous bed morphology on the chromatographic characteristics is shown. The applicability of modern microscopic analysis to evaluate the morphology of the continuous beds is demonstrated.

  16. Distinction of synthetic dl-α-tocopherol from natural vitamin E (d-α-tocopherol) by reversed-phase liquid chromatography. Enhanced selectivity of a polymeric C18 stationary phase at low temperature and/or at high pressure.

    Science.gov (United States)

    Yui, Yuko; Miyazaki, Shota; Ma, Yan; Ohira, Masayoshi; Fiehn, Oliver; Ikegami, Tohru; McCalley, David V; Tanaka, Nobuo

    2016-06-10

    Separation of diastereomers of dl-α-tocopherol was studied by reversed-phase liquid chromatography using three types of stationary phases, polymeric ODS, polymeric C30, and monomeric ODS. Polymeric ODS stationary phase (Inertsil ODS-P, 3mmID, 20cm) was effective for the separation of the isomers created by the presence of three chiral centers on the alkyl chain of synthetic dl-α-tocopherol. Considerable improvement of the separation of isomers was observed on ODS-P phase at high pressure and at low temperature. Complete separation of four pairs of diastereomers was achieved at 12.0°C, 536bar, while three peaks were observed when the separation was carried out either at 12.0°C at low pressure or at 20°C at 488bar. Higher temperature (30.0°C) with the ODS-P phase resulted in only partial separation of the diastereomers even at high pressure. Only slight resolution was observed for the mixture of diastereomers with the C30 stationary phase (Inertsil C30) at 12.0°C and 441bar, although the stationary phase afforded greater resolution for β- and γ-tocopherol than ODS-P. A monomeric C18 stationary phase did not show any separation at 12.0°C and 463bar. The results suggest that the binding site of the polymeric ODS-P phase is selective for flexible alkyl chains that provided the longest retention for the natural form, (R,R,R) form, and the enantiomer, (S,S,S) form, of dl-α-tocopherol. Copyright © 2016. Published by Elsevier B.V.

  17. Analysis of Stationary, Photovoltaic-based Surface Power System Designs at the Lunar South Pole

    Science.gov (United States)

    Freeh, Joshua E.

    2009-01-01

    Combinations of solar arrays and either batteries or regenerative fuel cells are analyzed for a surface power system module at the lunar south pole. The systems are required to produce 5 kW of net electrical power in sunlight and 2 kW of net electrical power during lunar night periods for a 10-year period between 2020 and 2030. Systems-level models for energy conservation, performance, degradation, and mass are used to compare to various systems. The sensitivities of important and/or uncertain variables including battery specific energy, fuel cell operating voltage, and DC-DC converter efficiency are compared to better understand the system. Switching unit efficiency, battery specific energy, and fuel cell operating voltage appear to be important system-level variables for this system. With reasonably sized solar arrays, the regenerative fuel cell system has significantly lower mass than the battery system based on the requirements and assumptions made herein. The total operational time is estimated at about 10,000 hours in battery discharge/fuel cell mode and about 4,000 and 8,000 hours for the battery charge and electrolyzer modes, respectively. The estimated number of significant depth-of-discharge cycles for either energy storage system is less than 100 for the 10-year period.

  18. ENVISAT Land Surface Processes. Phase 2

    Science.gov (United States)

    vandenHurk, B. J. J. M.; Su, Z.; Verhoef, W.; Menenti, M.; Li, Z.-L.; Wan, Z.; Moene, A. F.; Roerink, G.; Jia, I.

    2002-01-01

    This is a progress report of the 2nd phase of the project ENVISAT- Land Surface Processes, which has a 3-year scope. In this project, preparative research is carried out aiming at the retrieval of land surface characteristics from the ENVISAT sensors MERIS and AATSR, for assimilation into a system for Numerical Weather Prediction (NWP). Where in the 1st phase a number of first shot experiments were carried out (aiming at gaining experience with the retrievals and data assimilation procedures), the current 2nd phase has put more emphasis on the assessment and improvement of the quality of the retrieved products. The forthcoming phase will be devoted mainly to the data assimilation experiments and the assessment of the added value of the future ENVISAT products for NWP forecast skill. Referring to the retrieval of albedo, leaf area index and atmospheric corrections, preliminary radiative transfer calculations have been carried out that should enable the retrieval of these parameters once AATSR and MERIS data become available. However, much of this work is still to be carried out. An essential part of work in this area is the design and implementation of software that enables an efficient use of MODTRAN(sub 4) radiative transfer code, and during the current project phase familiarization with these new components has been achieved. Significant progress has been made with the retrieval of component temperatures from directional ATSR-images, and the calculation of surface turbulent heat fluxes from these data. The impact of vegetation cover on the retrieved component temperatures appears manageable, and preliminary comparison of foliage temperature to air temperatures were encouraging. The calculation of surface fluxes using the SEBI concept,which includes a detailed model of the surface roughness ratio, appeared to give results that were in reasonable agreement with local measurements with scintillometer devices. The specification of the atmospheric boundary conditions

  19. Involvement of GDH3-encoded NADP+-dependent glutamate dehydrogenase in yeast cell resistance to stress-induced apoptosis in stationary phase cells.

    Science.gov (United States)

    Lee, Yong Joo; Kim, Kyung Jin; Kang, Hong Yong; Kim, Hye-Rim; Maeng, Pil Jae

    2012-12-28

    Glutamate metabolism is linked to a number of fundamental metabolic pathways such as amino acid metabolism, the TCA cycle, and glutathione (GSH) synthesis. In the yeast Saccharomyces cerevisiae, glutamate is synthesized from α-ketoglutarate by two NADP(+)-dependent glutamate dehydrogenases (NADP-GDH) encoded by GDH1 and GDH3. Here, we report the relationship between the function of the NADP-GDH and stress-induced apoptosis. Gdh3-null cells showed accelerated chronological aging and hypersusceptibility to thermal and oxidative stress during stationary phase. Upon exposure to oxidative stress, Gdh3-null strains displayed a rapid loss in viability associated with typical apoptotic hallmarks, i.e. reactive oxygen species accumulation, nuclear fragmentation, DNA breakage, and phosphatidylserine translocation. In addition, Gdh3-null cells, but not Gdh1-null cells, had a higher tendency toward GSH depletion and subsequent reactive oxygen species accumulation than did WT cells. GSH depletion was rescued by exogenous GSH or glutamate. The hypersusceptibility of stationary phase Gdh3-null cells to stress-induced apoptosis was suppressed by deletion of GDH2. Promoter swapping and site-directed mutagenesis of GDH1 and GDH3 indicated that the necessity of GDH3 for the resistance to stress-induced apoptosis and chronological aging is due to the stationary phase-specific expression of GDH3 and concurrent degradation of Gdh1 in which the Lys-426 residue plays an essential role.

  20. Phase-shifting interferometer for surface inspection

    Science.gov (United States)

    Tam, Siu Chung; Low, Beng-Yew; Chua, Hock-Chuan; Ho, Anthony T. S.; Neo, Wah-Peng

    1997-08-01

    A phase-shifting Twyman-Green interferometer has been constructed. Using three consecutively captured interferograms, the phase profile of a reflective surface can be determined. Results using various fringe processing techniques are compared. These methods include uniform averaging, Gaussian mask and spin filtering. For simulated fringes superimposed with random noise and fixed-pattern noise, it has been observed that a combination of weighted averaging and spin filtering could generate the best results. The computerized system has been applied to the measurement of the form errors of a silicon wafer and a cosmetic mirror, respectively. The root-mean-square error of the wafer is determined to be 11.13 nm.

  1. Solid-phase equilibria on Pluto's surface

    Science.gov (United States)

    Tan, Sugata P.; Kargel, Jeffrey S.

    2018-03-01

    Pluto's surface is covered by volatile ices that are in equilibrium with the atmosphere. Multicomponent phase equilibria may be calculated using a thermodynamic equation of state and, without additional assumptions, result in methane-rich and nitrogen-rich solid phases. The former is formed at temperature range between the atmospheric pressure-dependent sublimation and condensation points, while the latter is formed at temperatures lower than the sublimation point. The results, calculated for the observed 11 μbar atmospheric pressure and composition, are consistent with recent work derived from observations by New Horizons.

  2. High-resolution peptide mapping separations with MS-friendly mobile phases and charge-surface-modified C18.

    Science.gov (United States)

    Lauber, Matthew A; Koza, Stephan M; McCall, Scott A; Alden, Bonnie A; Iraneta, Pamela C; Fountain, Kenneth J

    2013-07-16

    Ionic analytes, such as peptides, can be challenging to separate by reverse-phase chromatography with optimal efficiency. They tend, for instance, to exhibit poor peak shapes, particularly when eluted with mobile phases preferred for electrospray ionization mass spectrometry. We demonstrate that a novel charged-surface C18 stationary phase alleviates some of the challenges associated with reverse-phase peptide separations. This column chemistry, known as CSH (charged-surface hybrid) C18, improves upon an already robust organosilica hybrid stationary phase, BEH (ethylene-bridged hybrid) C18. Based on separations of a nine-peptide standard, CSH C18 was found to exhibit improved loadability, greater peak capacities, and unique selectivity compared to BEH C18. Its performance was also seen to be significantly less dependent on TFA-ion pairing, making it ideal for MS applications where high sensitivity is desired. These performance advantages were evaluated through application to peptide mapping, wherein CSH C18 was found to aid the development of a high-resolution, high-sensitivity LC-UV-MS peptide mapping method for the therapeutic antibody, trastuzumab. From these results, the use of a C18 stationary phase with a charged surface, such as CSH C18, holds significant promise for facilitating challenging peptide analyses.

  3. High performance liquid chromatographic separation of thirteen drugs collected in Chinese Pharmacopoeia 2010(Ch.P2010 on cellulose ramification chiral stationary phase

    Directory of Open Access Journals (Sweden)

    Ying Zhou

    2012-02-01

    Full Text Available The enantiomers separation of thirteen drugs collected in Ch.P2010 was performed on chiral stationary phase of cellulose ramification (chiralpak OD and chiralpak OJ by high performance liquid chromatographic (HPLC methods, which included ibuprofen (C1, ketoprofen (C2, nitrendipine (C3, nimodipine (C4, felodipine (C5, omeprazole (C6, praziquantel (C7, propranolol hydrochloride (C8, atenolol (C9, sulpiride (C10, clenbuterol hydrochloride (C11, verapamil hydrochloride (C12, and chlorphenamine maleate (C13. The mobile phase consisted of isopropanol and n-hexane. The detection wavelength was set at 254 nm and the flow rate was 0.7 mL/min. The enantiomers separation of these thirteen racemates on chiralpak OD column and chiralpak OJ column was studied, while the effects of proportion of organic additives, alcohol displacer and temperature on the separation were studied. And the mechanism of some of racemates was discussed. The results indicated that thirteen chiral drugs could be separated on chiral stationary phase of cellulose ramification in normal phase chromatographic system. The chromatographic retention and resolution of enantiomers could be adjusted by factors including column temperature and the concentration of alcohol displacer and organic alkaline modifier in mobile phase. It was shown that the resolution was improved with reducing concentration of alcohol displacer. When concentration of organic alkaline modifier was 0.2% (v/v, the resolution and the peak shape were fairly good. Most racemates mentioned above had better resolution at column temperature of 25 °C. When racemates were separated, the temperature should be kept so as to obtain stable separation results. Keywords: HPLC, Chiral stationary phase, Optical enantiomers, Cellulose ramification

  4. The phase diagram of crystalline surfaces

    International Nuclear Information System (INIS)

    Anagnostopoulos, K.N.; Bowick, M.J.; Catterall, S.M.

    1995-01-01

    We report the status of a high-statistics Monte Carlo simulation of non-self-avoiding crystalline surfaces with extrinsic curvature on lattices of size up to 128 2 nodes. We impose free boundary conditions. The free energy is a gaussian spring tethering potential together with a normal-normal bending energy. Particular emphasis is given to the behavior of the model in the cold phase where we measure the decay of the normal-normal correlation function

  5. Comparison of Various Types of Stationary Phases in Non-Aqueous Reversed-Phase High-Performance Liquid Chromatography–Mass Spectrometry of Glycerolipids in Blackcurrant Oil and Its Enzymatic Hydrolysis Mixture

    Czech Academy of Sciences Publication Activity Database

    Lísa, M.; Holčapek, M.; Sovová, Helena

    2009-01-01

    Roč. 1216, č. 47 (2009), s. 8371-8378 ISSN 0021-9673 Institutional research plan: CEZ:AV0Z40720504 Keywords : ultra high-performance liquid chromatography * C30 stationary phase * triacylglycerols Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 4.101, year: 2009

  6. Liquid chromatographic resolution of racemic rasagiline and its analogues on a chiral stationary phase based on (+)-(18-crown-6)-2,3,11,12-tetracarboxylic acid.

    Science.gov (United States)

    Tak, Kyung Mi; Park, Eun Ju; Hyun, Myung Ho

    2013-12-01

    A liquid chromatographic chiral stationary phase based on (+)-(18-crown-6)-2,3,11,12-tetracarboxylic acid was applied to the resolution of 15 analytes, including racemic rasagiline, a chiral drug for the treatment of Parkinson's disease, and its analogues. The composition of mobile phase was optimized to be ethanol/acetonitrile/acetic acid/triethylamine (80:20:0.2:0.3, v/v/v/v) by evaluating the chromatographic results for the resolution of five selected analytes under various mobile phase conditions. Under the optimized mobile phase conditions, racemic rasagiline was resolved quite well with a separation factor of 1.48 and resolution of 2.71 and its 14 analogues were also resolved reasonably well with separation factors of 1.06-1.54 and resolutions of 0.54-2.11. Among 15 analytes, racemic rasagiline was resolved best except for just one analyte. The analyte structure-enantioselectivity relationship indicated that racemic rasagiline has the most appropriate structural characteristics for resolution on the chiral stationary phase. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Application of a cholesterol stationary phase in the analysis of phosphorothioate oligonucleotides by means of ion pair chromatography coupled with tandem mass spectrometry.

    Science.gov (United States)

    Studzińska, Sylwia; Krzemińska, Katarzyna; Szumski, Michał; Buszewski, Bogusław

    2016-07-01

    The main aim of this study was the investigation of the influence of several ion pair reagents towards both the retention and the mass spectrometry sensitivity of phosphorothioate oligonucleotides. A cholesterol stationary phase was applied for the first time in the analysis of this group of compounds. The mobile phase composition was modified by changing the concentration and the type of amines and acetates or 1,1,1,3,3,3-hexafluoroisopropanol. It has been shown that the increase of amines concentration results in the retention factor increase for each oligonucleotide, on each adsorbent. The only exception was the mobile phase composed of triethylamine and 1,1,1,3,3,3-hexafluoroisopropanol. This is a consequence of interactions taking place between a cholesterol molecule and an alcohol. This effect was convenient when the mass spectrometry detection was applied, since it allowed an increase in the sensitivity. Moreover, optimization of the mobile phase composition and its impact on the efficiency of ionization process and on the sensitivity in mass spectrometry were also presented. The optimization of this new method, based on cholesterol stationary phase coupled with mass spectrometry detection, was finally applied for the determination of phosphorothioate oligonucleotides impurity in a real sample. Copyright © 2016 Elsevier B.V. All rights reserved.

  8. 2-DE based proteomic analysis of Saccharomyces cerevisiae wild and K+ transport-affected mutant (trk1,2) strains at the growth exponential and stationary phases.

    Science.gov (United States)

    Curto, Miguel; Valledor, Luis; Navarrete, Clara; Gutiérrez, Dolores; Sychrova, Hana; Ramos, José; Jorrin, Jesús

    2010-11-10

    By using a 2-DE based workflow, the proteome of wild and potassium transport mutant trk1,2 under optimal growth potassium concentration (50mM) has been analyzed. At the exponential and stationary phases, both strains showed similar growth, morphology potassium content, and Vmax of rubidium transport, the only difference found being the Km values for this potassium analogue transport, higher for the mutant (20mM) than for the wild (3-6mM) cells. Proteins were buffer-extracted, precipitated, solubilized, quantified, and subjected to 2-DE analysis in the 5-8 pH range. More differences in protein content (37-64mgg(-1) cell dry weight) and number of resolved spots (178-307) were found between growth phases than between strains. In all, 164 spots showed no differences between samples and a total of 105 were considered to be differential after ANOVA test. 171 proteins, corresponding to 71 unique gene products have been identified, this set being dominated by cytosolic species and glycolitic enzymes. The ranking of the more abundant spots revealed no differences between samples and indicated fermentative metabolism, and active cell wall biosynthesis, redox homeostasis, biosynthesis of amino acids, coenzymes, nucleotides, and RNA, and protein turnover, apart from cell division and growth. PCA analysis allowed the separation of growth phases (PC1 and 2) and strains at the stationary phase (PC3 and 4), but not at the exponential one. These results are also supported by clustering analysis. As a general tendency, a number of spots newly appeared at the stationary phase in wild type, and to a lesser extent, in the mutant. These up-accumulated spots corresponded to glycolitic enzymes, indicating a more active glucose catabolism, accompanied by an accumulation of methylglyoxal detoxification, and redox-homeostasis enzymes. Also, more extensive proteolysis was observed at the stationary phase with this resulting in an accumulation of low Mr protein species. Copyright © 2010

  9. Effect of pressure on the selectivity of polymeric C18 and C30 stationary phases in reversed-phase liquid chromatography. Increased separation of isomeric fatty acid methyl esters, triacylglycerols, and tocopherols at high pressure.

    Science.gov (United States)

    Okusa, Kensuke; Iwasaki, Yuki; Kuroda, Ikuma; Miwa, Shohei; Ohira, Masayoshi; Nagai, Toshiharu; Mizobe, Hoyo; Gotoh, Naohiro; Ikegami, Tohru; McCalley, David V; Tanaka, Nobuo

    2014-04-25

    A high-density, polymeric C18 stationary phase (Inertsil ODS-P) or a polymeric C30 phase (Inertsil C30) provided improved resolution of the isomeric fatty acids (FAs), FA methyl esters (FAMEs), triacylglycerols (TAGs), and tocopherols with an increase in pressure of 20-70MPa in reversed-phase HPLC. With respect to isomeric C18 FAMEs with one cis-double bond, ODS-P phase was effective for recognizing the position of a double bond among petroselinic (methyl 6Z-octadecenoate), oleic (methyl 9Z-octadecenoate), and cis-vaccenic (methyl 11Z-octadecenoate), especially at high pressure, but the differentiation between oleic and cis-vaccenic was not achieved by C30 phase regardless of the pressure. A monomeric C18 phase (InertSustain C18) was not effective for recognizing the position of the double bond in monounsaturated FAME, while the separation of cis- and trans-isomers was achieved by any of the stationary phases. The ODS-P and C30 phases provided increased separation for TAGs and β- and γ-tocopherols at high pressure. The transfer of FA, FAME, or TAG molecules from the mobile phase to the ODS-P stationary phase was accompanied by large volume reduction (-30∼-90mL/mol) resulting in a large increase in retention (up to 100% for an increase of 50MPa) and improved isomer separation at high pressure. For some isomer pairs, the ODS-P and C30 provided the opposite elution order, and in each case higher pressure improved the separation. The two stationary phases showed selectivity for the isomers having rigid structures, but only the ODS-P was effective for differentiating the position of a double bond in monounsaturated FAMEs. The results indicate that the improved isomer separation was provided by the increased dispersion interactions between the solute and the binding site of the stationary phase at high pressure. Copyright © 2014 Elsevier B.V. All rights reserved.

  10. Imaging of surface wave phase velocities from array phase observations

    Science.gov (United States)

    Weidle, Christian; Maupin, Valerie

    2010-05-01

    While temporary deployments some 10 years ago were largely based on short-period seismometers, the availability of broadband instruments in instrument pools increased strongly in recent years and as such modern temporary deployments for passive seismological recordings often consist to a large extent, if not exclusively, of broadband instruments. This opens for new analysis approaches as the broadband seismic wavefield is obtained at a relatively high spatial sampling relative to the wavelength. In an attempt to infer surface wave phase velocity anomalies beneath Southern Norway based on data from a temporary network of 41 broadband instruments, we present a new approach to overcome the limitations of two-station phase measurements (on the great circle with the source) and instead exploit the two-dimensional nature of the wavefield by taking into account phase measurements at all stations of the array from a single event. This is based on the assumption that the wavefield is at least piecewise linear within the study region. By triangulation of the network region and linear estimation of the phase gradient in each triangle we get without further a priori assumptions a coarse image of the phase velocity variations within our network. The image can be significantly refined for a single event recording by stacking multiple images based on arbitrary subsets of the available data. Phase velocity anomalies measured from single event recordings can be biased and blurred by non-plane arriving wavefield, reflections and diffractions of heterogeneities. Therefore, by averaging over velocity fields from different events with varying backazimuths, artefacts are reduced and the recovered image significantly improved. Another way to improve the recovered structures is to take into account the spatial variation of the amplitude field. However, while the phase between two neighboring stations may be (at least close to) linear, the amplitude may not, hence estimation of the second

  11. Novel bis(5-methyltetrazolium)amine ligand-bonded stationary phase with reduced leakage of metal ions in immobilized metal affinity chromatography of proteins.

    Science.gov (United States)

    Bo, Chunmiao; Wang, Chaozhan; Wei, Yinmao

    2016-11-01

    Immobilized metal affinity chromatography (IMAC) has been widely used for the specific separation of biopolymers. However, leakage of metal ions from IMAC adsorbents is of concern in IMAC. In this study, we designed a novel tridenate bis(5-methyltetrazolium)amine (BMTA) to reduce the leakage of metal ions by improving the affinity to immobilized metal ions. The ligand was bonded onto silica via three-step reaction to prepare a high-performance IMAC stationary phase. The chromatographic behaviors of ribonuclease A, cytochrome c, and lysozyme on the Cu(II)-, Ni(II)-, and Zn(II)-chelated stationary phase were investigated with respect to pH effect and elution with an imidazole gradient. The retention times of these three proteins increased by increasing the pH of the mobile phase but decreased by increasing the concentration of the competitive displacer. The retaining strength of the three proteins on the chelated stationary phase were in the order Cu(II) > Ni(II) > Zn(II). The behavior of these three proteins was consistent with the properties of a typical IMAC. The BMTA ligand exhibited a much stronger affinity for Cu(II) and Ni(II) than iminodiacetic acid (IDA), which is often regarded as a standard tridentate IMAC ligand. Quantum mechanical calculations at the B3LYP/6-31G level were used to image the coordination mode of the protein-metal ions-BMTA complex. In addition, a fused histidine-tagged cecropin b-human epidermal growth factor (CB-EGF) from Escherichia coli crude extract was purified by the Ni(II)-chelated stationary phase, and the purity of the CB-EGF was determined to be at least 90 %. These results suggest that the BMTA ligand may have potential applications in the preparation of therapeutics. Graphical Abstract A novel ligand of tridenate bis(5-methyltetrazolium)amine (BMTA) was designed to reduce the leakage of metal ions from the column in immobolized metal affinity chromatography (IMAC).

  12. Solvation molar enthalpies and heat capacities of n-alkanes and n-alkylbenzenes on stationary phases of wide-ranging polarity.

    Science.gov (United States)

    Lebrón-Aguilar, Rosa; Quintanilla-López, Jesús Eduardo; Santiuste, José María

    2010-12-03

    A comparison of the most usual gas chromatographic methods for the calculation of partial molar enthalpies of solvation (Δ(sol)H(o)) has been carried out. Those methods based on the fitting of lnV(g) or ln(k/T) vs. 1/T and ln(k/T) vs. (1/T and the temperature arrangement, T(a)) are the most adequate ones for obtaining Δ(sol)H(o) values. However, the latter is the only reliable option for Δ(sol)H(o) estimation when commercial WCOT capillary columns are used, since in this case the estimation of some variables involved in the V(g) determination is less accurate or even impossible. Consequently, in this paper, Δ(sol)H(o) obtained from ln(k/T) vs. (1/T+T(a)) fitting at 373.15 and 298.15K for n-alkanes and n-alkylbenzenes on 12 commercial capillary columns coated with stationary phases covering the 203-3608 McReynolds polarity range are reported. Moreover, molar heat capacities of solvation at constant pressure (Δ(sol)C(p)(o)) have also been calculated using this method. A clear influence on Δ(sol)H(o) of the type and content of the substitution group in the stationary phase was observed. In addition, a linear relationship of Δ(sol)C(p)(o) with the van der Waals volume of the n-alkanes and the temperature gradient of density of the stationary phase was found. The effect of the size of the hydrocarbon on both thermodynamic variables was also investigated. Copyright © 2010 Elsevier B.V. All rights reserved.

  13. Stationary Frame Current Control Evaluations for Three-Phase Grid-Connected Inverters with PVR-based Active Damped LCL Filters

    DEFF Research Database (Denmark)

    Han, Yang; Shen, Pan; Guerrero, Josep M.

    2016-01-01

    Grid-connected inverters (GCIs) with LCL output filter have the ability of attenuating high-frequency (HF) switching ripples. However, by using only grid-current control, the system is prone to resonances if it is not properly damped, and the current distortion would be amplified significantly...... to suppress the LCL resonance is proposed. Although both proportional-resonant (PR) controller in αβ stationary frame and PI controller in dq synchronous frame achieve zero steady-state error, the amplitude- and phase-frequency characteristics differ greatly from each other except for the reference tracking...

  14. The use of Stationary Phase Optimized Selectivity Liquid Chromatography for the development of herbal fingerprints to detect targeted plants in plant food supplements.

    Science.gov (United States)

    Deconinck, E; Djiogo, C A Sokeng; Kamugisha, A; Courselle, P

    2017-08-01

    The consumption of plant food supplements is increasing steadily and more and more, these products are bought through internet. Often the products sold through internet are not registered or declared with a national authority, meaning that no or minimal quality control is performed and that they could contain herbs or plants that are regulated. Stationary Phase Optimized Selectivity Liquid Chromatography (SOS-LC) was evaluated for the development of specific fingerprints, to be used for the detection of targeted plants in plant food supplements. Three commonly used plants in plant food supplements and two regulated plants were used to develop fingerprints with SOS-LC. It was shown that for all plants specific fingerprints could be obtained, allowing the detection of these targeted plants in triturations with different herbal matrices as well as in real samples of suspicious supplements seized by the authorities. For three of the five plants a more specific fingerprint was obtained, compared to the ones developed on traditional columns described in literature. It could therefore be concluded that the combination of segments of different types of stationary phases, as used in SOS-LC, has the potential of becoming a valuable tool in the quality control and the identification of crude herbal or plant material and in the detection of regulated plants in plant food supplements or other herbal preparations. Copyright © 2017 Elsevier B.V. All rights reserved.

  15. Novel tentacle-type polymer stationary phase grafted with anion exchange polymer chains for open tubular CEC of nucleosides and proteins.

    Science.gov (United States)

    Aydoğan, Cemil; Çetin, Kemal; Denizli, Adil

    2014-08-07

    A novel and simple method for preparation of a tentacle-type polymer stationary phase grafted with polyethyleneimine (PEI) anion exchanger was developed for open tubular capillary electrochromatography (OT-CEC) of nucleosides and proteins. The polymeric stationary phase was prepared using 3-chloro-2-hydroxypropyl methacrylate (HPMA-Cl)-based reactive monomer. The preparation procedure included pretreatment of the capillary inner wall, silanization, in situ graft polymerization with HPMA-Cl and PEI modification. To compare with the tentacle-type capillary column with PEI functionalization, a monolayer capillary column without PEI functionalization was also prepared. The electrochromatographic characterization of the prepared open tubular column was performed using alkylbenzenes. The electroosmotic flow (EOF) with regard to PEI concentrations and the running buffer pH was investigated. The separation conditions of the nucleosides and the proteins were optimized. The modified tentacle-type column with high anion exchange capacity has proven to afford better retention and resolution for the separation of nucleosides and proteins. The PEI functionalization column can also provide long-term stable use for biomolecule separation using a single capillary with relative standard deviation values of retention times of less than 2%. The results indicate that the present method for open tubular capillary preparation with a HPMA-Cl-based reactive monomer is promising for OT-CEC biomolecule separation.

  16. Separation of biomolecules by micro-high-performance anion-exchange chromatography using a tentacle-like stationary phase.

    Science.gov (United States)

    Marlin, Nicola Dawn; Smith, Norman William

    2005-05-01

    A variety of biomolecules and their variants, which have previously been problematic to separate, have been analysed using a novel anion-exchange resin based on a non-porous polystyrene polymeric support with a hydrophilic coating and grafted tentacular quaternary ammonium functional groups. The hydrophilic coating results in minimal interaction between the support and the biomolecule, while the highly flexible tentacular-like anion-exchange groups increase the ionic interaction potential and act as an umbrella to hold the proteins away from the surface. Because of the removal of silanophilic interactions, minimisation of hydrophobic interactions, and the highly flexible nature of the tentacle-like ion exchangers, ionic interactions can therefore dominate the separation. As such this phase is highly suited to the separation of highly charged biomolecules and their variants. This polymeric strong anion-exchange (SAX) support was packed into a fused-silica capillary column and, using a salt concentration gradient, various recombinant proteins were analysed by micro-HPLC resulting in baseline resolution.

  17. Comparison of the peak resolution and the stationary phase retention between the satellite and the planetary motions using the coil satellite centrifuge with counter-current chromatographic separation of 4-methylumbelliferyl sugar derivatives

    Science.gov (United States)

    Shinomiya, Kazufusa; Zaima, Kazumasa; Harada, Yukina; Yasue, Miho; Harikai, Naoki; Tokura, Koji; Ito, Yoichiro

    2016-01-01

    Coil satellite centrifuge (CSC) produces the complex satellite motion consisting of the triplicate rotation of the coiled column around three axes including the sun axis (the angular velocity, ω1), the planet axis (ω2) and the satellite axis (the central axis of the column) (ω3) according to the following formula: ω1 = ω2 + ω3. Improved peak resolution in the separation of 4-methylumbelliferyl sugar derivatives was achieved using the conventional multilayer coiled columns with ethyl acetate/1-butanol/water (3 : 2 : 5, v/v) for the lower mobile phase at the combination of the rotation speeds (ω1, ω2, ω3) = (300, 150, 150 rpm), and (1 : 4 : 5, v/v) for the upper mobile phase at (300 : 100 : 200 rpm). The effect of the satellite motion on the peak resolution and the stationary phase retention was evaluated by each CSC separation with the different rotation speeds of ω2 and ω3 under the constant revolution speed at ω1 = 300 rpm. With the lower mobile phase, almost constant peak resolution and stationary phase retention were yielded regardless of the change of ω2 and ω3, while with the upper mobile phase these two values were sensitively varied according to the different combination of ω2 and ω3. For example, when ω2 = 147 or 200 rpm is used, no stationary phase was retained in the coiled column while ω2 = 150 rpm could retain enough volume of stationary phase for separation. On the other hand, the combined rotation speeds at (ω1, ω2, ω3) = (300, 300, 0 rpm) or (300, 0, 300 rpm) produced insufficient peak resolution regardless of the choice of the mobile phase apparently due to the lack of rotation speed except at (300, 0, 300 rpm) with the upper mobile phase. At lower rotation speed of ω1 = 300 rpm, better peak resolution and stationary phase retention were obtained by the satellite motion (ω3) than by the planetary motion (ω2), or ω3 > ω2. The effect of the hydrophobicity of the two-phase solvent systems on the stationary phase retention was

  18. Innovative Deterministic Optical Surface Finishing, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — Increasing the optical surface finishing precision and reducing surface roughness will greatly benefit astronomy telescope and other optical systems. Conventional...

  19. Surface Modification of Exfoliated Graphite Nano-Reinforcements, Phase II

    Data.gov (United States)

    National Aeronautics and Space Administration — Phase I results showed that two surface treatments, oxidative plasma and reactive finishes, are effective means of modifying the surface chemistry of exfoliated...

  20. Dynamic high performance liquid chromatography on chiral stationary phases. Low temperature separation of the interconverting enantiomers of diazepam, flunitrazepam, prazepam and tetrazepam.

    Science.gov (United States)

    Sabia, Rocchina; Ciogli, Alessia; Pierini, Marco; Gasparrini, Francesco; Villani, Claudio

    2014-10-10

    Diazepam and the structurally related 1,4-benzodiazepin-2-ones tetrazepam, prazepam and flunitrazepam are chiral molecules because they adopt a ground state conformation featuring a non-planar seven membered ring devoid of any reflection-symmetry element. The two conformational enantiomers of this class of benzodiazepines interconvert rapidly at room temperature by a simple ring flipping process. Low temperature HPLC on the Whelk-O1 chiral stationary phase allowed us to separate the conformational enantiomers of diazepam and of the related 1,4-benzodiazepin-2-ones, under conditions where the interconversion rate is sufficiently low, compared to the chromatographic separation rate. Diazepam, tetrazepam and prazepam showed temperature dependent dynamic HPLC profiles with interconversion plateaus indicative of on-column enantiomer interconversion (enantiomerization) in the temperature range between -10 °C and -35 °C, whereas for flunitrazepam on-column interconversion was observed at temperatures between -40 °C and -66 °C. Simulation of exchange-deformed HPLC profiles using a computer program based on the stochastic model yielded the apparent rate constants for the on-column enantiomerization and the corresponding free energy activation barriers. At -20 °C the enantiomerization barriers, ΔG(≠), for diazepam, prazepam and tetrazepam were determined to be in the range 17.6-18.7 kcal/mol. At -55 °C ΔG(≠) for flunitrazepam was determined to be in the 15.6-15.7 kcal/mol range. The experimental dynamic chromatograms and the corresponding interconversion barriers reported in this paper call for a reinterpretation of previously published results on the HPLC behavior of diazepam on chiral stationary phases. Copyright © 2014 Elsevier B.V. All rights reserved.

  1. Diastereo- and enantioseparation of a Nα-Boc amino acid with a zwitterionic quinine-based stationary phase: Focus on the stereorecognition mechanism

    International Nuclear Information System (INIS)

    Ianni, Federica; Carotti, Andrea; Marinozzi, Maura; Marcelli, Gloria; Di Michele, Alessandro; Sardella, Roccaldo; Lindner, Wolfgang; Natalini, Benedetto

    2015-01-01

    Highlights: • The ZWIX(+) column allowed getting the Boc-Aph(Hor)-OH (1) isomeric peaks resolved. • ECD studies and molecular dynamic simulations allowed to assign the elution order. • Molecular descriptors revealed the active role of achiral elements of the CSP. - Abstract: A chiral chromatography method enabling the simultaneous diastereo- and enantioseparation of N α -Boc-N 4 -(hydroorotyl)-4-aminophenylalanine [Boc-Aph(Hor)-OH, 1] was optimized with a quinine-based zwitterionic stationary phase. The polar-ionic eluent system consisting of ACN:MeOH:water—49.7:49.7:0.6 (v/v/v) with formic acid (4.0 mM) and diethylamine (2.5 mM), allowed the successful separation of the four acid stereoisomers: α D,D-/D,L-1 = 1.08; α D,L-/L,D-1 = 1.08; α L,D-/L,L-1 = 1.40. According to the in-house developed synthetic procedure and the recorded electronic circular dichroism spectra, the following stereoisomeric elution order was readily established in the optimal chromatographic conditions: D,D-1 < D,L-1 < L,D-1 < L,L-1. With the aim of better understanding the molecular basis of the retention behaviour of the four stereoisomers in the employed chromatographic system and conditions, a computational protocol consisting in molecular dynamics simulations was applied. The use of the three descriptors INTER (in kcal mol −1 , encoding for the interaction energy between the selector SO unit and the whole system), INTER-SA (in kcal mol −1 , encoding for the interaction energy between SO and the sole selectand SA), and SELF (in kcal mol −1 , encoding for the conformational energy of SA relative to its minimum energy registered by the collected snapshots) revealed the active role of achiral sub-structural elements of the chiral stationary phase and eluent components in the overall stereorecognition mechanism

  2. Diastereo- and enantioseparation of a N(α)-Boc amino acid with a zwitterionic quinine-based stationary phase: focus on the stereorecognition mechanism.

    Science.gov (United States)

    Ianni, Federica; Carotti, Andrea; Marinozzi, Maura; Marcelli, Gloria; Di Michele, Alessandro; Sardella, Roccaldo; Lindner, Wolfgang; Natalini, Benedetto

    2015-07-23

    A chiral chromatography method enabling the simultaneous diastereo- and enantioseparation of N(α)-Boc-N(4)-(hydroorotyl)-4-aminophenylalanine [Boc-Aph(Hor)-OH, 1] was optimized with a quinine-based zwitterionic stationary phase. The polar-ionic eluent system consisting of ACN:MeOH:water-49.7:49.7:0.6 (v/v/v) with formic acid (4.0mM) and diethylamine (2.5mM), allowed the successful separation of the four acid stereoisomers: αd,d-/d,l-1=1.08; αd,l-/l,d-1=1.08; αl,d-/l,l-1=1.40. According to the in-house developed synthetic procedure and the recorded electronic circular dichroism spectra, the following stereoisomeric elution order was readily established in the optimal chromatographic conditions: d,d-1stationary phase and eluent components in the overall stereorecognition mechanism. Copyright © 2015 Elsevier B.V. All rights reserved.

  3. Novas fases estacionárias à base de sílica para cromatografia líquida de alta eficiência New stationary phases based on silica for high performance liquid chromatography

    Directory of Open Access Journals (Sweden)

    César R. Silva

    2004-04-01

    Full Text Available The present work reviews recent advances in the preparation of new reversed phase packing materials such as sterically protected, bidentate, hybrid organic-inorganic and monolithic phases and phases containing embedded polar groups. The bonding chemistry involved in the preparation of these phases as well as their advantages over conventional C8 and C18 reversed phases are discussed. Understanding the reasons behind the development of these newer column packings helps analysts select the best stationary phase for a given application.

  4. Anomalous Surface Wave Launching by Handedness Phase Control

    KAUST Repository

    Zhang, Xueqian

    2015-10-09

    Anomalous launch of a surface wave with different handedness phase control is achieved in a terahertz metasurface based on phase discontinuities. The polarity of the phase profile of the surface waves is found to be strongly correlated to the polarization handedness, promising polarization-controllable wavefront shaping, polarization sensing, and environmental refractive-index sensing. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Modeling, analysis, and design of stationary reference frame droop controlled parallel three-phase voltage source inverters

    DEFF Research Database (Denmark)

    Vasquez, Juan Carlos; Guerrero, Josep M.; Savaghebi, Mehdi

    2013-01-01

    Power electronics based MicroGrids consist of a number of voltage source inverters (VSIs) operating in parallel. In this paper, the modeling, control design, and stability analysis of parallel connected three-phase VSIs are derived. The proposed voltage and current inner control loops and the mat......Power electronics based MicroGrids consist of a number of voltage source inverters (VSIs) operating in parallel. In this paper, the modeling, control design, and stability analysis of parallel connected three-phase VSIs are derived. The proposed voltage and current inner control loops...... control restores the frequency and amplitude deviations produced by the primary control. Also, a synchronization algorithm is presented in order to connect the MicroGrid to the grid. Experimental results are provided to validate the performance and robustness of the parallel VSI system control...

  6. Evaluation of different hydrophilic stationary phases for the simultaneous determination of iminosugars and other low molecular weight carbohydrates in vegetable extracts by liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Rodríguez-Sánchez, S; Quintanilla-López, J E; Soria, A C; Sanz, M L

    2014-11-01

    Iminosugars are considered potential drug candidates for the treatment of several diseases, mainly as a result of their α-glycosidase inhibition properties. A method by hydrophilic interaction liquid chromatography tandem mass spectrometry has been optimized for the first time for the simultaneous determination of complex mixtures of bioactive iminosugars and other low molecular weight carbohydrates (LMWC) in vegetable extracts. Three hydrophilic stationary phases (sulfoalkylbetaine zwitterionic, polyhydroxyethyl aspartamide and ethylene bridge hybrid (BEH) with trifunctionally bonded amide) were compared under both basic and acidic conditions. The best sensitivity (limits of detection between 0.025 and 0.28ngmL -1 ) and overall chromatographic performance in terms of resolution, peak width and analysis time were obtained with the BEH amide column using 0.1% ammonium hydroxide as a mobile phase additive. The optimized method was applied to the analysis of extracts of hyacinth bulbs, buckwheat seeds and mulberry leaves. Iminosugar and other LMWC structures were tentatively assigned by their high resolution daughter ions mass spectra. Several iminosugars such as glycosyl-fagomine in mulberry extract were also described for the first time. Among the extracts analysed, mulberry showed the widest diversity of iminosugars, whereas the highest content of them was found in hyacinth bulb (2.5mgg -1 ) followed by mulberry (1.95 mgg -1 ). Copyright © 2014 Elsevier B.V. All rights reserved.

  7. Design, preparation and application of a Pirkle-type chiral stationary phase for enantioseparation of some racemic organic acids and molecular dynamics studies

    Directory of Open Access Journals (Sweden)

    Reşit Çakmak

    2017-08-01

    Full Text Available This study consists of two parts. In the first part of the study; a Pirkle-type chiral stationary phase was prepared by synthesizing an aromatic amine derivative of (R-2-amino-1-butanol as a chiral selectorand binding to L- tyrosine -modified cyanogen bromide (CNBr-activated Sepharose 4B and then, packed into the separation column. T he chromatographic performance of the separation column was evaluated w ith racemic mandelic acid and 2-phenylpropionic acid by using phosphate buffers at three different pHs as mobile phase. In the resolution processes, t he prepared solutions were loaded onto the separation column at two different concentrations and at three different pHs for each racemic organic acid, separately. Enantiomeric excess (ee % of the eluates was determined on CHIRALPAK AD-H chiral analytical column by HPLC. The maximum ee% for mandelic acid and 2-phenylpropionic acid was determined to be 60.84 and 27.4, respectively. Separation factors (k 1 ’, k 2 ’, α, and Rs were calculated for each acid. The structures of the obtained compounds were characterized using the spectroscopic methods (NMR, and elemental analysis. In the second part of the study; enantioselective interactions between the prepared CSP and the analytes have been widely studied by docking, molecular dynamics simulation and quantum mechanical computation methods. The reason of column eluation of rac-2-phenylpropionic acid with lower enantiomeric yield was explained by these techniques.

  8. DEFINITION OF DENSITY OF THE THERMAL STATIONARY STREAMS ON A SURFACES OF A SLEEVE OF CYLINDER COMBUSTION ENGINE BY A METHOD OF OPTIMUM FILTRATION KALMANA

    Directory of Open Access Journals (Sweden)

    ZARENBIN V. G.

    2016-01-01

    Full Text Available Problem statement. At research warmly intensity and thermal weariness of internal combustion engines (ICE the knowledge and the analysis of local temperatures and thermal streams in the basic details forming the chamber of combustion is defining. Theoretically the problem consists in the decision of the equation of heat conductivity at the set features of course of thermal processes on border of bodies. Thus there is a problem of accuracy of the decision since it depends on accuracy of the task of real boundary conditions which can be received only by means of physical experiment and corresponding metrological maintenance. Unlike temperature the thermal stream cannot be measured directly, therefore it define on a difference of temperatures (thermal gradient a method or a calorimetric method. Definition of density of streams with the help as named gauges of a thermal stream when the measured temperatures are used at the decision of a return problem of heat conductivity for chosen thermometric an element is most extended. In this case, except the requirement of one-dimensionality of distribution of temperatures, linearity and the minimum distortion of temperature fields of thermal system, there are considerable difficulties of calculation derivative of the measured temperature. To perspective it is possible to carry methods of researches which it is accepted to name cybernetic diagnostics or identification of systems. Their essence consists that the deformed information on object is compared to its mathematical model and then are defined its condition, parameters or entrance influences by minimization of square-law function are nonviscous. In work definition of density of thermal stationary streams on surfaces of a sleeve of cylinder ICE by a method of optimum filtration Kalmana and also an estimation of their reliability and accuracy is made. Possibility of application of filtration Kalmana is shown at experimental researches in ICE. The purpose

  9. Innovative Microbial Surface Sampler, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — The QS Team will develop an Innovative Microbial Surface Sampling (IMSS) device design and provide prototype kits for use in the International Space Station (ISS)....

  10. Wetting and phase separation at surfaces

    Indian Academy of Sciences (India)

    §2, we discuss microscopic and coarse-grained models for SDSD. In §3, we present analytical and numerical results for the case of a semi-infinite geometry. In §4, we discuss phase separation in confined geometries, e.g., pores, thin films. Finally, §5 concludes this paper with a summary and discussion of our results. 881 ...

  11. Correlations between retention indices and molecular structure of their benzoyl derivatives on phenyl substituted polysiloxane stationary phases

    International Nuclear Information System (INIS)

    Pias, J.B.; Gasco, L.

    1976-01-01

    The retention indices of aliphaticalcohols of carbon number up to Csub(g), and of their benzoyl derivatives up to C 7 , were determined in columns packed with Chromosorb G (AW-DMCS-HP) coated previously with 5% methyl, and methyl phenyl polysiloxanes with increasing polarity (SE-30, OV-3, OV-7; OV-11, OV-17 and OV-25). Correlations between retention indices and chain length for 1-alcohols, 2-alcohols, 3-alcohols, 1, on -3-alcohols, 2-methyl-1-alcohols and for their corresponding benzoyl derivatives were calculated at 100, 120 and 140 0 C. In alcohols, a -CH 2 - group increases I approximately 100 units, and in their benzoyl derivatives from 80 to 100 units. Dispersion indices ΔI, and positional and structural increments of I were evaluated for -OH and benzoyl groups in terms for phase polarity and chain length. Effects of chain length, chain branching and double bond location on retention parameters were also studied. (author)

  12. Diastereo- and enantioseparation of a N{sup α}-Boc amino acid with a zwitterionic quinine-based stationary phase: Focus on the stereorecognition mechanism

    Energy Technology Data Exchange (ETDEWEB)

    Ianni, Federica; Carotti, Andrea; Marinozzi, Maura; Marcelli, Gloria [Department of Pharmaceutical Sciences, University of Perugia, Via Fabretti 48, 06123 Perugia (Italy); Di Michele, Alessandro [Department of Physics and Geology, University of Perugia, Via Pascoli 1, 06123 Perugia (Italy); Sardella, Roccaldo, E-mail: roccaldo.sardella@unipg.it [Department of Pharmaceutical Sciences, University of Perugia, Via Fabretti 48, 06123 Perugia (Italy); Lindner, Wolfgang [Department of Analytical Chemistry, University of Vienna, Währinger Strasse 38, 1090 Vienna (Austria); Natalini, Benedetto [Department of Pharmaceutical Sciences, University of Perugia, Via Fabretti 48, 06123 Perugia (Italy)

    2015-07-23

    Highlights: • The ZWIX(+) column allowed getting the Boc-Aph(Hor)-OH (1) isomeric peaks resolved. • ECD studies and molecular dynamic simulations allowed to assign the elution order. • Molecular descriptors revealed the active role of achiral elements of the CSP. - Abstract: A chiral chromatography method enabling the simultaneous diastereo- and enantioseparation of N{sup α}-Boc-N{sup 4}-(hydroorotyl)-4-aminophenylalanine [Boc-Aph(Hor)-OH, 1] was optimized with a quinine-based zwitterionic stationary phase. The polar-ionic eluent system consisting of ACN:MeOH:water—49.7:49.7:0.6 (v/v/v) with formic acid (4.0 mM) and diethylamine (2.5 mM), allowed the successful separation of the four acid stereoisomers: α{sub D,D-/D,L-1} = 1.08; α{sub D,L-/L,D-1} = 1.08; α{sub L,D-/L,L-1} = 1.40. According to the in-house developed synthetic procedure and the recorded electronic circular dichroism spectra, the following stereoisomeric elution order was readily established in the optimal chromatographic conditions: D,D-1 < D,L-1 < L,D-1 < L,L-1. With the aim of better understanding the molecular basis of the retention behaviour of the four stereoisomers in the employed chromatographic system and conditions, a computational protocol consisting in molecular dynamics simulations was applied. The use of the three descriptors INTER (in kcal mol{sup −1}, encoding for the interaction energy between the selector SO unit and the whole system), INTER-SA (in kcal mol{sup −1}, encoding for the interaction energy between SO and the sole selectand SA), and SELF (in kcal mol{sup −1}, encoding for the conformational energy of SA relative to its minimum energy registered by the collected snapshots) revealed the active role of achiral sub-structural elements of the chiral stationary phase and eluent components in the overall stereorecognition mechanism.

  13. Surface phase transitions in cu-based solid solutions

    Science.gov (United States)

    Zhevnenko, S. N.; Chernyshikhin, S. V.

    2017-11-01

    We have measured surface energy in two-component Cu-based systems in H2 + Ar gas atmosphere. The experiments on solid Cu [Ag] and Cu [Co] solutions show presence of phase transitions on the surfaces. Isotherms of the surface energy have singularities (the minimum in the case of copper solid solutions with silver and the maximum in the case of solid solutions with cobalt). In both cases, the surface phase transitions cause deficiency of surface miscibility: formation of a monolayer (multilayer) (Cu-Ag) or of nanoscale particles (Cu-Co). At the same time, according to the volume phase diagrams, the concentration and temperature of the surface phase transitions correspond to the solid solution within the volume. The method permits determining the rate of diffusional creep in addition to the surface energy. The temperature and concentration dependence of the solid solutions' viscosity coefficient supports the fact of the surface phase transitions and provides insights into the diffusion properties of the transforming surfaces.

  14. Capillary electrochromatography using knitted aromatic polymer as the stationary phase for the separation of small biomolecules and drugs.

    Science.gov (United States)

    Tang, Pingxiu; Chen, Zilin

    2018-02-01

    Hypercrosslinked polymers (HCPs) are currently receiving great attention due to their unique characteristics and potential uses in diverse areas. However, the field of HCPs for open-tubular capillary electrochromatography (OT-CEC) separations has not been explored. Here, a knitted aromatic polymer (KAP) was in-situ grown on the inner wall of the capillary column for OT-CEC for the first time. The silylating reagent containing phenyl was served as monomer, immobilized on the inner wall of the capillary column, and then KAPs-modified capillary column was prepared through in-situ hypercrosslinking reaction. The surface structure and morphology of KAPs-modified capillary column was characterized by Fourier transform infrared spectra (FT-IR) and scanning electron microscopy (SEM). The prepared capillary columns showed good separation performance for neutral compounds, small biomolecules, such as nucleosides, amino acids, small peptides, and non-steroidal anti-inflammatory drugs, sulfa drugs. In addition, the KAPs-modified capillaries showed good reproducibility, with relative standard deviations for intra-day, inter-day and column-to-column runs less than 1.59%, 2.55%, and 5.19% respectively. The strategy of in-situ immobilization of KAPs provides a new approach for the application of the material in the analytical fields. Copyright © 2017 Elsevier B.V. All rights reserved.

  15. Surface field theories of point group symmetry protected topological phases

    Science.gov (United States)

    Huang, Sheng-Jie; Hermele, Michael

    2018-02-01

    We identify field theories that describe the surfaces of three-dimensional bosonic point group symmetry protected topological (pgSPT) phases. The anomalous nature of the surface field theories is revealed via a dimensional reduction argument. Specifically, we study three different surface field theories. The first field theory is quantum electrodynamics in three space-time dimensions (QED3) with four flavors of fermions. We show this theory can describe the surfaces of a majority of bosonic pgSPT phases protected by a single mirror reflection, or by Cn v point group symmetry for n =2 ,3 ,4 ,6 . The second field theory is a variant of QED3 with charge-1 and charge-3 Dirac fermions. This field theory can describe the surface of a reflection symmetric pgSPT phase built by placing an E8 state on the mirror plane. The third field theory is an O (4 ) nonlinear sigma model with a topological theta term at θ =π , or, equivalently, a noncompact CP1 model. Using a coupled wire construction, we show this is a surface theory for bosonic pgSPT phases with U (1 ) ×Z2P symmetry. For the latter two field theories, we discuss the connection to gapped surfaces with topological order. Moreover, we conjecture that the latter two field theories can describe surfaces of more general bosonic pgSPT phases with Cn v point group symmetry.

  16. Scalable Lunar Surface Networks and Adaptive Orbit Access, Phase II

    Data.gov (United States)

    National Aeronautics and Space Administration — Based on our proposed innovations and accomplished work in Phase I, we will focus on developing the new MAC protocol and hybrid routing protocol for lunar surface...

  17. Modeling and predicting chiral stationary phase enantioselectivity: An efficient random forest classifier using an optimally balanced training dataset and an aggregation strategy.

    Science.gov (United States)

    Piras, Patrick; Sheridan, Robert; Sherer, Edward C; Schafer, Wes; Welch, Christopher J; Roussel, Christian

    2018-03-01

    Predicting whether a chiral column will be effective is a daily task for many analysts. Moreover, finding the best chiral column for separating a particular racemic compound is mostly a matter of trial and error that may take up to a week in some cases. In this study we have developed a novel prediction approach based on combining a random forest classifier and an optimized discretization method for dealing with enantioselectivity as a continuous variable. Using the optimization results, models were trained on data sets divided into four enantioselectivity classes. The best model performances were achieved by over-sampling the minority classes (α ≤ 1.10 and α ≥ 2.00), down-sampling the majority class (1.2 ≤ α < 2.0), and aggregating multicategory predictions into binary classifications. We tested our method on 41 chiral stationary phases using layered fingerprints as descriptors. Experimental results show that this learning methodology was successful in terms of average area under the Receiver Operating Characteristic curve, Kappa indices and F-measure for structure-based prediction of the enantioselective behavior of 34 chiral columns. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Chiral recognition of N-phthaloyl, N-tetrachlorophthaloyl, and N-naphthaloyl α-amino acids and their esters on polysaccharide-derived chiral stationary phases.

    Science.gov (United States)

    Kim, Byoung-Hyoun; Lee, Sang Uck; Moon, Dong Cheul

    2012-12-01

    Enantiomeric separations of N-phthaloyl (N-PHT), N-tetrachlorophthaloyl (N-TCPHT), and N-naphthaloyl (N-NPHT) α-amino acids and their esters were examined on several kinds of polysaccharide-derived chiral stationary phases (CSPs). Resolution capability of CSPs was greater Chiralcel OF than the others for N-PHT and N-NPHT α-amino acids and their esters. In N-TCPHT α-amino acids and their esters, good enantioselectivities showed Chiralcel OG for N-TCPHT α-amino acids, Chiralpak AD for N-TCPHT α-amino acid methyl esters, and Chiralcel OD for N-TCPHT α-amino acid ethyl esters, respectively. From the results of liquid chromatography and computational chemistry, it is concluded that l-form is preferred and more retained with electrostatic interaction in case of interaction between N-PHT α-amino acid derivatives and Chiralcel OF, N-TCPHT α-amino acid derivatives and Chiralcel OD, and N-NPHT α-amino acid derivatives and Chiracel OF. On the other hand, d-form is preferred and more retained with van der Waals interaction in case of interaction between N-TCPHT α-amino acid ester derivatives and Chiralcel OG and Chiralpak AD. Copyright © 2012 Wiley Periodicals, Inc.

  19. Enantioseparation of α-Hydroxyallylphosphonates and Phosphonoallylic Carbonate Derivatives on Chiral Stationary Phases Using Sequential UV, Polarimetric, and Refractive Index Detection.

    Science.gov (United States)

    Hamper, Bruce C; Mannino, Michael P; Mueller, Melissa E; Harrison, Liam T; Spilling, Christopher D

    2016-09-01

    Chromatographic separation of the enantiomers of parent compounds dimethyl α-hydroxyallyl phosphonate and 1-(dimethoxyphosphoryl) allyl methyl carbonate was demonstrated by high-performance liquid chromatography (HPLC) using Chiralpak AS-H and ad-H chiral stationary phases (CSP), respectively, using a combination of UV, polarimetric, and refractive index detectors. A comparison was made of the separation efficiency and elution order of enantiomeric α-hydroxyallyl phosphonates and their carbonate derivatives on commercially available polysaccharide AS, ad, OD, IC-3, and Whelk-O 1 CSPs. In general, the α-hydroxyallyl phosphonates were resolved on the AS-H CSP, whereas the carbonate derivatives and were preferentially resolved on the ad-H CSP. The impact of aryl substitution on the resolution of analytes and was evaluated. Thermodynamic parameters determined for enantioselective adsorption hydroxyphosphonates and on the AS-H CSP and carbonate on the ad-H CSP demonstrated enthalpic control for separation of the enantiomers. Chirality 28:656-662, 2016. © 2016 Wiley Periodicals, Inc. © 2016 Wiley Periodicals, Inc.

  20. Sensitive immunoassay-based detection of Vibrio parahaemolyticus using capture and labeling particles in a stationary liquid phase lab-on-a-chip.

    Science.gov (United States)

    Park, Byunghee; Choi, Suk-Jung

    2017-04-15

    In the present study, a method was developed for detection of Vibrio parahaemolyticus based on a stationary liquid phase lab-on-a-chip (SLP LOC). The present SLP LOC comprises a sample chamber, washing chamber, and detection chamber connected by two channels. The method utilizes two types of particles: capture particles (CPs), which are magnetic nanoparticles functionalized with antibody; and labeling particles (LPs), which are silica nanoparticles functionalized with horseradish peroxidase and antibody. Samples were added to the sample chamber with CPs and LPs, forming a CP-bacteria-LP complex, and the complex was transported to the detection chamber containing chromogenic substrate solution. The method allowed the detection of V. parahaemolyticus in the range of 10 1 -10 5 cfu within 45min. Additionally, contamination of oyster samples with V. parahaemolyticus was detected within 2.5h, including 2h of culturing. The present method has the advantage of being highly rapid and facile, and enabling the detection of bacteria with high sensitivity. Moreover, the LOC and LOC processing device used in this method possess simple structures, making the detection process economical and allowing miniaturization. Therefore, the present SLP LOC detection method is potentially useful for in situ determination of food safety. Copyright © 2016 Elsevier B.V. All rights reserved.

  1. Microcanonical rates, gap times, and phase space dividing surfaces

    NARCIS (Netherlands)

    Ezra, Gregory S.; Waalkens, Holger; Wiggins, Stephen

    2009-01-01

    The general approach to classical unimolecular reaction rates due to Thiele is revisited in light of recent advances in the phase space formulation of transition state theory for multidimensional systems. Key concepts, such as the phase space dividing surface separating reactants from products, the

  2. Phase spectral composition of wind generated ocean surface waves

    Digital Repository Service at National Institute of Oceanography (India)

    Varkey, M.J.

    A study of the composition of the phase spectra of wind generated ocean surface waves is carried out using wave records collected employing a ship borne wave recorder. It is found that the raw phase spectral estimates could be fitted by the Uniform...

  3. Synthesis and evaluation of a maltose-bonded silica gel stationary phase for hydrophilic interaction chromatography and its application in Ginkgo Biloba extract separation in two-dimensional systems.

    Science.gov (United States)

    Sheng, Qianying; Yang, Kaiya; Ke, Yanxiong; Liang, Xinmiao; Lan, Minbo

    2016-09-01

    Maltose covalently bonded to silica was prepared by using carbonyl diimidazole as a cross-linker and employed as a stationary phase for hydrophilic interaction liquid chromatography. The column efficiency and the effect of water content, buffer concentration, and pH value influenced on retention were investigated. The separation or enrichment selectivity was also studied with nucleosides, saccharides, amino acids, peptides, and glycopeptides. The results indicated that the stationary phase processed good separation efficiency and separation selectivity in hydrophilic interaction liquid chromatography mode. Moreover, a two-dimensional hydrophilic interaction liquid chromatography× reversed-phase liquid chromatography method with high orthogonality was developed to analyze the Ginkgo Biloba extract fractions. The development of this two-dimensional chromatographic system would be an effective tool for the separation of complex samples of different polarities and contents. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Enantioseparation of 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate tagged amino acids and other zwitterionic compounds on cinchona-based chiral stationary phases.

    Science.gov (United States)

    Hellinger, Roland; Horak, Jeannie; Lindner, Wolfgang

    2013-10-01

    The fluorescent tag 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate (AQC; AccQ Fluor reagent kit from Waters) is a commercial N-terminal label for proteinogenic amino acids (AAs), designed for reversed-phase separation and quantification of the AA racemates. The applicability of AQC-tagged AAs and AA-type zwitterionic compounds was tested for enantiomer separation on the tert-butyl carbamate modified quinine and quinidine based chiral stationary phases, QN-AX and QD-AX employing polar-organic elution conditions. The investigated test analytes included the enantiomers of the positional isomers of isoleucine (Ile), threonine, homoserine, and 4-hydroxyproline. Furthermore, β-AAs, cyclic, and heterocyclic AAs including trans-2-amino-cyclohexane carboxylic acid and trans-2-aminocyclohexyl sulfonic acid, phenylalanine derivatives substituted with halides with increasing electronegativity and 3,4-dihydroxyphenylalanine, cysteine-related derivatives including homocysteic acid, methionine sulfone, cysteine-S-acetic acid, and cysteine-S-acetamide as well as a small range of aminophosphonic acids were enantioseparated. A mechanistic interaction study of AQC-AAs in comparison with fluoresceine isothiocyanate-labeled AAs was performed. The chiral and chemoselective recognition processes involved in enantiomer separation and retention was systematically discussed. Special emphasis was set on the influential factors exhibited by the chemistry, branching position, and spatial properties of the investigated zwitterionic analytes. The general interest to separate and distinguish between different types of branched-chained AAs and metabolic side products thereof lies in the toxicity of some of these compounds, which makes for instance allo-Ile an attractive candidate in disease-related biomarker research.

  5. C₁₈-bound porous silica monolith particles as a low-cost high-performance liquid chromatography stationary phase with an excellent chromatographic performance.

    Science.gov (United States)

    Ali, Faiz; Cheong, Won Jo

    2014-12-01

    Ground porous silica monolith particles with an average particle size of 2.34 μm and large pores (363 Å) exhibiting excellent chromatographic performance have been synthesized on a relatively large scale by a sophisticated sol-gel procedure. The particle size distribution was rather broad, and the d(0.1)/d(0.9) ratio was 0.14. The resultant silica monolith particles were chemically modified with chlorodimethyloctadecylsilane and end-capped with a mixture of hexamethyldisilazane and chlorotrimethylsilane. Very good separation efficiency (185,000/m) and chromatographic resolution were achieved when the C18 -bound phase was evaluated for a test mixture of five benzene derivatives after packing in a stainless-steel column (1.0 mm × 150 mm). The optimized elution conditions were found to be 70:30 v/v acetonitrile/water with 0.1% trifluoroacetic acid at a flow rate of 25 μL/min. The column was also evaluated for fast analysis at a flow rate of 100 μL/min, and all the five analytes were eluted within 3.5 min with reasonable efficiency (ca. 60,000/m) and resolution. The strategy of using particles with reduced particle size and large pores (363 Å) combined with C18 modification in addition to partial-monolithic architecture has resulted in a useful stationary phase (C18 -bound silica monolith particles) of low production cost showing excellent chromatographic performance. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Comparison of high-accuracy numerical simulations of black-hole binaries with stationary-phase post-Newtonian template waveforms for initial and advanced LIGO

    International Nuclear Information System (INIS)

    Boyle, Michael; Brown, Duncan A; Pekowsky, Larne

    2009-01-01

    We study the effectiveness of stationary-phase approximated post-Newtonian waveforms currently used by ground-based gravitational-wave detectors to search for the coalescence of binary black holes by comparing them to an accurate waveform obtained from numerical simulation of an equal-mass non-spinning binary black hole inspiral, merger and ringdown. We perform this study for the initial- and advanced-LIGO detectors. We find that overlaps between the templates and signal can be improved by integrating the match filter to higher frequencies than used currently. We propose simple analytic frequency cutoffs for both initial and advanced LIGO, which achieve nearly optimal matches, and can easily be extended to unequal-mass, spinning systems. We also find that templates that include terms in the phase evolution up to 3.5 post-Newtonian (pN) order are nearly always better, and rarely significantly worse, than 2.0 pN templates currently in use. For initial LIGO we recommend a strategy using templates that include a recently introduced pseudo-4.0 pN term in the low-mass (M ≤ 35 M o-dot ) region, and 3.5 pN templates allowing unphysical values of the symmetric reduced mass η above this. This strategy always achieves overlaps within 0.3% of the optimum, for the data used here. For advanced LIGO we recommend a strategy using 3.5 pN templates up to M = 12 M o-dot , 2.0 pN templates up to M = 21 M o-dot , pseudo-4.0 pN templates up to 65 M o-dot , and 3.5 pN templates with unphysical η for higher masses. This strategy always achieves overlaps within 0.7% of the optimum for advanced LIGO.

  7. I. Diamino telechelic polybutadienes: Synthesis, characterization and melt coupling. II. Poly(epsilon-caprolactone-beta-poly(ethylene glycol) polymeric nanoparticles for drug delivery. III. Zirconia based cellulosic HPLC chiral stationary phase for enantioseparations

    Science.gov (United States)

    Ji, Shengxiang

    surfaces was measured and ˜51-67% conjugation was obtained. Chemical modification of celluloses leads to the production of high value-added materials. Phosphonic acid, carboxylic acid, and methacrylate functionalized carbamate celluloses were synthesized through direct alkylation of carbamate celluloses. These functionalized carbamate celluloses were then deposited on zirconia particles, which were used as chiral stationary phases for HPLC. The separation and retention factors of columns packed by cellulose coated zirconia were evaluated on thirteen pairs of racemates. The results were also compared with the results of a commercial cellulosic silica column under same test conditions.

  8. Phase diagram for droplet impact on superheated surfaces

    NARCIS (Netherlands)

    Staat, Erik-Jan; Tran, Tuan; Geerdink, B.M.; Riboux, G.; Sun, Chao; Gordillo, J.M.; Lohse, Detlef

    2015-01-01

    We experimentally determine the phase diagram for impacting ethanol droplets on a smooth, sapphire surface in the parameter space of Weber number We versus surface temperature T. We observe two transitions, namely the one towards splashing (disintegration of the droplet) with increasing We, and the

  9. [[Chiral separation of five arylpropionic acid drugs and determination of their enantiomers in pharmaceutical preparations by reversed-phase high performance liquid chromatography with cellulose-tris-(4-methylbenzoate) stationary phase

    Science.gov (United States)

    Luo, An; Wan, Qiang; Fan, Huajun; Chen, Zhi; Wu, Xuehao; Huang, Xiaowen; Zang, Linquan

    2014-09-01

    Chromatographic behaviors for enantiomeric separation of arylpropionic acid drugs were systematically developed by reversed phase-high performance liquid chromatography (RP-HPLC) using cellulose-tris-(4-methylbenzoate) (CTMB) as chiral stationary phase (CSP). The effects of the composition of the mobile phase, additives and temperature on chiral separation of flurbiprofen, pranoprofen, naproxen, ibuprofen and loxoprofen were further investigated. The enantiomers had been successfully separated on CSP of CTMB by the mobile phase of methanol-0.1% (v/v) formic acid except naproxen by acetonitrile-0.1% (v/v) formic acid at 25 °C. The mechanisms of the racemic resolution for the above mentioned five drugs are discussed thermodynamically and structurally. The resolutions between respective enantiomers for arylpropionic acid drugs on CTMB had significant differences due to their chromatographic behaviors. The order of resolutions ranked pranoprofen, loxoprofen, flurbiprofen, ibuprofen and naproxen. The method established has been successfully applied to the determination of the enantiomers of the five drugs in commercial preparations under the optimized conditions. It proved that the method is simple, reliable and accurate.

  10. Surface Plasmons Carry the Pancharatnam-Berry Geometric Phase

    Science.gov (United States)

    Daniel, Salman; Saastamoinen, Kimmo; Saastamoinen, Toni; Vartiainen, Ismo; Friberg, Ari T.; Visser, Taco D.

    2017-12-01

    Surface plasmon polaritons (SPPs) are electromagnetic surface waves that travel along the boundary of a metal and a dielectric medium. They can be generated when freely propagating light is scattered by structural metallic features such as gratings or slits. In plasmonics, SPPs are manipulated, amplified, or routed before being converted back into light by a second scattering event. In this process, the light acquires a dynamic phase and perhaps an additional geometric phase associated with polarization changes. We examine the possibility that SPPs mediate the Pancharatnam-Berry phase, which follows from a closed path of successive in-phase polarization-state transformations on the Poincaré sphere and demonstrate that this is indeed the case. The geometric phase is shown to survive the light →SPP →light process and, moreover, its magnitude agrees with Pancharatnam's rule. Our findings are fundamental in nature and highly relevant for photonics applications.

  11. Wide-range high-resolution transmission electron microscopy reveals morphological and distributional changes of endomembrane compartments during log to stationary transition of growth phase in tobacco BY-2 cells.

    Science.gov (United States)

    Toyooka, Kiminori; Sato, Mayuko; Kutsuna, Natsumaro; Higaki, Takumi; Sawaki, Fumie; Wakazaki, Mayumi; Goto, Yumi; Hasezawa, Seiichiro; Nagata, Noriko; Matsuoka, Ken

    2014-09-01

    Rapid growth of plant cells by cell division and expansion requires an endomembrane trafficking system. The endomembrane compartments, such as the Golgi stacks, endosome and vesicles, are important in the synthesis and trafficking of cell wall materials during cell elongation. However, changes in the morphology, distribution and number of these compartments during the different stages of cell proliferation and differentiation have not yet been clarified. In this study, we examined these changes at the ultrastructural level in tobacco Bright yellow 2 (BY-2) cells during the log and stationary phases of growth. We analyzed images of the BY-2 cells prepared by the high-pressure freezing/freeze substitution technique with the aid of an auto-acquisition transmission electron microscope system. We quantified the distribution of secretory and endosomal compartments in longitudinal sections of whole cells by using wide-range gigapixel-class images obtained by merging thousands of transmission electron micrographs. During the log phase, all Golgi stacks were composed of several thick cisternae. Approximately 20 vesicle clusters (VCs), including the trans-Golgi network and secretory vesicle cluster, were observed throughout the cell. In the stationary-phase cells, Golgi stacks were thin with small cisternae, and only a few VCs were observed. Nearly the same number of multivesicular body and small high-density vesicles were observed in both the stationary and log phases. Results from electron microscopy and live fluorescence imaging indicate that the morphology and distribution of secretory-related compartments dramatically change when cells transition from log to stationary phases of growth. © The Author 2014. Published by Oxford University Press on behalf of Japanese Society of Plant Physiologists. All rights reserved. For permissions, please email: journals.permissions@oup.com.

  12. Temperature dependences of the retention indices of mono- and polyethylene glycol acetals and ethers on stationary phase DB-1 and enthalpies of their sorption from the gas phase

    Science.gov (United States)

    Zhabina, A. A.; Krasnykh, E. L.

    2017-12-01

    Gas chromatography is used to study the sorption characteristics and retention of a series of mono-, di-, and triethylene glycol ethers on nonpolar phase DB-1 in the temperature range of 70-180°C. Temperature dependences of the retention indices of the compounds are obtained and their linear character in the investigated range of temperatures is demonstrated. The enthalpies of sorption of the investigated compounds are calculated and analyzed, based on the temperature dependences of the retention factors.

  13. TLC-MS versus TLC-LC-MS fingerprints of herbal extracts. Part III. Application of the reversed-phase liquid chromatography systems with C18 stationary phase.

    Science.gov (United States)

    Sajewicz, Mieczysław; Staszek, Dorota; Natic, Maja; Waksmundzka-Hajnos, Monika; Kowalska, Teresa

    2011-08-01

    In the previous paper from this series, we proposed mass spectrometric fingerprinting of complex botanical samples upon the examples of the pharmacologically important phenolic acids and flavonoids selectively extracted from Salvia lavandulifolia. In this study, we explore fingerprinting efficiency with a novel two-dimensional analytical system composed of the reversed-phase thin-layer chromatography and the reversed-phase high performance liquid chromatography with mass spectrometric detection (2D RP-TLC-RP-LC-MS). We also compare its efficiency with that of the one-dimensional analytical system (the reversed-phase thin-layer chromatography with mass spectrometric detection; 1D RP-TLC-MS). As our present study is basically focused on the method development, we considered it as justified to carry out our comparison with the phenolic acid extracts selectively derived from the Salvia lavandulifolia species, similar as it was done in Part II from this series. Upon the results obtained, it was established that the 1D RP-TLC-MS mode and the 2D RP-TLC-RP-LC-MS mode can be applied to fingerprinting of herbal extracts, and that the 2D RP-TLC-RP-LC mode can provide a more abundant information than that originating from the 1D RP-TLC mode.

  14. Gene encoding gamma-carbonic anhydrase is cotranscribed with argC and induced in response to stationary phase and high CO2 in Azospirillum brasilense Sp7.

    Science.gov (United States)

    Kaur, Simarjot; Mishra, Mukti N; Tripathi, Anil K

    2010-07-04

    Carbonic anhydrase (CA) is a ubiquitous enzyme catalyzing the reversible hydration of CO2 to bicarbonate, a reaction underlying diverse biochemical and physiological processes. Gamma class carbonic anhydrases (gamma-CAs) are widespread in prokaryotes but their physiological roles remain elusive. At present, only gamma-CA of Methanosarcina thermophila (Cam) has been shown to have CA activity. Genome analysis of a rhizobacterium Azospirillum brasilense, revealed occurrence of ORFs encoding one beta-CA and two gamma-CAs. One of the putative gamma-CA encoding genes of A. brasilense was cloned and overexpressed in E. coli. Electrometric assays for CA activity of the whole cell extracts overexpressing recombinant GCA1 did not show CO2 hydration activity. Reverse transcription-PCR analysis indicated that gca1 in A. brasilense is co-transcribed with its upstream gene annotated as argC, which encodes a putative N-acetyl-gamma-glutamate-phosphate reductase. 5'-RACE also demonstrated that there was no transcription start site between argC and gca1, and the transcription start site located upstream of argC transcribed both the genes (argC-gca1). Using transcriptional fusions of argC-gca1 upstream region with promoterless lacZ, we further demonstrated that gca1 upstream region did not have any promoter and its transcription occurred from a promoter located in the argC upstream region. The transcription of argC-gca1 operon was upregulated in stationary phase and at elevated CO2 atmosphere. This study shows lack of CO2 hydration activity in a recombinant protein expressed from a gene predicted to encode a gamma-carbonic anhydrase in A. brasilense although it cross reacts with anti-Cam antibody raised against a well characterized gamma-CA. The organization and regulation of this gene along with the putative argC gene suggests its involvement in arginine biosynthetic pathway instead of the predicted CO2 hydration.

  15. Synthesis of Optically Active Poly(diphenylacetylenes Using Polymer Reactions and an Evaluation of Their Chiral Recognition Abilities as Chiral Stationary Phases for HPLC

    Directory of Open Access Journals (Sweden)

    Katsuhiro Maeda

    2016-11-01

    Full Text Available A series of optically active poly(diphenylacetylene derivatives bearing a chiral substituent (poly-2S or chiral and achiral substituents (poly-(2Sx-co-31−x on all of their pendant phenyl rings were synthesized by the reaction of poly(bis(4-carboxyphenylacetylene with (S-1-phenylethylamine ((S-2 or benzylamine (3 in the presence of a condensing reagent. Their chiroptical properties and chiral recognition abilities as chiral stationary phases (CSPs for high-performance liquid chromatography (HPLC were investigated. Poly-2S and poly-(2Sx-co-31−x (0.06 < x < 0.71 formed a preferred-handed helical conformation with opposite helical senses after thermal annealing despite possessing the same chiral pendant (h-poly-2S and h-poly-(2Sx-co-31−x. Furthermore, h-poly-2S and h-poly-(2S0.36-co-30.64 emitted circularly polarized luminescence with opposite signs. h-Poly-2S showed higher chiral recognition abilities toward a larger number of racemates than poly-2S without a preferred-handed helicity and the previously reported preferred-handed poly(diphenylacetylene derivative bearing the same chiral substituent on half of its pendant phenyl rings. h-Poly-(2S0.36-co-30.64 also exhibited good chiral recognition abilities toward several racemates, though the elution order of some enantiomers was reversed compared with h-poly-2S.

  16. PlcRa, a new quorum-sensing regulator from Bacillus cereus, plays a role in oxidative stress responses and cysteine metabolism in stationary phase.

    Science.gov (United States)

    Huillet, Eugénie; Tempelaars, Marcel H; André-Leroux, Gwenaëlle; Wanapaisan, Pagakrong; Bridoux, Ludovic; Makhzami, Samira; Panbangred, Watanalai; Martin-Verstraete, Isabelle; Abee, Tjakko; Lereclus, Didier

    2012-01-01

    We characterized a new quorum-sensing regulator, PlcRa, which is present in various members of the B. cereus group and identified a signaling heptapeptide for PlcRa activity: PapRa(7). We demonstrated that PlcRa is a 3D structural paralog of PlcR using sequence analysis and homology modeling. A comparison of the transcriptomes at the onset of stationary phase of a ΔplcRa mutant and the wild-type B. cereus ATCC 14579 strain showed that 68 genes were upregulated and 49 genes were downregulated in the ΔplcRa mutant strain (>3-fold change). Genes involved in the cysteine metabolism (putative CymR regulon) were downregulated in the ΔplcRa mutant strain. We focused on the gene with the largest difference in expression level between the two conditions, which encoded -AbrB2- a new regulator of the AbrB family. We demonstrated that purified PlcRa bound specifically to the abrB2 promoter in the presence of synthetic PapRa(7), in an electrophoretic mobility shift assay. We further showed that the AbrB2 regulator controlled the expression of the yrrT operon involved in methionine to cysteine conversion. We found that the ΔplcRa mutant strain was more sensitive to hydrogen peroxide- and disulfide-induced stresses than the wild type. When cystine was added to the culture of the ΔplcRa mutant, challenged with hydrogen peroxide, growth inhibition was abolished. In conclusion, we identified a new RNPP transcriptional regulator in B. cereus that activated the oxidative stress response and cysteine metabolism in transition state cells.

  17. PlcRa, a new quorum-sensing regulator from Bacillus cereus, plays a role in oxidative stress responses and cysteine metabolism in stationary phase.

    Directory of Open Access Journals (Sweden)

    Eugénie Huillet

    Full Text Available We characterized a new quorum-sensing regulator, PlcRa, which is present in various members of the B. cereus group and identified a signaling heptapeptide for PlcRa activity: PapRa(7. We demonstrated that PlcRa is a 3D structural paralog of PlcR using sequence analysis and homology modeling. A comparison of the transcriptomes at the onset of stationary phase of a ΔplcRa mutant and the wild-type B. cereus ATCC 14579 strain showed that 68 genes were upregulated and 49 genes were downregulated in the ΔplcRa mutant strain (>3-fold change. Genes involved in the cysteine metabolism (putative CymR regulon were downregulated in the ΔplcRa mutant strain. We focused on the gene with the largest difference in expression level between the two conditions, which encoded -AbrB2- a new regulator of the AbrB family. We demonstrated that purified PlcRa bound specifically to the abrB2 promoter in the presence of synthetic PapRa(7, in an electrophoretic mobility shift assay. We further showed that the AbrB2 regulator controlled the expression of the yrrT operon involved in methionine to cysteine conversion. We found that the ΔplcRa mutant strain was more sensitive to hydrogen peroxide- and disulfide-induced stresses than the wild type. When cystine was added to the culture of the ΔplcRa mutant, challenged with hydrogen peroxide, growth inhibition was abolished. In conclusion, we identified a new RNPP transcriptional regulator in B. cereus that activated the oxidative stress response and cysteine metabolism in transition state cells.

  18. Determination of pore size distributions in capillary-channeled polymer fiber stationary phases by inverse size-exclusion chromatography and implications for fast protein separations.

    Science.gov (United States)

    Wang, Zhengxin; Marcus, R Kenneth

    2014-07-18

    Capillary-channeled polymer (C-CP) fibers have been utilized as liquid chromatography stationary phases, primarily for biomacromolecule separations on the analytical and preparative scales. The collinear packing of the eight-channeled C-CP fibers provides for very efficient flow, allowing operation at high linear velocity (u>100mm s(-1)) and low backpressure (chromatography (iSEC) has been employed to determine the pore size distribution (PSD) within C-CP fibers. A diversity of test species (from metal ions to large proteins) was used as probes under non-retaining conditions to obtain a response curve reflecting the apparent partition coefficient (Kd) versus hydrodynamic radii (rm). A mean pore radius (rp) of 4.2nm with standard deviation (sp) of ±1.1nm was calculated by fitting the Kd versus rm data to model equations with a Gaussian pore size distribution, and a pore radius of 4.0±0.1nm was calculated based on a log-normal distribution. The derived mean pore radius is much smaller than traditional support materials, with the standard deviation showing a relatively uniform pore distribution. van Deemter plots were analyzed to provide practical confirmation of the structural implications. Large molecules (e.g., proteins) that are fully excluded from pores have no significant C-terms in the van Deemter plots whereas small molecules that can access the pore volumes display appreciable C-terms, as expected. Fitting of retention data to the Knox equation suggests that the columns operate with a characteristic particle diameter (dp) of ∼53μm. Copyright © 2014 Elsevier B.V. All rights reserved.

  19. A chemometric approach to determine the phenolic compounds in different barley samples by two different stationary phases: a comparison between C18 and pentafluorophenyl core shell columns.

    Science.gov (United States)

    Gómez-Caravaca, Ana María; Verardo, Vito; Berardinelli, Annachiara; Marconi, Emanuele; Caboni, Maria Fiorenza

    2014-08-15

    Barley (Hordeum vulgare L.) is a cereal crop that has been cultivated since ancient times. However, its interest as nutritional food and as food ingredient is relatively new. Thus, in this study, the phenolic compounds of eighteen different varieties of barley (4 waxy and 14 non-waxy) grown under the same agronomic conditions in the same experimental field have been determined by HPLC-DAD-MS. Two new methodologies were developed using new generation superficially porous HPLC columns with different stationary phases: C18 and pentafluorophenyl (PFP). Twelve free phenolic compounds and eight bound phenolic compounds could be identified in barley samples in less than 22min. The study of different method parameters showed that C18 column was more suitable for the analysis of phenolic compounds of barley. Hierarchical cluster analysis (HCA) was conducted in order to assess the different ability of the two different core shell HPLC columns in the discrimination between "waxy" and "non-waxy" varieties, and only HCA of C18 column could separate waxy and non-waxy genotypes. Significant differences in the content of phenolic compounds between waxy and non-waxy samples were found, being waxy barley samples the ones which presented higher content of free and bound phenolic compounds. Once the best discriminant HPLC column was established, principal component analysis (PCA) was applied and it was able to discriminate between "waxy" and "non-waxy" varieties; however it discriminated the barley samples based only in free phenolic compounds. Because of that, partial least squares discriminant analysis (PLS-DA) and Artificial Neural Networks (ANN) were carried out. PLS-DA and ANN permitted the classification of waxy and non-waxy genotypes from both free and bound phenolic compounds. Copyright © 2014 Elsevier B.V. All rights reserved.

  20. Group separation of transplutonium and rare earth elements by liquid chromatography with free stationary phase using 2,4,6-tris[ditolylphosphoryl] - 1,3,5 - triazine as extractant

    International Nuclear Information System (INIS)

    Chmutova, M.K.; Ivanova, L.A.; Bodrin, G.B.; Polikarpov, Yu.M.; Myasoedov, B.F.

    1994-01-01

    Methods of group separation of trace amounts of transplutonium elements (TPE) and weight amounts of rare earth elements (REE) in the systems on the basis of bifunctional neutral organophosphoric compounds by the method of liquid chromatography with a free stationary phase have been developed. When solution of 2,4,6 - tris[ditolylphosphoryl] - 1,3,5 - triazine in chloroform was used as stationary phase, REE were the first to be washed out by 0.5 mol/l NH 4 SCN-1 mol/l HCl solution, then TPE - by 0.025 mol/l of oxyethylidenediphosphonic acid in water. the fractions contained about 100% of one of the groups without impurity of the other. 7 refs.; 6 figs

  1. iTRAQ quantitative analysis of Francisella tularensis ssp. holarctica live vaccine strain and Francisella tularensis ssp. tularensis SCHU S4 response to different temperatures and stationary phases of growth.

    Science.gov (United States)

    Lenco, Juraj; Link, Marek; Tambor, Vojtech; Zaková, Jitka; Cerveny, Lukas; Stulik, And Jiri

    2009-05-01

    Proteomics has been shown to significantly contribute to the investigation of the pathogenicity of the extremely infectious bacteria Francisella tularensis. In this study, the authors employed iTRAQ quantitative proteomic analysis in order to monitor alterations in proteomes of F. tularensis ssp. holarctica live vaccine strain and F. tularensis ssp. tularensis SCHU S4 associated with the cultivation at different temperatures or in the stationary phase. Correlated production of the identified proteins studied by the exploratory statistical analysis revealed novel candidates for virulence factors that were regulated in a similar manner to the genes encoded in the Francisella Pathogenicity Island. Moreover, the assessment of the adaptation of live vaccine strain and SCHU S4 strain to the examined stimuli uncovered differences in their physiological responses to the stationary phase of growth.

  2. X-Ray Studies of Phase Transitions on Surfaces

    DEFF Research Database (Denmark)

    Als-Nielsen, Jens Aage

    1984-01-01

    The density variation across the surface from vapor to liquid in liquid crystal materials has been measured in the isotropic, nematic and smectic A phases by specular reflection of X rays with grazing angles from θc to θB (total reflection angle and Bragg angle for smectic A layering, respectively......) using synchroton X-rays in HASYLAB, Hamburg. Crystalline surface structures may be deduced from X-ray diffraction, utilizing the evanescent beam occuring for grazing angles less than θc to obtain surface sensitivity. Results from the reconstruction of Au(110) surface are reviewed....

  3. Phase transitions and adsorbate restructuring at metal surface

    CERN Document Server

    King, DA

    1994-01-01

    The objective in initiating this series in 1980 was to provide an in-depth review of advances made in the understanding key aspects of surface chemistry and physics through the application of new techniques to the study of well-defined surfaces. Since then the field of surface science has greatly matured, and further important techniques, particularly scanning probe microscopies, have been successfully assimilated into the applications armoury of the surface scientist. The present volume is a series of timely reviews by many of the current experts in the field of phase transitions an

  4. Multi-phase-field method for surface tension induced elasticity

    Science.gov (United States)

    Schiedung, Raphael; Steinbach, Ingo; Varnik, Fathollah

    2018-01-01

    A method, based on the multi-phase-field framework, is proposed that adequately accounts for the effects of a coupling between surface free energy and elastic deformation in solids. The method is validated via a number of analytically solvable problems. In addition to stress states at mechanical equilibrium in complex geometries, the underlying multi-phase-field framework naturally allows us to account for the influence of surface energy induced stresses on phase transformation kinetics. This issue, which is of fundamental importance on the nanoscale, is demonstrated in the limit of fast diffusion for a solid sphere, which melts due to the well-known Gibbs-Thompson effect. This melting process is slowed down when coupled to surface energy induced elastic deformation.

  5. Differences in stationary-phase cells of a commercial Saccharomyces cerevisiae wine yeast grown in aerobic and microaerophilic batch cultures assessed by electric particle analysis, light diffraction and flow cytometry.

    Science.gov (United States)

    Portell, X; Ginovart, M; Carbó, R; Vives-Rego, J

    2011-01-01

    We applied electric particle analysis, light diffraction and flow cytometry to obtain information on the morphological changes during the stationary phase of Saccharomyces cerevisiae. The reported analyses of S. cerevisiae populations were obtained under two different conditions, aerobic and microaerophilic, at 27°C. The samples analysed were taken at between 20 and 50 h from the beginning of culture. To assist in the interpretation of the observed distributions a complexity index was used. The aerobically grown culture reached significantly greater cell density. Under these conditions, the cell density experienced a much lower reduction (3%) compared with the microaerophilic conditions (30%). Under aerobic conditions, the mean cell size determined by both electric particle analysis and light diffraction was lower and remained similar throughout the experiment. Under microaerophilic conditions, the mean cell size determined by electric particle analysis decreased slightly as the culture progressed through the stationary phase. Forward and side scatter distributions revealed two cell subpopulations under both growth conditions. However, in the aerobic growing culture the two subpopulations were more separated and hence easier to distinguish. The distributions obtained with the three experimental techniques were analysed using the complexity index. This analysis suggested that a complexity index is a good descriptor of the changes that take place in a yeast population in the stationary phase, and that it aids in the discussion and understanding of the implications of these distributions obtained by these experimental techniques.

  6. Ultra high phase sensitive surface plasmon resonance biosensor

    Science.gov (United States)

    Li, Ying-Chang; Chou, Chien

    2009-02-01

    This study demonstrates a novel phase-sensitive surface plasman resonance biosensor (PS-SPRB) which is able to convert the phase modulation into amplitude modulation analytically via a differential amplifier. PS-SPRB is able to measure biomolecule interactions at ultra-low concentration relying on the properties of phase sensitive detection at shot-noise detection in a real-time. The common-phase noise-rejection mode is provided in PS-SPRB to be able to immune the background phase noise efficiently. The experimental results confirm the detection sensitivity of 0.00001 wt % concentration of sucrose solution and 10 fg/ml mouse IgG interaction with anti IgG in real time.

  7. Formation, transformation and dissolution of phases formed on surfaces

    International Nuclear Information System (INIS)

    Shoesmith, D.W.

    1983-03-01

    The basic mechanisms of film growth, transformation, and dissolution of phases formed on surfaces are discussed. Film growth can occur via solid-state processes or via substrate (usally metal or alloy) dissolution, followed by local supersaturation and precipitation of an insoluble phase. The phase(s) formed may be metastable and transform to a more stable phase, via either solid-state or dissolution-reprecipitation processes. Film dissolution reactions can also occur via a variety of mechanisms, including: (i) direct chemical dissolution when no oxidation state change occurs; (ii) redox dissolution when the film dissolves via a redox reaction involving a reducing or oxidizing agent in solution; and (iii) autoreduction, where film dissolution is coupled to metal dissolution. Such film-growth and dissolution processes, which often produce complex multilayer films, are common in the nuclear industry. A number of examples are discussed

  8. Gene encoding γ-carbonic anhydrase is cotranscribed with argC and induced in response to stationary phase and high CO2 in Azospirillum brasilense Sp7

    Science.gov (United States)

    2010-01-01

    Background Carbonic anhydrase (CA) is a ubiquitous enzyme catalyzing the reversible hydration of CO2 to bicarbonate, a reaction underlying diverse biochemical and physiological processes. Gamma class carbonic anhydrases (γ-CAs) are widespread in prokaryotes but their physiological roles remain elusive. At present, only γ-CA of Methanosarcina thermophila (Cam) has been shown to have CA activity. Genome analysis of a rhizobacterium Azospirillum brasilense, revealed occurrence of ORFs encoding one β-CA and two γ-CAs. Results One of the putative γ-CA encoding genes of A. brasilense was cloned and overexpressed in E. coli. Electrometric assays for CA activity of the whole cell extracts overexpressing recombinant GCA1 did not show CO2 hydration activity. Reverse transcription-PCR analysis indicated that gca1 in A. brasilense is co-transcribed with its upstream gene annotated as argC, which encodes a putative N-acetyl-γ-glutamate-phosphate reductase. 5'-RACE also demonstrated that there was no transcription start site between argC and gca1, and the transcription start site located upstream of argC transcribed both the genes (argC-gca1). Using transcriptional fusions of argC-gca1 upstream region with promoterless lacZ, we further demonstrated that gca1 upstream region did not have any promoter and its transcription occurred from a promoter located in the argC upstream region. The transcription of argC-gca1 operon was upregulated in stationary phase and at elevated CO2 atmosphere. Conclusions This study shows lack of CO2 hydration activity in a recombinant protein expressed from a gene predicted to encode a γ-carbonic anhydrase in A. brasilense although it cross reacts with anti-Cam antibody raised against a well characterized γ-CA. The organization and regulation of this gene along with the putative argC gene suggests its involvement in arginine biosynthetic pathway instead of the predicted CO2 hydration. PMID:20598158

  9. Gene encoding γ-carbonic anhydrase is cotranscribed with argC and induced in response to stationary phase and high CO2 in Azospirillum brasilense Sp7

    Directory of Open Access Journals (Sweden)

    Mishra Mukti N

    2010-07-01

    Full Text Available Abstract Background Carbonic anhydrase (CA is a ubiquitous enzyme catalyzing the reversible hydration of CO2 to bicarbonate, a reaction underlying diverse biochemical and physiological processes. Gamma class carbonic anhydrases (γ-CAs are widespread in prokaryotes but their physiological roles remain elusive. At present, only γ-CA of Methanosarcina thermophila (Cam has been shown to have CA activity. Genome analysis of a rhizobacterium Azospirillum brasilense, revealed occurrence of ORFs encoding one β-CA and two γ-CAs. Results One of the putative γ-CA encoding genes of A. brasilense was cloned and overexpressed in E. coli. Electrometric assays for CA activity of the whole cell extracts overexpressing recombinant GCA1 did not show CO2 hydration activity. Reverse transcription-PCR analysis indicated that gca1 in A. brasilense is co-transcribed with its upstream gene annotated as argC, which encodes a putative N-acetyl-γ-glutamate-phosphate reductase. 5'-RACE also demonstrated that there was no transcription start site between argC and gca1, and the transcription start site located upstream of argC transcribed both the genes (argC-gca1. Using transcriptional fusions of argC-gca1 upstream region with promoterless lacZ, we further demonstrated that gca1 upstream region did not have any promoter and its transcription occurred from a promoter located in the argC upstream region. The transcription of argC-gca1 operon was upregulated in stationary phase and at elevated CO2 atmosphere. Conclusions This study shows lack of CO2 hydration activity in a recombinant protein expressed from a gene predicted to encode a γ-carbonic anhydrase in A. brasilense although it cross reacts with anti-Cam antibody raised against a well characterized γ-CA. The organization and regulation of this gene along with the putative argC gene suggests its involvement in arginine biosynthetic pathway instead of the predicted CO2 hydration.

  10. Simultaneous determination of clobutinol hydrochloride and doxylamine succinate from syrups by RP HPLC using a new stationary phase containing embedded urea polar groups

    Directory of Open Access Journals (Sweden)

    Paulo Cesar Pires Rosa

    2012-06-01

    Full Text Available A new, simple, fast, reproducible and sensitive reversed phase HPLC method, using a new stationary phase containing embedded urea polar groups, has been developed and validated for the simultaneous determination of clobutinol hydrochloride (CLO and doxylamine succinate (DOX in syrups. The determination was carried out on a C8 urea column (125 mm x 3.9 mm i.d., 5 µm particle size synthetized at the Liquid Chomatography Laboratory (LabCrom of the Chemistry Institute of Unicamp. The mobile phase consisted of a mixture of acetonitrile:methanol:phosphate buffer (pH 2.5 in the gradient mode. The diode array detector (DAD was operated at 230 nm for CLO and 262 nm for DOX. The method showed adequate precision, with relative standard deviations (RSD less than 1%. The presence of the excipients did not interfere in the results of the analysis. Accuracy was determined by adding standards of the drugs to a placebo and good recovery values were obtained. The analytical curves were linear (r² 0.9999 for CLO and 0.9998 for DOX over a wide concentration range (2.4-336 µg mL-1 for CLO and 2.3-63 µg mL-1 for DOX. The solutions were stable for at least 72 hours at room temperature. The criteria for validation using the ICH guidelines were fulfilled.Um novo método simples, fácil e reprodutível, de fase reversa para CLAE, usando uma fase estacionária contendo um grupo polar, uréia, embutido, foi desenvolvido e validado para determinação simultânea de cloridrato de clobutinol (CLO e succinato de doxilamina (DOX em xarope. A determinação foi realizada em uma coluna C8 uréia (125 mm x 3,9 mm d.i., 5 µm tamanho de partícula sintetizada em nosso laboratório (LabCrom. A fase móvel consistiu de mistura de acetonitrila:metanol:tampão fosfato pH 2,5, em eluição por gradiente. O detector por arranjos de diodo (DAD foi utilizado a 230 nm para CLO e a 262 nm para DOX. O método apresentou precisão adequada, com desvio padrão relativo menor que 1%. A

  11. Orientation of liquid crystalline blue phases on unidirectionally orienting surfaces

    Science.gov (United States)

    Takahashi, Misaki; Ohkawa, Takuma; Yoshida, Hiroyuki; Fukuda, Jun-ichi; Kikuchi, Hirostugu; Ozaki, Masanori

    2018-03-01

    Liquid crystalline cholesteric blue phases (BPs) continue to attract interest due to their fast response times and quasi-polarization-independent phase modulation capabilities. Various approaches have recently been proposed to control the crystal orientation of BPs on substrates; however, their basic orientation properties on standard, unidirectionally orienting alignment layers have not been investigated in detail. Through analysis of the azimuthal orientation of Kossel diagrams, we study the 3D crystal orientation of a BP material—with a phase sequence of cholesteric, BP I, and BP II—on unidirectionally orienting surfaces prepared using two methods: rubbing and photoalignment. BP II grown from the isotropic phase is sensitive to surface conditions, with different crystal planes orienting on the two substrates. On the other hand, strong thermal hysteresis is observed in BPs grown through a different liquid crystal phase, implying that the preceding structure determines the orientation. More specifically, the BP II–I transition is accompanied by a rotation of the crystal such that the crystal direction defined by certain low-value Miller indices transform into different directions, and within the allowed rotations, different azimuthal configurations are obtained in the same cell depending on the thermal process. Our findings demonstrate that, for the alignment control of BPs, the thermal process is as important as the properties of the alignment layer.

  12. Surface magnetic phase transitions in Dy/Lu superlattices

    International Nuclear Information System (INIS)

    Goff, J.P.; Sarthour, R.S.; Micheletti, C.; Langridge, S.; Wilkins, C.J.T.; Ward, R.C.C.; Wells, M.R.

    1999-01-01

    Dy/Lu superlattices comprising ferromagnetic Dy blocks coupled antiferromagnetically across the Lu blocks may be modelled as a chain of XY spins with antiferromagnetic exchange and six-fold anisotropy. We have calculated the stable magnetic phases for the cases of large anisotropy and a field applied along an easy direction. For an infinite chain an intermediate phase (1, 5,...) is predicted, where the notation gives the angle between the moment and the applied field in units of π/3. Furthermore, the effects of surface reconstruction are determined for finite chains. A [Dy 20 Lu 12 ] 20 superlattice has been studied using bulk magnetization and polarized neutron reflectivity. The (1, 5,...) phase has been identified and the results provide direct evidence in support of the theoretical predictions. Dipolar forces are shown to account for the magnitude of the observed exchange coupling. (Copyright (c) 1999 Elsevier Science B.V., Amsterdam. All rights reserved.)

  13. Berry's phase, chaos, and the deformations of Riemann surfaces

    Science.gov (United States)

    Lévay, Péter

    1997-11-01

    Parametrized families of Landau Hamiltonians on compact Riemann surfaces corresponding to classically chaotic families of geodesic motion are investigated. The parameters describe deformations of such surfaces with genus g>=1. It is shown that the adiabatic curvature (responsible for Berry's phase) of the lowest Landau level for g>1 is the sum of two terms. The first term is proportional to the natural symplectic form on deformation space, and the second is a fluctuating term reflecting the chaos of the geodesic motion for g>1. For g=1 (integrable motion on the torus) we have no fluctuating term. We propose our result to be interpreted as a curvature analog of the well-known semiclassical trace formulas. Connections with the viscosity properties of quantum Hall fluids on such surfaces are also pointed out. An interesting possibility in this respect is the fractional quantization of certain components of the viscosity tensor of such fluids.

  14. Random phase mask as a model of a rough surface

    International Nuclear Information System (INIS)

    Svitasheva, S.N.

    2011-01-01

    Artificial roughness was created on sample surfaces by etching through a two-dimensional orthogonal grating with a stochastic distribution of square 'defects' of size. 'Defects' depth was varied from 0.02 μm up to 1.005 μm. The experimental dependences of the scattering of polarized light were studied on four types of surface roughness for two materials: quartz and aluminum. The defect sizes of the random phase mask were 25 x 25 μm and 2.5 x 2.5 μm. The impacts of the sizes and density of artificial defects of rough surfaces on the polarization of reflected light were investigated by multiple-angle-of-incidence (MAI) ellipsometry at a wavelength of 0.63 μm.

  15. New potential humic acid stationary phase toward drug components: Development of a chemometric-assisted RP-HPLC method for the determination of paracetamol and caffeine in tablet formulations.

    Science.gov (United States)

    Topkafa, Mustafa; Ayyildiz, Hamide Filiz; Memon, Fakhar N; Kara, Huseyin

    2016-07-01

    A new humic acid based stationary phase has been used, for the first time, to achieve the separation and quantification of paracetamol and caffeine in pharmaceutical preparations under reversed-phase high-performance liquid chromatography conditions. Central composite design was applied as a powerful tool to optimize the most dominant parameters that influence the resolution of reversed-phase high-performance liquid chromatography, that is, mobile phase composition (acetonitrile percentage in water), flow rate, and column temperature. The optimum conditions were obtained as 21.69%, 1.5 mL/min, and 15°C, respectively, with the aid of a second-order quadratic model and desirability function. Under the optimum conditions, the peaks could be baseline separated within 10 min. For the developed reversed-phase high-performance liquid chromatography method, the linearity was investigated in the concentration ranges of 2-160 mg/mL (R(2) = 0.999) for paracetamol and 2-9.9 mg/mL (R(2) = 0.991) for caffeine. Mean recoveries for paracetamol and caffeine were 95.90 and 95.68%, respectively. The limits of detection and quantification were 4.1 × 10(-4) and 1.3 × 10(-3) mg/mL for paracetamol and 1.6 × 10(-4) and 5.0 × 10(-4) mg/mL for caffeine. The results showed that the new humic acid based stationary phase is very suitable for the separation of paracetamol and caffeine in pharmaceutical preparations and, thus it can be used effectively in the pharmaceutical industry. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Stationary nonlinear Airy beams

    International Nuclear Information System (INIS)

    Lotti, A.; Faccio, D.; Couairon, A.; Papazoglou, D. G.; Panagiotopoulos, P.; Tzortzakis, S.; Abdollahpour, D.

    2011-01-01

    We demonstrate the existence of an additional class of stationary accelerating Airy wave forms that exist in the presence of third-order (Kerr) nonlinearity and nonlinear losses. Numerical simulations and experiments, in agreement with the analytical model, highlight how these stationary solutions sustain the nonlinear evolution of Airy beams. The generic nature of the Airy solution allows extension of these results to other settings, and a variety of applications are suggested.

  17. Surface wake in the random-phase approximation

    International Nuclear Information System (INIS)

    Garcia de Abajo, F.J.; Echenique, P.M.

    1993-01-01

    The scalar-electric-potential distribution set up by an ion traveling in the vicinity of a plane solid-vacuum interface, that is, the surface-wake potential, is investigated with the specular-reflection model to describe the response of the surface and with the random-phase approximation for the dielectric function of the bulk material. This permits us to address the study of the low-velocity surface wake: the static potential is found to have a dip at the position of the ion; that dip is shifted towards the direction opposite to the velocity vector for velocities smaller than the threshold of creation of plasmons (∼1.3v F ). Extensive numerical calculations are presented for an ion both inside and outside aluminum. Comparison to the results obtained with the plasmon-pole dielectric function indicates excellent agreement for velocities larger than ∼1.3v F . On the other side, the possibility of surface-wake riding is suggested, by analogy with bulk-wake riding postulated in the past. In it, the electron would be bound in the first trough of the surface-wake potential set up when the ion describes a grazing trajectory. The main feature introduced by the surface with respect to the bulk consists of allowing the use of ions of higher charge, reducing in this way the relative importance of the electron self-energy, and in addition, giving rise to larger binding energies. When the ion beam is directed along a special direction of an oriented crystal surface, the mechanism of resonant coherent excitation could provide a way for experimentally detecting this phenomenon through the emission of the bound electron with well-defined energy and around a preferential direction

  18. Unwrapped phase inversion for near surface seismic data

    KAUST Repository

    Choi, Yun Seok

    2012-11-04

    The Phase-wrapping is one of the main obstacles of waveform inversion. We use an inversion algorithm based on the instantaneous-traveltime that overcomes the phase-wrapping problem. With a high damping factor, the frequency-dependent instantaneous-traveltime inversion provides the stability of refraction tomography, with higher resolution results, and no arrival picking involved. We apply the instantaneous-traveltime inversion to the synthetic data generated by the elastic time-domain modeling. The synthetic data is a representative of the near surface seismic data. Although the inversion algorithm is based on the acoustic wave equation, the numerical examples show that the instantaneous-traveltime inversion generates a convergent velocity model, very similar to what we see from traveltime tomography.

  19. Phase shift reflectometry for sub-surface defect detection

    Science.gov (United States)

    Asundi, Anand; Lei, Huang; Eden, Teoh Kang Min; Sreemathy, Parthasarathy; May, Watt Sook

    2012-11-01

    Phase Shift Reflectometry has recently been seen as a novel alternative to interferometry since it can provide warpage measurement over large areas with no need for large optical components. To confirm its capability and to explore the use of this method for sub-surface defect detection, a Chinese magic mirror is used. This bronze mirror which dates back to the Chinese Han Dynasty appears at first sight to be an ordinary convex mirror. However, unlike a normal mirror, when illuminated by a beam of light, an image is formed onto a screen. It has been hypothesized that there are indentations inside the mirror which alter the path of reflected light rays and hence the reflected image. This paper explores various methods to measure these indentations. Of the methods test Phase Shift Reflectometry (PSR) was found suitable to be the most suitable both in terms of the sensitivity and the field of view.

  20. The synthesis of surface-glycosylated porous monolithic column via aqueous two-phase graft copolymerization and its application in capillary-liquid chromatography.

    Science.gov (United States)

    Xiong, Xiyue; He, Haiqin; Shu, Yan; Li, Yuxin; Yang, Zihui; Chen, Yingzhuang; Ma, Ming; Chen, Bo

    2016-12-01

    A facile, flexible process was developed for the preparation of surface-glycosylated porous monolithic columns via aqueous two-phase graft copolymerization of polyethylene glycol diacrylate (PEGDA) and water-soluble dextran (dextran sulfate). The formation of poly(PEGDA) porous skeletons and surface glycosylation were achieved via a one-step process without pre-modification of the dextran. The synthesis conditions were thoroughly optimized. The optimal monolithic column exhibited a large dry state surface area (greater than 400m 2 /g), and it was evaluated as a hydrophilic liquid chromatography (HILIC) stationary phase. A typical HILIC mechanism was observed at high organic solvent content (≥65% acetonitrile). In addition, the resulting monolithic column demonstrated the potential use in analysis of complex biological sample and enviroment water. Copyright © 2016 Elsevier B.V. All rights reserved.

  1. Holographic partition functions and phases for higher genus Riemann surfaces

    International Nuclear Information System (INIS)

    Maxfield, Henry; Ross, Simon F; Way, Benson

    2016-01-01

    We describe a numerical method to compute the action of Euclidean saddle points for the partition function of a two-dimensional holographic CFT on a Riemann surface of arbitrary genus, with constant curvature metric. We explicitly evaluate the action for the saddles for genus two and map out the phase structure of dominant bulk saddles in a two-dimensional subspace of the moduli space. We discuss spontaneous breaking of discrete symmetries, and show that the handlebody bulk saddles always dominate over certain non-handlebody solutions. (paper)

  2. Surface wave phase velocities between Bulgaria and the Czech Republic

    Czech Academy of Sciences Publication Activity Database

    Gaždová, Renata; Kolínský, Petr; Popova, I.; Dimitrova, L.

    2011-01-01

    Roč. 18, č. 2 (2011), s. 16-23 ISSN 1803-1447. [OVA´11 – New Knowledge and Measurements in Seismology, Engineering Geophysics and Geotechnics. Ostrava, 12.04.2011-14.04.2011] R&D Projects: GA ČR GA205/09/1244 Institutional research plan: CEZ:AV0Z30460519 Keywords : surface waves * phase velocity * shear wave velocity Subject RIV: DC - Siesmology, Volcanology, Earth Structure http://www.caag.cz/egrse/2011-2/03%20gazdova_ova.pdf

  3. Interaction of stress and phase transformations during thermochemical surface engineering

    DEFF Research Database (Denmark)

    Jespersen, Freja Nygaard

    dissolution. The present project is devoted to understanding the mutual interaction of stresses and phase transformations during thermochemical surface engineering by combining numerical modelling with experimental materials science. The modelling was done by combining solid mechanics with thermodynamics...... by chromium atoms, and the effect of composition-induced stress on surface concentration and diffusive flux. The effect of plasticity was also included. Temperature and concentration dependencies of mechanical and diffusion material properties were studied, and the effect of incorporation in the model...... examined. The effect of pre-stressing the sample was also tested, to investigate the effects of a residual stress-state that might be present from processing of the metal specimen. Controlled thermochemical treatment of austenitic stainless steel was investigated experimentally by in-diffusion of nitrogen...

  4. Silicate Phases on the Surfaces of Trojan Asteroids

    Science.gov (United States)

    Martin, Audrey; Emery, Joshua P.; Lindsay, Sean S.

    2017-10-01

    Determining the origin of asteroids provides an effective means of constraining the solar system’s dynamic past. Jupiter Trojan asteroids (hereafter Trojans) may help in determining the amount of radial mixing that occurred during giant planet migration. Previous studies aimed at characterizing surface composition show that Trojans have low albedo surfaces and are spectrally featureless in the near infrared. The thermal infrared (TIR) wavelength range has advantages for detecting silicates on low albedo asteroids such as Trojans. The 10 μm region exhibits strong features due to the Si-O fundamental molecular vibrations. Silicates that formed in the inner solar system likely underwent thermal annealing, and thus are crystalline, whereas silicates that accreted in the outer solar system experienced less thermal processing, and therefore are more likely to have remained in an amorphous phase. We hypothesize that the Trojans formed in the outer solar system (i.e., the Kuiper Belt), and therefore will have a more dominant amorphous spectral silicate component. With TIR spectra from the Spitzer Space Telescope, we identify mineralogical features from the surface of 11 Trojan asteroids. Fine-grain mixtures of crystalline pyroxene and olivine exhibit a 10 μm feature with sharp cutoffs between about 9 μm and 12 μm, which create a broad flat plateau. Amorphous phases, when present, smooth the sharp emission features, resulting in a dome-like shape. Preliminary results indicate that the surfaces of analyzed Trojans contain primarily amorphous silicates. Emissivity spectra of asteroids 1986 WD and 4709 Ennomos include small peaks in the 10 μm region, diagnostic of small amounts of crystalline olivine. One explanation is that Trojans formed in the same region as Kuiper Belt objects, and when giant planet migration ensued, they were swept into Jupiter’s stable Lagrange points where they are found today. As such, it is possible that an ancestral group of Kuiper Belt

  5. Particle separation by phase modulated surface acoustic waves.

    Science.gov (United States)

    Simon, Gergely; Andrade, Marco A B; Reboud, Julien; Marques-Hueso, Jose; Desmulliez, Marc P Y; Cooper, Jonathan M; Riehle, Mathis O; Bernassau, Anne L

    2017-09-01

    High efficiency isolation of cells or particles from a heterogeneous mixture is a critical processing step in lab-on-a-chip devices. Acoustic techniques offer contactless and label-free manipulation, preserve viability of biological cells, and provide versatility as the applied electrical signal can be adapted to various scenarios. Conventional acoustic separation methods use time-of-flight and achieve separation up to distances of quarter wavelength with limited separation power due to slow gradients in the force. The method proposed here allows separation by half of the wavelength and can be extended by repeating the modulation pattern and can ensure maximum force acting on the particles. In this work, we propose an optimised phase modulation scheme for particle separation in a surface acoustic wave microfluidic device. An expression for the acoustic radiation force arising from the interaction between acoustic waves in the fluid was derived. We demonstrated, for the first time, that the expression of the acoustic radiation force differs in surface acoustic wave and bulk devices, due to the presence of a geometric scaling factor. Two phase modulation schemes are investigated theoretically and experimentally. Theoretical findings were experimentally validated for different mixtures of polystyrene particles confirming that the method offers high selectivity. A Monte-Carlo simulation enabled us to assess performance in real situations, including the effects of particle size variation and non-uniform acoustic field on sorting efficiency and purity, validating the ability to separate particles with high purity and high resolution.

  6. Phase behavior of charged colloids on spherical surfaces

    Science.gov (United States)

    Kelleher, Colm; Guerra, Rodrigo; Chaikin, Paul

    For a broad class of 2D materials, the transition from isotropic fluid to crystalline solid is described by the theory of melting due to Kosterlitz, Thouless, Halperin, Nelson and Young. According to this theory, long-range order is achieved via elimination of the topological defects which proliferate in the fluid phase. However, many natural and man-made 2D systems posses spatial curvature and/or non-trivial topology, which require the presence of defects, even at T = 0 . In principle, the presence of these defects could profoundly affect the phase behavior of such a system. In this presentation, we describe experiments and simulations we have performed on repulsive particles which are bound to the surface of a sphere. We observe spatial structures and inhomogeneous dynamics that cannot be captured by the measures traditionally used to describe flat-space phase behavior. We show that ordering is achieved by a novel mechanism: sequestration of topological defects into freely-terminating grain boundaries (``scars''), and simultaneous spatial organization of the scars themselves on the vertices of an icosahedron. The emergence of icosahedral order coincides with the localization of mobility into isolated ``lakes'' of fluid or glassy particles, situated at the icosahedron vertices.

  7. Ultrasonic phased array with surface acoustic wave for imaging cracks

    Directory of Open Access Journals (Sweden)

    Yoshikazu Ohara

    2017-06-01

    Full Text Available To accurately measure crack lengths, we developed a real-time surface imaging method (SAW PA combining an ultrasonic phased array (PA with a surface acoustic wave (SAW. SAW PA using a Rayleigh wave with a high sensitivity to surface defects was implemented for contact testing using a wedge with the third critical angle that allows the Rayleigh wave to be generated. Here, to realize high sensitivity imaging, SAW PA was optimized in terms of the wedge and the imaging area. The improved SAW PA was experimentally demonstrated using a fatigue crack specimen made of an aluminum alloy. For further verification in more realistic specimens, SAW PA was applied to stainless-steel specimens with a fatigue crack and stress corrosion cracks (SCCs. The fatigue crack was visualized with a high signal-to-noise ratio (SNR and its length was measured with a high accuracy of better than 1 mm. The SCCs generated in the heat-affected zones (HAZs of a weld were successfully visualized with a satisfactory SNR, although responses at coarse grains appeared throughout the imaging area. The SCC lengths were accurately measured. The imaging results also precisely showed complicated distributions of SCCs, which were in excellent agreement with the optically observed distributions.

  8. Fully Printed, Flexible, Phased Array Antenna for Lunar Surface Communication

    Science.gov (United States)

    Subbaraman, Harish; Hen, Ray T.; Lu, Xuejun; Chen, Maggie Yihong

    2013-01-01

    NASAs future exploration missions focus on the manned exploration of the Moon, Mars, and beyond, which will rely heavily on the development of a reliable communications infrastructure from planetary surface-to-surface, surface-to-orbit, and back to Earth. Flexible antennas are highly desired in many scenarios. Active phased array antennas (active PAAs) with distributed control and processing electronics at the surface of an antenna aperture offer numerous advantages for radar communications. Large-area active PAAs on flexible substrates are of particular interest in NASA s space radars due to their efficient inflatable package that can be rolled up during transportation and deployed in space. Such an inflatable package significantly reduces stowage volume and mass. Because of these performance and packaging advantages, large-area inflatable active PAAs are highly desired in NASA s surface-to-orbit and surface-to-relay communications. To address the issues of flexible electronics, a room-temperature printing process of active phased-array antennas on a flexible Kapton substrate was developed. Field effect transistors (FETs) based on carbon nanotubes (CNTs), with many unique physical properties, were successfully proved feasible for the PAA system. This innovation is a new type of fully inkjet-printable, two-dimensional, high-frequency PAA on a flexible substrate at room temperature. The designed electronic circuit components, such as the FET switches in the phase shifter, metal interconnection lines, microstrip transmission lines, etc., are all printed using a special inkjet printer. Using the developed technology, entire 1x4, 2x2, and 4x4 PAA systems were developed, packaged, and demonstrated at 5.3 GHz. Several key solutions are addressed in this work to solve the fabrication issues. The source/drain contact is developed using droplets of silver ink printed on the source/drain areas prior to applying CNT thin-film. The wet silver ink droplets allow the silver to

  9. Investigating the Effect of Growth Phase on the Surface-Layer Associated Proteome of Lactobacillus acidophilus Using Quantitative Proteomics

    Directory of Open Access Journals (Sweden)

    Courtney Klotz

    2017-11-01

    Full Text Available Bacterial surface-layers (S-layers are semi-porous crystalline arrays that self-assemble to form the outermost layer of some cell envelopes. S-layers have been shown to act as scaffolding structures for the display of auxiliary proteins externally. These S-layer associated proteins have recently gained attention in probiotics due to their direct physical contact with the intestinal mucosa and potential role in cell proliferation, adhesion, and immunomodulation. A number of studies have attempted to catalog the S-layer associated proteome of Lactobacillus acidophilus NCFM under a single condition. However, due to the versatility of the cell surface, we chose to employ a multiplexing-based approach with the intention of accurately contrasting multiple conditions. In this study, a previously described lithium chloride isolation protocol was used to release proteins bound to the L. acidophilus S-layer during logarithmic and early stationary growth phases. Protein quantification values were obtained via TMT (tandem mass tag labeling combined with a triple-stage mass spectrometry (MS3 method. Results showed significant growth stage-dependent alterations to the surface-associated proteome while simultaneously highlighting the sensitivity and reproducibility of the technology. Thus, this study establishes a framework for quantifying condition-dependent changes to cell surface proteins that can easily be applied to other S-layer forming bacteria.

  10. Stationary-State Mutagenesis in Escherichia coli

    Indian Academy of Sciences (India)

    Stationary-phase mutagenesis in nondividing E. coli cells exposed to a nonlethal stress was, a few years ago, claimed to be a likely case of a Lamarckian mechanism capable of producing exclusively useful mutations in a directed manner. After a heated debate over the last decade it now appears to involve a Darwinian ...

  11. Conformational variability of the stationary phase survival protein E from Xylella fastidiosa revealed by X-ray crystallography, small-angle X-ray scattering studies, and normal mode analysis.

    Science.gov (United States)

    Machado, Agnes Thiane Pereira; Fonseca, Emanuella Maria Barreto; Reis, Marcelo Augusto Dos; Saraiva, Antonio Marcos; Santos, Clelton Aparecido Dos; de Toledo, Marcelo Augusto Szymanski; Polikarpov, Igor; de Souza, Anete Pereira; Aparicio, Ricardo; Iulek, Jorge

    2017-10-01

    Xylella fastidiosa is a xylem-limited bacterium that infects a wide variety of plants. Stationary phase survival protein E is classified as a nucleotidase, which is expressed when bacterial cells are in the stationary growth phase and subjected to environmental stresses. Here, we report four refined X-ray structures of this protein from X. fastidiosa in four different crystal forms in the presence and/or absence of the substrate 3'-AMP. In all chains, the conserved loop verified in family members assumes a closed conformation in either condition. Therefore, the enzymatic mechanism for the target protein might be different of its homologs. Two crystal forms exhibit two monomers whereas the other two show four monomers in the asymmetric unit. While the biological unit has been characterized as a tetramer, differences of their sizes and symmetry are remarkable. Four conformers identified by Small-Angle X-ray Scattering (SAXS) in a ligand-free solution are related to the low frequency normal modes of the crystallographic structures associated with rigid body-like protomer arrangements responsible for the longitudinal and symmetric adjustments between tetramers. When the substrate is present in solution, only two conformers are selected. The most prominent conformer for each case is associated to a normal mode able to elongate the protein by moving apart two dimers. To our knowledge, this work was the first investigation based on the normal modes that analyzed the quaternary structure variability for an enzyme of the SurE family followed by crystallography and SAXS validation. The combined results raise new directions to study allosteric features of XfSurE protein. © 2017 Wiley Periodicals, Inc.

  12. Relativistic elasticity of stationary fluid branes

    DEFF Research Database (Denmark)

    Armas, J.; Obers, N.A.

    2013-01-01

    Fluid mechanics can be formulated on dynamical surfaces of arbitrary codimension embedded in a background space-time. This has been the main object of study of the blackfold approach in which the emphasis has primarily been on stationary fluid configurations. Motivated by this approach we show un...

  13. Stationary Double Layers in a Collisionless Magnetoplasma

    DEFF Research Database (Denmark)

    Noriyoshi, Sato; Mieno, Tetsu; Hatakeyama, Rikizo

    1983-01-01

    Stationary double layers are generated in a magnetoplasma by applying potential differences between two heated plates on which the plasma is produced by surface ionization. By measuring the double-layer formation process, a localized potential drop is found to be formed initially in front of the ...

  14. Stationary Double Layers in a Collisionless Magnetoplasma

    DEFF Research Database (Denmark)

    Noriyoshi, Sato; Mieno, Tetsu; Hatakeyama, Rikizo

    1983-01-01

    Stationary double layers are generated in a magnetoplasma by applying potential differences between two heated plates on which the plasma is produced by surface ionization. By measuring the double-layer formation process, a localized potential drop is found to be formed initially in front...... of the plate on the low-potential side, being accompanied with current limitation. This localized potential drop moves along the plasma column, but finally stops and results in the formation of the stationary double layer in the presence of sufficient plasma supply from the plate on the high-potential side....

  15. Substrate integrated ferrite phase shifters and active frequency selective surfaces

    International Nuclear Information System (INIS)

    Cahill, B.M.

    2002-01-01

    There are two distinct parts to this thesis; the first investigates the use of ferrite tiles in the construction of printed phase shifting transmission lines, culminating in the design of two compact electromagnetic controlled beam steered patch and slot antenna arrays. The second part investigates the use of active frequency selective surfaces (AFSS), which are later used to cover a uPVC constructed enclosure. Field intensity measurements are taken from within the enclosure to determine the dynamic screening effectiveness. Trans Tech G-350 Ferrite is investigated to determine its application in printed microstrip and stripline phase shifting transmission lines. 50-Ohm transmission lines are constructed using the ferrite tile and interfaced to Rogers RT Duroid 5870 substrate. Scattering parameter measurements are made under the application of variable magnetic fields to the ferrite. Later, two types of planar microwave beam steering antennas are constructed. The first uses the ferrites integrated into the Duroid as microstrip lines with 3 patch antennas as the radiating elements. The second uses stripline transmission lines, with slot antennas as the radiating sources etched into the ground plane of the triplate. Beam steering is achieved by the application of an external electromagnet. An AFSS is constructed by the interposition of PIN diodes into a dipole FSS array. Transmission response measurements are then made for various angles of electromagnetic wave incidence. Two states of operation exist: when a current is passed through the diodes and when the diodes are switched off. These two states form a high pass and band stop space filter respectively. An enclosure covered with the AFSS is constructed and externally illuminated in the range 2.0 - 2.8GHz. A probe antenna inside the enclosure positioned at various locations through out the volume is used to establish the effective screening action of the AFSS in 3 dimensional space. (author)

  16. Evaluation of the chiral recognition properties and the column performances of three chiral stationary phases based on cellulose for the enantioseparation of six dihydropyridines by high-performance liquid chromatography.

    Science.gov (United States)

    Yu, Jia; Tang, Jing; Yuan, Xiaowei; Guo, Xingjie; Zhao, Longshan

    2017-03-01

    Separations of six dihydropyridine enantiomers on three commercially available cellulose-based chiral stationary phases (Chiralcel OD-RH, Chiralpak IB, and Chiralpak IC) were evaluated with high-performance liquid chromatography (HPLC). The best enantioseparation of the six chiral drugs was obtained with a Chiralpak IC (250 × 4.6 mm i.d., 5 μm) column. Then the influence of the mobile phase including an alcohol-modifying agent and alkaline additive on the enantioseparation were investigated and optimized. The optimal mobile phase conditions and maximum resolution for every analyte were as follows respectively: n-hexane/isopropanol (85:15, v/v) for nimodipine (R = 5.80) and cinildilpine (R = 5.65); n-hexane/isopropanol (92:8, v/v) for nicardipine (R = 1.76) and nisoldipine (R = 1.92); and n-hexane/isopropanol/ethanol (97:2:1, v/v/v) for felodipine (R = 1.84) and lercanidipine (R = 1.47). Relative separation mechanisms are discussed based on the separation results, and indicate that the achiral parts in the analytes' structure showed an important influence on the separation of the chiral column. © 2017 Wiley Periodicals, Inc.

  17. The staphylococcal accessory regulator, SarA, is an RNA-binding protein that modulates the mRNA turnover properties of late-exponential and stationary phase Staphylococcus aureus cells

    Directory of Open Access Journals (Sweden)

    John M Morrison

    2012-03-01

    Full Text Available The modulation of mRNA turnover is gaining recognition as a mechanism by which Staphylococcus aureus regulates gene expression, but the factors that orchestrate alterations in transcript degradation are poorly understood. In that regard, we previously found that 138 mRNA species, including the virulence factors protein A (spa and collagen binding protein (cna, are stabilized in a sarA-dependent manner during exponential phase growth, suggesting that SarA protein may directly or indirectly effect the RNA turnover properties of these transcripts. Herein, we expanded our characterization of the effects of sarA on mRNA turnover during late exponential and stationary phases of growth. Results revealed that the locus affects the RNA degradation properties of cells during both growth phases. Further, using gel mobility shift assays and RIP-ChIP, it was found that SarA protein is capable of binding mRNA species that it stabilizes both in vitro and within bacterial cells. Taken together, these results suggest that SarA post-transcriptionally regulates S. aureus gene expression in a manner that involves binding to and consequently altering the mRNA turnover properties of target transcripts.

  18. Evaluation of the chiral recognition properties as well as the column performance of four chiral stationary phases based on cellulose (3,5-dimethylphenylcarbamate) by parallel HPLC and SFC.

    Science.gov (United States)

    Nelander, Hanna; Andersson, Shalini; Ohlén, Kristina

    2011-12-30

    The performance of four commercially available cellulose tris(3,5-dimethylphenylcarbamate) based chiral stationary phases (CSPs) was evaluated with parallel high performance liquid chromatography (HPLC) and super critical fluid chromatography (SFC). Retention, enantioselectivity, resolution and efficiency were compared for a set of neutral, basic and acidic compounds having different physico-chemical properties by using different mobile phase conditions. Although the chiral selector is the same in all the four CSPs, a large difference in the ability to retain and resolve enantiomers was observed under the same chromatographic conditions. We believe that this is mainly due to differences in the silica matrix and immobilization techniques used by the different vendors. An extended study of metoprolol and structure analogues gave a deeper understanding of the accessibility of the chiral discriminating interactions and its impact on the resolution of the racemic compounds on the four CSPs studied. Also, a clear difference in enantioselectivity is observed between SFC and LC mode, hydrogen bonding was found to play an important role in the differential binding of the enantiomers to the CSPs. Copyright © 2011 Elsevier B.V. All rights reserved.

  19. Comparative study on the liquid chromatographic enantioseparation of cyclic β-amino acids and the related cyclic β-aminohydroxamic acids on Cinchona alkaloid-based zwitterionic chiral stationary phases.

    Science.gov (United States)

    Bajtai, Attila; Fekete, Beáta; Palkó, Márta; Fülöp, Ferenc; Lindner, Wolfgang; Kohout, Michal; Ilisz, István; Péter, Antal

    2018-03-01

    The enantiomeric pairs of cis and trans stereoisomers of cyclic β-aminohydroxamic acids and their related cis and trans cyclic β-amino acids containing two chiral centers were directly separated on four structurally related chiral stationary phases derived from quinine and quinidine modified with (R,R)- and (S,S)-aminocyclohexanesulfonic acids. Applying these zwitterionic ion-exchangers as chiral selectors, the effects of the composition of the bulk solvent, the acid and base additives, the structures of the analytes, and temperature on the enantioresolution were investigated. To study the effects of temperature and obtain thermodynamic parameters, experiments were carried out at constant mobile phase compositions in the temperature range 5-50°C. The differences in the changes in standard enthalpy Δ(ΔH°), entropy Δ(ΔS°), and free energy Δ(ΔG°) were calculated from the linear van't Hoff plots derived from the ln α versus 1/T curves in the studied temperature range. Results thus obtained indicated enthalpy-driven separations in all cases. The sequence of elution of the enantiomers was determined and found to be reversed when ZWIX(-)™ was changed to ZWIX(+)™ or ZWIX(-A) to ZWIX(+A). © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Capillary-channeled polymer (C-CP) fibers as a stationary phase for sample clean-up of protein solutions for matrix-assisted laser/desorption ionization mass spectrometry.

    Science.gov (United States)

    Manard, Benjamin T; Marcus, R Kenneth

    2012-08-01

    Capillary-channeled polymer (C-CP) fibers are employed in a micropipette tip format to affect a stationary phase for the solid phase extraction (SPE) of proteins from buffer solutions prior to MALDI-MS analysis. Proteins readily adsorb to the polypropylene (PP) C-CP fibers while buffer species are easily washed off the tips using DI-H(2)O. Elution of the solutes is achieved with an aliquot of 50:50 ACN:H(2)O, which is compatible with the subsequent spotting on the MALDI target with the matrix solution. Lysozyme and cytochrome c are used as test species, with a primary buffer composition of 100 mM Tris-HCl. In this case, direct MALDI-MS produces no discernible protein signals. SPE on the C-CP fibers yields high fidelity mass spectra for 1 μL sample volumes. Limits of detection for cytochrome c in 100 mM Tris-HCl are on the order of 40 nM. Extraction of cytochrome c from buffer concentrations of up to 1 M Tris-HCl, provides signal recoveries that are suppressed by only ~50% versus neat protein solutions. Finally, extraction of 3.1 μM cytochrome c from a synthetic urine matrix exhibits excellent recovery.

  1. Capillary-Channeled Polymer (C-CP) Fibers as a Stationary Phase for Sample Clean-Up of Protein Solutions for Matrix-Assisted Laser/Desorption Ionization Mass Spectrometry

    Science.gov (United States)

    Manard, Benjamin T.; Marcus, R. Kenneth

    2012-08-01

    Capillary-channeled polymer (C-CP) fibers are employed in a micropipette tip format to affect a stationary phase for the solid phase extraction (SPE) of proteins from buffer solutions prior to MALDI-MS analysis. Proteins readily adsorb to the polypropylene (PP) C-CP fibers while buffer species are easily washed off the tips using DI-H2O. Elution of the solutes is achieved with an aliquot of 50:50 ACN:H2O, which is compatible with the subsequent spotting on the MALDI target with the matrix solution. Lysozyme and cytochrome c are used as test species, with a primary buffer composition of 100 mM Tris-HCl. In this case, direct MALDI-MS produces no discernible protein signals. SPE on the C-CP fibers yields high fidelity mass spectra for 1 μL sample volumes. Limits of detection for cytochrome c in 100 mM Tris-HCl are on the order of 40 nM. Extraction of cytochrome c from buffer concentrations of up to 1 M Tris-HCl, provides signal recoveries that are suppressed by only ~50 % versus neat protein solutions. Finally, extraction of 3.1 μM cytochrome c from a synthetic urine matrix exhibits excellent recovery.

  2. Large Area Diamond Tribological Surfaces with Negligible Wear in Extreme Environments, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — In Phase I we propose to demonstrate the processing of very large area diamond sliding bearings and tribological surfaces. The bearings and surfaces will experience...

  3. Ortho-substituent correlated retention of polychlorinated biphenyls on a 50% n-octyl-methylpolysiloxane stationary phase by HRGC/MSD

    Energy Technology Data Exchange (ETDEWEB)

    Fischer, R.; Ballschmiter, K.

    1988-11-01

    Polychlorinated biphenyls (PCB) have been known as ubiquitous environmental pollutants since the late 60s. They are found partitioned between all environmental compartments according to their physico-chemical properties. Investigation of their partitioning, degradation, and transport behaviour demands sensitive and selective analytical methods for this complex mixture of up to 209 theoretically possible compounds. Congener-specific separation by high-resolution gas chromatography coupled with mass-selective detection would be a suitable approach to this multi-compound problem. In this paper, the separation of PCB congeners by capillary gas chromatography (HRGC) on a 50% n-octyl-methylpolysiloxane phase is presented.

  4. Automated Hybrid Microwave Heating for Lunar Surface Solidification, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — This SBIR project addresses the need for a system that will provide automated lunar surface stabilization via hybrid microwave heating. Surface stabilization is...

  5. Surface Operations Data Analysis and Adaptation Tool, Phase II

    Data.gov (United States)

    National Aeronautics and Space Administration — This effort undertook the creation of a Surface Operations Data Analysis and Adaptation (SODAA) tool to store data relevant to airport surface research and...

  6. Enantiomer separation of a powerful chiral auxiliary, 2-methoxy-2-(1-naphthyl)propionic acid by liquid chromatography using chiral anion exchanger-type stationary phases in polar-organic mode; investigation of molecular recognition aspects.

    Science.gov (United States)

    Gyimesi-Forrás, Krisztina; Akasaka, Kazuaki; Lämmerhofer, Michael; Maier, Norbert M; Fujita, Takuma; Watanabe, Masataka; Harada, Nobuyuki; Lindner, Wolfgang

    2005-01-01

    The enantiodiscriminating potential of the weak anion exchange-type quinine-based chiral stationary phases (CSPs) for direct enantiomer separation of racemic 2-methoxy-2-(1-naphthyl)propionic acid (selectand, SA) was studied. The influence of structure variations of the selector (SO) in the carbamate functional group and/or in the C6' position of quinoline moiety on retention and enantioselectivity was investigated. Systematic chromatographic studies were made to gain more insight into the overall chiral recognition mechanism for a given mobile phase. In this context, the tert-butylcarbamoyl quinine and the corresponding diisopropylphenyl-derived selector provided the highest resolution and enantioselectivity under polar-organic conditions with the elution order of (R) before the (S) enantiomer. When the bulkiness of the substituents in the C6' position of the SO was increased, the selectivity was decreased in all cases. Alkylation of the nitrogen atom in the carbamate functionality of the SO resulted in the complete loss of enantiomer separation, confirming the crucial importance of the hydrogen-bond formation involved in the stereodiscriminating events. In addition, ten different mono-, bi-, or trivalent acids, necessary as competitor molecules (counter-ions) of the mobile phase, were screened to judge their influence on retention and overall enantioselectivity. Among them, acetic acid, formic acid, N-acetylglycine, and glycolic acid proved to be the most promising counter-ions with R(S) values of 6.35, 6.81, 8.19, and 7.34, respectively. On the basis of chromatographic data, a tentative molecular recognition model was proposed. Simultaneous ion-pairing and hydrogen bonding, in concert with pi-pi stacking and steric interactions, were expected to be responsible for chiral recognition mechanism. This was partially corroborated by structural and/or conformational analysis of the tert-butylcarbamoyl quinine-2-methoxy-2-(1-naphthyl)propionic acid (SO-SA) complex

  7. High pressure size exclusion chromatography (HPSEC) determination of dissolved organic matter molecular weight revisited: Accounting for changes in stationary phases, analytical standards, and isolation methods

    Science.gov (United States)

    McAdams, Brandon C.; Aiken, George R.; McKnight, Diane M.; Arnold, William A.; Chin, Yu-Ping

    2018-01-01

    We reassessed the molecular weight of dissolved organic matter (DOM) determined by high pressure size exclusion chromatography (HPSEC) using measurements made with different columns and various generations of polystyrenesulfonate (PSS) molecular weight standards. Molecular weight measurements made with a newer generation HPSEC column and PSS standards from more recent lots are roughly 200 to 400 Da lower than initial measurements made in the early 1990s. These updated numbers match DOM molecular weights measured by colligative methods and fall within a range of values calculated from hydroxyl radical kinetics. These changes suggest improved accuracy of HPSEC molecular weight measurements that we attribute to improved accuracy of PSS standards and changes in the column packing. We also isolated DOM from wetlands in the Prairie Pothole Region (PPR) using XAD-8, a cation exchange resin, and PPL, a styrene-divinylbenzene media, and observed little difference in molecular weight and specific UV absorbance at 280 nm (SUVA280) between the two solid phase extraction resins, suggesting they capture similar DOM moieties. PPR DOM also showed lower SUVA280 at similar weights compared to DOM isolates from a global range of environments, which we attribute to oxidized sulfur in PPR DOM that would increase molecular weight without affecting SUVA280.

  8. High Pressure Size Exclusion Chromatography (HPSEC) Determination of Dissolved Organic Matter Molecular Weight Revisited: Accounting for Changes in Stationary Phases, Analytical Standards, and Isolation Methods.

    Science.gov (United States)

    McAdams, Brandon C; Aiken, George R; McKnight, Diane M; Arnold, William A; Chin, Yu-Ping

    2018-01-16

    We reassessed the molecular weight of dissolved organic matter (DOM) determined by high pressure size exclusion chromatography (HPSEC) using measurements made with different columns and various generations of polystyrenesulfonate (PSS) molecular weight standards. Molecular weight measurements made with a newer generation HPSEC column and PSS standards from more recent lots are roughly 200 to 400 Da lower than initial measurements made in the early 1990s. These updated numbers match DOM molecular weights measured by colligative methods and fall within a range of values calculated from hydroxyl radical kinetics. These changes suggest improved accuracy of HPSEC molecular weight measurements that we attribute to improved accuracy of PSS standards and changes in the column packing. We also isolated DOM from wetlands in the Prairie Pothole Region (PPR) using XAD-8, a cation exchange resin, and PPL, a styrene-divinylbenzene media, and observed little difference in molecular weight and specific UV absorbance at 280 nm (SUVA 280 ) between the two solid phase extraction resins, suggesting they capture similar DOM moieties. PPR DOM also showed lower SUVA 280 at similar weights compared to DOM isolates from a global range of environments, which we attribute to oxidized sulfur in PPR DOM that would increase molecular weight without affecting SUVA 280 .

  9. Correlations Between retention indices and molecular structure of aliphatic alcohols and of their benzoyl derivatives on phenyl substituted polysiloxane stationary phases

    International Nuclear Information System (INIS)

    Pias, J. B.; Gasco, L.

    1976-01-01

    The retention indices of aliphatic alcohols of carbon number up to C g , and of their benzoyl derivatives up to C 7 , were determined in columns packed with Chromo sorb G (AW-DMCS-HP) coated previously with 5% methyl, and methyl phenyl polysiloxanes with increasing polarity (SE-30, 0V-3, 0V-7, 0V-11, 0V-17 and OV-25). Correlations between retention indices and chain length for 1-alcohols, 2-alcohols, 3-alcohols, 1 , on -3-alcohols, 2-methyl-1-alcohols and for their corresponding benzoyl derivatives were calculated at 100, 120 and 140 degree centigree. In alcohols, a -CH 2 - group increases I approximately 100 units, and in their benzoyl derivatives from 80 to 100 units. Dispersion indices Δl , and positional and structural increments δI, were evaluated for -OH and benzoyl groups in terms of phase polarity and chain length. Effects of chain length, chain branching and double bond location on retention parameters were also studied. (Author) 23 refs

  10. Airport Surface Management Tools for NAS Users, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — Decision support tools that make use of surface surveillance technologies data can potentially make it possible to increase airport throughput, better accommodate...

  11. Scalable Lunar Surface Networks and Adaptive Orbit Access, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — Innovative network architecture, protocols, and algorithms are proposed for both lunar surface networks and orbit access networks. Firstly, an overlaying...

  12. Low Friction Surfaces for Low Temperature Applications, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — Lunar and other extraterrestrial environments put extreme demands on moving mechanical components. Gears must continue to function and surfaces must continue to...

  13. Phase transformations during machining and properties of surface layers in zirconium dioxide ceramics

    International Nuclear Information System (INIS)

    Grigor'ev, O.N.; Krivoshej, G.S.; Stel'mashenko, N.A.; Trefilov, V.I.; Shevchenko, A.V.

    1991-01-01

    The methods of X-ray allow studying phase composition and inner stresses in the surface layers of partially stabilized zirconium dioxide after mashining. It is shown that under conditions of abrasive treatment transitions from tetragonal into rhomboedric and monoclinic phases initiate. As a result of phase transitions fields of compressible stresses achieving 900 MPa under grinding with ACM abrasive are created on the surface. An essential increase of hardness due to growth of the brittle fauilure resistance and deformation hardening is revealed

  14. A Comet Surface Sample Return System, Phase II

    Data.gov (United States)

    National Aeronautics and Space Administration — The proposed Phase II investigation will focus on the development of spacecraft systems required to obtain a sample from the nucleus of a comet, hermetically seal...

  15. A Novel Two-Step Liquid-Liquid Extraction Procedure Combined with Stationary Phase Immobilized Human Serum Albumin for the Chiral Separation of Cetirizine Enantiomers along with M and P Parabens

    Directory of Open Access Journals (Sweden)

    Aleksandra Chmielewska

    2016-12-01

    Full Text Available The research into the separation of drug enantiomers is closely related to the safety and efficiency of the drugs. The aim of this study was to develop a simple and validated HPLC method to analyze cetirizine enantiomers. In the case of liquid dosage forms, besides the active substance in large amounts there are usually also inactive ingredients such as methyl- and propylparaben. Unfortunately, these compounds can interfere with the analyte, inter alia during chiral separation of the analyte enantiomers. The proposed innovative two-step liquid-liquid extraction procedure allowed for the determination of cetirizine enantiomers (along with M and P parabens also in liquid dosage forms. The main focus of this study was the chromatographic activity of cetirizine dihydrochloride on the proteinate-based chiral stationary phase. The chromatographic separation of cetirizine enantiomers was performed on an immobilized human serum albumin (HSA column for the first time. Measurements were performed at a wavelength of 227 nm. Under optimal conditions, baseline separation of two enantiomers was obtained with 1.43 enantioseparation factor (α and 1.82 resolution (Rs. Finally, the proposed method was successfully applied to the selected pharmaceutical formulations.

  16. A Novel Two-Step Liquid-Liquid Extraction Procedure Combined with Stationary Phase Immobilized Human Serum Albumin for the Chiral Separation of Cetirizine Enantiomers along with M and P Parabens.

    Science.gov (United States)

    Chmielewska, Aleksandra; Konieczna, Lucyna; Bączek, Tomasz

    2016-12-07

    The research into the separation of drug enantiomers is closely related to the safety and efficiency of the drugs. The aim of this study was to develop a simple and validated HPLC method to analyze cetirizine enantiomers. In the case of liquid dosage forms, besides the active substance in large amounts there are usually also inactive ingredients such as methyl- and propylparaben. Unfortunately, these compounds can interfere with the analyte, inter alia during chiral separation of the analyte enantiomers. The proposed innovative two-step liquid-liquid extraction procedure allowed for the determination of cetirizine enantiomers (along with M and P parabens) also in liquid dosage forms. The main focus of this study was the chromatographic activity of cetirizine dihydrochloride on the proteinate-based chiral stationary phase. The chromatographic separation of cetirizine enantiomers was performed on an immobilized human serum albumin (HSA) column for the first time. Measurements were performed at a wavelength of 227 nm. Under optimal conditions, baseline separation of two enantiomers was obtained with 1.43 enantioseparation factor (α) and 1.82 resolution ( R s ). Finally, the proposed method was successfully applied to the selected pharmaceutical formulations.

  17. Surface Tension of Multi-phase Flow with Multiple Junctions Governed by the Variational Principle

    International Nuclear Information System (INIS)

    Matsutani, Shigeki; Nakano, Kota; Shinjo, Katsuhiko

    2011-01-01

    We explore a computational model of an incompressible fluid with a multi-phase field in three-dimensional Euclidean space. By investigating an incompressible fluid with a two-phase field geometrically, we reformulate the expression of the surface tension for the two-phase field found by Lafaurie et al. (J Comput Phys 113:134–147, 1994) as a variational problem related to an infinite dimensional Lie group, the volume-preserving diffeomorphism. The variational principle to the action integral with the surface energy reproduces their Euler equation of the two-phase field with the surface tension. Since the surface energy of multiple interfaces even with singularities is not difficult to be evaluated in general and the variational formulation works for every action integral, the new formulation enables us to extend their expression to that of a multi-phase (N-phase, N ≥ 2) flow and to obtain a novel Euler equation with the surface tension of the multi-phase field. The obtained Euler equation governs the equation for motion of the multi-phase field with different surface tension coefficients without any difficulties for the singularities at multiple junctions. In other words, we unify the theory of multi-phase fields which express low dimensional interface geometry and the theory of the incompressible fluid dynamics on the infinite dimensional geometry as a variational problem. We apply the equation to the contact angle problems at triple junctions. We computed the fluid dynamics for a two-phase field with a wall numerically and show the numerical computational results that for given surface tension coefficients, the contact angles are generated by the surface tension as results of balances of the kinematic energy and the surface energy.

  18. Surface-Mount Rotor Motion Sensing System, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — A surface-mounted instrumentation system for measuring rotor blade motions on rotorcraft, for use both in flight and in wind tunnel testing, is proposed for...

  19. Surface Micromachined Arrays of Transition-Edge Detectors, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — An innovative surface micromachining technique is described for the fabrication of closely-packed arrays of transition edge sensor (TES) x-ray microcalorimeters....

  20. Robust Prediction of High Lift Using Surface Vorticity, Phase II

    Data.gov (United States)

    National Aeronautics and Space Administration — FlightStream has been developed a fast, accurate, aerodynamic prediction code based on vorticity computations on the surface of an aircraft. The code, though still a...

  1. Microscopic Analysis and Modeling of Airport Surface Sequencing, Phase II

    Data.gov (United States)

    National Aeronautics and Space Administration — Although a number of airportal surface models exist and have been successfully used for analysis of airportal operations, only recently has it become possible to...

  2. V-Band Wireless Surface Networks, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — NASA GLENN RESEARCH CENTER in Topic O1.10 has identified the need to provide surface communications networks for human and robotic missions to explore the Moon and...

  3. Inhibition of Biofilm Formation Using Novel Nanostructured Surfaces, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — Biofilms are ubiquitous in the environment. Few surfaces resist biofilm formation, most promote it. Biofilm formation poses problems in water systems as they can...

  4. Engineered Multifunction Surfaces for Fluid Handling, Phase II

    Data.gov (United States)

    National Aeronautics and Space Administration — ORBITEC will investigate new nanocoating and other engineered surfaces and apply them to passive control of humidity within confined spaces while minimizing power,...

  5. Microscopic Analysis and Modeling of Airport Surface Sequencing, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — The complexity and interdependence of operations on the airport surface motivate the need for a comprehensive and detailed, yet flexible and validated analysis and...

  6. Dust Mitigation for the Lunar Surface, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — The lunar surface is to a large extent covered with a dust layer several meters thick. Known as lunar regolith, it poses a hazard in the form of dust clouds being...

  7. Dust Mitigation for the Lunar Surface, Phase II

    Data.gov (United States)

    National Aeronautics and Space Administration — The lunar surface is, to a large extent, covered with a dust layer several meters thick. Known as lunar regolith, it has been produced by meteorite impacts since the...

  8. Surface Operations Data Analysis and Adaptation Tool, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — The Surface Management System (SMS), developed by NASA Ames Research Center in cooperation with the FAA, has received wide and significant acceptance by the air...

  9. In-Situ Extended Lateral Range Surface Metrology, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — We propose to develop an extended lateral range capability for a dynamic optical profiling system to enable non-contact, surface roughness measurement of large and...

  10. Morphing Flight Control Surface for Advanced Flight Performance, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — In this SBIR project, a new Morphing Flight Control Surface (MFCS) will be developed. The distinction of the research effort is that the SenAnTech team will employ...

  11. Surface Optimization Techniques for Deployable Reflectors, Phase II

    Data.gov (United States)

    National Aeronautics and Space Administration — Under this and several other programs, CTD has developed TEMBOREG deployable solid-surface reflectors (TEMBOREG Reflectors) to provide future NASA and Air Force...

  12. Enhanced Prediction of Gear Tooth Surface Fatigue Life, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — Sentient will develop an enhanced prediction of gear tooth surface fatigue life with rigorous analysis of the tribological phenomena that contribute to pitting...

  13. Figuring and Polishing Precision Optical Surfaces, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — The requirements for cost effective manufacturing and metrology of large optical surfaces is instrumental for the success of future NASA programs such as LISA,...

  14. Flexible and Safe Control of Mobile Surface Systems, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — The primary innovation of this work is a novel Petri net based approach for safe and flexible control of highly capable mobile surface systems, such as long-duration...

  15. Flexible and Safe Control of Mobile Surface Systems, Phase II

    Data.gov (United States)

    National Aeronautics and Space Administration — The primary innovation of this work is a novel approach for flexible and safe control of highly capable mobile surface systems, such as long-duration science rovers,...

  16. Multifunctional Coating for Crew Cabin Surfaces and Fabrics, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — NASA's crewed spacecrafts require routine cleaning of particulate, moisture, organic, and salt contaminants on the crew cabin surfaces and fabrics. Self-cleaning...

  17. A Surface-Mounted Rotor State Sensing System, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — A surface-mounted instrumentation system for measuring rotor blade motions on rotorcraft, for use both in flight and in wind tunnel testing, is proposed for...

  18. Derivation of the Wenzel and Cassie Equations from a Phase Field Model for Two Phase Flow on Rough Surface

    KAUST Repository

    Xu, Xianmin

    2010-01-01

    In this paper, the equilibrium behavior of an immiscible two phase fluid on a rough surface is studied from a phase field equation derived from minimizing the total free energy of the system. When the size of the roughness becomes small, we derive the effective boundary condition for the equation by the multiple scale expansion homogenization technique. The Wenzel and Cassie equations for the apparent contact angles on the rough surfaces are then derived from the effective boundary condition. The homogenization results are proved rigorously by the F-convergence theory. © 2010 Society for Industrial and Applied Mathematics.

  19. Surface and upper air meteorological features during onset phase

    Indian Academy of Sciences (India)

    There was a sharp fall in the temperature difference between 850 and 500 hPa, and the height of zero degree isotherm about 2–3 days before the monsoon onset. The flux of sensible heat was positive (sea to air) over south Arabian Sea during the onset phase. Over the Bay of Bengal higher negative (air to sea) values of ...

  20. Stationary plume induced by carbon dioxide dissolution

    International Nuclear Information System (INIS)

    Nadal, F.; Meunier, P.; Pouligny, B.; Laurichesse, E.

    2013-01-01

    In this paper, laminar convection flows induced by carbon dioxide absorption are addressed from experimental, numerical and theoretical points of view. A vertical glass tube (of centimetre scale) filled with distilled water is subjected to a sudden increase in the partial pressure of carbon dioxide. As a result of the diffusion of the gas into the unsaturated solution, a thin layer of fluid located underneath the surface becomes heavier. This initial density gradient first destabilizes to form a plume, which goes downwards through the entire cell. After a first transient pulsating regime (periodic succession of such Rayleigh-Benard plumes), a stationary flow settles in the tube, which is maintained by the constant supply of gas at the surface. At late stages, this stationary regime is followed by an aperiodic regime, which lasts until the complete saturation of the solution (thermodynamic equilibrium). The present study only focuses on the stationary regime, whose characteristics appear to be almost independent of the Bond number and the aspect ratio but strongly dependent on the chemical Rayleigh number. Three decades of Rayleigh numbers are explored using particle image velocimetry measurements, which allows for a precise determination of the scaling exponents for the vertical velocity amplitude and the plume width. The assumption that gravity and a constant pressure gradient balance the viscous effects enables us to derive an analytic expression for the stationary vertical velocity on the axis, which scales as Ra 2/3 (ln Ra) 1/3 . As a consequence, the width of the plume scales as Ra -1/6 (ln Ra) -1/3 and the mass Nusselt number as (Ra= ln Ra) 1/3 . These scalings are in excellent agreement with the experimental and numerical results. The multiplicative constants of these scalings can also be calculated and show a fairly good agreement if a rigid boundary condition (no-slip) is assumed at the free surface. (authors)

  1. A Two-Phase Cooling Loop for Fission Surface Power Waste Heat Transport, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — Current lunar-based Fission Surface Power (FSP) Systems that will support sustained surface outposts consist of a nuclear reactor with power converters, whose waste...

  2. Measurement range of phase retrieval in optical surface and wavefront metrology

    International Nuclear Information System (INIS)

    Brady, Gregory R.; Fienup, James R.

    2009-01-01

    Phase retrieval employs very simple data collection hardware and iterative algorithms to determine the phase of an optical field. We have derived limitations on phase retrieval, as applied to optical surface and wavefront metrology, in terms of the speed of beam (i.e., f-number or numerical aperture) and amount of aberration using arguments based on sampling theory and geometrical optics. These limitations suggest methodologies for expanding these ranges by increasing the complexity of the measurement arrangement, the phase-retrieval algorithm, or both. We have simulated one of these methods where a surface is measured at unusual conjugates

  3. Surface and upper air meteorological features during onset phase of ...

    Indian Academy of Sciences (India)

    Over the Bay of Bengal higher negative (air to sea) values of sensible flux prevailed before the monsoon onset which became less negative with the advance of monsoon over that region. The pre-onset period was characterized by large sea surface temperature (SST) gradient over the Arabian Sea with rapid decrease ...

  4. Study on removal of phase lines in welding pool surface shape sensing

    Science.gov (United States)

    Wei, Yiqing; Liu, Nansheng; Hu, Xian; Ai, Xiaopu; Wei, Sheng; Liu, Xiaorui

    2009-11-01

    In recent years, arc welding pool surface shape sensing becomes a hot spot in the field of welding automation. In order to restore the pool surface shape, we first need to photograph the pool surface, and then extract useful information from the acquired images. In arc welding surface shape sensing system based on structured light projection, the raster images obtained by charge-coupled device (CCD) are seriously affected by strong arc and spatter, etc. resulting in errors of phase unwrapping, and thus seriously affecting the surface shape recovery. To address phase lines of unwrapping errors, this paper presents a two-neighborhood method. First we analyzed the characteristics of phase lines in the phase diagram, then by comparison of phase diagrams or phase difference diagrams processed before and after, the effectiveness of two-neighborhood method was confirmed, finally this method was applied to the actual pool phase diagram processing, experimental results also confirmed this two-neighborhood method is feasible in removal of phase lines.

  5. Identification of IbeR as a Stationary-Phase Regulator in Meningitic Escherichia coli K1 that Carries a Loss-of-Function Mutation in rpoS

    Directory of Open Access Journals (Sweden)

    Feng Chi

    2009-01-01

    Full Text Available IbeR is a regulator present in meningitic Escherichia coli strain E44 that carries a loss-of-function mutation in the stationary-phase (SP regulatory gene rpoS. In order to determine whether IbeR is an SP regulator in E44, two-dimensional gel electrophoresis and LC-MS were used to compare the proteomes of a noninvasive ibeR deletion mutant BR2 and its parent strain E44 in the SP. Four up-regulated (TufB, GapA, OmpA, AhpC and three down-regulated (LpdA, TnaA, OpmC proteins in BR2 were identified when compared to E44. All these proteins contribute to energy metabolism or stress resistance, which is related to SP regulation. One of the down-regulated proteins, tryptophanase (TnaA, which is regulated by RpoS in other E. coli strains, is associated with SP regulation via production of a signal molecule indole. Our studies demonstrated that TnaA was required for E44 invasion, and that indole was able to restore the noninvasive phenotype of the tnaA mutant. The production of indole was significantly reduced in BR2, indicating that ibeR is required for the indole production via tnaA. Survival studies under different stress conditions indicated that IbeR contributed to bacteria stress resistance in the SP. Taken together, IbeR is a novel regulator contributing to the SP regulation.

  6. High Sensitivity Semiconductor Sensor Skins for Multi-Axis Surface Pressure Characterization, Phase II

    Data.gov (United States)

    National Aeronautics and Space Administration — This NASA Phase II SBIR program would fabricate high sensitivity semiconductor nanomembrane 'sensor skins' capable of multi-axis surface pressure characterization on...

  7. High Sensitivity Semiconductor Sensor Skins for Multi-Axis Surface Pressure Characterization, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — This NASA Phase I SBIR program would fabricate high sensitivity semiconductor nanomembrane 'sensor skins' capable of multi-axis surface pressure characterization on...

  8. Thermal Infrared Spectra of Microcrystalline Sedimentary Phases: Effects of Natural Surface Roughness on Spectral Feature Shape

    Science.gov (United States)

    Hardgrove, C.; Rogers, A. D.

    2012-03-01

    Thermal infrared spectral features of common microcrystalline phases (chert, alabaster, micrite) are presented. Spectra are sensitive to mineralogy and micron-scale (~1-25 µm) surface roughness. Roughness is on the scale of the average crystal size.

  9. Effect of phase coupling on surface amplitude distribution of wind waves

    Digital Repository Service at National Institute of Oceanography (India)

    Varkey, M.J.

    Nonlinear features of wind generated surface waves are considered here to be caused by nonrandomness (non-Uniform) in the phase spectrum. Nonrandomness in recorded waves, if present, would be generally obscured within the error level of observations...

  10. Ocean Surface Current Vectors from MODIS Terra/Aqua Sea Surface Temperature Image Pairs, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — Satellites that record imagery of the same sea surface area, at times separated by a few hours, can be used to estimate ocean surface velocity fields based on the...

  11. Phase mixing and surface wave decay in an inhomogeneous plasma

    International Nuclear Information System (INIS)

    Cally, P.S.; Sedlacek, Z.

    1992-02-01

    The decay rate is calculated of an Alfven or plasma surface wave propagating along an inhomogeneous layer of plasma. The inhomogeneous profile is thin and odd, but otherwise arbitrary. The wave's decay rate is determined using two fundamentally different methods, the integral-differential equation approach of Sedlacek and the Fourier expansion technique of Cally, and found by both to depend only on the slope of the Alfven or plasma frequency profile at the r esonant point , and not on other details of its shape. The result is verified numerically. This problem represents a good example with which to compare and contrast the two methods. (author) 3 figs., 7 refs

  12. Modeling and computation of two phase geometric biomembranes using surface finite elements

    OpenAIRE

    Elliott, Charles M.; Stinner, Björn

    2010-01-01

    Biomembranes consisting of multiple lipids may involve phase separation phenomena leading to coexisting domains of different lipid compositions. The modeling of such biomembranes involves an elastic or bending energy together with a line energy associated with the phase interfaces. This leads to a free boundary problem for the phase interface on the unknown equilibrium surface which minimizes an energy functional subject to volume and area constraints. In this paper we propose a new computati...

  13. Stationary Random Metrics on Hierarchical Graphs Via {(min,+)}-type Recursive Distributional Equations

    Science.gov (United States)

    Khristoforov, Mikhail; Kleptsyn, Victor; Triestino, Michele

    2016-07-01

    This paper is inspired by the problem of understanding in a mathematical sense the Liouville quantum gravity on surfaces. Here we show how to define a stationary random metric on self-similar spaces which are the limit of nice finite graphs: these are the so-called hierarchical graphs. They possess a well-defined level structure and any level is built using a simple recursion. Stopping the construction at any finite level, we have a discrete random metric space when we set the edges to have random length (using a multiplicative cascade with fixed law {m}). We introduce a tool, the cut-off process, by means of which one finds that renormalizing the sequence of metrics by an exponential factor, they converge in law to a non-trivial metric on the limit space. Such limit law is stationary, in the sense that glueing together a certain number of copies of the random limit space, according to the combinatorics of the brick graph, the obtained random metric has the same law when rescaled by a random factor of law {m} . In other words, the stationary random metric is the solution of a distributional equation. When the measure m has continuous positive density on {mathbf{R}+}, the stationary law is unique up to rescaling and any other distribution tends to a rescaled stationary law under the iterations of the hierarchical transformation. We also investigate topological and geometric properties of the random space when m is log-normal, detecting a phase transition influenced by the branching random walk associated to the multiplicative cascade.

  14. Analysis of free-surface flows through energy considerations: Single-phase versus two-phase modeling.

    Science.gov (United States)

    Marrone, Salvatore; Colagrossi, Andrea; Di Mascio, Andrea; Le Touzé, David

    2016-05-01

    The study of energetic free-surface flows is challenging because of the large range of interface scales involved due to multiple fragmentations and reconnections of the air-water interface with the formation of drops and bubbles. Because of their complexity the investigation of such phenomena through numerical simulation largely increased during recent years. Actually, in the last decades different numerical models have been developed to study these flows, especially in the context of particle methods. In the latter a single-phase approximation is usually adopted to reduce the computational costs and the model complexity. While it is well known that the role of air largely affects the local flow evolution, it is still not clear whether this single-phase approximation is able to predict global flow features like the evolution of the global mechanical energy dissipation. The present work is dedicated to this topic through the study of a selected problem simulated with both single-phase and two-phase models. It is shown that, interestingly, even though flow evolutions are different, energy evolutions can be similar when including or not the presence of air. This is remarkable since, in the problem considered, with the two-phase model about half of the energy is lost in the air phase while in the one-phase model the energy is mainly dissipated by cavity collapses.

  15. Extended averaging phase-shift schemes for Fizeau interferometry on high-numerical-aperture spherical surfaces

    Science.gov (United States)

    Burke, Jan

    2010-08-01

    Phase-shifting Fizeau interferometry on spherical surfaces is impaired by phase-shift errors increasing with the numerical aperture, unless a custom optical set-up or wavelength shifting is used. This poses a problem especially for larger numerical apertures, and requires good error tolerance of the phase-shift method used; but it also constitutes a useful testing facility for phase-shift formulae, because a vast range of phase-shift intervals can be tested in a single measurement. In this paper I show how the "characteristic polynomials" method can be used to generate a phase-shifting method for the actual numerical aperture, and analyse residual cyclical phase errors by comparing a phase map from an interferogram with a few fringes to a phase mpa from a nulled fringe. Unrelated to the phase-shift miscalibration, thirdharmonic error fringes are found. These can be dealt with by changing the nominal phase shift from 90°/step to 60°/step and re-tailoring the evaluation formula for third-harmonic rejection. The residual error has the same frequency as the phase-shift signal itself, and can be removed by averaging measurements. Some interesting features of the characteristic polynomials for the averaged formulae emerge, which also shed some light on the mechanism that generates cyclical phase errors.

  16. Final report on the surface-based investigation phase (phase 1) at the Mizunami Underground Research Laboratory project

    International Nuclear Information System (INIS)

    Saegusa, Hiromitsu; Matsuoka, Toshiyuki

    2011-03-01

    The Mizunami Underground Research Laboratory (MIU) Project is a comprehensive research project investigating the deep underground environment within crystalline rock being conducted by Japan Atomic Energy Agency at Mizunami City in Gifu Prefecture, central Japan and its role is defined in 'Framework for Nuclear Energy Policy' by Japan Atomic Energy Commission. The MIU Project has three overlapping phases: Surface-based Investigation phase (Phase I), Construction phase (Phase II), and Operation phase (Phase III), with a total duration of 20 years. The overall project goals of the MIU Project from Phase I through to Phase III are: 1) to establish techniques for investigation, analysis and assessment of the deep geological environment, and 2) to develop a range of engineering for deep underground application. During Phase I, the overall project goals were supported by Phase I goals. For the overall project goals 1), the Phase I goals were set to construct models of the geological environment from all surface-based investigation results that describe the geological environment prior to excavation and predict excavation response. For the overall project goals 2), the Phase I goals were set to formulate detailed design concepts and a construction plan for the underground facilities. This report summarizes the Phase I investigation which was completed in March 2005. The authors believe this report will make an important milestone, since this report clarifies how the Phase I goals are achieved and evaluate the future issues thereby direct the research which will be conducted during Phase II. With regard to the overall project goals 1), 'To establish techniques for investigation, analysis and assessment of the deep geological environment,' a step-wise investigation was conducted by iterating investigation, interpretation, and assessment, thereby understanding of geologic environment was progressively and effectively improved with progress of investigation. An optimal

  17. Coherent Surface Clutter Suppression Techniques with Topography Estimation for Multi-Phase-Center Radar Ice Sounding

    DEFF Research Database (Denmark)

    Nielsen, Ulrik; Dall, Jørgen; Kristensen, Steen Savstrup

    2012-01-01

    Radar ice sounding enables measurement of the thickness and internal structures of the large ice sheets on Earth. Surface clutter masking the signal of interest is a major obstacle in ice sounding. Algorithms for surface clutter suppression based on multi-phase-center radars are presented...

  18. Coherent Surface Clutter Suppression Techniques with Topography Estimation for Multi-Phase-Center Radar Ice Sounding

    DEFF Research Database (Denmark)

    Nielsen, Ulrik; Dall, Jørgen; Kristensen, Steen Savstrup

    2012-01-01

    Radar ice sounding enables measurement of the thickness and internal structures of the large ice sheets on Earth. Surface clutter masking the signal of interest is a major obstacle in ice sounding. Algorithms for surface clutter suppression based on multi-phase-center radars are presented. These ...

  19. Lateral phase separation in polymer-blend thin films: surface bifurcation.

    Science.gov (United States)

    Coveney, Sam; Clarke, Nigel

    2014-06-01

    We use simulations of a binary polymer blend confined between selectively attracting walls to identify and explain the mechanism of lateral phase separation via a transient wetting layer. We first show that equilibrium phases in the film are described by one-dimensional phase equilibria in the vertical (depth) dimension, and demonstrate that effective boundary conditions imposed by the film walls pin the film profile at the walls. We then show that, prior to lateral phase separation, distortion of the interface in a transient wetting layer is coupled to lateral phase separation at the walls. Using Hamiltonian phase portraits, we explain a "surface bifurcation mechanism" whereby the volume fraction at the walls evolves and controls the dynamics of the phase separation. We suggest how solvent evaporation may assist our mechanism.

  20. Contributions of gas-phase plasma chemistry to surface modifications and gas-surface interactions: investigations of fluorocarbon rf plasmas

    Science.gov (United States)

    Cuddy, Michael F., II

    The fundamental aspects of inductively coupled fluorocarbon (FC) plasma chemistry were examined, with special emphasis on the contributions of gas-phase species to surface modifications. Characterization of the gas-phase constituents of single-source CF4-, C2F6-, C3F 8-, and C3F6-based plasmas was performed using spectroscopic and mass spectrometric techniques. The effects of varying plasma parameters, including applied rf power (P) and system pressure (p) were examined. Optical emission spectroscopy (OES) and laser-induced fluorescence (LIF) spectroscopy were employed to monitor the behavior of excited and ground CFx (x = 1,2) radicals, respectively. Mass spectrometric techniques, including ion energy analyses, elucidated behaviors of nascent ions in the FC plasmas. These gas-phase data were correlated with the net effect of substrate processing for Si and ZrO2 surfaces. Surface-specific analyses were performed for post-processed substrates via x-ray photoelectron spectroscopy (XPS) and contact angle goniometry. Generally, precursors with lower F/C ratios tended to deposit robust FC films of high surface energy. Precursors of higher F/C ratio, such as CF4, were associated with etching or removal of material from surfaces. Nonetheless, a net balance between deposition of FC moieties and etching of material exists for each plasma system. The imaging of radicals interacting with surfaces (IRIS) technique provided insight into the phenomena occurring at the interface of the plasma gas-phase and substrate of interest. IRIS results demonstrate that CFx radicals scatter copiously, with surface scatter coefficients, S, generally greater than unity under most experimental conditions. Such considerable S values imply surface-mediated production of the CFx radicals at FC-passivated sites. It is inferred that the primary route to surface production of CFx arises from energetic ion bombardment and ablation of surface FC films. Other factors which may influence the observed CFx

  1. Phase analysis for three-dimensional surface reconstruction of apples using structured-illumination reflectance imaging

    Science.gov (United States)

    Lu, Yuzhen; Lu, Renfu

    2017-05-01

    Three-dimensional (3-D) shape information is valuable for fruit quality evaluation. This study was aimed at developing phase analysis techniques for reconstruction of the 3-D surface of fruit from the pattern images acquired by a structuredillumination reflectance imaging (SIRI) system. Phase-shifted sinusoidal patterns, distorted by the fruit geometry, were acquired and processed through phase demodulation, phase unwrapping and other post-processing procedures to obtain phase difference maps relative to the phase of a reference plane. The phase maps were then transformed into height profiles and 3-D shapes in a world coordinate system based on phase-to-height and in-plane calibrations. A reference plane-based approach, coupled with the curve fitting technique using polynomials of order 3 or higher, was utilized for phase-to-height calibrations, which achieved superior accuracies with the root-mean-squared errors (RMSEs) of 0.027- 0.033 mm for a height measurement range of 0-91 mm. The 3rd-order polynomial curve fitting technique was further tested on two reference blocks with known heights, resulting in relative errors of 3.75% and 4.16%. In-plane calibrations were performed by solving a linear system formed by a number of control points in a calibration object, which yielded a RMSE of 0.311 mm. Tests of the calibrated system for reconstructing the surface of apple samples showed that surface concavities (i.e., stem/calyx regions) could be easily discriminated from bruises from the phase difference maps, reconstructed height profiles and the 3-D shape of apples. This study has laid a foundation for using SIRI for 3-D shape measurement, and thus expanded the capability of the technique for quality evaluation of horticultural products. Further research is needed to utilize the phase analysis techniques for stem/calyx detection of apples, and optimize the phase demodulation and unwrapping algorithms for faster and more reliable detection.

  2. Surface roughness of Saturn's rings and ring particles inferred from thermal phase curves

    Science.gov (United States)

    Morishima, Ryuji; Turner, Neal; Spilker, Linda

    2017-10-01

    We analyze thermal phase curves of all the main rings of Saturn (the A, B, C rings, and the Cassini division) measured by both the far-IR and mid-IR detectors of the Cassini Composite InfraRed Spectrometer (CIRS). All the rings show temperature increases toward zero phase angle, known as an opposition effect or thermal beaming. For the C ring and Cassini division, which have low optical depths, intra-particle shadowing is considered the dominant mechanism causing the effect. On the other hand, the phase curves of the optically thick B and A rings steepen significantly with decreasing absolute solar elevation angle from 21° to 14°, suggesting inter-particle shadowing plays an important role in these rings. We employ an analytic roughness model to estimate the degrees of surface roughness of the rings or ring particles. For optically thin rings, an isolated particle covered by spherical segment craters is employed while for the thick rings we approximate a packed particle layer as a slab covered by craters. The particles in the thin rings are found to have generally rough surfaces, except in the middle C ring. Across the C ring, the optical depth correlates with the degree of surface roughness. This may indicate that surface roughness comes mainly from particle clumping, while individual particles have rather smooth surfaces. For the optically thick rings, the surface roughness of the particle layer is found to be moderate. The modeled phase curves of optically thick rings are shallow if the phase angle change is primarily due to change of observer azimuthal angle. On the other hand, the phase curves are steep if the phase angle change is due to change of observer elevation angle, as inter-particle shadows become visible at higher observer elevation. In addition, the area of shadowed facets increases with decreasing solar elevation angle. These combined effects explain the large seasonal change of the phase curve steepness observed for the thick rings. The degrees

  3. Surface morphology changes of acrylic resins during finishing and polishing phases

    Directory of Open Access Journals (Sweden)

    Glaucio Serra

    2013-12-01

    Full Text Available INTRODUCTION: The finishing and polishing phases are essential to improve smoothness and shining on the surface of acrylic resins used to make removable orthodontic appliances. A good surface finishing reduces roughness, which facilitates hygiene, prevents staining and provides greater comfort to the patients. OBJECTIVE: The aim of this paper was to analyze the changes on surface morphology of acrylic resins during finishing and polishing phases. METHODS: Thirty discs (10 mm in diameter and 5 mm in length were made with acrylic resin and randomly divided into ten groups. The control group did not receive any treatment while the other groups received gradual finishing and polishing. The last group received the entire finishing and polishing procedures. Surface morphology was qualitatively analyzed through scanning electron microscopy and quantitatively analyzed through a laser profilometer test. RESULTS: The acrylic resin surfaces without treatment showed bubbles which were not observed in the subsequent phases. Wearing out with multilaminated burs, finishing with wood sandpaper and finishing with water sandpaper resulted in surfaces with decreasing irregularities. The surfaces that were polished with pumice and with low abrasive liquids showed high superficial smoothness. CONCLUSION: Highly smooth acrylic resin surfaces can be obtained after mechanical finishing and polishing performed with multilaminated burs, wood sandpaper, water sandpaper, pumice and low abrasive liquids.

  4. The Changing Relationship between Surface Temperatures and Indian Monsoon Rainfall with the Phase of ESI Tendency

    Directory of Open Access Journals (Sweden)

    S. B. Kakade

    2012-01-01

    Full Text Available Effective Strength Index (ESI is the relative strength of NAO and SO. ESI tendency is the algebraic difference between April-ESI and January-ESI and it represents the simultaneous evolution of NAO and SO from winter to spring. During positive (negative phase of ESI tendency, NAO restores positive (negative phase and SO restores negative (positive phase before the beginning of summer season. Thus during contrasting phases (positive and negative of ESI tendency, the evolution of NAO and SO is out of phase. In this paper we have studied the spatial and temporal variability of winter-time temperature field over Europe, Arabian Sea and Bay of Bengal during contrasting phases of ESI tendency. The study reveals that during positive (negative ESI tendency, smaller (larger region of Europe is showing significant winter-time cooling (warming at surface. The relationship between winter-time surface temperature over above regions and Indian summer monsoon rainfall (ISMR also shows spatial and temporal variability. The probable explanation for this change in the relationship is discussed in the paper. Two sets of temperature parameters for two different phases of ESI tendency are found out. Multiple regression equations are developed for the prediction of ISMR in each phase of ESI tendency. The performance of these equations is also discussed in this paper.

  5. Calculation of the surface potential and surface charge density by measurement of the three-phase contact angle.

    Science.gov (United States)

    Horiuchi, H; Nikolov, A; Wasan, D T

    2012-11-01

    The silica/silicon wafer is widely used in the semiconductor industry in the manufacture of electronic devices, so it is essential to understand its physical chemistry and determine the surface potential at the silica wafer/water interface. However, it is difficult to measure the surface potential of a silica/silicon wafer directly due to its high electric resistance. In the present study, the three-phase contact angle (TPCA) on silica is measured as a function of the pH. The surface potential and surface charge density at the silica/water surface are calculated by a model based on the Young-Lippmann equation in conjunction with the Gouy-Chapman model for the electric double layer. In measurements of the TPCA on silica, two distinct regions were identified with a boundary at pH 9.5-showing a dominance of the surface ionization of silanol groups below pH 9.5 and a dominance of the dissolution of silica into the aqueous solution above pH 9.5. Since the surface chemistry changes above pH 9.5, the model is applied to solutions below pH 9.5 (ionization dominant) for the calculation of the surface potential and surface charge density at the silica/aqueous interface. In order to evaluate the model, a galvanic mica cell was made of a mica sheet and the surface potential was measured directly at the mica/water interface. The model results are also validated by experimental data from the literature, as well as the results obtained by the potentiometric titration method and the electro-kinetic measurements. Copyright © 2012 Elsevier Inc. All rights reserved.

  6. Surface based cardiac and respiratory motion extraction for pulmonary structures from multi-phase CT

    Science.gov (United States)

    von Berg, Jens; Barschdorf, Hans; Blaffert, Thomas; Kabus, Sven; Lorenz, Cristian

    2007-03-01

    During medical imaging and therapeutic interventions, pulmonary structures are in general subject to cardiac and respiratory motion. This motion leads potentially to artefacts and blurring in the resulting image material and to uncertainties during interventions. This paper presents a new automatic approach for surface based motion tracking of pulmonary structures and reports on the results for cardiac and respiratory induced motion. The method applies an active shape approach to ad-hoc generated surface representations of the pulmonary structures for phase to phase surface tracking. Input of the method are multi-phase CT data, either cardiac or respiratory gated. The iso-surface representing the transition between air or lung parenchyma to soft tissue, is triangulated for a selected phase p 0. An active shape procedure is initialised in the image of phase p I using the generated surface in p 0. The used internal energy term penalizes shape deformation as compared to p 0. The process is iterated for all phases p i to p i+1 of the complete cycle. Since the mesh topology is the same for all phases, the vertices of the triangular mesh can be treated as pseudo-landmarks defining tissue trajectories. A dense motion field is interpolated. The motion field was especially designed to estimate the error margins for radiotherapy. In the case of respiratory motion extraction, a validation on ten biphasic thorax CT images (2.5mm slice distance) was performed with expert landmarks placed at vessel bifurcations. The mean error on landmark position was below 2.6mm. We further applied the method to ECG gated images and estimated the influence of the heart beat on lung tissue displacement.

  7. Influence of Stationary Crossflow Modulation on Secondary Instability

    Science.gov (United States)

    Choudhari, Meelan M.; Li, Fei; Paredes, Pedro

    2016-01-01

    A likely scenario for swept wing transition on subsonic aircraft with natural laminar flow involves the breakdown of stationary crossflow vortices via high frequency secondary instability. A majority of the prior research on this secondary instability has focused on crossflow vortices with a single dominant spanwise wavelength. This paper investigates the effects of the spanwise modulation of stationary crossflow vortices at a specified wavelength by a subharmonic stationary mode. Secondary instability of the modulated crossflow pattern is studied using planar, partial-differential-equation based eigenvalue analysis. Computations reveal that weak modulation by the first subharmonic of the input stationary mode leads to mode splitting that is particularly obvious for Y-type secondary modes that are driven by the wall-normal shear of the basic state. Thus, for each Y mode corresponding to the fundamental wavelength of results in unmodulated train of crossflow vortices, the modulated flow supports a pair of secondary modes with somewhat different amplification rates. The mode splitting phenomenon suggests that a more complex stationary modulation such as that induced by natural surface roughness would yield a considerably richer spectrum of secondary instability modes. Even modest levels of subharmonic modulation are shown to have a strong effect on the overall amplification of secondary disturbances, particularly the Z-modes driven by the spanwise shear of the basic state. Preliminary computations related to the nonlinear breakdown of these secondary disturbances provide interesting insights into the process of crossflow transition in the presence of the first subharmonic of the dominant stationary vortex.

  8. High-performance liquid chromatography separation of cis-trans anthocyanin isomers from wild Lycium ruthenicum Murr. employing a mixed-mode reversed-phase/strong anion-exchange stationary phase.

    Science.gov (United States)

    Jin, Hongli; Liu, Yanfang; Guo, Zhimou; Yang, Fan; Wang, Jixia; Li, Xiaolong; Peng, Xiaojun; Liang, Xinmiao

    2015-01-21

    The cis-trans isomerism is a common phenomenon for acylated anthocyanins. Nevertheless, few studies reported effective methods for the preparation of isomeric anthocyanins from natural products. In this work, a high-performance liquid chromatography (HPLC) method was developed to efficiently purify anthocyanin isomers from Lycium ruthenicum Murr. based on a mixed-mode reversed-phase/strong anion-exchange column (named XCharge C8SAX). Four commercially available columns were evaluated with a pair of isomeric anthocyanins, and the results demonstrated that the XCharge C8SAX column exhibited improved selectivity and column efficiency for the isomers. The chromatographic parameters, including pH, organic content, and ionic strength, were investigated. Optimal separation quality for the anthocyanin isomers was achieved on the XCharge C8SAX column. Six pure anthocyanins, including two pairs of cis-trans isomeric anthocyanins with one new anthocyanin, were purified from L. ruthenicum and identified. All of the results indicated that this method is an effective way to separate anthocyanins, especially for cis-trans isomers.

  9. Surface crystalline phases and nanoindentation hardness of explanted zirconia femoral heads.

    Science.gov (United States)

    Catledge, Shane A; Cook, Monique; Vohra, Yogesh K; Santos, Erick M; McClenny, Michelle D; David Moore, K

    2003-10-01

    One new and nine explanted zirconia femoral heads were studied using glancing angle X-ray diffraction, scanning electron microscopy, and nanoindentation hardness techniques. All starting zirconia implants consisted only of tetragonal zirconia polycrystals (TZP). For comparison, one explanted alumina femoral head was also studied. Evidence for a surface tetragonal-to-monoclinic zirconia phase transformation was observed in some implants, the extent of which was varied for different in-service conditions. A strong correlation was found between increasing transformation to the monoclinic phase and decreasing surface hardness. Microscopic investigations of some of the explanted femoral heads revealed ultra high molecular weight polyethylene and metallic transfer wear debris.

  10. Carbon-based nanostructured surfaces for enhanced phase-change cooling

    Science.gov (United States)

    Selvaraj Kousalya, Arun

    To maintain acceptable device temperatures in the new generation of electronic devices under development for high-power applications, conventional liquid cooling schemes will likely be superseded by multi-phase cooling solutions to provide substantial enhancement to the cooling capability. The central theme of the current work is to investigate the two-phase thermal performance of carbon-based nanostructured coatings in passive and pumped liquid-vapor phase-change cooling schemes. Quantification of the critical parameters that influence thermal performance of the carbon nanostructured boiling surfaces presented herein will lead to improved understanding of the underlying evaporative and boiling mechanisms in such surfaces. A flow boiling experimental facility is developed to generate consistent and accurate heat transfer performance curves with degassed and deionized water as the working fluid. New means of boiling heat transfer enhancement by altering surface characteristics such as surface energy and wettability through light-surface interactions is explored in this work. In this regard, carbon nanotube (CNT) coatings are exposed to low-intensity irradiation emitted from a light emitting diode and the subcooled flow boiling performance is compared against a non-irradiated CNT-coated copper surface. A considerable reduction in surface superheat and enhancement in average heat transfer coefficient is observed. In another work involving CNTs, the thermal performance of CNT-integrated sintered wick structures is evaluated in a passively cooled vapor chamber. A physical vapor deposition process is used to coat the CNTs with varying thicknesses of copper to promote surface wetting with the working fluid, water. Thermal performance of the bare sintered copper powder sample and the copper-functionalized CNT-coated sintered copper powder wick samples is compared using an experimental facility that simulates the capillary fluid feeding conditions of a vapor chamber

  11. Corrugation of Phase-Separated Lipid Bilayers Supported by Nanoporous Silica Xerogel Surfaces

    Energy Technology Data Exchange (ETDEWEB)

    Goksu, E I; Nellis, B A; Lin, W; Satcher Jr., J H; Groves, J T; Risbud, S H; Longo, M L

    2008-10-30

    Lipid bilayers supported by substrates with nanometer-scale surface corrugations holds interest in understanding both nanoparticle-membrane interactions and the challenges of constructing models of cell membranes on surfaces with desirable properties, e.g. porosity. Here, we successfully form a two-phase (gel-fluid) lipid bilayer supported by nanoporous silica xerogel. Surface topology, diffusion, and lipid density in comparison to mica-supported lipid bilayers were characterized by AFM, FRAP, FCS, and quantitative fluorescence microscopy, respectively. We found that the two-phase lipid bilayer follows the xerogel surface contours. The corrugation imparted on the lipid bilayer results in a lipid density that is twice that on a flat mica surface. In direct agreement with the doubling of actual bilayer area in a projected area, we find that the lateral diffusion coefficient (D) of lipids on xerogel ({approx}1.7 {micro}m{sup 2}/s) is predictably lower than on mica ({approx}4.1 {micro}m{sup 2}/s) by both FRAP and FCS techniques. Furthermore, the gel-phase domains on xerogel compared to mica were larger and less numerous. Overall, our results suggest the presence of a relatively defect-free continuous two-phase bilayer that penetrates approximately midway into the first layer of {approx}50 nm xerogel beads.

  12. Phase Retrieval System for Assessing Diamond Turning and Optical Surface Defects

    Science.gov (United States)

    Dean, Bruce; Maldonado, Alex; Bolcar, Matthew

    2011-01-01

    An optical design is presented for a measurement system used to assess the impact of surface errors originating from diamond turning artifacts. Diamond turning artifacts are common by-products of optical surface shaping using the diamond turning process (a diamond-tipped cutting tool used in a lathe configuration). Assessing and evaluating the errors imparted by diamond turning (including other surface errors attributed to optical manufacturing techniques) can be problematic and generally requires the use of an optical interferometer. Commercial interferometers can be expensive when compared to the simple optical setup developed here, which is used in combination with an image-based sensing technique (phase retrieval). Phase retrieval is a general term used in optics to describe the estimation of optical imperfections or aberrations. This turnkey system uses only image-based data and has minimal hardware requirements. The system is straightforward to set up, easy to align, and can provide nanometer accuracy on the measurement of optical surface defects.

  13. Stationary wave patterns in deep water | Doyle | Quaestiones ...

    African Journals Online (AJOL)

    ship" or an obstacle in a stream, is revisited. The wave patterns are calculated using the results of the method of stationary phase. This allows for an elegant geometrical construction in which the reciprocal polar of the wave normal diagram ...

  14. A Variational Model for Two-Phase Immiscible Electroosmotic Flow at Solid Surfaces

    KAUST Repository

    Shao, Sihong

    2012-01-01

    We develop a continuum hydrodynamic model for two-phase immiscible flows that involve electroosmotic effect in an electrolyte and moving contact line at solid surfaces. The model is derived through a variational approach based on the Onsager principle of minimum energy dissipation. This approach was first presented in the derivation of a continuum hydrodynamic model for moving contact line in neutral two-phase immiscible flows (Qian, Wang, and Sheng, J. Fluid Mech. 564, 333-360 (2006)). Physically, the electroosmotic effect can be formulated by the Onsager principle as well in the linear response regime. Therefore, the same variational approach is applied here to the derivation of the continuum hydrodynamic model for charged two-phase immiscible flows where one fluid component is an electrolyte exhibiting electroosmotic effect on a charged surface. A phase field is employed to model the diffuse interface between two immiscible fluid components, one being the electrolyte and the other a nonconductive fluid, both allowed to slip at solid surfaces. Our model consists of the incompressible Navier-Stokes equation for momentum transport, the Nernst-Planck equation for ion transport, the Cahn-Hilliard phase-field equation for interface motion, and the Poisson equation for electric potential, along with all the necessary boundary conditions. In particular, all the dynamic boundary conditions at solid surfaces, including the generalized Navier boundary condition for slip, are derived together with the equations of motion in the bulk region. Numerical examples in two-dimensional space, which involve overlapped electric double layer fields, have been presented to demonstrate the validity and applicability of the model, and a few salient features of the two-phase immiscible electroosmotic flows at solid surface. The wall slip in the vicinity of moving contact line and the Smoluchowski slip in the electric double layer are both investigated. © 2012 Global-Science Press.

  15. Ceramic Stationary Gas Turbine Development. Technical progress report, April 1, 1993--October 31, 1994

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    1994-12-01

    This report summarizes work performed by Solar Technologies Inc. and its subcontractors, during the period April 1, 1993 through October 31, 1994 under Phase II of the DOE Ceramic Stationary Gas Turbine Development program. The objective of the program is to improve the performance of stationary gas turbines in cogeneration through the implementation of selected ceramic components.

  16. Dispersive and Covalent Interactions between Graphene and Metal Surfaces from the Random Phase Approximation

    DEFF Research Database (Denmark)

    Olsen, Thomas; Yan, Jun; Mortensen, Jens Jørgen

    2011-01-01

    We calculate the potential energy surfaces for graphene adsorbed on Cu(111), Ni(111), and Co(0001) using density functional theory and the random phase approximation (RPA). For these adsorption systems covalent and dispersive interactions are equally important and while commonly used approximations...... for exchange-correlation functionals give inadequate descriptions of either van der Waals or chemical bonds, RPA accounts accurately for both. It is found that the adsorption is a delicate competition between a weak chemisorption minimum close to the surface and a physisorption minimum further from the surface....

  17. Lateral phase separation of mixed polymer brushes on planar and spherical surfaces

    Science.gov (United States)

    van Lehn, Reid; Alexander-Katz, Alfredo

    2012-02-01

    A mixed polymer brush consists of two (or more) polymer species grafted to a surface at a high density, inducing the polymers to highly stretch to maximize favorable solvent interactions while minimizing polymer overlap. The enthalpic and entropic interactions between the different polymers give rise to lateral phase behavior on the surface. Understanding this phase separation behavior is interesting for applications in nanotemplating and controlled protein adsorption. In this work, we present a novel theoretical model to quickly predict lateral phase separated morphologies of mixed polymer brushes on planar, cylindrical and spherical surfaces. The model combines a Flory-Huggins model for enthalpic interactions between the polymer components with an Alexander-de Gennes model for the entropy of the brush layers. When there is a length difference between the polymer components, these two interactions along with the conformational entropy of the system lead to a range of morphologies including stripes, dimples, mixing, and complete phase separation. The computational efficiency of this model allows for phase diagrams to be generated with great accuracy. The results of our model thus allow for the fast prediction of lateral morphologies on different geometries.

  18. Resolution potential of surface wave phase velocity measurements at small arrays

    Science.gov (United States)

    Bodin, Thomas; Maupin, Valérie

    2008-02-01

    The deployment of temporary arrays of broadband seismological stations over dedicated targets is common practice. Measurement of surface wave phase velocity across a small array and its depth-inversion gives us information about the structure below the array which is complementary to the information obtained from body-wave analysis. The question is however: what do we actually measure when the array is much smaller than the wave length, and how does the measured phase velocity relates to the real structure below the array? We quantify this relationship by performing a series of numerical simulations of surface wave propagation in 3-D structures and by measuring the apparent phase velocity across the array on the synthetics. A principal conclusion is that heterogeneities located outside the array can map in a complex way onto the phase velocities measured by the array. In order to minimize this effect, it is necessary to have a large number of events and to average measurements from events well-distributed in backazimuth. A second observation is that the period of the wave has a remarkably small influence on the lateral resolution of the measurement, which is dominantly controlled by the size of the array. We analyse if the artefacts created by heterogeneities can be mistaken for azimuthal variations caused by anisotropy. We also show that if the amplitude of the surface waves can be measured precisely enough, phase velocities can be corrected and the artefacts which occur due to reflections and diffractions in 3-D structures greatly reduced.

  19. Cycle-to-cycle control of swing phase of paraplegic gait induced by surface electrical stimulation

    NARCIS (Netherlands)

    Franken, H.M.; Franken, H.M.; Veltink, Petrus H.; Baardman, G.; Redmeijer, R.A.; Boom, H.B.K.

    1995-01-01

    Parameterised swing phase of gait in paraplegics was obtained using surface electrical stimulation of the hip flexors, hamstrings and quadriceps; the hip flexors were stimulated to obtain a desired hip angle range, the hamstrings to provide foot clearance in the forward swing, and the quadriceps to

  20. On measuring surface wave phase velocity from station–station cross-correlation of ambient signal

    DEFF Research Database (Denmark)

    Boschi, Lapo; Weemstra, Cornelis; Verbeke, Julie

    2012-01-01

    We apply two different algorithms to measure surface wave phase velocity, as a function of frequency, from seismic ambient noise recorded at pairs of stations from a large European network. The two methods are based on consistent theoretical formulations, but differ in the implementation: one met...

  1. Stabilization of the ceria ι-phase (Ce7O12) surface on Si(111)

    Science.gov (United States)

    Wilkens, H.; Schuckmann, O.; Oelke, R.; Gevers, S.; Schaefer, A.; Bäumer, M.; Zoellner, M. H.; Schroeder, T.; Wollschläger, J.

    2013-03-01

    In this work a 250 nm CeO2(111) film grown on a hex-Pr2O3(0001)/Si(111) system is annealed at 660 °C for 30 min to form the ι bulk phase of Ce7O12 as controlled by x-ray photoelectron spectroscopy. The (111) surface of the stabilized ι phase is characterized via high-resolution low-energy electron diffraction. The ι-phase surface exhibits a (√7 ×√7 )R19.1° superstructure with two mirror domains. This structure is attributed to a periodic ordering of oxygen vacancies compared to the fluorite structure of CeO2.

  2. Surface-initiated phase transition in solid hydrogen under the high-pressure compression

    Science.gov (United States)

    Lei, Haile; Lin, Wei; Wang, Kai; Li, Xibo

    2018-03-01

    The large-scale molecular dynamics simulations have been performed to understand the microscopic mechanism governing the phase transition of solid hydrogen under the high-pressure compression. These results demonstrate that the face-centered-cubic-to-hexagonal close-packed phase transition is initiated first at the surfaces at a much lower pressure than in the volume and then extends gradually from the surface to volume in the solid hydrogen. The infrared spectra from the surface are revealed to exhibit a different pressure-dependent feature from those of the volume during the high-pressure compression. It is thus deduced that the weakening intramolecular H-H bonds are always accompanied by hardening surface phonons through strengthening the intermolecular H2-H2 coupling at the surfaces with respect to the counterparts in the volume at high pressures. This is just opposite to the conventional atomic crystals, in which the surface phonons are softening. The high-pressure compression has further been predicted to force the atoms or molecules to spray out of surface to degrade the pressure. These results provide a glimpse of structural properties of solid hydrogen at the early stage during the high-pressure compression.

  3. Tailorable Surface Morphology of 3D Scaffolds by Combining Additive Manufacturing with Thermally Induced Phase Separation.

    Science.gov (United States)

    Di Luca, Andrea; de Wijn, Joost R; van Blitterswijk, Clemens A; Camarero-Espinosa, Sandra; Moroni, Lorenzo

    2017-08-01

    The functionalization of biomaterials substrates used for cell culture is gearing towards an increasing control over cell activity. Although a number of biomaterials have been successfully modified by different strategies to display tailored physical and chemical surface properties, it is still challenging to step from 2D substrates to 3D scaffolds with instructive surface properties for cell culture and tissue regeneration. In this study, additive manufacturing and thermally induced phase separation are combined to create 3D scaffolds with tunable surface morphology from polymer gels. Surface features vary depending on the gel concentration, the exchanging temperature, and the nonsolvent used. When preosteoblasts (MC-3T3 cells) are cultured on these scaffolds, a significant increase in alkaline phosphatase activity is measured for submicron surface topography, suggesting a potential role on early cell differentiation. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Flood frequency analysis of historical flood data under stationary and non-stationary modelling

    Science.gov (United States)

    Machado, M. J.; Botero, B. A.; López, J.; Francés, F.; Díez-Herrero, A.; Benito, G.

    2015-06-01

    Historical records are an important source of information on extreme and rare floods and fundamental to establish a reliable flood return frequency. The use of long historical records for flood frequency analysis brings in the question of flood stationarity, since climatic and land-use conditions can affect the relevance of past flooding as a predictor of future flooding. In this paper, a detailed 400 yr flood record from the Tagus River in Aranjuez (central Spain) was analysed under stationary and non-stationary flood frequency approaches, to assess their contribution within hazard studies. Historical flood records in Aranjuez were obtained from documents (Proceedings of the City Council, diaries, chronicles, memoirs, etc.), epigraphic marks, and indirect historical sources and reports. The water levels associated with different floods (derived from descriptions or epigraphic marks) were computed into discharge values using a one-dimensional hydraulic model. Secular variations in flood magnitude and frequency, found to respond to climate and environmental drivers, showed a good correlation between high values of historical flood discharges and a negative mode of the North Atlantic Oscillation (NAO) index. Over the systematic gauge record (1913-2008), an abrupt change on flood magnitude was produced in 1957 due to constructions of three major reservoirs in the Tagus headwaters (Bolarque, Entrepeñas and Buendia) controlling 80% of the watershed surface draining to Aranjuez. Two different models were used for the flood frequency analysis: (a) a stationary model estimating statistical distributions incorporating imprecise and categorical data based on maximum likelihood estimators, and (b) a time-varying model based on "generalized additive models for location, scale and shape" (GAMLSS) modelling, which incorporates external covariates related to climate variability (NAO index) and catchment hydrology factors (in this paper a reservoir index; RI). Flood frequency

  5. Construção de câmara de luz ultravioleta para fotopolimerização de fases estacionárias monolíticas Coinstruction of ultraviolet-light chamber for monolithic stationary phases photo-polymerization

    Directory of Open Access Journals (Sweden)

    Fernando Antonio Simas Vaz

    2008-01-01

    Full Text Available The assembly of a photochemical reactor with six fluorescent lamps, used for photopolymerizations is described. This chamber presents a mobile support, allowing the placement of samples at different heights and a safety lock that interrupts the radiation, if it is opened during operation. The mirrored internal walls avoid the dispersion and non-uniform distribution of light. There is no high heating because the own character of the used lamps. All parts could be purchased in commerce with less than U$ 150,00. This reactor was successfully used for monolithic stationary phase photopolymerization.

  6. Virtual Stationary Automata for Mobile Networks

    National Research Council Canada - National Science Library

    Dolev, Shlomi; Gilbert, Seth; Lahiani, Limor; Lynch, Nancy; Nolte, Tina

    2005-01-01

    We define a programming abstraction for mobile networks called the Virtual Stationary Automata programming layer, consisting of real mobile clients, virtual timed I/O automata called virtual stationary automata (VSAs...

  7. Formation and structural phase transition in Co atomic chains on a Cu(775) surface

    International Nuclear Information System (INIS)

    Syromyatnikov, A. G.; Kabanov, N. S.; Saletsky, A. M.; Klavsyuk, A. L.

    2017-01-01

    The formation of Co atomic chains on a Cu(775) surface is investigated by the kinetic Monte Carlo method. It is found that the length of Co atomic chains formed as a result of self-organization during epitaxial growth is a random quantity and its mean value depends on the parameters of the experiment. The existence of two structural phases in atomic chains is detected using the density functional theory. In the first phase, the separations between an atom and its two nearest neighbors in a chain are 0.230 and 0.280 nm. In the second phase, an atomic chain has identical atomic spacings of 0.255 nm. It is shown that the temperature of the structural phase transition depends on the length of the atomic chain.

  8. A surface plasmon resonance interferometer based on spatial phase modulation for protein array detection

    Science.gov (United States)

    Yu, Xinglong; Ding, Xiang; Liu, Fangfang; Wei, Xing; Wang, Dingxin

    2008-01-01

    Thousands of kinds of proteins exist in a single cell. Proteomics research aims to characterize these proteins and simultaneously analyse modifications and interactions on a large scale. Here we present a label-free surface plasmon resonance (SPR) imaging interferometer based on spatial phase modulation, which can be useful in this field. It consists of a light source, a SPR sensing unit, a special phase modulator, a photoelectric conversion unit and a computer. Collimated light is projected into a prism and reflected at the gold-glass interface. The p- and s-polarized components of the reflected light pass through a one-dimensional beam expander and a Wollaston prism, and form an interference pattern on a CCD. Interference images are acquired and transferred to the computer for data processing. Protein interaction on the gold surface leads to a local refractive index change and results in interference fringe phase shift. By calculating the phase shift, interaction information can be obtained. It is demonstrated that this technique can detect different concentrations of NaCl solutions, and the phase change generated by a 0.9% NaCl solution is about 10°. In protein-protein interaction experiments, a model system of rabbit IgG and goat-anti-rabbit IgG is tested. The maximum phase change is up to 12°. The phase resolution of the system is 0.2°, equivalent to the refractive index resolution of 3 × 10-5 RIU, and this value can be improved to 2 × 10-6 RIU just by increasing the gold thickness of the sensing chip. It is concluded that the sensitivity of the interferometer is enough to achieve larger capacity than that detected by the present protein micro-array products. These results suggest that the SPR interferometer based on spatial phase modulation provides a potential facility to meet the requirements in proteomics research.

  9. Stationary measure in the multiverse

    Energy Technology Data Exchange (ETDEWEB)

    Linde, Andrei [Department of Physics, Stanford University, Stanford, CA 94305 (United States); Vanchurin, Vitaly; Winitzki, Sergei, E-mail: alinde@stanford.edu, E-mail: vitaly@cosmos2.phy.tufts.edu, E-mail: winitzki@physik.uni-muenchen.de [Department of Physics, Ludwig-Maximilians University, Munich (Germany)

    2009-01-15

    We study the recently proposed ''stationary measure'' in the context of the string landscape scenario. We show that it suffers neither from the ''Boltzmann brain'' problem nor from the ''youngness'' paradox that makes some other measures predict a high CMB temperature at present. We also demonstrate a good performance of this measure in predicting the results of local experiments, such as proton decay.

  10. A stationary q-metric

    Science.gov (United States)

    Toktarbay, S.; Quevedo, H.

    2014-10-01

    We present a stationary generalization of the static $q-$metric, the simplest generalization of the Schwarzschild solution that contains a quadrupole parameter. It possesses three independent parameters that are related to the mass, quadrupole moment and angular momentum. We investigate the geometric and physical properties of this exact solution of Einstein's vacuum equations, and show that it can be used to describe the exterior gravitational field of rotating, axially symmetric, compact objects.

  11. Surface Termination of M1 Phase and Rational Design of Propane Ammoxidation Catalysts

    Energy Technology Data Exchange (ETDEWEB)

    Guliants, Vadim [Univ. of Cincinnati, OH (United States)

    2015-02-16

    This final report describes major accomplishments in this research project which has demonstrated that the M1 phase is the only crystalline phase required for propane ammoxidation to acrylonitrile and that a surface monolayer terminating the ab planes of the M1 phase is responsible for their activity and selectivity in this reaction. Fundamental studies of the topmost surface chemistry and mechanism of propane ammoxidation over the Mo-V-(Te,Sb)-(Nb,Ta)-O M1 and M2 phases resulted in the development of quantitative understanding of the surface molecular structure – reactivity relationships for this unique catalytic system. These oxides possess unique catalytic properties among mixed metal oxides, because they selectively catalyze three alkane transformation reactions, namely propane ammoxidation to acrylonitrile, propane oxidation to acrylic acid and ethane oxidative dehydrogenation, all of considerable economic significance. Therefore, the larger goal of this research was to expand this catalysis to other alkanes of commercial interest, and more broadly, demonstrate successful approaches to rational design of improved catalysts that can be applied to other selective (amm)oxidation processes.

  12. Diurnal variability of gas phase and surface water ethanol in southeastern North Carolina, USA

    Science.gov (United States)

    Kieber, R. J.; Powell, J. P.; Foley, L.; Mead, R. N.; Willey, J. D.; Avery, G. B.

    2017-11-01

    Diurnal variations in gas phase and surface water concentrations of ethanol and acetaldehyde were investigated at five locations in southeastern North Carolina, USA. There were distinct diurnal oscillations observed in gas phase concentrations with maxima occurring in late afternoon suggesting that photochemical production is an important process in the cycling of these analytes in the troposphere. The rapid decrease in concentrations after the mid day maximum suggests that there is also an atmospheric photochemical sink for both analytes most likely involving photo produced hydroxyl radicals with a half-life on the order of hours rather than days at ground level. Ethanol concentrations in the surface microlayer taken at the same time as gas phase samples had a very similar diurnal profile suggesting photochemical processes, in addition to atmospheric deposition, play a role in the aqueous phase cycling of both analytes. The concentration of ethanol and acetaldehyde increased significantly in flasks containing freshwater collected from the Cape Fear River exposed to simulated sunlight for 6 h underscoring the importance of in situ photochemical production. Results of this study are significant because they represent the first simultaneous analyses of the temporal variability of ethanol and acetaldehyde concentrations in the gas and aqueous phases. These measurements are essential in order to better define the processes involved in the global biogeochemical cycling of ethanol both now and in the future as our use of the biofuel continues to grow.

  13. Calcium and initial surface binding phase of pinocytosis in Amoeba proteus

    Energy Technology Data Exchange (ETDEWEB)

    Prusch, R.D.

    1986-08-01

    The uptake of membrane-bound solute and external medium by bulk-phase pinocytosis in Amoeba proteus is influenced by the level of Ca/sup 2 +/ in the external medium. Increasing external Ca/sup 2 +/ to approx.10/sup -4/ M increases pinocytotic intensity, while increases in Ca/sup 2 +/ above this level decrease the intensity of pinocytosis. The initial interaction of pinocytotic inducers and Ca/sup +2/ at the surface of A moeba proteus was therefore examined. Alcain blue and Na/sup +/, both inducers of pinocytosis, differ in the manner with which they associate with the amoeba surface, suggesting the possibility of different pinocytosis-inducing sites on the amoeba surface. Low levels of external Ca/sup 2 +/ in the range of 3 x 10/sup -5/ to 4.5 x 10/sup -4/ M increase the amount of cationic inducer associated with the cell surface while, at the same time, decreasing anion association with the cell surface. It is suggested that Ca/sup 2 +/ influences ion association with the cell surface by controlling the availability of negative surface sites, which in turn influences pinocytotic intensity. Surface binding of Na/sup +/, Ca/sup 2 +/ and Cl/sup -/ was determined by adding /sup 22/Na, /sup 45/Ca or /sup 36/Cl.

  14. An in situ vapour phase hydrothermal surface doping approach for fabrication of high performance Co3O4 electrocatalysts with an exceptionally high S-doped active surface.

    Science.gov (United States)

    Tan, Zhijin; Liu, Porun; Zhang, Haimin; Wang, Yun; Al-Mamun, Mohammad; Yang, Hua Gui; Wang, Dan; Tang, Zhiyong; Zhao, Huijun

    2015-04-04

    A facile in situ vapour phase hydrothermal (VPH) surface doping approach has been developed for fabrication of high performance S-doped Co3O4 electrocatalysts with an unprecedentedly high surface S content (>47%). The demonstrated VPH doping approach could be useful for enrichment of surface active sites for other metal oxide electrocatalysts.

  15. Synthesis and HPLC evaluation of carboxylic acid phases on a hydride surface.

    Science.gov (United States)

    Pesek, Joseph J; Matyska, Maria T; Gangakhedkar, Surekha; Siddiq, Rukhsana

    2006-04-01

    Three organic moieties containing carboxylic acid functional groups are attached to a particulate silica surface through silanization/hydrosilation. Two compounds (undecylenic acid and 10-undecynoic acid) have 11 carbon chains and the other is a five-carbon acid (pentenoic acid). Bonding is confirmed through carbon elemental analysis, diffuse reflectance infrared fourier transform spectroscopy, and carbon-13 and silicon-29 CP-MAS NMR spectroscopy. The bonded phases are tested by HPLC using PTH amino acids, nucleic acids, theophylline-related compounds, anilines, benzoic acid compounds, choline, and tobramycin. The latter two compounds are used to investigate the aqueous normal phase properties of the three bonded materials.

  16. Non-Stationary Internal Tides Observed with Satellite Altimetry

    Science.gov (United States)

    Ray, Richard D.; Zaron, E. D.

    2011-01-01

    Temporal variability of the internal tide is inferred from a 17-year combined record of Topex/Poseidon and Jason satellite altimeters. A global sampling of along-track sea-surface height wavenumber spectra finds that non-stationary variance is generally 25% or less of the average variance at wavenumbers characteristic of mode-l tidal internal waves. With some exceptions the non-stationary variance does not exceed 0.25 sq cm. The mode-2 signal, where detectable, contains a larger fraction of non-stationary variance, typically 50% or more. Temporal subsetting of the data reveals interannual variability barely significant compared with tidal estimation error from 3-year records. Comparison of summer vs. winter conditions shows only one region of noteworthy seasonal changes, the northern South China Sea. Implications for the anticipated SWOT altimeter mission are briefly discussed.

  17. First Principles Calculations of Transition Metal Binary Alloys: Phase Stability and Surface Effects

    Science.gov (United States)

    Aspera, Susan Meñez; Arevalo, Ryan Lacdao; Shimizu, Koji; Kishida, Ryo; Kojima, Kazuki; Linh, Nguyen Hoang; Nakanishi, Hiroshi; Kasai, Hideaki

    2017-06-01

    The phase stability and surface effects on binary transition metal nano-alloy systems were investigated using density functional theory-based first principles calculations. In this study, we evaluated the cohesive and alloying energies of six binary metal alloy bulk systems that sample each type of alloys according to miscibility, i.e., Au-Ag and Pd-Ag for the solid solution-type alloys (SS), Pd-Ir and Pd-Rh for the high-temperature solid solution-type alloys (HTSS), and Au-Ir and Ag-Rh for the phase-separation (PS)-type alloys. Our results and analysis show consistency with experimental observations on the type of materials in the bulk phase. Varying the lattice parameter was also shown to have an effect on the stability of the bulk mixed alloy system. It was observed, particularly for the PS- and HTSS-type materials, that mixing gains energy from the increasing lattice constant. We furthermore evaluated the surface effects, which is an important factor to consider for nanoparticle-sized alloys, through analysis of the (001) and (111) surface facets. We found that the stability of the surface depends on the optimization of atomic positions and segregation of atoms near/at the surface, particularly for the HTSS and the PS types of metal alloys. Furthermore, the increase in energy for mixing atoms at the interface of the atomic boundaries of PS- and HTSS-type materials is low enough to overcome by the gain in energy through entropy. These, therefore, are the main proponents for the possibility of mixing alloys near the surface.

  18. Dry phase titanium dioxide-mediated photocatalysis: Basis for in situ surface destruction of hazardous chemicals

    Energy Technology Data Exchange (ETDEWEB)

    Jones, A.P.; Watts, R.J. [Washington State Univ., Pullman, WA (United States). Dept. of Civil and Environmental Engineering

    1997-10-01

    The photocatalytic oxidation of 2,4,6-trichlorophenol (TCP) on the surface of titanium dioxide (TiO{sub 2}) at varying water contents was investigated to provide fundamental data for incorporating photocatalysts into the surface of pavements to promote the destruction of spilled organic chemicals. 2,4,6-Trichlorophenol, spiked onto a thin layer of TiO{sub 2}, was degraded to 20% of its original concentration over 24 h; the release of chloride confirmed the degradation of the parent compound on the surface of the dry TiO{sub 2}. Addition of water ({ge}25% by weight) to the TiO{sub 2} increased the rate of photocatalysis resulting in degradation of TCP to below detectable levels after 20 h. Based on competition studies using the hydroxyl radical scavengers, bicarbonate and 1-octanol, the proposed mechanisms for the dry phase photocatalytic degradation of TCP was oxidation by the valence band hole on the surface of the TiO{sub 2} particle or dehalogenation by superoxide radical anions. Competition studies also confirmed that the more rapid TCP oxidation on wet TiO{sub 2} was primarily the result of generation of hydroxyl radicals through oxidation of water by the valence band hole. The results show that dry phase TiO{sub 2}-mediated photocatalysis may be a potential system for the in situ surface destruction of chemicals that can be oxidized by nonhydroxyl radical mechanisms, such as valence band electron holes and dehalogenation processes.

  19. Surface Wave Multipathing and its Influence on Phase Velocities Measured by Small Networks

    Science.gov (United States)

    Maupin, V.

    2011-12-01

    Networks of temporary broadband seismological stations are commonly deployed over dedicated targets. Measurement of surface wave phase velocity across the network and its depth-inversion gives us information about the structure below the network which is complementary to the information obtained from body-wave analysis. For small networks, we face however the fundamental problem that the dimensions of the heterogeneities to image are not large compared to the wavelengths of the surface waves used to image them. In addition, multipathing is very common is teleseismic surface waves at moderate frequencies and the complexity of the incoming wavefield has to be taken into account during the tomographic process. We perform a series of numerical simulations of surface wave propagation in 3-D structures using complex incoming wavefields in order to analyse how the nature of the incoming wavefield plays together with the 3-D structure to determine phases and amplitudes at the different stations of a network. We analyse how different tomographic methods cope with the complex wavefield, the consequences on the resolution of the resulting tomographic models and we try to provide recommendations for data selection. The numerical simulations are done using a multiple-scattering mode coupling scheme. The amount of multipathing is taken from a recent study using teleseismic surface waves recorded on a temporary network in Southern Norway. The period range of 20 to 200s and the 450km x 600km dimension of the network is also taken form the same study.

  20. TEM observation on phase separation and interfaces of laser surface alloyed high-entropy alloy coating.

    Science.gov (United States)

    Cai, Zhaobing; Cui, Xiufang; Jin, Guo; Liu, Zhe; Li, Yang; Dong, Meiling

    2017-12-01

    Phase separation is a common phenomenon in traditional alloys. Under the condition of appropriate undercooling, the segregation phenomenon can be also found in blue-chip high-entropy alloys (HEAs). In this work, the phase separation behavior and interfacial investigation of laser surface alloyed HEA coating with high content Ti were studied principally by transmission electron microscopy. The results show that crystal structure and elementary composition on both sides of the interface of coating/substrate are quite different, and the interfaces between different phases are incoherent or semi-coherent boundarys, resolved by high resolution transmission electron microscopy. In the interface of (Co, Ni)Ti 2 phase/β-Ti phase, there is angle of 80° between BCC〈100〉 and FCC〈201〉. An interesting 'island' structure, that β-Ti phases are embraced by (Co, Ni)Ti 2 compounds in the BCC matrix, was observed definitely, which is attributed to the combined action of Ti segregation and inter-attraction of Ti and other elements. Copyright © 2017 Elsevier Ltd. All rights reserved.

  1. Photocatalytic Reaction of Gas-Phase Naphthalene on Paint- and Sunscreen-Coated Surfaces

    OpenAIRE

    Ashley, Nicholas A.; McBride, Noelle; Krumholt, Jason; Baker, Breeana; Valsaraj, Kalliat T.

    2012-01-01

    The uses of metal oxide nanoparticles in modern paint and sunscreen formulations are widespread. Through materials characterization and kinetic experiments, it is demonstrated that fresh surface coatings of paint and sunscreen photocatalytically degrade gaseous naphthalene. The primary metal oxides are TiO2 in the form of the rutile phase in paint and as anatase in sunscreen formulations. Other metal oxides present are Al2O3 and ZnO. Several organic fillers that are photochemically active are...

  2. Solitary waves of surface plasmon polariton via phase shifts under Doppler broadening and Kerr nonlinearity

    Science.gov (United States)

    Ahmad, S.; Ahmad, A.; Bacha, B. A.; Khan, A. A.; Abdul Jabar, M. S.

    2017-12-01

    Surface Plasmon Polaritons (SPPs) are theoretically investigated at the interface of a dielectric metal and gold. The output pulse from the dielectric is used as the input pulse for the generation of SPPs. The SPPs show soliton-like behavior at the interface. The solitary form of a SPP is maintained under the effects of Kerr nonlinearity, Doppler broadening and Fresnel dragging whereas its phase shift is significantly modified. A 0.3radian phase shift is calculated in the presence of both Kerr nonlinearity and Fresnel dragging in the absence of plasma motion. The phase shift is enhanced to 60radian due to the combined effect of Doppler broadening, Kerr nonlinearity and Fresnel dragging. The results may have significant applications in nano-photonics, optical tweezers, photovoltaic devices, plasmonster and sensing technology.

  3. Temperature dependence of {sigma} phase formation in surface melted duplex stainless steel

    Energy Technology Data Exchange (ETDEWEB)

    Knezevic, V.; Cvijovic, Z.; Mihajlovic, D. [Faculty of Technology and Metallurgy, Univ. of Belgrade, Belgrade (Yugoslavia)

    2000-07-01

    The {sigma} phase formation in GTA surface melted 22/7/2 copper-bearing duplex stainless steel was investigated in the range of 800 C to 1150 C. Annealing at 1050 C and below resulted in {sigma} phase formation, which was preceded by the {delta}{yields}{gamma}{sub 2} transformation. At 800 C and 900 C, the {sigma} phase forms by the in situ transformation and via the eutectoid reaction {delta}{yields}{sigma}+{gamma}{sub 2}, while at 1050 C it precipitates directly from the {delta} ferrite. This observation is supported by the Johnson-Mehl analysis. From a C shaped TTT diagram, the precipitation is most rapid at about 950 C. At 1150 C, total {sigma} dissolution occurs. (orig.)

  4. Liquid-solid surface phase transformation of fluorinated fullerene on monolayer tungsten diselenide

    KAUST Repository

    Song, Zhibo

    2018-04-04

    Hybrid van der Waals heterostructures constructed by the integration of organic molecules and two-dimensional (2D) transition metal dichalcogenide (TMD) materials have useful tunable properties for flexible electronic devices. Due to the chemically inert and atomically smooth nature of the TMD surface, well-defined crystalline organic films form atomically sharp interfaces facilitating optimal device performance. Here, the surface phase transformation of the supramolecular packing structure of fluorinated fullerene (C60F48) on single-layer tungsten diselenide (WSe2) is revealed by low-temperature scanning tunneling microscopy, from thermally stable liquid to solid phases as the coverage increases. Statistical analysis of the intermolecular interaction potential reveals that the repulsive dipole-dipole interaction induced by interfacial charge transfer and substrate-mediated interactions play important roles in stabilizing the liquid C60F48 phases. Theoretical calculations further suggest that the dipole moment per C60F48 molecule varies with the surface molecule density, and the liquid-solid transformation could be understood from the perspective of the thermodynamic free energy for open systems. This study offers insights into the growth behavior at 2D organic/TMD hybrid heterointerfaces.

  5. Liquid-solid surface phase transformation of fluorinated fullerene on monolayer tungsten diselenide

    Science.gov (United States)

    Song, Zhibo; Wang, Qixing; Li, Ming-Yang; Li, Lain-Jong; Zheng, Yu Jie; Wang, Zhuo; Lin, Tingting; Chi, Dongzhi; Ding, Zijing; Huang, Yu Li; Thye Shen Wee, Andrew

    2018-04-01

    Hybrid van der Waals heterostructures constructed by the integration of organic molecules and two-dimensional (2D) transition metal dichalcogenide (TMD) materials have useful tunable properties for flexible electronic devices. Due to the chemically inert and atomically smooth nature of the TMD surface, well-defined crystalline organic films form atomically sharp interfaces facilitating optimal device performance. Here, the surface phase transformation of the supramolecular packing structure of fluorinated fullerene (C60F48 ) on single-layer tungsten diselenide (WSe2) is revealed by low-temperature scanning tunneling microscopy, from thermally stable liquid to solid phases as the coverage increases. Statistical analysis of the intermolecular interaction potential reveals that the repulsive dipole-dipole interaction induced by interfacial charge transfer and substrate-mediated interactions play important roles in stabilizing the liquid C60F48 phases. Theoretical calculations further suggest that the dipole moment per C60F48 molecule varies with the surface molecule density, and the liquid-solid transformation could be understood from the perspective of the thermodynamic free energy for open systems. This study offers insights into the growth behavior at 2D organic/TMD hybrid heterointerfaces.

  6. Noise-and delay-induced phase transitions of the dimer–monomer surface reaction model

    International Nuclear Information System (INIS)

    Zeng Chunhua; Wang Hua

    2012-01-01

    Highlights: ► We study the dimer–monomer surface reaction model. ► We show that noise induces first-order irreversible phase transition (IPT). ► Combination of noise and time-delayed feedback induce first- and second-order IPT. ► First- and second-order IPT is viewed as noise-and delay-induced phase transitions. - Abstract: The effects of noise and time-delayed feedback in the dimer–monomer (DM) surface reaction model are investigated. Applying small delay approximation, we construct a stochastic delayed differential equation and its Fokker–Planck equation to describe the state evolution of the DM reaction model. We show that the noise can only induce first-order irreversible phase transition (IPT) characteristic of the DM model, however the combination of the noise and time-delayed feedback can simultaneously induce first- and second-order IPT characteristics of the DM model. Therefore, it is shown that the well-known first- and second-order IPT characteristics of the DM model may be viewed as noise-and delay-induced phase transitions.

  7. Surface modification-induced phase transformation of hexagonal close-packed gold square sheets

    KAUST Repository

    Fan, Zhanxi

    2015-03-13

    Conventionally, the phase transformation of inorganic nanocrystals is realized under extreme conditions (for example, high temperature or high pressure). Here we report the complete phase transformation of Au square sheets (AuSSs) from hexagonal close-packed (hcp) to face-centered cubic (fcc) structures at ambient conditions via surface ligand exchange, resulting in the formation of (100)f-oriented fcc AuSSs. Importantly, the phase transformation can also be realized through the coating of a thin metal film (for example, Ag) on hcp AuSSs. Depending on the surfactants used during the metal coating process, two transformation pathways are observed, leading to the formation of (100)f-oriented fcc Au@Ag core-shell square sheets and (110)h/(101)f-oriented hcp/fcc mixed Au@Ag nanosheets. Furthermore, monochromated electron energy loss spectroscopy reveals the strong surface plasmon resonance absorption of fcc AuSS and Au@Ag square sheet in the infrared region. Our findings may offer a new route for the crystal-phase and shape-controlled synthesis of inorganic nanocrystals. © 2015 Macmillan Publishers Limited. All rights reserved.

  8. Cell surface acid-base properties of the cyanobacterium Synechococcus: Influences of nitrogen source, growth phase and N:P ratios

    Science.gov (United States)

    Liu, Yuxia; Alessi, D. S.; Owttrim, G. W.; Kenney, J. P. L.; Zhou, Qixing; Lalonde, S. V.; Konhauser, K. O.

    2016-08-01

    The distribution of many trace metals in the oceans is controlled by biological uptake. Recently, Liu et al. (2015) demonstrated the propensity for a marine cyanobacterium to adsorb cadmium from seawater, suggesting that cell surface reactivity might also play an important role in the cycling of metals in the oceans. However, it remains unclear how variations in cyanobacterial growth rates and nutrient supply might affect the chemical properties of their cellular surfaces. In this study we used potentiometric titrations and Fourier Transform Infrared (FT-IR) spectrometry to profile the key metabolic changes and surface chemical responses of a Synechococcus strain, PCC 7002, during different growth regimes. This included testing various nitrogen (N) to phosphorous (P) ratios (both nitrogen and phosphorous dependent), nitrogen sources (nitrate, ammonium and urea) and growth stages (exponential, stationary, and death phase). FT-IR spectroscopy showed that varying the growth substrates on which Synechococcus cells were cultured resulted in differences in either the type or abundance of cellular exudates produced or a change in the cell wall components. Potentiometric titration data were modeled using three distinct proton binding sites, with resulting pKa values for cells of the various growth conditions in the ranges of 4.96-5.51 (pKa1), 6.67-7.42 (pKa2) and 8.13-9.95 (pKa3). According to previous spectroscopic studies, these pKa ranges are consistent with carboxyl, phosphoryl, and amine groups, respectively. Comparisons between the titration data (for the cell surface) and FT-IR spectra (for the average cellular changes) generally indicate (1) that the nitrogen source is a greater determinant of ligand concentration than growth phase, and (2) that phosphorus limitation has a greater impact on Synechococcus cellular and extracellular properties than does nitrogen limitation. Taken together, these techniques indicate that nutritional quality during cell growth can

  9. First-principles surface interaction studies of aluminum-copper and aluminum-copper-magnesium secondary phases in aluminum alloys

    Science.gov (United States)

    da Silva, Thiago H.; Nelson, Eric B.; Williamson, Izaak; Efaw, Corey M.; Sapper, Erik; Hurley, Michael F.; Li, Lan

    2018-05-01

    First-principles density functional theory-based calculations were performed to study θ-phase Al2Cu, S-phase Al2CuMg surface stability, as well as their interactions with water molecules and chloride (Cl-) ions. These secondary phases are commonly found in aluminum-based alloys and are initiation points for localized corrosion. Density functional theory (DFT)-based simulations provide insight into the origins of localized (pitting) corrosion processes of aluminum-based alloys. For both phases studied, Cl- ions cause atomic distortions on the surface layers. The nature of the distortions could be a factor to weaken the interlayer bonds in the Al2Cu and Al2CuMg secondary phases, facilitating the corrosion process. Electronic structure calculations revealed not only electron charge transfer from Cl- ions to alloy surface but also electron sharing, suggesting ionic and covalent bonding features, respectively. The S-phase Al2CuMg structure has a more active surface than the θ-phase Al2Cu. We also found a higher tendency of formation of new species, such as Al3+, Al(OH)2+, HCl, AlCl2+, Al(OH)Cl+, and Cl2 on the S-phase Al2CuMg surface. Surface chemical reactions and resultant species present contribute to establishment of local surface chemistry that influences the corrosion behavior of aluminum alloys.

  10. Optically transparent, mechanically durable, nanostructured superhydrophobic surfaces enabled by spinodally phase-separated glass thin films

    International Nuclear Information System (INIS)

    Aytug, Tolga; Simpson, John T; Lupini, Andrew R; Trejo, Rosa M; Jellison, Gerald E; Ivanov, Ilia N; Pennycook, Stephen J; Hillesheim, Daniel A; Winter, Kyle O; Christen, David K; Hunter, Scott R; Allen Haynes, J

    2013-01-01

    We describe the formation and properties of atomically bonded, optical quality, nanostructured thin glass film coatings on glass plates, utilizing phase separation by spinodal decomposition in a sodium borosilicate glass system. Following deposition via magnetron sputtering, thermal processing and differential etching, these coatings are structurally superhydrophilic (i.e., display anti-fogging functionality) and demonstrate robust mechanical properties and superior abrasion resistance. After appropriate chemical surface modification, the surfaces display a stable, non-wetting Cassie–Baxter state and exhibit exceptional superhydrophobic performance, with water droplet contact angles as large as 172°. As an added benefit, in both superhydrophobic and superhydrophilic states these nanostructured surfaces can block ultraviolet radiation and can be engineered to be anti-reflective with broadband and omnidirectional transparency. Thus, the present approach could be tailored toward distinct coatings for numerous markets, such as residential windows, windshields, specialty optics, goggles, electronic and photovoltaic cover glasses, and optical components used throughout the US military. (paper)

  11. Quality investigation of surface mount technology using phase-shifting digital holography

    Science.gov (United States)

    Boonsri, Chantira; Buranasiri, Prathan

    2016-09-01

    Applying of a phase-shifting digital holography combined with compressive sensing to inspect the soldering quality of surface mount technology (SMT) which is a method for producing electronic circuits. In SMT, the components are mounted and connected with each other directly onto the surface of printed circuit boards (PCBs). By reconstructing the multidimensional images from a few samples of SMT, the results are solved by an optimization problem. In this paper, two problems have been concerned. The first one is to examine the devices and the soldering quality of connections between them, which are in micro-scaled. The second is to observe the effect of heat treatment of soldering material and devices on the surface mount board.

  12. Evaporation phase change processes of water/methanol mixtures on superhydrophobic nanostructured surfaces

    Science.gov (United States)

    Chiang, Cheng-Kun; Lu, Yen-Wen

    2011-07-01

    Evaporation phenomena are a critical and frequently seen phase change process in many heat transfer applications. In this paper, we study the evaporation process of a sessile droplet on two topologically different surfaces, including smooth and nanostructured surfaces. The nanostructured surface has an array of high-aspect-ratio nanowires (height/diameter ~ 125) and is implemented by using a simple template-based nanofabrication method. It possesses superhydrophobicity (>140°) and low contact angle hysteresis (1.2-2.1°), allowing the liquid droplets to remain in the 'fakir' state throughout the evaporation processes. Sessile droplets of deionized (DI) water and water/methanol binary mixture test liquids with their contact angles and base diameters are monitored. The results show that the nanostructures play a critical role in the droplet dynamics during evaporation.

  13. Evaporation phase change processes of water/methanol mixtures on superhydrophobic nanostructured surfaces

    International Nuclear Information System (INIS)

    Chiang, Cheng-Kun; Lu, Yen-Wen

    2011-01-01

    Evaporation phenomena are a critical and frequently seen phase change process in many heat transfer applications. In this paper, we study the evaporation process of a sessile droplet on two topologically different surfaces, including smooth and nanostructured surfaces. The nanostructured surface has an array of high-aspect-ratio nanowires (height/diameter ∼ 125) and is implemented by using a simple template-based nanofabrication method. It possesses superhydrophobicity (>140°) and low contact angle hysteresis (1.2–2.1°), allowing the liquid droplets to remain in the 'fakir' state throughout the evaporation processes. Sessile droplets of deionized (DI) water and water/methanol binary mixture test liquids with their contact angles and base diameters are monitored. The results show that the nanostructures play a critical role in the droplet dynamics during evaporation

  14. Optically transparent, mechanically durable, nanostructured superhydrophobic surfaces enabled by spinodally phase-separated glass thin films

    Science.gov (United States)

    Aytug, Tolga; Simpson, John T.; Lupini, Andrew R.; Trejo, Rosa M.; Jellison, Gerald E.; Ivanov, Ilia N.; Pennycook, Stephen J.; Hillesheim, Daniel A.; Winter, Kyle O.; Christen, David K.; Hunter, Scott R.; Haynes, J. Allen

    2013-08-01

    We describe the formation and properties of atomically bonded, optical quality, nanostructured thin glass film coatings on glass plates, utilizing phase separation by spinodal decomposition in a sodium borosilicate glass system. Following deposition via magnetron sputtering, thermal processing and differential etching, these coatings are structurally superhydrophilic (i.e., display anti-fogging functionality) and demonstrate robust mechanical properties and superior abrasion resistance. After appropriate chemical surface modification, the surfaces display a stable, non-wetting Cassie-Baxter state and exhibit exceptional superhydrophobic performance, with water droplet contact angles as large as 172°. As an added benefit, in both superhydrophobic and superhydrophilic states these nanostructured surfaces can block ultraviolet radiation and can be engineered to be anti-reflective with broadband and omnidirectional transparency. Thus, the present approach could be tailored toward distinct coatings for numerous markets, such as residential windows, windshields, specialty optics, goggles, electronic and photovoltaic cover glasses, and optical components used throughout the US military.

  15. Monte Carlo simulation of the surface magnetic phase transition in chromium

    International Nuclear Information System (INIS)

    Mata, G.J.; Valera, M.

    1995-03-01

    Antiferromagnetic chromium is known to have a surface magnetic phase transition at a temperature T s = 780K, which is well above its bulk Neel temperature, T N = 311K. Electronic structure calculations predict an enhancement of the magnetic moment at the surface, due to changes in the local electronic environment. In order to ascertain the role of such an enhancement in the surface magnetic transition, we have modelled the surface by means of a classical Heisenberg model in which: a) the magnitude of a given spin is equal to the value of the corresponding magnetic moment predicted by band structure calculations, b) the exchange interaction J between spins is the same throughout the system, and c) the exchange interaction is chosen so as to reproduce the bulk transition temperature. We find a ratio of surface to bulk transition temperature of T S /T N = 2.5, which is an excellent agreement with the experimental result. Our results suggest that the surface magnetic transition in chromium is driven by fluctuations in the orientation of the magnetic moments and that quantum fluctuations play a minor role. (author). 18 refs, 5 figs

  16. Development of Phase Detection Schemes Based on Surface Plasmon Resonance Using Interferometry

    Directory of Open Access Journals (Sweden)

    Muhammad Kashif

    2014-08-01

    Full Text Available Surface plasmon resonance (SPR is a novel optical sensing technique with a unique ability to monitor molecular binding in real-time for biological and chemical sensor applications. Interferometry is an excellent tool for accurate measurement of SPR changes, the measurement and comparison is made for the sensitivity, dynamic range and resolution of the different analytes using interferometry techniques. SPR interferometry can also employ phase detection in addition to the amplitude of the reflected light wave, and the phase changes more rapidly compared with other approaches, i.e., intensity, angle and wavelength. Therefore, the SPR phase interferometer offers the advantages of spatial phase resolution and high sensitivity. This work discusses the advancements in interferometric SPR methods to measure the phase shifts due to refractive index changes. The main application areas of SPR sensors are demonstrated, i.e., the Fabry-Perot interferometer, Michelson interferometer and Mach-Zehnder interferometer, with different configurations. The three interferometers are discussed in detail, and solutions are suggested to enhance the performance parameters that will aid in future biological and chemical sensors.

  17. Oxidation of elemental mercury by chlorine: Gas phase, Surface,and Photo-induced reaction pathways

    Energy Technology Data Exchange (ETDEWEB)

    Yan, Nai-Qiang; Liu, Shou-Heng; Chang, Shih-Ger

    2004-10-22

    Accurate oxidation rate constants of mercury gas are needed for determining its dispersion and lifetime in the atmosphere. They would also help in developing a technology for the control of mercury emissions from coal-fired power plants. However, it is difficult to establish the accurate rate constants primarily due to the fact that mercury easily adsorbs on solid surface and its reactions can be catalyzed by the surface. We have demonstrated a procedure that allows the determination of gas phase, surface-induced, and photo-induced contributions in the kinetic study of the oxidation of mercury by chlorine gas. The kinetics was studied using reactors with various surface to volume ratios. The effect of the surface and the photo irradiation on the reaction was taken into consideration. The pressure dependent study revealed that the gas phase oxidation was a three-body collision process. The third order rate constant was determined to be 7.5({+-}0.2) x 10{sup -39} mL{sup 2} molecules{sup -2}s{sup -1} with N{sub 2} as the third body at 297 {+-} 1 K. The surface induced reaction on quartz window was second order and the rate constant was 2.7 x 10{sup -17} mL{sup 2} molecules{sup -1} cm{sup -2} sec. Meanwhile, the 253.7 nm photon employed for mercury detection was found to accelerate the reaction. The utilization efficiency of 253.7 nm photon for Hg{sup 0} oxidation was 6.7 x 10{sup -4} molecules photon{sup -1} under the conditions employed in this study.

  18. Surface modification induced phase transformation and structure variation on the rapidly solidified recast layer of titanium

    Energy Technology Data Exchange (ETDEWEB)

    Tsai, Ming-Hung [Department of Mechanical Engineering and Graduate Institute of Mechanical and Precision Engineering, National Kaoshiung University of Applied Sciences, Kaoshiung 807, Taiwan (China); School of Dentistry, College of Oral Medicine, Taipei Medical University, Taipei 110, Taiwan (China); Haung, Chiung-Fang [School of Dental Technology, College of Oral Medicine, Taipei Medical University, Taipei 110, Taiwan (China); Division of Family and Operative Dentistry, Department of Dentistry, Taipei Medical University Hospital, Taipei 110, Taiwan (China); Research Center for Biomedical Devices and Prototyping Production, Taipei Medical University, Taipei 110, Taiwan (China); Shyu, Shih-Shiun [Department of Dentistry, Taipei Tzu Chi Hospital, Buddhist Tzu Chi Medical Foundation, New Taipei City 231, Taiwan (China); Chou, Yen-Ru [Research Center for Biomedical Devices and Prototyping Production, Taipei Medical University, Taipei 110, Taiwan (China); Graduate Institute of Biomedical Materials and Tissue Engineering, College of Oral Medicine, Taipei Medical University, Taipei 110, Taiwan (China); Research Center for Biomedical Implants and Microsurgery Devices, Taipei Medical University, Taipei 110, Taiwan (China); Lin, Ming-Hong [Department of Mechanical Engineering and Graduate Institute of Mechanical and Precision Engineering, National Kaoshiung University of Applied Sciences, Kaoshiung 807, Taiwan (China); Peng, Pei-Wen, E-mail: apon@tmu.edu.tw [School of Dental Technology, College of Oral Medicine, Taipei Medical University, Taipei 110, Taiwan (China); and others

    2015-08-15

    In this study, neodymium-doped yttrium orthovanadate (Nd:YVO{sub 4}) as a laser source with different scanning speeds was used on biomedical Ti surface. The microstructural and biological properties of laser-modified samples were investigated by means of optical microscope, electron microscope, X-ray diffraction, surface roughness instrument, contact angle and cell cytotoxicity assay. After laser modification, the rough volcano-like recast layer with micro-/nanoporous structure and wave-like recast layer with nanoporous structure were generated on the surfaces of laser-modified samples, respectively. It was also found out that, an α → (α + rutile-TiO{sub 2}) phase transition occurred on the recast layers of laser-modified samples. The Ti surface becomes hydrophilic at a high speed laser scanning. Moreover, the cell cytotoxicity assay demonstrated that laser-modified samples did not influence the cell adhesion and proliferation behaviors of osteoblast (MG-63) cell. The laser with 50 mm/s scanning speed induced formation of rough volcano-like recast layer accompanied with micro-/nanoporous structure, which can promote cell adhesion and proliferation of MG-63 cell on Ti surface. The results indicated that the laser treatment was a potential technology to enhance the biocompatibility for titanium. - Highlights: • Laser induced the formation of recast layer with micro-/nanoporous structure on Ti. • An α → (α + rutile-TiO{sub 2}) phase transition was observed within the recast layer. • The Ti surface becomes hydrophilic at a high speed laser scanning. • Laser-modified samples exhibit good biocompatibility to osteoblast (MG-63) cell.

  19. Anatomy of successive helium-shell flashes: Stationary shell burning

    International Nuclear Information System (INIS)

    Sackmann, I.

    1980-01-01

    For successive helium-shell flashes, the amounts of helium and hydrogen burned were computed over the peak flash phase, over the total flash cycle, and over the quiet, interflash phase. It was found that the frequently made assumption of stationary shell burning is violated by the helium-shell flash for the first few flashes; here, over a total flash cycle, the helium-burning shell always progresses considerably faster outward than the hydrogen-burning shell. However, after about 15 flashes, coincident with the leveling out of the peaks of the helium shell, agreement with stationary shell burning is attained, both for the 3 M/sub sun/ and 6 M/sub sun/ cases

  20. Stationary analysis of signals and ratio decay determination in BWR type reactors by neuronal network

    International Nuclear Information System (INIS)

    Sanchis, R.; Palomo, M. J.; Munoz-Cobo, J. L.

    1998-01-01

    The signals registered in the nuclear plants have non stationary characteristics, in numerous times. This made difficult the application of the methods of analysis. There are determinate temporal intervals in that the signal is stationary with determinate mean, value together of zones with corrupt registers, and other zones with mean value distinct, but stationary during a temporal interval. The methodology consist in a stationary analysis to the signal received of the nuclear plant. With the Gabor Transformation are determined the temporal intervals of the stationary signals, synthesised it, as previous phase to the application of the methods of the analysis of stability parameters with methods ARMA, SVD, Neural Net,... to the reconstructed signal. 4 refs. (Author)

  1. One-sided asymptotically mean stationary channels

    OpenAIRE

    Simon, Francois

    2014-01-01

    This paper proposes an analysis of asymptotically mean stationary (AMS) communication channels. A hierarchy based on stability properties (stationarity, quasi-stationarity, recurrence and asymptotically mean stationarity) of channels is identified. Stationary channels are a subclass of quasi-stationary channels which are a subclass of recurrent AMS channels which are a subclass of AMS channels. These classes are proved to be stable under Markovian composition of channels (e.g., the cascade of...

  2. Phase diagram of a diluted surface of a disordered Ising film

    International Nuclear Information System (INIS)

    Bengrine, M.; Benyoussef, A.; Ez-Zahraouy, H.; Mhirech, F.

    1998-09-01

    The effects of amorphized film and diluted surface on phase diagrams and magnetic properties of a spin-1/2 Ising film are investigated within a finite cluster approximation. Depending on the value of the concentration p of the dilution couplings at the surface, it is found that there exists a critical value p c , when increasing the thickness of the film the critical temperature T c decreases for p greater than p c , while it increases for p less than p c . Moreover, the critical concentration depends on the amorphization δ. Indeed, p c increasing with increasing δ. Besides, the phase diagram represented in (T c ,α), where α represents the strength of the strong coupling at the surface, shows that there exists a critical value of the amorphization δ c =δ c (p) for p not= 1, for δ≤δ c (p) a long range order occurs for any value of α at low temperature, while for δ>δ c (p) an order-disorder transition occurs at T=0 and α=α c (δ). Magnetization is calculated as a function of the amorphization δ, the concentration p and the strength α of the strong coupling. (author)

  3. Surface modification of the MoSiON phase shift mask to reduce critical dimension variation

    Science.gov (United States)

    Choo, Hyeokseong; Seo, Dongwan; Lim, Sangwoo

    2013-10-01

    Phase shift masks (PSMs) were introduced to extend the limits of optical lithography. However, cleaning a MoSiON-based PSM pattern with an ammonium hydroxide/hydrogen peroxide mixture (APM), although efficient at cleaning the PSM pattern, etches the PSM layer, inducing changes in the phase angle and transmittance due to the introduction of variation of the critical dimension (CD). In this study, we investigated the effects of plasma treatment and furnace annealing on the etching of the MoSiON PSM in APM. In particular, we found that the etch behavior and surface chemical state after each treatment were correlated. We also compared variations in the CD between patterned PSM layers and blank masks. After O2 or N2 plasma treatment, the top surface of MoSiON had a thicker transition layer with an extreme increase in O, and a huge variation in CD was also observed after APM treatment. However, CD variation of the patterned MoSiON layer was minimal when the sample was first annealed in NH3 ambient gas and then subjected to APM treatment. This phenomenon may be related to an increase in the portion of the SiO2-like state at the top surface of the MoSiON PSM layer and its optimization without a change in the transition layer thickness.

  4. Short-period surface-wave phase velocities across the conterminous United States

    Science.gov (United States)

    Ekström, G.

    2017-09-01

    Surface-wave phase-velocity maps for the full footprint of the USArray Transportable Array (TA) across the conterminous United States are developed and tested. Three-component, long-period continuous seismograms recorded on more than 1800 seismometers, most of which were deployed for 18 months or longer, are processed using a noise cross-correlation technique to derive inter-station Love and Rayleigh dispersion curves at periods between 5 and 40 s. The phase-velocity measurements are quality controlled using an automated algorithm and then used in inversions for Love and Rayleigh phase-velocity models at discrete periods on a 0.25°-by-0.25° pixel grid. The robustness of the results is examined using comparisons of maps derived from subsets of the data. A winter-summer division of the cross-correlation data results in small model differences, indicating relatively minor sensitivity of the results to seasonal variations in the distribution of noise sources. Division of the dispersion data based on inter-station azimuth does not result in geographically coherent model differences, suggesting that azimuthal anisotropy at the regional scale is weak compared with variations in isotropic velocities and does not substantially influence the results for isotropic velocities. The phase-velocity maps and dispersion measurements are documented and made available as data products of the 10-year-long USArray TA deployment.

  5. Existence of several surface-reconstructed phases in a two-dimensional lattice model

    Science.gov (United States)

    Huckaby, Dale A.; Rys, Franz S.

    1992-03-01

    The zero-temperature phase diagram is rigorously obtained for a two-dimensional lattice model with four energy parameters. It is shown that the parameter space can be divided into regions, together with their boundaries, such that in each region the ground-state configurations are of one of seven different types. These types include one which is nondegenerate, four which are doubly degenerate, one which is infinitely degenerate but with no residual entropy, and one which is infinitely degenerate and has a nonzero residual entropy. The Pirogov-Sinai extension of the Peierls argument is used to establish the existence at low temperatures of four different types of ordered surface-reconstructed phases.

  6. Condensational theory of stationary tornadoes

    International Nuclear Information System (INIS)

    Makarieva, A.M.; Gorshkov, V.G.; Nefiodov, A.V.

    2011-01-01

    Using the Bernoulli integral for air streamline with condensing water vapor a stationary axisymmetric tornado circulation is described. The obtained profiles of vertical, radial and tangential velocities are in agreement with observations for the Mulhall tornado, world's largest on record and longest-lived among the three tornadoes for which 3D velocity data are available. Maximum possible vortex velocities are estimated. -- Highlights: → Water vapor condensation causes a logarithmic drop of air pressure towards tornado center. → The first ever theoretical description of tornado velocities is obtained. → The maximum vortex velocity grows logarithmically with decreasing tornado eye radius. → Air motion with high velocities can only develop in sufficiently large condensation areas.

  7. Phase transformations on the surface of YAG composite ceramics under the action of directed laser treatment

    Energy Technology Data Exchange (ETDEWEB)

    Vlasova, M., E-mail: vlasovamarina@inbox.ru; Márquez Aguilar, P.A.; Escobar Martinez, A.; Kakazey, M.; Guardian Tapia, R.; Trujillo Estrada, A.

    2016-07-30

    Highlights: • During directed laser treatment of the surface of the composite ceramics consisting of predominantly Y{sub 3}Al{sub 5}O{sub 12} and Al{sub 2}O{sub 3}, the oriented crystallization of YAG and Al{sub 2}O{sub 3} takes place. • As a result of high-temperature heating, in the surface layer of tracks, the partial dissociation of Y{sub 3}Al{sub 5}O{sub 12}, Y{sub 2}Ti{sub 2}O{sub 7}, and Al{sub 2}Y{sub 4}O{sub 9} and enrichment in YAlO{sub 3} occur. • The content of YAlO{sub 3}, the size of YAG crystallites, and their crystallographic texturing depend on the irradiation mode. • After laser treatment, the ceramic material transforms into a three-layer macrostructure consisting of the basic ceramic material, near-surface textured layer, and surface layer. - Abstract: The laser treatment of composite ceramics based on Y{sub 3}Al{sub 5}O{sub 12} with Y{sub 2}Ti{sub 2}O{sub 7}, Al{sub 2}Y{sub 4}O{sub 9}, and Al{sub 2}O{sub 3} additives is accompanied by the melting of the surface layer and formation of tracks. In the volume of tracks, the partial dissociation of Y{sub 3}Al{sub 5}O{sub 12}, Y{sub 2}Ti{sub 2}O{sub 7}, and Al{sub 2}Y{sub 4}O{sub 9}, and the formation of new phases such as YAlO{sub 3} of orthorhombic and hexagonal modifications along with the appearance of additional content of Y{sub 3}Al{sub 5}O{sub 12} and Al{sub 2}O{sub 3} are observed. The content of all these phases depends on the irradiation mode and the phase composition of the ceramics. With increase in the corundum content in ceramic specimens, in the tracks, the Al{sub 2}O{sub 3} content increases, and the Y{sub 3}Al{sub 5}O{sub 12} content decreases. In the volume of tracks, Y{sub 3}Al{sub 5}O{sub 12} crystallites are textured. The size of YAG crystallites and their crystallographic texturing depend on the irradiation mode and Y{sub 3}Al{sub 5}O{sub 12}/Al{sub 2}O{sub 3} phase ratio. On the surface of tracks, a layer enriched in YAlO{sub 3} forms. Thus, as a result of laser

  8. Operable Unit 3-13, Group 3, Other Surface Soils (Phase II) Field Sampling Plan

    Energy Technology Data Exchange (ETDEWEB)

    G. L. Schwendiman

    2006-07-27

    This Field Sampling Plan describes the Operable Unit 3-13, Group 3, Other Surface Soils, Phase II remediation field sampling activities to be performed at the Idaho Nuclear Technology and Engineering Center located within the Idaho National Laboratory Site. Sampling activities described in this plan support characterization sampling of new sites, real-time soil spectroscopy during excavation, and confirmation sampling that verifies that the remedial action objectives and remediation goals presented in the Final Record of Decision for Idaho Nuclear Technology and Engineering Center, Operable Unit 3-13 have been met.

  9. Phase study of the generated surface plasmon waves in light transmission through a subwavelength aperture

    DEFF Research Database (Denmark)

    Hashemi, Mahdieh; Xiao, Sanshui; Farzad, Mahmood Hosseini

    2014-01-01

    Interference of surface plasmon (SP) waves plays a key role in light transmission through a subwavelength aperture surrounded by groove structures. In order to characterize interference of the hole and groove-generated SP waves, their phase information was carefully investigated using finite...... difference time domain simulations. In a structure with only one groove, constructive interference of the generated SP waves will enhance transmitted light by a factor of 5.4 compared with that of a single hole. Increasing the groove number to 3 in the design, which supports constructive interference of SP...... waves, will enhance the transmission coefficient to 10.5 times that for the single-hole transmission coefficient....

  10. Versatile gas-phase reactions for surface to bulk esterification of cellulose microfibrils aerogels.

    Science.gov (United States)

    Fumagalli, Matthieu; Ouhab, Djamila; Boisseau, Sonia Molina; Heux, Laurent

    2013-09-09

    Aqueous suspensions of microfibrillated cellulose obtained by a high pressure homogenization process were freeze-dried after solvent exchange into tert-butanol. The resulting aerogels, which displayed a remarkable open morphology with a surface area reaching 100 m(2)/g, were subjected to a gas-phase esterification with palmitoyl chloride. Under these conditions, variations of the reaction temperature from 100 to 200 °C, of the reaction time from 0.5 to 2 h, and of the initial quantity of reagent, led to the preparation of a library of cellulose palmitates with DS varying from zero to 2.36. These products were characterized by gravimetry, FTIR, and (13)C solid-state NMR spectroscopy. Of special interest were the cellulose palmitate samples of low DS in the range of 0.1-0.4, which corresponded to hydrophobic cellulose microfibrils exclusively esterified at their surface while keeping intact their inner structure.

  11. DPPC Monolayers Exhibit an Additional Phase Transition at High Surface Pressure

    DEFF Research Database (Denmark)

    Shen, Chen; de la Serna, Jorge B.; Struth, Bernd

    2015-01-01

    Pulmonary surfactant forms a monolayer at the air/aqueous interface within the lung. During the breath process, the surface pressure (Π) periodically varies from ~40mN/m up to ~70mN/m. The film is mechanically stable during this rapid and reversible expansion. Pulmonary surfactant consists of ~90......% of lipid with 10% integrated proteins. Among its lipid compounds, di-palmitoyl-phosphatidylcholine (DPPC) dominates (~45wt%). DPPC is the only known lipid that can be compressed to very high surface pressure (~70mN/m) before its monolayer collapses. Most probably, this feature contributes to the mechanical...... stability of the alveoli monolayer. Still, to the best of our knowledge, some details of the compression isotherm presented here and the related structures of the DPPC monolayer were not studied so far. The liquid-expanded/liquid-condensed phase transition of the DPPC monolayer at ~10mN/m is well known...

  12. Expressions to Rayleigh circumferential phase velocity and dispersion relation for a cylindrical surface under mechanical pressure

    Science.gov (United States)

    Sebold, Jean Eduardo; de Lacerda, Luiz Alkimin

    2018-04-01

    This paper describes a substantiated mathematical theory for Rayleigh waves propagated on some types of metal cylinders. More specifically, it presents not only a new way to express the dispersion relation of Rayleigh waves propagated on the cylindrical surface, but also how it can be used to construct a mathematical equation showing that the applied static mechanical pressure affects the shear modulus of the metal cylinder. All steps, required to conclude the process, consider the equation of motion as a function of radial and circumferential coordinates only, while the axial component can be overlooked without causing any problems. Some numerical experiments are done to illustrate the changes in the Rayleigh circumferential phase velocity in a metal cylindrical section due to static mechanical pressure around its external surface.

  13. The influence of surface microchemistry in protective film formation on multi-phase magnesium alloys

    International Nuclear Information System (INIS)

    Gray-Munro, J.E.; Luan, B.; Huntington, L.

    2008-01-01

    The high strength:weight ratio of magnesium alloys makes them an ideal metal for automotive and aerospace applications where weight reduction is of significant concern. Unfortunately, magnesium alloys are highly susceptible to corrosion particularly in salt-spray conditions. This has limited their use in the automotive and aerospace industries, where exposure to harsh service conditions is unavoidable. The simplest way to avoid corrosion is to coat the magnesium-based substrate by a process such as electroless plating, which is a low-cost, non line of sight process. Magnesium is classified as a difficult to plate metal due to its high reactivity. This means that in the presence of air magnesium very quickly forms a passive oxide layer that must be removed prior to plating. Furthermore, high aluminium content alloys are especially difficult to plate due to the formation of intermetallic species at the grain boundaries, resulting in a non-uniform surface potential across the substrate and thereby further complicating the plating process. The objective of this study is to understand how the magnesium alloy microstructure influences the surface chemistry of the alloy during both pretreatment and immersion copper coating of the substrate. A combination of scanning electron microscopy, energy dispersive spectroscopy and scanning Auger microscopy has been used to study the surface chemistry at the various stages of the coating process. Our results indicate that the surface chemistry of the alloy is different on the aluminum rich β phase of the material compared to the magnesium matrix which leads to preferential deposition of the metal on the aluminum rich phase of the alloy

  14. Turbulence Driven by Common Non-stationary Weak Winds

    Science.gov (United States)

    Mahrt, L.

    2015-12-01

    Complications with analysis of turbulence in common non-stationary weak-wind conditions are briefly surveyed. The behavior of turbulent transport in the weak-wind stably stratified boundary layer is then examined in terms of the non-stationarity of the wind field using measurements from three field programs with towers ranging from 12 to 20 m and an extensive horizontal network of sonic anemometers. The relationship of the friction velocity to the stratification and small non-stationary submeso motions are studied from several points of view and nominally quantified. The relationship of the turbulence to the stratification is less systematic than expected due to the important submeso motions. Cause and effect relationships are difficult to isolate because the non-stationary momentum flux significantly modifies the profile of the non-stationary mean flow. The link between the turbulence and accelerations at the surface is examined in terms of the changing vertical structure of the wind profile and sudden increases of downward transport of momentum. The relationship between the heat flux, wind speed and stratification is investigated. Weak wind conditions include frequent vertical convergence of the heat flux and implied temperature advection.

  15. Stationary strings near a higher-dimensional rotating black hole

    International Nuclear Information System (INIS)

    Frolov, Valeri P.; Stevens, Kory A.

    2004-01-01

    We study stationary string configurations in a space-time of a higher-dimensional rotating black hole. We demonstrate that the Nambu-Goto equations for a stationary string in the 5D (five-dimensional) Myers-Perry metric allow a separation of variables. We present these equations in the first-order form and study their properties. We prove that the only stationary string configuration that crosses the infinite redshift surface and remains regular there is a principal Killing string. A worldsheet of such a string is generated by a principal null geodesic and a timelike at infinity Killing vector field. We obtain principal Killing string solutions in the Myers-Perry metrics with an arbitrary number of dimensions. It is shown that due to the interaction of a string with a rotating black hole, there is an angular momentum transfer from the black hole to the string. We calculate the rate of this transfer in a space-time with an arbitrary number of dimensions. This effect slows down the rotation of the black hole. We discuss possible final stationary configurations of a rotating black hole interacting with a string

  16. Removal of contaminated concrete surfaces by microwave heating: Phase 1 results

    International Nuclear Information System (INIS)

    White, T.L.; Grubb, R.G.; Pugh, L.P.; Foster, D. Jr.; Box, W.D.

    1992-01-01

    Oak Ridge National Laboratory (ORNL) is developing a microwave heating process to remove radiologically contaminated surface layers from concrete. The microwave energy is directed at the concrete surface and heats the concrete and free water present in the concrete matrix. Continued heating produces steam-pressure-induced mechanical stresses that cause the concrete surface to burst. The concrete particles from this steam explosion are small enough to be removed by a vacuum system, yet less than 1% of the debris is small enough to pose an airborne contamination hazard. The first phase of this program has demonstrated reliable removal of noncontaminated concrete surfaces at frequencies of 2.45 GHz and 10.6 GHz. Continuous concrete removal rates of 1.07 cm 3 /s with 5.2 kW of 2.45.-GHz power and 2.11 cm 3 /s with 3.6 kW of 10.6-GHz power have been demonstrated. Figures-of-merit for microwave removal of concrete have been calculated to be 0.21 cm 3 /s/kW at 2.45 GHz and 0.59 cm 3 /s/kW at 10.6 GHz. The amount of concrete removed in a single pass can be controlled by choosing the frequency and power of the microwave system

  17. High-frequency instabilities of stationary crossflow vortices in a hypersonic boundary layer

    Science.gov (United States)

    Li, Fei; Choudhari, Meelan; Paredes, Pedro; Duan, Lian

    2016-09-01

    Hypersonic boundary layer flows over a circular cone at moderate incidence angle can support strong crossflow instability in between the windward and leeward rays on the plane of symmetry. Due to more efficient excitation of stationary crossflow vortices by surface roughness, such boundary layer flows may transition to turbulence via rapid amplification of the high-frequency secondary instabilities of finite-amplitude stationary crossflow vortices. The amplification characteristics of these secondary instabilities are investigated for crossflow vortices generated by an azimuthally periodic array of roughness elements over a 7° half-angle circular cone in a Mach 6 free stream. The analysis is based on both quasiparallel stability theory in the form of a partial-differential-equation-based eigenvalue analysis and plane marching parabolized stability equations that account for the effects of the nonparallel basic state on the growth of secondary disturbances. Depending on the local amplitude of the stationary crossflow mode, the most unstable high-frequency disturbances either originate from the second (i.e., Mack) mode instabilities of the unperturbed boundary layer or correspond to genuine secondary instabilities that reduce to stable disturbances at sufficiently small amplitudes of the stationary crossflow vortex. The predicted frequencies of the dominant secondary disturbances of either type are similar to those measured during wind tunnel experiments at Purdue University and the Technical University of Braunschweig, Germany. Including transverse surface curvature within the quasiparallel predictions does not alter the topology of the unstable modes; however, the resulting changes in both mode shape and disturbance growth rate are rather significant and curvature can be either stabilizing or destabilizing depending on the disturbance frequency and mode type. Nonparallel effects are shown to be strongly destabilizing for secondary instabilities originating from

  18. Imaging metal-like monoclinic phase stabilized by surface coordination effect in vanadium dioxide nanobeam

    Science.gov (United States)

    Li, Zejun; Wu, Jiajing; Hu, Zhenpeng; Lin, Yue; Chen, Qi; Guo, Yuqiao; Liu, Yuhua; Zhao, Yingcheng; Peng, Jing; Chu, Wangsheng; Wu, Changzheng; Xie, Yi

    2017-06-01

    In correlated systems, intermediate states usually appear transiently across phase transitions even at the femtosecond scale. It therefore remains an open question how to determine these intermediate states--a critical issue for understanding the origin of their correlated behaviour. Here we report a surface coordination route to successfully stabilize and directly image an intermediate state in the metal-insulator transition of vanadium dioxide. As a prototype metal-insulator transition material, we capture an unusual metal-like monoclinic phase at room temperature that has long been predicted. Coordinate bonding of L-ascorbic acid molecules with vanadium dioxide nanobeams induces charge-carrier density reorganization and stabilizes metallic monoclinic vanadium dioxide, unravelling orbital-selective Mott correlation for gap opening of the vanadium dioxide metal-insulator transition. Our study contributes to completing phase-evolution pathways in the metal-insulator transition process, and we anticipate that coordination chemistry may be a powerful tool for engineering properties of low-dimensional correlated solids.

  19. Translational Symmetry and Microscopic Constraints on Symmetry-Enriched Topological Phases: A View from the Surface

    Directory of Open Access Journals (Sweden)

    Meng Cheng

    2016-12-01

    Full Text Available The Lieb-Schultz-Mattis theorem and its higher-dimensional generalizations by Oshikawa and Hastings require that translationally invariant 2D spin systems with a half-integer spin per unit cell must either have a continuum of low energy excitations, spontaneously break some symmetries, or exhibit topological order with anyonic excitations. We establish a connection between these constraints and a remarkably similar set of constraints at the surface of a 3D interacting topological insulator. This, combined with recent work on symmetry-enriched topological phases with on-site unitary symmetries, enables us to develop a framework for understanding the structure of symmetry-enriched topological phases with both translational and on-site unitary symmetries, including the effective theory of symmetry defects. This framework places stringent constraints on the possible types of symmetry fractionalization that can occur in 2D systems whose unit cell contains fractional spin, fractional charge, or a projective representation of the symmetry group. As a concrete application, we determine when a topological phase must possess a “spinon” excitation, even in cases when spin rotational invariance is broken down to a discrete subgroup by the crystal structure. We also describe the phenomena of “anyonic spin-orbit coupling,” which may arise from the interplay of translational and on-site symmetries. These include the possibility of on-site symmetry defect branch lines carrying topological charge per unit length and lattice dislocations inducing degeneracies protected by on-site symmetry.

  20. Inversion of Surface Wave Phase Velocities for Radial Anisotropy to an Depth of 1200 km

    Science.gov (United States)

    Xing, Z.; Beghein, C.; Yuan, K.

    2012-12-01

    This study aims to evaluate three dimensional radial anisotropy to an depth of 1200 km. Radial anisotropy describes the difference in velocity between horizontally polarized Rayleigh waves and vertically polarized Love waves. Its presence in the uppermost 200 km mantle has well been documented by different groups, and has been regarded as an indicator of mantle convection which aligns the intrinsically anisotropic minerals, largely olivine, to form large scale anisotropy. However, there is no global agreement on whether anisotropy exists in the region below 200 km. Recent models also associate a fast vertically polarized shear wave with vertical upwelling mantle flow. The data used in this study is the globally isotropic phase velocity models of fundamental and higher mode Love and Rayleigh waves (Visser, 2008). The inclusion of higher mode surface wave phase velocity provides sensitivities to structure at depth that extends to below the transition zone. While the data is the same as used by Visser (2008), a quite different parameterization is applied. All the six parameters - five elastic parameters A, C, F, L, N and density - are now regarded as independent, which rules out possible biased conclusions induced by scaling relation method used in several previous studies to reduce the number of parameters partly due to limited computing resources. The data need to be modified by crustal corrections (Crust2.0) as we want to look at the mantle structure only. We do this by eliminating the perturbation in surface wave phase velocity caused by the difference in crustal structure with respect to the referent model PREM. Sambridge's Neighborhood Algorithm is used to search the parameter space. The introduction of such a direct search technique pales the traditional inversion method, which requires regularization or some unnecessary priori restriction on the model space. On the contrary, the new method will search the full model space, providing probability density

  1. Stable water isotope simulation by current land-surface schemes:Results of IPILPS phase 1

    Energy Technology Data Exchange (ETDEWEB)

    Henderson-Sellers, A.; Fischer, M.; Aleinov, I.; McGuffie, K.; Riley, W.J.; Schmidt, G.A.; Sturm, K.; Yoshimura, K.; Irannejad, P.

    2005-10-31

    Phase 1 of isotopes in the Project for Intercomparison of Land-surface Parameterization Schemes (iPILPS) compares the simulation of two stable water isotopologues ({sup 1}H{sub 2} {sup 18}O and {sup 1}H{sup 2}H{sup 16}O) at the land-atmosphere interface. The simulations are off-line, with forcing from an isotopically enabled regional model for three locations selected to offer contrasting climates and ecotypes: an evergreen tropical forest, a sclerophyll eucalypt forest and a mixed deciduous wood. Here we report on the experimental framework, the quality control undertaken on the simulation results and the method of intercomparisons employed. The small number of available isotopically-enabled land-surface schemes (ILSSs) limits the drawing of strong conclusions but, despite this, there is shown to be benefit in undertaking this type of isotopic intercomparison. Although validation of isotopic simulations at the land surface must await more, and much more complete, observational campaigns, we find that the empirically-based Craig-Gordon parameterization (of isotopic fractionation during evaporation) gives adequately realistic isotopic simulations when incorporated in a wide range of land-surface codes. By introducing two new tools for understanding isotopic variability from the land surface, the Isotope Transfer Function and the iPILPS plot, we show that different hydrological parameterizations cause very different isotopic responses. We show that ILSS-simulated isotopic equilibrium is independent of the total water and energy budget (with respect to both equilibration time and state), but interestingly the partitioning of available energy and water is a function of the models' complexity.

  2. Growth, intermixing, and surface phase formation for zinc tin oxide nanolaminates produced by atomic layer deposition

    Energy Technology Data Exchange (ETDEWEB)

    Hägglund, Carl, E-mail: carl.hagglund@angstrom.uu.se [Department of Chemical Engineering, Stanford University, Stanford, California 94305 and Department of Engineering Sciences, Division of Solid State Electronics, Uppsala University, 75121 Uppsala (Sweden); Grehl, Thomas; Brongersma, Hidde H. [ION-TOF GmbH, Heisenbergstraße 15, 48149 Münster (Germany); Tanskanen, Jukka T.; Mullings, Marja N.; Mackus, Adriaan J. M.; MacIsaac, Callisto; Bent, Stacey Francine, E-mail: sbent@stanford.edu [Department of Chemical Engineering, Stanford University, Stanford, California 94305 (United States); Yee, Ye Sheng [Department of Electrical Engineering, Stanford University, Stanford, California 94305 (United States); Clemens, Bruce M. [Department of Material Science and Engineering, Stanford University, Stanford, California 94305 (United States)

    2016-03-15

    A broad and expanding range of materials can be produced by atomic layer deposition at relatively low temperatures, including both oxides and metals. For many applications of interest, however, it is desirable to grow more tailored and complex materials such as semiconductors with a certain doping, mixed oxides, and metallic alloys. How well such mixed materials can be accomplished with atomic layer deposition requires knowledge of the conditions under which the resulting films will be mixed, solid solutions, or laminated. The growth and lamination of zinc oxide and tin oxide is studied here by means of the extremely surface sensitive technique of low energy ion scattering, combined with bulk composition and thickness determination, and x-ray diffraction. At the low temperatures used for deposition (150 °C), there is little evidence for atomic scale mixing even with the smallest possible bilayer period, and instead a morphology with small ZnO inclusions in a SnO{sub x} matrix is deduced. Postannealing of such laminates above 400 °C however produces a stable surface phase with a 30% increased density. From the surface stoichiometry, this is likely the inverted spinel of zinc stannate, Zn{sub 2}SnO{sub 4}. Annealing to 800 °C results in films containing crystalline Zn{sub 2}SnO{sub 4}, or multilayered films of crystalline ZnO, Zn{sub 2}SnO{sub 4}, and SnO{sub 2} phases, depending on the bilayer period.

  3. The Research of Phase Retrieval Holography Method Based on the Active Deformation of the Active Reflector Surface

    Science.gov (United States)

    Wang, Z. Q.; Chen, M. Z.; Pei, X.; Wang, J.

    2017-09-01

    The surface accuracy of a large reflector radio telescope is one of the important factors influencing the performance of the antenna. The effects of panel processing, installation, as well as gravity, temperature, and wind load, will greatly limit the observation efficiency of the antenna. Focused on the technology of active surface which is more accurately controllable than the minor reflector surface of six-ploe, the continuous distribution of active deformation phase factor described by Zernike polynomials is adopted for the first time. Only getting the far field amplitude through adjusting the active surface, the surface error can be detected. By building the models of numerical simulation, the retrieval error of arbitrary surface deformation is calculated, and the retrieval results of surface deformation in a variety of continuous active surface deformation is also studied. It is indicated that this method can stably and accurately detect surface deformation, and can also improve the efficiency of radio telescope observations effectively.

  4. Comparison of Approaches to the Prediction of Surface Wave Phase Velocity

    Science.gov (United States)

    Godfrey, K. E.; Dalton, C. A.; Hjorleifsdottir, V.; Ekstrom, G.

    2017-12-01

    Global seismic models provide crucial information about the state, composition, and dynamics of the Earth's interior, and in the shallow mantle these models are primarily constrained by observations of surface waves. Models developed by different groups have been constructed using different data sets and different techniques. While these models exhibit good agreement on the long-wavelength features, there is less consistency in the patterns and amplitude of smaller-scale heterogeneity. Here we investigate how approximations in the theoretical treatment of wave propagation and excitation influence the interpretation of measured phase delays and the tomographic images that result from inverting them. Synthetic seismograms were generated using SPECFEM3D_GLOBE for 42 earthquakes, 134 receiver locations, and two 3-D models of elastic Earth structure: S362ANI (Kustowski et al., 2008) and a rougher model constructed by adding realistic small-scale structure to S362ANI. Fundamental-mode Rayleigh and Love wave phase delays in the period range 35-250 seconds were measured using the approach of Ekström et al. (1997), for which PREM is the assumed reference Earth model. These measurements were compared to phase-delay predictions generated for the great-circle ray approximation, exact ray theory, and finite-frequency theory. We find that for both 3-D earth models exact ray theory provides the best fit to the measurements at short periods. At longer periods finite frequency theory provides the best fit. For the smooth earth model, the differences in fit for the various predictions are less significant at long periods than at shorter periods. The differences at long periods become more significant with increasing model roughness. In all cases, the agreement between predictions and measurements is best for paths located away from nodes in the source radiation pattern. The ability of the measured phase delays to recover the input Earth models is assessed through tests that explore

  5. Theoretical investigation of phase transition on GaAs(0 0 1)-c(4 x 4) surface

    International Nuclear Information System (INIS)

    Ishizaki, Hirotoshi; Akiyama, Toru; Nakamura, Kohji; Shiraishi, Kenji; Taguchi, Akihito; Ito, Tomonori

    2005-01-01

    The surface phase transition between GaAs(0 0 1)-c(4 x 4) and -(2 x 4)β2 surfaces is systematically investigated by using our ab initio-based approach. The phase diagram calculations for the c(4 x 4) surfaces as functions of temperature and As pressure reveal that three kinds of c(4 x 4) surfaces consisting of Ga-As dimers and/or Ga-Ga dimers become stable near the phase transition temperature. The electron counting Monte Carlo simulation and ab initio calculations are also performed to investigate the structural change of the c(4 x 4) surface after predepositing a 0.5 monolayer of Ga on the three kinds of c(4 x 4) surfaces. The calculated results suggest that the c(4 x 4) surfaces consisting of three Ga-As dimers or one Ga-Ga dimer and two Ga-As dimers in the (4 x 4) surface unit cell possibly change their structures to (2 x 4)β2 structures with Ga-As surface dimers. The conventional (2 x 4)β2 surface consisting of As dimers finally appears due to destabilization of Ga-As dimers at high temperature and high pressure

  6. Thermal performance of a phase change material on a nickel-plated surface

    International Nuclear Information System (INIS)

    Nurmawati, M.H.; Siow, K.S.; Rasiah, I.J.

    2004-01-01

    Thermal control becomes increasingly vital with IC chips becoming faster and smaller. The need to keep chips within acceptable operating temperatures is a growing challenge. Thermal interface materials (TIM) form the interfaces that improve heat transfer from the heat-generating chip to the heat dissipating thermal solution. One of the most commonly used materials in today's electronics industry is phase change material (PCM). Typically, the heat spreader is a nickel-plated copper surface. The compatibility of the PCM to this surface is crucial to the performance of the TIM. In this paper, we report on the performance of this interface. To that end, an instrument to suitably measure critical parameters, like the apparent and contact thermal resistance of the TIM, is developed according to the ASTM D5470 and calibrated. A brief theory of TIM is described and the properties of the PCM were investigated using the instrument. Thermal resistance measurements were made to investigate the effects of physical parameters like pressure, temperature and supplied power on the thermal performance of the material on nickel-plated surface. Conclusions were drawn on the effectiveness of the interface and their application in IC packages

  7. Angle - resolved photoemission study of two phases of the GaAs(100)-c(4x4) surface

    Czech Academy of Sciences Publication Activity Database

    Cukr, Miroslav; Jiříček, Petr; Bartoš, Igor; Sadowski, J.

    2008-01-01

    Roč. 100, - (2008), 072017/1-072017/4 ISSN 1742-6588 R&D Projects: GA AV ČR IAA100100628; GA ČR GA202/07/0601 Institutional research plan: CEZ:AV0Z10100521 Keywords : gallium arsenide * molecular beam epitaxy * photoelectron spectroscopy * surface reconstruction * surface phases * electron states Subject RIV: BM - Solid Matter Physics ; Magnetism

  8. Theoretical Investigation of the Structural Stabilities of Ceria Surfaces and Supported Metal Nanocluster in Vapor and Aqueous Phases

    Energy Technology Data Exchange (ETDEWEB)

    Ren, Zhibo [State Key Laboratory of Chemical Resource Engineering, Beijing University of Chemical Technology, Beijing 100029, China; Institute for Integrated Catalysis, Pacific Northwest National Laboratory, Richland, Washington 99352, United States; Liu, Ning [State Key Laboratory of Chemical Resource Engineering, Beijing University of Chemical Technology, Beijing 100029, China; Institute for Integrated Catalysis, Pacific Northwest National Laboratory, Richland, Washington 99352, United States; Chen, Biaohua [State Key Laboratory of Chemical Resource Engineering, Beijing University of Chemical Technology, Beijing 100029, China; Li, Jianwei [State Key Laboratory of Chemical Resource Engineering, Beijing University of Chemical Technology, Beijing 100029, China; Mei, Donghai [Institute for Integrated Catalysis, Pacific Northwest National Laboratory, Richland, Washington 99352, United States

    2018-01-25

    Understanding the structural stability and dynamics at the interface between the solid metal oxide and aqueous phase is significant in a variety of industrial applications including heterogeneous catalysis and environmental remediation. In the present work, the stabilities of three low-index ceria (CeO2) surfaces, i.e., (111), (110) and (100) in vapor and aqueous phases were studied using ab initio molecular dynamics simulations and density functional theory (DFT) calculations. Gibbs surface free energies as a function of temperature, water partial pressure, and water coverages were calculated using DFT based atomistic thermodynamic approach. On the basis of surface free energies, the morphology and exposed surface structures of the CeO2 nanoparticle were predicted using Wulff construction principle. It is found that the partially hydroxylated (111) and (100) are two major surface structures of CeO2 nanoparticles in vapor phase at ambient temperature (300 K). As the temperature increases, the fully dehydrated (111) surface gradually becomes the most dominant surface structure. While in aqueous phase, the exposed surface of the CeO2 nanoparticle is dominated by the hydroxylated (110) structure at 393 K. Finally, the morphology and stability of a cuboctahedron Pt13 nanocluster supported on CeO2 surfaces in both gas and aqueous phases were investigated. In gas phase, the supported Pt13 nanocluster has the tendency to wetting the CeO2 surface due to the strong metal-support interaction. The calculated interaction energies suggest the CeO2(110) surface provides the best stability for the Pt13 nanocluster. The CeO2 supported Pt13 nanoclusters are oxidized. Compared to the gas phase, the morphology of the CeO2 supported Pt13 nanocluster is less distorted due to the solvation effect provided by surrounding water molecules in aqueous phase. More electrons are transferred from the Pt13 nanocluster to the CeO2 support, implying the supported Pt13 nanocluster is further

  9. Free-Surface Optical Scattering as an Indicator of the Shock-Induced Solid-Liquid Phase Transition in Tin

    Energy Technology Data Exchange (ETDEWEB)

    Stevens, G. D.; Lutz, S. S.; Marshall, B. R.; Turley, W. D.; Veeser, L. R.; Furlanetto, M. R.; Hixson, R. S.; Holtkamp, D. B.; Jensen, B. J.; Rigg, P. A.; Wilke, M. D.

    2008-07-01

    When highly polished metal surfaces melt upon release after shock loading, they exhibit features that suggest significant surface changes accompany the phase transition. The reflection of light from such surfaces changes from specular (pre-shock) to diffuse upon melting. A familiar manifestation of this phenomenon is the loss of signal light in VISAR measurements, which occurs at pressures high enough to melt the free surface. Unlike many other potential material phase-sensitive diagnostics (e.g., reflectometry, conductivity) that show relatively small (1%–10%) changes, the specularity of reflection provides a more sensitive and definitive indication of the solid-liquid phase transition. Data will be presented that support the hypothesis that specularity changes indicate melt in a way that can be measured easily and unambiguously.

  10. Single-drop liquid phase microextraction accelerated by surface acoustic wave.

    Science.gov (United States)

    Zhang, Anliang; Zha, Yan

    2013-03-01

    A single-drop liquid phase microextraction method is presented, in which surface acoustic wave (SAW) is used for accelerating extraction speed. A pair of interdigital transducers with 27.5 MHz center frequency is fabricated on a 128° yx-LiNbO3 substrate. A radio frequency signal is applied to one of interdigital transducers to excite SAW. Plastic straw is filled with PDMS, leaving 1 mL for holding sample solution. Plastic straw with sample solution droplet is then dipping into extractant, into which SAW is radiated. Mass transportation from sample solution to extractant drop is accelerated due to acoustic streaming, and extraction time is decreased. An ionic liquid and an acid green-25 solution are used for extraction experiments. Results show that the extraction process is almost finished within 2 min, and extraction speed is increased with radio frequency signal power. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Regolith Advanced Surface Systems Operations Robot (RASSOR) Phase 2 and Smart Autonomous Sand-Swimming Excavator

    Science.gov (United States)

    Sandy, Michael

    2015-01-01

    The Regolith Advanced Surface Systems Operations Robot (RASSOR) Phase 2 is an excavation robot for mining regolith on a planet like Mars. The robot is programmed using the Robotic Operating System (ROS) and it also uses a physical simulation program called Gazebo. This internship focused on various functions of the program in order to make it a more professional and efficient robot. During the internship another project called the Smart Autonomous Sand-Swimming Excavator was worked on. This is a robot that is designed to dig through sand and extract sample material. The intern worked on programming the Sand-Swimming robot, and designing the electrical system to power and control the robot.

  12. Dynamics of two-phase interfaces and surface tensions: A density-functional theory perspective

    Science.gov (United States)

    Yatsyshin, Petr; Sibley, David N.; Duran-Olivencia, Miguel A.; Kalliadasis, Serafim

    2016-11-01

    Classical density functional theory (DFT) is a statistical mechanical framework for the description of fluids at the nanoscale, where the inhomogeneity of the fluid structure needs to be carefully accounted for. By expressing the grand free-energy of the fluid as a functional of the one-body density, DFT offers a theoretically consistent and computationally accessible way to obtain two-phase interfaces and respective interfacial tensions in a ternary solid-liquid-gas system. The dynamic version of DFT (DDFT) can be rigorously derived from the Smoluchowsky picture of the dynamics of colloidal particles in a solvent. It is generally agreed that DDFT can capture the diffusion-driven evolution of many soft-matter systems. In this context, we use DDFT to investigate the dynamic behaviour of two-phase interfaces in both equilibrium and dynamic wetting and discuss the possibility of defining a time-dependent surface tension, which still remains in debate. We acknowledge financial support from the European Research Council via Advanced Grant No. 247031 and from the Engineering and Physical Sciences Research Council of the UK via Grants No. EP/L027186 and EP/L020564.

  13. Micropatterned surfaces through moisture-induced phase-separation of polystyrene-clay nanocomposite particles.

    Science.gov (United States)

    Nair, Bindu P; Pavithran, Chorappan

    2010-08-03

    We report micropatterned polystyrene-clay nanocomposite (PCN) surfaces with concavities by moisture-induced phase separation of PCN particles. Micropatterned film with concavity size of 800 nm to 1.3 microm and a high number density of 2 x 10(8) features/cm(2) was obtained by drop-casting PCN solution (20 mg/mL PCN/THF) under ambient relative humidity of 70-80%. It is proposed that water droplets were channeled through the hydrophilic interfaces between the PCN particles, and the two-dimensional array of concavities was formed by spontaneous phase separation due to the presence of rigid clay platelets. The concavity size and number density can be tuned by varying the solvent for PCN. Micropatterned film with concavity size in the range of 650 nm to 1.1 microm with a number density of 5 x 10(7) features/cm(2) was obtained using chloroform as solvent, whereas a concavity size of 150-740 nm and number density of 10(8) features/cm(2) were obtained using carbon disulfide.

  14. Evaluation of flyash surface phenomena and the application of surface analysis technology. Summary report: Phase I. [44 elements; 86 references

    Energy Technology Data Exchange (ETDEWEB)

    Smith, R.D.

    1981-06-01

    The factors governing the formation of flyash surfaces during and following coal combustion are reviewed. The competing chemical and physical processes during the evolution of inorganic material in coal during combustion into flyash are described with respect to various surface segregation processes. Two mechanisms leading to surface enrichment are volatilization-condensation processes and diffusion processes within individual flyash particles. The experimental evidence for each of these processes is reviewed. It is shown that the volatilization-condensation process is the major factor leading to trace element enrichment in smaller flyash particles. Evidence also exists from surface analyses of flyash and representative mineral matter that diffusion processes may lead to surface enrichment of elements not volatilized or cause transport of surface-condensed elements into the flyash matrix. The semiquantitative determination of the relative importance of these two processes can be determined by comparison of concentration versus particle size profiles with surface-depth profiles obtained using surface analysis techniques. A brief description of organic transformations on flyash surfaces is also presented. The various surface analytical techniques are reviewed and the relatively new technique of Static-Secondary Ion Mass Spectroscopy is suggested as having significant advantages in studies of surfaces and diffusion processes in model systems. Several recommendations are made for research relevant to flyash formation and processes occurring on flyash surfaces.

  15. Surface modification of superaustenitic and maraging stainless steels by low-temperature gas-phase carburization

    Science.gov (United States)

    Gentil, Johannes

    Low-temperature gas-phase carburization of 316L austenitic stainless steel was developed in recent years by the Swagelok company. This process generates great mechanical and electrochemical surface properties. Hardness, wear resistance, fatigue behavior, and corrosion resistance are dramatically improved, while the formation of carbides is effectively suppressed. This new technique is of technical, economical, but especially of scientific interest because the surface properties of common stainless steel can be enhanced to a level of more sophisticated and more expensive superalloys. The consequential continuation of previous research is the application of the carburization process to other steel grades. Differences in chemical composition, microstructure, and passivity between the various alloys may cause technical problems and it is expected that the initial process needs to be optimized for every specific material. This study presents results of low-temperature carburization of AL-6XN (superaustenitic stainless steel) and PH13-8Mo (precipitation-hardened martensitic stainless steel). Both alloys have been treated successfully in terms of creating a hardened surface by introducing high amounts of interstitially dissolved carbon. The surface hardness of AL-6XN was increased to 12GPa and is correlated with a colossal carbon supersaturation at the surface of up to 20 at.%. The hardened case develops a carburization time-dependent thickness between 10mum after one carburization cycle and up to 35mum after four treatments and remains highly ductile. Substantial broadening of X-ray diffraction peaks in low-temperature carburized superaustenitic stainless steels are attributed to the generation of very large compressive biaxial residual stresses. Those large stresses presumably cause relaxations of the surface, so-called undulations. Heavily expanded regions of carburized AL-6XN turn ferromagnetic. Non-carburized AL-6XN is known for its outstanding corrosion resistance

  16. Near-surface test facility. Phase I. Geologic site characterization report

    Energy Technology Data Exchange (ETDEWEB)

    Moak, D.J.; Wintczak, T.M.

    1980-08-01

    The report is a description of the geology and characterization of the rock mass of the area in which the Phase I qualification tests at the Near-Surface Test Facility (NSTF) are being performed. The NSTF is located on Gable Mountain within the Hanford Site near Richland, Washington. It is located in the entablature of the Pomona Member, an upper flow in the Columbia River Basalt Group, and is approximately 150 feet (47.5 meters) below the surface. Core logging from the instrument boreholes coupled with joint mapping, statistics, and other test data provided the basis for a detailed characterization of the 16-foot x 20-foot x 28-foot (5-meter x 6-meter x 9-meter) rock masses surrounding Full-Scale Heater Tests No. 1 and No. 2. The Pomona entablature contains three joint sets delineated by their degree of dip, each with apertures averaging 0.25 millimeter and having no preferred strike orientation. Although joint frequencies in the study area exceed 4 joints per foot (13 per meter), the rock-mass classification rating is good.

  17. The structure optimization of gas-phase surface discharge and its application for dye degradation

    Science.gov (United States)

    Ying, CAO; Jie, LI; Nan, JIANG; Yan, WU; Kefeng, SHANG; Na, LU

    2018-05-01

    A gas-phase surface discharge (GSD) was employed to optimize the discharge reactor structure and investigate the dye degradation. A dye mixture of methylene blue, acid orange and methyl orange was used as a model pollutant. The results indicated that the reactor structure of the GSD system with the ratio of tube inner surface area and volume of 2.48, screw pitch between a high-voltage electrode of 9.7 mm, high-voltage electrode wire diameter of 0.8 mm, dielectric tube thickness of 2.0 mm and tube inner diameter of 16.13 mm presented a better ozone (O3) generation efficiency. Furthermore, a larger screw pitch and smaller wire diameter enhanced the O3 generation. After the dye mixture degradation by the optimized GSD system, 73.21% and 50.74% of the chemical oxygen demand (COD) and total organic carbon removal rate were achieved within 20 min, respectively, and the biochemical oxygen demand (BOD) and biodegradability (BOD/COD) improved.

  18. Tuning colloidal quantum dot band edge positions through solution-phase surface chemistry modification

    Science.gov (United States)

    Kroupa, Daniel M.; Vörös, Márton; Brawand, Nicholas P.; McNichols, Brett W.; Miller, Elisa M.; Gu, Jing; Nozik, Arthur J.; Sellinger, Alan; Galli, Giulia; Beard, Matthew C.

    2017-05-01

    Band edge positions of semiconductors determine their functionality in many optoelectronic applications such as photovoltaics, photoelectrochemical cells and light emitting diodes. Here we show that band edge positions of lead sulfide (PbS) colloidal semiconductor nanocrystals, specifically quantum dots (QDs), can be tuned over 2.0 eV through surface chemistry modification. We achieved this remarkable control through the development of simple, robust and scalable solution-phase ligand exchange methods, which completely replace native ligands with functionalized cinnamate ligands, allowing for well-defined, highly tunable chemical systems. By combining experiments and ab initio simulations, we establish clear relationships between QD surface chemistry and the band edge positions of ligand/QD hybrid systems. We find that in addition to ligand dipole, inter-QD ligand shell inter-digitization contributes to the band edge shifts. We expect that our established relationships and principles can help guide future optimization of functional organic/inorganic hybrid nanostructures for diverse optoelectronic applications.

  19. Elucidation of the Oxygen Surface Kinetics in a Coated Dual-Phase Membrane for Enhancing Oxygen Permeation Flux.

    Science.gov (United States)

    Na, Beom Tak; Park, Jeong Hwan; Park, Jong Hyuk; Yu, Ji Haeng; Joo, Jong Hoon

    2017-06-14

    The dual-phase membrane has received much attention as the solution to the instability of the oxygen permeation membrane. It has been reported that the oxygen flux of the dual-phase membrane is greatly enhanced by the active coating layer. However, there has been little discussion about the enhancement mechanism by surface coating in the dual-phase membrane. This study investigates the oxygen flux of the Ce 0.9 Gd 0.1 O 2-δ -La 0.7 Sr 0.3 MnO 3±δ (GDC 80 vol %/LSM 20 vol %) composite membrane depending on the oxygen partial pressure (P O 2 ) to elucidate the mechanism of enhanced oxygen flux by the surface modification in the fluorite-rich phase dual-phase membrane. The oxygen permeation resistances were obtained from the oxygen flux as a function of P O 2 using the oxygen permeation model. The surface exchange coefficient (k) and the bulk diffusion coefficient (D) were calculated from these resistances. According to the calculated k and D values, we concluded that the active coating layer (La 0.6 Sr 0.4 CoO 3-δ ) significantly increased the k value of the membrane. Furthermore, the surface exchange reaction on the permeate side was more sluggish than that at the feed side under operating conditions (feed: 0.21 atm/permeate side: 4.7 × 10 -4 atm). Therefore, the enhancement of the oxygen surface exchange kinetics at the permeate side is more important in improving the oxygen permeation flux of the thin film-based fluorite-rich dual-phase membrane. These results provide new insight about the function of the surface coating to enhance the oxygen permeation flux of the dual-phase membrane.

  20. Stationary infinitely divisible processes

    DEFF Research Database (Denmark)

    Barndorff-Nielsen, Ole E.

    Several recent strands of work has led to the consideration of various types of continuous time stationary and infinitely divisible processes. A review of these types, with some new results, is presented.......Several recent strands of work has led to the consideration of various types of continuous time stationary and infinitely divisible processes. A review of these types, with some new results, is presented....

  1. Laboratory Investigations of Stationary Methane Anemometer

    Science.gov (United States)

    Kruczkowski, Janusz; Krawczyk, Jerzy; Ostrogórski, Piotr

    2017-12-01

    This paper presents a new stationary device that can perform simultaneous measurements of air flow velocity and methane concentration in a mine heading (stationary methane anemometer). The test station is designed to use the instrument to test the effect of various parameters on the air-methane stream. The air velocities and methane concentrations were fed to the measuring area via an injector and recorded. The results present numerical simulations of flow phenomena that occurred during measurement experiments.

  2. Dampers for Stationary Labyrinth Seals

    Science.gov (United States)

    El-Aini, Yehia; Mitchell, William; Roberts, Lawrence; Montgomery, Stuart; Davis, Gary

    2011-01-01

    Vibration dampers have been invented that are incorporated as components within the stationary labyrinth seal assembly. These dampers are intended to supplement other vibration-suppressing features of labyrinth seals in order to reduce the incidence of high-cycle-fatigue failures, which have been known to occur in the severe vibratory environments of jet engines and turbopumps in which labyrinth seals are typically used. A vibration damper of this type includes several leaf springs and/or a number of metallic particles (shot) all held in an annular seal cavity by a retaining ring. The leaf springs are made of a spring steel alloy chosen, in conjunction with design parameters, to maintain sufficient preload to ensure effectiveness of damping at desired operating temperatures. The cavity is vented via a small radial gap between the retaining ring and seal housing. The damping mechanism is complex. In the case of leaf springs, the mechanism is mainly friction in the slippage between the seal housing and individual dampers. In the case of a damper that contains shot, the damping mechanism includes contributions from friction between individual particles, friction between particles and cavity walls, and dissipation of kinetic energy of impact. The basic concept of particle/shot vibration dampers has been published previously; what is new here is the use of such dampers to suppress traveling-wave vibrations in labyrinth seals. Damping effectiveness depends on many parameters, including, but not limited to, coefficient of friction, mode shape, and frequency and amplitude of vibrational modes. In tests, preloads of the order of 6 to 15 lb (2.72 to 6.8 kilograms) per spring damper were demonstrated to provide adequate damping levels. Effectiveness of shot damping of vibrations having amplitudes from 20 to 200 times normal terrestrial gravitational acceleration (196 to 1,960 meters per square second) and frequencies up to 12 kHz was demonstrated for shot sizes from 0.032 to

  3. A new damage diagnosis approach for NC machine tools based on hybrid Stationary subspace analysis

    Science.gov (United States)

    Gao, Chen; Zhou, Yuqing; Ren, Yan

    2017-05-01

    This paper focused on the damage diagnosis for NC machine tools and put forward a damage diagnosis method based on hybrid Stationary subspace analysis (SSA), for improving the accuracy and visibility of damage identification. First, the observed single sensor signal was reconstructed to multi-dimensional signals by the phase space reconstruction technique, as the inputs of SSA. SSA method was introduced to separate the reconstructed data into stationary components and non-stationary components without the need for independency and prior information of the origin signals. Subsequently, the selected non-stationary components were analysed for training LS-SVM (Least Squares Support Vector Machine) classifier model, in which several statistic parameters in the time and frequency domains were exacted as the sample of LS-SVM. An empirical analysis in NC milling machine tools is developed, and the result shows high accuracy of the proposed approach.

  4. Stationary Liquid Fuel Fast Reactor

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Won Sik [Purdue Univ., West Lafayette, IN (United States); Grandy, Andrew [Argonne National Lab. (ANL), Argonne, IL (United States); Boroski, Andrew [Argonne National Lab. (ANL), Argonne, IL (United States); Krajtl, Lubomir [Argonne National Lab. (ANL), Argonne, IL (United States); Johnson, Terry [Argonne National Lab. (ANL), Argonne, IL (United States)

    2015-09-30

    For effective burning of hazardous transuranic (TRU) elements of used nuclear fuel, a transformational advanced reactor concept named SLFFR (Stationary Liquid Fuel Fast Reactor) was proposed based on stationary molten metallic fuel. The fuel enters the reactor vessel in a solid form, and then it is heated to molten temperature in a small melting heater. The fuel is contained within a closed, thick container with penetrating coolant channels, and thus it is not mixed with coolant nor flow through the primary heat transfer circuit. The makeup fuel is semi- continuously added to the system, and thus a very small excess reactivity is required. Gaseous fission products are also removed continuously, and a fraction of the fuel is periodically drawn off from the fuel container to a processing facility where non-gaseous mixed fission products and other impurities are removed and then the cleaned fuel is recycled into the fuel container. A reference core design and a preliminary plant system design of a 1000 MWt TRU- burning SLFFR concept were developed using TRU-Ce-Co fuel, Ta-10W fuel container, and sodium coolant. Conservative design approaches were adopted to stay within the current material performance database. Detailed neutronics and thermal-fluidic analyses were performed to develop a reference core design. Region-dependent 33-group cross sections were generated based on the ENDF/B-VII.0 data using the MC2-3 code. Core and fuel cycle analyses were performed in theta-r-z geometries using the DIF3D and REBUS-3 codes. Reactivity coefficients and kinetics parameters were calculated using the VARI3D perturbation theory code. Thermo-fluidic analyses were performed using the ANSYS FLUENT computational fluid dynamics (CFD) code. Figure 0.1 shows a schematic radial layout of the reference 1000 MWt SLFFR core, and Table 0.1 summarizes the main design parameters of SLFFR-1000 loop plant. The fuel container is a 2.5 cm thick cylinder with an inner radius of 87.5 cm. The fuel

  5. Effect of focusing flow on stationary spot machining properties in elastic emission machining.

    Science.gov (United States)

    Takei, Yoshinori; Mimura, Hidekazu

    2013-05-16

    Ultraprecise optical elements are applied in advanced optical apparatus. Elastic emission machining (EEM) is one of the ultraprecision machining methods used to fabricate shapes with 0.1-nm accuracy. In this study, we proposed and experimentally tested the control of the shape of a stationary spot profile by introducing a focusing-flow state between the nozzle outlet and the workpiece surface in EEM. The simulation results indicate that the focusing-flow nozzle sharpens the distribution of the velocity on the workpiece surface. The results of machining experiments verified those of the simulation. The obtained stationary spot conditions will be useful for surface processing with a high spatial resolution.

  6. Study of surface activity of piroxicam at the interface of palm oil esters and various aqueous phases.

    Science.gov (United States)

    Abdulkarim, Muthanna Fawzy; Abdullah, Ghassan Zuhair; Chitneni, Mallikarjun; Yam, Mun Fei; Mahdi, Elrashid Saleh; Salman, Ibrahim Muhammad; Ameer, Omar Ziad; Sattar, Munavvar Abdul; Basri, Mahiran; Noor, Azmin Mohd

    2012-04-01

    The surface activity of some non-steroidal anti-inflammatory agents like ibuprofen was investigated extensively. This fact has attracted the researchers to extend this behavior to other agents like piroxicam. Piroxicam molecules are expected to orient at the interface of oil and aqueous phase. The aim of this study was, firstly, to assess the surface and interfacial tension behaviour of newly synthesised palm oil esters and various pH phosphate buffers. Furthermore, the surface and interfacial tension activity of piroxicam was studied. All the measurements of surface and interfacial tension were made using the tensiometer. The study revealed that piroxicam has no effect on surface tension values of all pH phosphate buffers and palm oil esters. Similarly, various concentrations of piroxicam did not affect the interfacial tensions between the oil phase and the buffer phases. Accordingly, the interfacial tension values of all mixtures of oil and phosphate buffers were considerably high which indicates the immiscibility. It could be concluded that piroxicam has no surface activity. Additionally, there is no surface pressure activity of piroxicam at the interface of plam oil esters and phosphate buffers in the presence of Tweens and Spans.

  7. Influence of stationary and non-stationary conditions on drying time and mechanical properties of a porcelain slab

    Science.gov (United States)

    Hammouda, Imen; Mihoubi, Daoued

    2017-12-01

    This work deals with a numerical study of the response of a porcelain slab when subjected to convective drying in stationary and non-stationary conditions. The used model describes heat, mass, and momentum transfers is applied to an unsaturated viscoelastic medium described by a Maxwell model. The numerical code allows us to determine the effect of the surrounding air temperature on drying kinetics and on mechanical stress intensities. Von Mises stresses are analysed in order to foresee an eventual damage that may occur during drying. Simulation results for several temperatures in the range of [30 °C, 90 °C] shows that for the temperature from 30 °C to 60 °C, Von Mises stresses are always lower than the yield strength. But above 70 °C, Von Mises stresses are higher than the ultimate strength, and consequently there is a risk of crack at the end of the constant drying rate period. The idea proposed in this work is to integrate a reducing temperature phase when the predicted Von Mises stress intensity exceeds the admissible stress. Simulation results shows that a non-stationary convective drying (90-60 °C) allows us to optimize costs and quality by reducing the drying time and maintaining Von Mises stress values under the admissible stress.

  8. Prediction and Optimization of Phase Transformation Region After Spot Continual Induction Hardening Process Using Response Surface Method

    Science.gov (United States)

    Qin, Xunpeng; Gao, Kai; Zhu, Zhenhua; Chen, Xuliang; Wang, Zhou

    2017-09-01

    The spot continual induction hardening (SCIH) process, which is a modified induction hardening, can be assembled to a five-axis cooperating computer numerical control machine tool to strengthen more than one small area or relatively large area on complicated component surface. In this study, a response surface method was presented to optimize phase transformation region after the SCIH process. The effects of five process parameters including feed velocity, input power, gap, curvature and flow rate on temperature, microstructure, microhardness and phase transformation geometry were investigated. Central composition design, a second-order response surface design, was employed to systematically estimate the empirical models of temperature and phase transformation geometry. The analysis results indicated that feed velocity has a dominant effect on the uniformity of microstructure and microhardness, domain size, oxidized track width, phase transformation width and height in the SCIH process while curvature has the largest effect on center temperature in the design space. The optimum operating conditions with 0.817, 0.845 and 0.773 of desirability values are expected to be able to minimize ratio (tempering region) and maximize phase transformation width for concave, flat and convex surface workpieces, respectively. The verification result indicated that the process parameters obtained by the model were reliable.

  9. Cell cycle phase-specific surface expression of nerve growth factor receptors TrkA and p75(NTR).

    Science.gov (United States)

    Urdiales, J L; Becker, E; Andrieu, M; Thomas, A; Jullien, J; van Grunsven, L A; Menut, S; Evan, G I; Martín-Zanca, D; Rudkin, B B

    1998-09-01

    Expression of the nerve growth factor (NGF) receptors TrkA and p75(NTR) was found to vary at the surface of PC12 cells in a cell cycle phase-specific manner. This was evidenced by using flow cytometric and microscopic analysis of cell populations labeled with antibodies to the extracellular domains of both receptors. Differential expression of these receptors also was evidenced by biotinylation of surface proteins and Western analysis, using antibodies specific for the extracellular domains of TrkA and p75(NTR). TrkA is expressed most strongly at the cell surface in M and early G1 phases, whereas p75(NTR) is expressed mainly in late G1, S, and G2 phases. This expression reflects the molecular and cellular responses to NGF in specific phases of the cell cycle; in the G1 phase NGF elicits both the anti-mitogenic effect, i.e., inhibition of the G1 to S transition, and the differentiation response whereas a survival effect is provoked elsewhere in the cell cycle. A model is proposed relating these responses to the surface expression of the two receptors. These observations open the way for novel approaches to the investigation of the mechanism of NGF signal transduction.

  10. Effect of elemental composition of ion beam on the phase formation and surface strengthening of structural materials

    International Nuclear Information System (INIS)

    Avdienko, K.I.; Avdienko, A.A.; Kovalenko, I.A.

    2001-01-01

    The investigation results are reported on the influence of ion beam element composition on phase formation, wear resistance and microhardness of surface layers of titanium alloys VT-4 and VT-16 as well as stainless steel 12Kh18N10T implanted with nitrogen, oxygen and boron. It is stated that ion implantation into structural materials results in surface hardening and is directly dependent on element composition of implanted ion beam. The presence of oxygen in boron or nitrogen ion beams prevents the formation of boride and nitride phases thus decreasing a hardening effect [ru

  11. Phase contrast imaging reveals low lung volumes and surface areas in the developing marsupial.

    Directory of Open Access Journals (Sweden)

    Shannon J Simpson

    Full Text Available Marsupials are born with immature lungs when compared to eutherian mammals and rely, to various extents, on cutaneous gas exchange in order to meet metabolic requirements. Indeed, the fat-tailed dunnart is born with lungs in the canalicular stage of development and relies almost entirely on the skin for gas exchange at birth; consequently undergoing the majority of lung development in air. Plane radiographs and computed tomography data sets were acquired using phase contrast imaging with a synchrotron radiation source for two marsupial species, the fat-tailed dunnart and the larger tammar wallaby, during the first weeks of postnatal life. Phase contrast imaging revealed that only two lung sacs contain air after the first hour of life in the fat-tailed dunnart. While the lung of the tammar wallaby was comparatively more developed, both species demonstrated massive increases in air sac number and architectural complexity during the postnatal period. In addition, both the tammar wallaby and fat-tailed dunnart had lower lung volumes and parenchymal surface areas than were expected from morphometrically determined allometric equations relating these variables to body mass during the neonatal period. However, lung volume is predicted to scale with mass as expected after the neonatal marsupial reaches a body mass of ∼1 g and no longer relies on the skin for gas exchange. Decreased lung volume in the marsupial neonate further supports the maxim that cutaneous gas exchange occurs in the marsupial neonate because the respiratory apparatus is not yet capable of meeting the gas exchange requirements of the newborn.

  12. The coupling effect of gas-phase chemistry and surface reactions on oxygen permeation and fuel conversion in ITM reactors

    KAUST Repository

    Hong, Jongsup

    2015-08-01

    © 2015 Elsevier B.V. The effect of the coupling between heterogeneous catalytic reactions supported by an ion transport membrane (ITM) and gas-phase chemistry on fuel conversion and oxygen permeation in ITM reactors is examined. In ITM reactors, thermochemical reactions take place in the gas-phase and on the membrane surface, both of which interact with oxygen permeation. However, this coupling between gas-phase and surface chemistry has not been examined in detail. In this study, a parametric analysis using numerical simulations is conducted to investigate this coupling and its impact on fuel conversion and oxygen permeation rates. A thermochemical model that incorporates heterogeneous chemistry on the membrane surface and detailed chemical kinetics in the gas-phase is used. Results show that fuel conversion and oxygen permeation are strongly influenced by the simultaneous action of both chemistries. It is shown that the coupling somewhat suppresses the gas-phase kinetics and reduces fuel conversion, both attributed to extensive thermal energy transfer towards the membrane which conducts it to the air side and radiates to the reactor walls. The reaction pathway and products, in the form of syngas and C2 hydrocarbons, are also affected. In addition, the operating regimes of ITM reactors in which heterogeneous- or/and homogeneous-phase reactions predominantly contribute to fuel conversion and oxygen permeation are elucidated.

  13. A local leaky-box model for the local stellar surface density-gas surface density-gas phase metallicity relation

    Science.gov (United States)

    Zhu, Guangtun Ben; Barrera-Ballesteros, Jorge K.; Heckman, Timothy M.; Zakamska, Nadia L.; Sánchez, Sebastian F.; Yan, Renbin; Brinkmann, Jonathan

    2017-07-01

    We revisit the relation between the stellar surface density, the gas surface density and the gas-phase metallicity of typical disc galaxies in the local Universe with the SDSS-IV/MaNGA survey, using the star formation rate surface density as an indicator for the gas surface density. We show that these three local parameters form a tight relationship, confirming previous works (e.g. by the PINGS and CALIFA surveys), but with a larger sample. We present a new local leaky-box model, assuming star-formation history and chemical evolution is localized except for outflowing materials. We derive closed-form solutions for the evolution of stellar surface density, gas surface density and gas-phase metallicity, and show that these parameters form a tight relation independent of initial gas density and time. We show that, with canonical values of model parameters, this predicted relation match the observed one well. In addition, we briefly describe a pathway to improving the current semi-analytic models of galaxy formation by incorporating the local leaky-box model in the cosmological context, which can potentially explain simultaneously multiple properties of Milky Way-type disc galaxies, such as the size growth and the global stellar mass-gas metallicity relation.

  14. Prediction of deformations during gas-tungsten-arc stationary welds

    International Nuclear Information System (INIS)

    Duncan, D.B.; Giedt, W.H.

    1980-10-01

    Local temperature measurements on the heated and unheated surfaces, and strain measurements on the unheated surfaces of unrestrained circular weld specimens of annealed and cold-rolled Nitronic 40 stainless steel during stationary welding, are compared with values predicted from finite-element programs for temperature and strain variations. Experimental and predicted temperature histories agree within 10%. Predicted and measured hoop strain profiles (using a moire fringe technique), for the unheated surface are compared, showing significant deviations near the central region. Transient deflection measurements of the unheated specimen surfaces show good agreement with theory during the period the arc is operating. Close agreement in deflection behavior was observed during the cooling portion of the weld cycle for the annealed specimen, whereas substantial deviations occurred for the cold-rolled specimens

  15. Stationary radiation of objects with scattering media

    International Nuclear Information System (INIS)

    Vasil'eva, Inna A

    2001-01-01

    The radiation observed inside or outside a stationary radiator with a scattering medium is a sum of components, each being determined by, first, the primary radiation from some part of the radiator and, second, the probability of this radiation reaching the region where it is observed. In this review, general and rather simple relations between these components are discussed. These relations, unlike the components themselves, are independent of the specific optical characteristics of the object as well as of its geometry, inhomogeneity, etc. In deriving the relations, the situations in which geometrical optics is either applicable or inapplicable to radiation in a scattering medium are considered. For the case where geometrical optics does apply, stationary relations are derived from the probabilistic stationarity condition for radiation passing through the medium, i.e., from the fact that all radiation emitted in a stationary regime disappears with probability unity. Equilibrium relations are derived from the stationary relations in the particular case of a thermal radiator in an isothermal cavity. To derive the stationary relations in the geometrical optics approximation, we obtain general solutions of the linear equation of transfer using the Green function approach. If geometrical optics cannot be applied to a scattering and radiating medium, only relations for the components of outgoing thermal radiation are obtained, and the generalized Kirchhoff law, obtained by Levin and Rytov using statistical radio-physics methods, is employed. In this case, stationary relations are also derived from a probabilistic stationarity condition; the equilibrium relations follow from the stationary ones as well as from the equilibrium condition for radiation in the isothermal cavity. The quantities involved in all the relations obtained are a subject of experimental and computational spectroscopic studies. Examples of current and potential applications are given. The relations

  16. Analyzing Non Stationary Processes in Radiometers

    Science.gov (United States)

    Racette, Paul

    2010-01-01

    The lack of well-developed techniques for modeling changing statistical moments in our observations has stymied the application of stochastic process theory for many scientific and engineering applications. Non linear effects of the observation methodology is one of the most perplexing aspects to modeling non stationary processes. This perplexing problem was encountered when modeling the effect of non stationary receiver fluctuations on the performance of radiometer calibration architectures. Existing modeling approaches were found not applicable; particularly problematic is modeling processes across scales over which they begin to exhibit non stationary behavior within the time interval of the calibration algorithm. Alternatively, the radiometer output is modeled as samples from a sequence random variables; the random variables are treated using a conditional probability distribution function conditioned on the use of the variable in the calibration algorithm. This approach of treating a process as a sequence of random variables with non stationary stochastic moments produce sensible predictions of temporal effects of calibration algorithms. To test these model predictions, an experiment using the Millimeter wave Imaging Radiometer (MIR) was conducted. The MIR with its two black body calibration references was configured in a laboratory setting to observe a third ultra-stable reference (CryoTarget). The MIR was programmed to sequentially sample each of the three references in approximately a 1 second cycle. Data were collected over a six-hour interval. The sequence of reference measurements form an ensemble sample set comprised of a series of three reference measurements. Two references are required to estimate the receiver response. A third reference is used to estimate the uncertainty in the estimate. Typically, calibration algorithms are designed to suppress the non stationary effects of receiver fluctuations. By treating the data sequence as an ensemble

  17. Mechanics of the Separating Surface for a Two-Phase Co-current Flow in a Porous Medium

    DEFF Research Database (Denmark)

    Shapiro, Alexander A.

    2016-01-01

    A mechanical description of an unsteady two-phase co-current flow in a porous medium is developed based on the analysis of the geometry and motion of the surface separating the two phases. It is demonstrated that the flow should be considered as essentially three-dimensional, even if the phase...... velocities are co-directed, since the phase interface is on average inclined to the direction of the flow. Kinematics of the flow is described, distinguishing between the average velocities of the bulk phases and their velocity near the interface between them. Dynamics of the flow is analyzed by means...... of the extended Maxwell-Stefan formalism, as in our previous paper (Shapiro 2015). Force balances are formulated in the directions parallel and orthogonal to the flow. A complete system of the flow equations, generalizing the traditional Buckley–Leverett and Rappoport–Leas system, is derived. Sample computations...

  18. Correlations Between retention indices and molecular structure of aliphatic alcohols and of their benzoyl derivatives on phenyl substituted polysiloxane stationary phases; Cromatografia en fase gaseosa sobre metilfenilpolisiloxanos. Estructura molecular y parametros de retencion para alcoholes y sus derivados benzoilados

    Energy Technology Data Exchange (ETDEWEB)

    Pias, J. B.; Gasco, L.

    1976-07-01

    The retention indices of aliphatic alcohols of carbon number up to C{sub g}, and of their benzoyl derivatives up to C{sub 7}, were determined in columns packed with Chromo sorb G (AW-DMCS-HP) coated previously with 5% methyl, and methyl phenyl polysiloxanes with increasing polarity (SE-30, 0V-3, 0V-7, 0V-11, 0V-17 and OV-25). Correlations between retention indices and chain length for 1-alcohols, 2-alcohols, 3-alcohols, 1 , on -3-alcohols, 2-methyl-1-alcohols and for their corresponding benzoyl derivatives were calculated at 100, 120 and 140 degree centigree. In alcohols, a -CH{sub 2}- group increases I approximately 100 units, and in their benzoyl derivatives from 80 to 100 units. Dispersion indices {delta}l , and positional and structural increments {delta}I, were evaluated for -OH and benzoyl groups in terms of phase polarity and chain length. Effects of chain length, chain branching and double bond location on retention parameters were also studied. (Author) 23 refs.

  19. A layered Dirac system candidate: Fermi surface and anomalous Berry phase in ZrSiSe

    Science.gov (United States)

    Chiu, Yu-Che; Chen, Kuan-Wen; Graf, David; Zhou, Qiong; Martin, Thomas J.; Chan, Julia Y.; Johannes, Michelle; Baumbach, Ryan E.; Balicas, Luis

    ZrSiSe was recently claimed to correspond to a novel type of nodal Dirac system. We synthesized single crystals through a combination of solid state reaction and chemical vapor transport. The as-grown single crystals display residual resistivities on the order of 100 nOhmcm at 2K yielding a resistivity ratio surpassing 200. Magnetoresistance (MR) measurements reveal a non-saturating increase in the resistivity by a factor of 500000% under fields up to 35 Tesla. De Haas van Alphen measurements under high magneticfields reveal a Fermi surface that is more complex than previously reported, although its geometry generally agrees with band structure calculations that indicate Dirac-like dispersion in the bulk around the Fermi energy. The charge carrier effective masses extracted from Lifshitz-Kosevich (LK) fits to the amplitude of quantum oscillations were found to range between 0.08me to 0.5me where me is the free electron mass. Fittings of the oscillatory signal to the LK formalism further reveal the existence of cyclotron orbits displaying non-trivial Berry phases approaching pi, which is consistent with the expectations from band structure calculations. funded by DOE, NSF, NHMFL.

  20. A Synthetic Phased Array Surface Acoustic Wave Sensor for Quantifying Bolt Tension

    Directory of Open Access Journals (Sweden)

    Rasim Guldiken

    2012-09-01

    Full Text Available In this paper, we report our findings on implementing a synthetic phased array surface acoustic wave sensor to quantify bolt tension. Maintaining proper bolt tension is important in many fields such as for ensuring safe operation of civil infrastructures. Significant advantages of this relatively simple methodology is its capability to assess bolt tension without any contact with the bolt, thus enabling measurement at inaccessible locations, multiple bolt measurement capability at a time, not requiring data collection during the installation and no calibration requirements. We performed detailed experiments on a custom-built flexible bench-top experimental setup consisting of 1018 steel plate of 12.7 mm (½ in thickness, a 6.4 mm (¼ in grade 8 bolt and a stainless steel washer with 19 mm (¾ in of external diameter. Our results indicate that this method is not only capable of clearly distinguishing properly bolted joints from loosened joints but also capable of quantifying how loose the bolt actually is. We also conducted detailed signal-to-noise (SNR analysis and showed that the SNR value for the entire bolt tension range was sufficient for image reconstruction.

  1. CdSe Nanoparticles with Clean Surfaces: Gas Phase Synthesis and Optical Properties

    Directory of Open Access Journals (Sweden)

    Zhang Hongwei

    2015-01-01

    Full Text Available CdSe nanoparticles (NPs were generated in gas phase with a magnetron plasma gas aggregation cluster beam source. Coagulation-free CdSe nanocrystals with very clean particle surface and interface, as well as a fairly uniform spatial distribution were obtained. The deposited NPs have a good dispersity with a mean diameter of about 4.8nm. A strong photoluminescence band corresponding to the near- band-edge transition of the CdSe NPs was observed. The CdSe NP films show a significant photoconductance induced by laser irradiation. With an applied bias voltage of 10V, the photo- induced current can be as high as 0.4mA under 0.01mW/mm2 405nm laser illumination. Our approach offers an alternative method for CdSe NP synthesis, which has the advantages such as high purity, good process and product control, as well as mass production, as compared to the existing methods.

  2. Organoselenium Surface Modification of Stainless Steel Surfaces To Prevent Biofouling in Treatment of Space Wastestreams, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — The objective of this work is to quantify the reduction of biofilm formation in a water distribution system resulting from an organoselenium surface coating on...

  3. A Cassie-Like Law Using Triple Phase Boundary Line Fractions for Faceted Droplets on Chemically Heterogeneous Surfaces

    DEFF Research Database (Denmark)

    Larsen, Simon Tylsgaard; Taboryski, Rafael Jozef

    2009-01-01

    We present experimental contact angle data for surfaces, which were surface-engineered with a hydrophobic micropattern of hexagonal geometry. The chemically heterogeneous surface of the same hexagonal pattern of defects resulted in faceted droplets of hexagonal shape. When measuring the advancing...... contact angles with a viewing position aligned parallel to rows of defects, we found that an area averaged Cassie-law failed in describing the data. By replacing the area fractions by line fractions of the triple phase boundary Line segments in the Cassie equation, we found excellent agreement with data....

  4. Ku Band Phased Array Feed Development for Surface Water Ocean Topography Mission

    Data.gov (United States)

    National Aeronautics and Space Administration — The purpose of this project is to design components essential to the development of phased arrays and phased array feeds for use in remote sensing. Specifically the...

  5. Numerical simulation of wind wave surface profiles with tuned phase spectra

    Digital Repository Service at National Institute of Oceanography (India)

    Varkey, M.J.

    It is known that the phases of the individual harmonic components in a linear narrow band wave spectrum are uniformly random. It has been suggested by some workers that some sort of phase coupling and `locking' between the different spectral...

  6. Lateral gas phase diffusion length of boron atoms over Si/B surfaces during CVD of pure boron layers

    NARCIS (Netherlands)

    Mohammadi, V.; Nihtianov, S.

    2016-01-01

    The lateral gas phase diffusion length of boron atoms, LB, along silicon and boron surfaces during chemical vapor deposition(CVD) using diborane (B2H6) is reported. The value of LB is critical for reliable and uniform boron layer coverage. The presented information was obtained experimentally and

  7. Stability and instability of stationary solutions for sublinear parabolic equations

    Science.gov (United States)

    Kajikiya, Ryuji

    2018-01-01

    In the present paper, we study the initial boundary value problem of the sublinear parabolic equation. We prove the existence of solutions and investigate the stability and instability of stationary solutions. We show that a unique positive and a unique negative stationary solutions are exponentially stable and give the exact exponent. We prove that small stationary solutions are unstable. For one space dimensional autonomous equations, we elucidate the structure of stationary solutions and study the stability of all stationary solutions.

  8. Microstructures and phase formations in the surface layer of an AISI D2 steel treated with pulsed electron beam

    International Nuclear Information System (INIS)

    Zou, J.X.; Grosdidier, T.; Zhang, K.M.; Gao, B.; Hao, S.Z.; Dong, C.

    2007-01-01

    The nanostructures and metastable phase transformations in the surface layer of an AISI D2 steel treated with high current pulsed electron beam (HCPEB) were investigated. The surface structure is marked by two distinct features, i.e. the formation of sub-micrometer fine austenite γ grains (50-150 nm), and the disappearance of carbides via dissolution and crater eruption. The γ phase directly grows from the melt and is retained down to room temperature. Although the cooling rate is as high as 10 7 K/s in our case, the martensitic transformation could completely be suppressed. Such an effect is due to the increased stability of the austenite phase through grain refinement and chemistry modification

  9. SURFACE CHEMKIN-III: A Fortran package for analyzing heterogeneous chemical kinetics at a solid-surface - gas-phase interface

    Energy Technology Data Exchange (ETDEWEB)

    Coltrin, M.E.; Kee, R.J.; Rupley, F.M.; Meeks, E.

    1996-05-01

    This document is the user`s manual for the SURFACE CHEMKIN-III package. Together with CHEMKIN-III, this software facilitates the formation, solution, and interpretation of problems involving elementary heterogeneous and gas-phase chemical kinetics in the presence of a solid surface. The package consists of two major software components: an Interpreter and a Surface Subroutine Library. The Interpreter is a program that reads a symbolic description of a user-specified chemical reaction mechanism. One output from the Interpreter is a data file that forms a link to the Surface Subroutine Library, which is a collection of about seventy modular Fortran subroutines that may be called from a user`s application code to return information on chemical production rates and thermodynamic properties. This version of SURFACE CHEMKIN-III includes many modifications to allow treatment of multi-fluid plasma systems, for example modeling the reactions of highly energetic ionic species with a surface. Optional rate expressions allow reaction rates to depend upon ion energy rather than a single thermodynamic temperature. In addition, subroutines treat temperature as an array, allowing an application code to define a different temperature for each species. This version of SURFACE CHEMKIN-III allows use of real (non-integer) stoichiometric coefficients; the reaction order with respect to species concentrations can also be specified independent of the reaction`s stoichiometric coefficients. Several different reaction mechanisms can be specified in the Interpreter input file through the new construct of multiple materials.

  10. 2.5D constructs for characterizing phase separated polymer blend surface morphology in tissue engineering scaffolds.

    Science.gov (United States)

    Marszalek, Jolanta E; Simon, Carl G; Thodeti, Charles; Adapala, Ravi Kumar; Murthy, Ananth; Karim, Alamgir

    2013-05-01

    Previously, we used 2D films to identify an annealed PCL-PDLLA phase-separated blend morphology which provided nanoscale surface texture and patterning that stimulated osteoblast differentiation. In order to translate these 2D surface nanopatterning effects to the walls of 3D salt-leached scaffolds, the blend phase morphology of scaffold walls must be characterized. For salt-leached scaffolds, NaCl is used as a porogen, which may affect phase separation in PCL-PDLLA blends. However, it is not possible to characterize the surface blend morphology of 3D scaffold walls using standard approaches such as AFM or optical microscopy, since scaffolds are too rough for AFM and do not transmit light for optical microscopy. We introduce a 2.5D approach that mimics the processing conditions of 3D salt-leached scaffolds, but has a geometry amenable to surface characterization by AFM and optical microscopy. For the 2.5D approach, PCL-PDLLA blend films were covered with NaCl crystals prior to annealing. The presence of NaCl significantly influenced blend morphology in PCL-PDLLA 2.5D constructs causing increased surface roughness, higher percent PCL area on the surface and a smaller PCL domain size. During cell culture on 2.5D constructs, osteoblast (MC3T3-E1) and dermal endothelial cell (MDEC) adhesion were enhanced on PCL-PDLLA blends that were annealed with NaCl while chondrogenic cell (ATDC5) adhesion was diminished. This work introduces a 2.5D approach that mimicked 3D salt-leached scaffold processing, but enabled characterization of scaffold surface properties by AFM and light microscopy, to demonstrate that the presence of NaCl during annealing strongly influenced polymer blend surface morphology and cell adhesion. Copyright © 2012 Wiley Periodicals, Inc.

  11. Enhancement of optical nonlinearities with stationary light

    DEFF Research Database (Denmark)

    Iakoupov, Ivan

    Stationary light arises in atomic ensembles with certain energy level configurations, when two counter-propagating classical drives (lasers) are applied. Probe light coupled to a different energy level transition than the classical drives can be completely stopped, while still retaining its light...... character. We will be interested in the regime of stationary light, where the probe light still propagates through the atomic ensemble, but extremely slowly. In other words, probe field has a very low group velocity, which increases its interaction time with any optical nonlinearity. The enhancement...

  12. Pre-sintered Y-TZP sandblasting: effect on surface roughness, phase transformation, and Y-TZP/veneer bond strength

    Directory of Open Access Journals (Sweden)

    Carla Müller Ramos-Tonello

    Full Text Available Abstract Sandblasting is a common method to try to improve the Y-TZP/veneer bond strength of dental prostheses, however, it may put stress on zirconia surfaces and could accelerate the t→m phase transformation. Y-TZP sandblasting before sintering could be an alternative to improve surface roughness and bonding strength of veneering ceramic. Objectives. The aim of this study was to analyze the effect of Y-TZP pre-sintering sandblasting on surface roughness, phase transformation, and the Y-TZP/veneer shear bond strength. Material and Methods. The Y-TZP specimen surface underwent sandblasting with aluminum oxide (50 μm pre-sintering (Z-PRE and post-sintering (Z-POS. Z-CTR was not subjected to surface treatment. After ceramic veneer application, the specimens were subjected to shear bond testing. Surface roughness was analyzed by confocal microscopy. Y-TZP monoclinic and tetragonal phases were evaluated by micro-Raman spectroscopy. Shear bond strength and surface roughness data were analyzed by One-way ANOVA and Tukey tests (α=0.05. Differences in the wave numbers and the broadening bands of the Raman spectra were compared among groups. Results. Z-POS (9.73±5.36 MPa and Z-PRE (7.94±2.52 MPa showed the highest bond strength, significantly higher than that of Z-CTR (5.54±2.14 MPa. The Ra of Z-PRE (1.59±0.23 µm was much greater and significantly different from that of Z-CTR (0.29±0.05 µm and Z-POS (0.77±0.13 µm. All groups showed bands typical of the tetragonal (T and monoclinic (M phases. Y-TZP sandblasting before sintering resulted in rougher surfaces but did not increase the shear bond strength compared to post-sintering and increased surface defects. Conclusions. Surface treatment with Al3O2, regardless of the moment and application, improves the results of Y-TZP/veneer bonding and is not a specific cause of t→m transformation.

  13. 4. Workshop - Measurement techniques of stationary and transient multiphase flow

    Energy Technology Data Exchange (ETDEWEB)

    Prasser, H.M. (ed.)

    2001-05-01

    In November 2000, the 4th Workshop on Measurement Techniques for Stationary and Transient Multiphase Flows took place in Rossendorf. Three previous workshops of this series were national meetings; this time participants from different countries took part. The programme comprised 14 oral presentations, 9 of which are included in these proceedings in full length. A special highlight of the meeting was the main lecture ''Ultrasonic doppler method for bubbly flow measurement'' of Professor Masanori Aritomi, Dr. Hiroshige Kikura and Dr. Yumiko Suzuki. The workshop again dealt with high-resolution phase distribution and phase velocity measurement techniques based on electrical conductivity, ultrasound, laser light and high-speed cinematography. A number of presentations were dedicated to the application of wire-mesh sensors developed by FZR for different applications used by the Technical Universities of Delft and Munich and the Tokyo Institute of Technology. (orig.)

  14. 4. Workshop - Measurement techniques of stationary and transient multiphase flow

    International Nuclear Information System (INIS)

    Prasser, H.M.

    2001-05-01

    In November 2000, the 4th Workshop on Measurement Techniques for Stationary and Transient Multiphase Flows took place in Rossendorf. Three previous workshops of this series were national meetings; this time participants from different countries took part. The programme comprised 14 oral presentations, 9 of which are included in these proceedings in full length. A special highlight of the meeting was the main lecture ''Ultrasonic doppler method for bubbly flow measurement'' of Professor Masanori Aritomi, Dr. Hiroshige Kikura and Dr. Yumiko Suzuki. The workshop again dealt with high-resolution phase distribution and phase velocity measurement techniques based on electrical conductivity, ultrasound, laser light and high-speed cinematography. A number of presentations were dedicated to the application of wire-mesh sensors developed by FZR for different applications used by the Technical Universities of Delft and Munich and the Tokyo Institute of Technology. (orig.)

  15. Electromigration-Induced Surface Drift and Slit Propagation in Polycrystalline Interconnects: Insights from Phase-Field Simulations

    Science.gov (United States)

    Mukherjee, Arnab; Ankit, Kumar; Selzer, Michael; Nestler, Britta

    2018-04-01

    We employ the phase-field method to assess electromigration (EM) damage in wide polycrystalline interconnects due to grain-boundary grooving. An interplay of surface and grain-boundary diffusion is shown to drastically influence the mode of progressive EM damage. Rapid atomic transport along the surface leads to shape-preserving surface drift reminiscent of Blech drift-velocity experiments. On the other hand, a comparatively faster grain-boundary transport localizes the damage, resulting in the proliferation of intergranular slits with a shape-preserving tip. At steady state, the two regimes exhibit exponents of 1 and 3 /2 , respectively, in Black's law. While surface drift obeys an inverse scaling with grain size, slits exhibit a direct relationship at small sizes, with the dependence becoming weaker at larger ones. Furthermore, we explain the influence of curvature- or EM-mediated healing fluxes running along the surface on groove replenishment. Insights derived from phase-field simulations of EM in bicrystals are extended to investigate the multiphysics of mixed-mode damage of a polycrystalline interconnect line that is characterized by a drift of small grain surfaces, slit propagation, and coarsening. The triple and quadruple junctions are identified as prominent sites of failure.

  16. Rover Radar for Surface Navigation, Hazard Detection and Negative Obstacle Avoidance, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — In Topic X1.03 NASA (JPL) is seeking to extend and implement long distance exploratory surface rover missions to gain knowledge of surface topology and roughness....

  17. Optical Feather and Foil for Shape and Dynamic Load Sensing of Critical Flight Surfaces, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — Future flight vehicles may comprise complex flight surfaces requiring coordinated in-situ sensing and actuation. Inspired by the complexity of the flight surfaces on...

  18. Stationary Cycling and Children with Cerebral Palsy: Case Reports for Two Participants

    Science.gov (United States)

    Siebert, Kara L.; DeMuth, Sharon K.; Knutson, Loretta M.; Fowler, Eileen G.

    2010-01-01

    These case reports describe a stationary cycling intervention and outcomes for two child participants (P1 and P2) with spastic diplegic cerebral palsy. Each child completed a 12-week, 30-session cycling intervention consisting of strengthening and cardiorespiratory fitness phases. P1 exhibited higher training intensities, particularly during the…

  19. Universal phase and force diagrams for a microbubble or pendant drop in static fluid on a surface

    Science.gov (United States)

    Wei, P. S.; Hsiao, C. C.; Chen, K. Y.

    2008-01-01

    Dimensionless three-dimensional universal phase and lift force diagrams of a microbubble (or pendant drop) in static liquid on a solid surface (or orifice) are presented in this work. Microbubble dynamics has been found to play a vital role in mass, momentum, energy, and concentration transfer rates in contemporary micro- and nanosciences and technologies. In this study, dimensionless phase and force diagrams are introduced by utilizing the analytical solutions of the microbubble shape reported in the literature. It shows that phase and force diagrams can be universally specified by two dimensionless independent parameters, Bond number, and contact angle (or base radius). Based on the presence of an inflection point or neck on the microbubble surface, each diagram exhibits three regions. Growth, detachment, and entrapment of a microbubble can be described by path lines in three regions. The corresponding universal total lift forces include hydrostatic buoyancy, difference in gas, and hydrostatic pressures at the base, capillary pressure, as well as surface tension induced by the variation of circumference, which has not been treated in the literature so far. In the absence of viscous stress and Marangoni force, the total lift force equals surface tension induced by the variation of circumference. The latter can be an attaching or lifting force, depending on whether the state in the distinct regions and contact angle is less than or greater than a critical angle. The critical angle, which is slightly less than the inclination angle at the inflection point, is decreased with increasing Bond number.

  20. Polarization fluctuations in stationary light beams

    International Nuclear Information System (INIS)

    Shevchenko, A.; Setaelae, T.; Kaivola, M.; Friberg, A.T.; Royal Institute of Technology , Department of Microelectronics and Applied Physics; Sweden)

    2009-01-01

    For stationary beams the degree of polarization contains only limited information on time dependent polarization. Two approaches towards assessing a beams polarization dynamics, one based on Poincare and the other on Jones vector formalism, are described leading to the notion of polarization time. Specific examples of partially temporally coherent electromagnetic beams are discussed. (Author)