Sample records for t3 analytical column

  1. Radial heterogeneity of some analytical columns used in high-performance liquid chromatography.

    PubMed

    Abia, Jude A; Mriziq, Khaled S; Guiochon, Georges A

    2009-04-10

    An on-column electrochemical microdetector was used to determine accurately the radial distribution of the mobile phase velocity and of the column efficiency at the exit of three common analytical columns, namely a 100 mm x 4.6mm C18 bonded silica-based monolithic column, a 150 mm x 4.6mm column packed with 2.7 microm porous shell particles of C18 bonded silica (HALO), and a 150 mm x 4.6mm column packed with 3 microm fully porous C18 bonded silica particles (LUNA). The results obtained demonstrate that all three columns are not radially homogeneous. In all three cases, the efficiency was found to be lower in the wall region of the column than in its core region (the central core with a radius of 1/3 the column inner radius). The decrease in local efficiency from the core to the wall regions was lower in the case of the monolith (ca. 25%) than in that of the two particle-packed columns (ca. 35-50%). The mobile phase velocity was found to be ca. 1.5% higher in the wall than in the core region of the monolithic column while, in contrast, it was ca. 2.5-4.0% lower in the wall region for the two particle-packed columns.

  2. Microwave assisted solvent extraction and coupled-column reversed-phase liquid chromatography with UV detection use of an analytical restricted-access-medium column for the efficient multi-residue analysis of acidic pesticides in soils.

    PubMed

    Hogendoom, E A; Huls, R; Dijkman, E; Hoogerbrugge, R

    2001-12-14

    A screening method has been developed for the determination of acidic pesticides in various types of soils. Methodology is based on the use of microwave assisted solvent extraction (MASE) for fast and efficient extraction of the analytes from the soils and coupled-column reversed-phase liquid chromatography (LC-LC) with UV detection at 228 nm for the instrumental analysis of uncleaned extracts. Four types of soils, including sand, clay and peat, with a range in organic matter content of 0.3-13% and ten acidic pesticides of different chemical families (bentazone, bromoxynil, metsulfuron-methyl, 2,4-D, MCPA, MCPP, 2,4-DP, 2,4,5-T, 2,4-DB and MCPB) were selected as matrices and analytes, respectively. The method developed included the selection of suitable MASE and LC-LC conditions. The latter consisted of the selection of a 5-microm GFF-II internal surface reversed-phase (ISRP, Pinkerton) analytical column (50 x 4.6 mm, I.D.) as the first column in the RAM-C18 configuration in combination with an optimised linear gradient elution including on-line cleanup of sample extracts and reconditioning of the columns. The method was validated with the analysis of freshly spiked samples and samples with aged residues (120 days). The four types of soils were spiked with the ten acidic pesticides at levels between 20 and 200 microg/kg. Weighted regression of the recovery data showed for most analyte-matrix combinations, including freshly spiked samples and aged residues, that the method provides overall recoveries between 60 and 90% with relative standard deviations of the intra-laboratory reproducibility's between 5 and 25%; LODs were obtained between 5 and 50 microg/kg. Evaluation of the data set with principal component analysis revealed that the parameters (i) increase of organic matter content of the soil samples and (ii) aged residues negatively effect the recovery of the analytes.

  3. Enantiomeric separation of triazole fungicides with 3-μm and 5-μml particle chiral columns by reverse-phase high-performance liquid chromatography.

    PubMed

    Qiu, Jing; Dai, Shouhui; Zheng, Chuangmu; Yang, Shuming; Chai, Tingting; Bie, Mei

    2011-07-01

    This study used chiral columns packed with 3-μm and 5-μm particles to comparatively separate enantiomers of 9 triazole fungicides, and Lux Cellulose-1 columns with chiral stationary phase of cellulose-tris-(3,5-dimethylphenylcarbamate) were used on reverse-phase high-performance liquid chromatography with flow rates of 0.3 and 1.0 mL min(-1) for 3-μm and 5-μm columns, respectively. The (+)-enantiomers of hexaconazole (1), tetraconazole (4), myclobutanil (7), fenbuconazole (8) and the (-)-enantiomers of flutriafol (2), diniconazole (3), epoxiconazole (5), penconazole (6), triadimefon (9) were firstly eluted from both columns, the elution orders identified with an optical rotation detector didn't change with variety of column particles and mobile phases (acetronitrile/water and methanol/water). The plots of natural logarithms of the selectivity factors (ln α) for all fungicides except penconazole (6) versus the inverse of temperature (1/T) were linear in range of 5-40°C. The thermodynamic parameters (ΔH°, ΔS°, ΔΔH° and ΔΔS°) were calculated using Van't Hoff equations to understand the thermosynamic driving forces for enantioseparation. This work will be very helpful to obtain good enantiomeric separation and establish more efficient analytical method for triazole fungicides. Chirality, 2011. © 2011 Wiley-Liss, Inc. Copyright © 2011 Wiley-Liss, Inc.

  4. Simultaneous quantification of T4, T3, rT3, 3,5-T2 and 3,3'-T2 in larval zebrafish (Danio rerio) as a model to study exposure to polychlorinated biphenyls.

    PubMed

    Chen, Xiaopeng; Walter, Kyla M; Miller, Galen W; Lein, Pamela J; Puschner, Birgit

    2018-06-01

    Environmental toxicants that interfere with thyroid hormone (TH) signaling can impact growth and development in animals and humans. Zebrafish represent a model to study chemically induced TH disruption, prompting the need for sensitive detection of THs. Simultaneous quantification of 3,3',5-triiodo-l-thyronine (T3), thyroxine (T4), 3,3',5'-triiodo-l-thyronine (rT3), 3,5-diiodo-l-thyronine (3,5-T2) and 3,3'-diiodo-l-thyronine (3,3'-T2) in zebrafish larvae was achieved by ultra-performance liquid chromatography-tandem mass spectrometry in positive ion mode. Solid-phase extraction with SampliQ cartridges and derivatization with 3 m hydrochloric acid in n-butanol reduced matrix effects. Derivatized compounds were separated on an Acquity UPLC BEH C 18 column with mobile phases consisting of 0.1% acetic acid in deionized water and 0.1% acetic acid in methanol. The limits of detection ranged from 0.5 to 0.6 pg injected on column. The method was validated by evaluating recovery (77.1-117.2%), accuracy (87.3-123.9%) and precision (0.5-12.4%) using diluted homogenized zebrafish embryos spiked with all target compounds. This method was then applied to zebrafish larvae collected after 114 h of exposure to polychlorinated biphenyls (PCBs), including PCB 28, PCB 66 and PCB 95, or the technical mixture Aroclor 1254. Exposure to PCB 28 and PCB 95 increased the T4:T3 ratio and decreased the T3:rT3 ratio, demonstrating that this method can effectively detect PCB-induced alterations in THs. Copyright © 2018 John Wiley & Sons, Ltd.

  5. The column strength of aluminum alloy 75S-T extruded shapes

    NASA Technical Reports Server (NTRS)

    Holt, Marshall; Leary, J R

    1946-01-01

    Because the tensile strength and tensile yield strength of alloy 75S-T are appreciably higher than those of the materials used in the tests leading to the use of the straight-line column curve, it appeared advisable to establish the curve of column strength by test rather than by extrapolation of relations determined empirically in the earlier tests. The object of this investigation was to determine the curve of column strength for extruded aluminum alloy 75S-T. In addition to three extruded shapes, a rolled-and-drawn round rod was included. Specimens of various lengths covering the range of effective slenderness ratios up to about 100 were tested.

  6. Semi-permeable surface analytical reversed-phase column for the improved trace analysis of acidic pesticides in water with coupled-column reversed-phase liquid chromatography with UV detection. Determination of bromoxynil and bentazone in surface water.

    PubMed

    Hogendoorn, E A; Westhuis, K; Dijkman, E; Heusinkveld, H A; den Boer, A C; Evers, E A; Baumann, R A

    1999-10-08

    The coupled-column (LC-LC) configuration consisting of a 3 microm C18 column (50 x 4.6 mm I.D.) as the first column and a 5 microm C18 semi-permeable-surface (SPS) column (150 x 4.6 mm I.D.) as the second column appeared to be successful for the screening of acidic pesticides in surface water samples. In comparison to LC-LC employing two C18 columns, the combination of C18/SPS-C18 significantly decreased the baseline deviation caused by the hump of the co-extracted humic substances when using UV detection (217 nm). The developed LC-LC procedure allowed the simultaneous determination of the target analytes bentazone and bromoxynil in uncleaned extracts of surface water samples to a level of 0.05 microg/l in less than 15 min. In combination with a simple solid-phase extraction step (200 ml of water on a 500 mg C18-bonded silica) the analytical procedure provides a high sample throughput. During a period of about five months more than 200 ditch-water samples originating from agricultural locations were analyzed with the developed procedure. Validation of the method was performed by randomly analyzing recoveries of water samples spiked at levels of 0.1 microg/l (n=10), 0.5 microg/l (n=7) and 2.5 microg/l (n=4). Weighted regression of the recovery data showed that the method provides overall recoveries of 95 and 100% for bentazone and bromoxynil, respectively, with corresponding intra-laboratory reproducibilities of 10 and 11%, respectively. Confirmation of the analytes in part of the samples extracts was carried out with GC-negative ion chemical ionization MS involving a derivatization step with bis(trifluoromethyl)benzyl bromide. No false negatives or positives were observed.

  7. Two-Dimensional Model for Reactive-Sorption Columns of Cylindrical Geometry: Analytical Solutions and Moment Analysis.

    PubMed

    Khan, Farman U; Qamar, Shamsul

    2017-05-01

    A set of analytical solutions are presented for a model describing the transport of a solute in a fixed-bed reactor of cylindrical geometry subjected to the first (Dirichlet) and third (Danckwerts) type inlet boundary conditions. Linear sorption kinetic process and first-order decay are considered. Cylindrical geometry allows the use of large columns to investigate dispersion, adsorption/desorption and reaction kinetic mechanisms. The finite Hankel and Laplace transform techniques are adopted to solve the model equations. For further analysis, statistical temporal moments are derived from the Laplace-transformed solutions. The developed analytical solutions are compared with the numerical solutions of high-resolution finite volume scheme. Different case studies are presented and discussed for a series of numerical values corresponding to a wide range of mass transfer and reaction kinetics. A good agreement was observed in the analytical and numerical concentration profiles and moments. The developed solutions are efficient tools for analyzing numerical algorithms, sensitivity analysis and simultaneous determination of the longitudinal and transverse dispersion coefficients from a laboratory-scale radial column experiment. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  8. Column-to-column packing variation of disposable pre-packed columns for protein chromatography.

    PubMed

    Schweiger, Susanne; Hinterberger, Stephan; Jungbauer, Alois

    2017-12-08

    In the biopharmaceutical industry, pre-packed columns are the standard for process development, but they must be qualified before use in experimental studies to confirm the required performance of the packed bed. Column qualification is commonly done by pulse response experiments and depends highly on the experimental testing conditions. Additionally, the peak analysis method, the variation in the 3D packing structure of the bed, and the measurement precision of the workstation influence the outcome of qualification runs. While a full body of literature on these factors is available for HPLC columns, no comparable studies exist for preparative columns for protein chromatography. We quantified the influence of these parameters for commercially available pre-packed and self-packed columns of disposable and non-disposable design. Pulse response experiments were performed on 105 preparative chromatography columns with volumes of 0.2-20ml. The analyte acetone was studied at six different superficial velocities (30, 60, 100, 150, 250 and 500cm/h). The column-to-column packing variation between disposable pre-packed columns of different diameter-length combinations varied by 10-15%, which was acceptable for the intended use. The column-to-column variation cannot be explained by the packing density, but is interpreted as a difference in particle arrangement in the column. Since it was possible to determine differences in the column-to-column performance, we concluded that the columns were well-packed. The measurement precision of the chromatography workstation was independent of the column volume and was in a range of±0.01ml for the first peak moment and±0.007 ml 2 for the second moment. The measurement precision must be considered for small columns in the range of 2ml or less. The efficiency of disposable pre-packed columns was equal or better than that of self-packed columns. Copyright © 2017 The Author(s). Published by Elsevier B.V. All rights reserved.

  9. Modelling by partial least squares the relationship between the HPLC mobile phases and analytes on phenyl column.

    PubMed

    Markopoulou, Catherine K; Kouskoura, Maria G; Koundourellis, John E

    2011-06-01

    Twenty-five descriptors and 61 structurally different analytes have been used on a partial least squares (PLS) to latent structure technique in order to study chromatographically their interaction mechanism on a phenyl column. According to the model, 240 different retention times of the analytes, expressed as Y variable (log k), at different % MeOH mobile-phase concentrations have been correlated with their theoretical most important structural or molecular descriptors. The goodness-of-fit was estimated by the coefficient of multiple determinations r(2) (0.919), and the root mean square error of estimation (RMSEE=0.1283) values with a predictive ability (Q(2)) of 0.901. The model was further validated using cross-validation (CV), validated by 20 response permutations r(2) (0.0, 0.0146), Q(2) (0.0, -0.136) and validated by external prediction. The contribution of certain mechanism interactions between the analytes, the mobile phase and the column, proportional or counterbalancing is also studied. Trying to evaluate the influence on Y of every variable in a PLS model, VIP (variables importance in the projection) plot provides evidence that lipophilicity (expressed as Log D, Log P), polarizability, refractivity and the eluting power of the mobile phase are dominant in the retention mechanism on a phenyl column. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. The influence of salt chaotropicity, column hydrophobicity and analytes' molecular properties on the retention of pramipexole and its impurities.

    PubMed

    Vemić, Ana; Kalinić, Marko; Erić, Slavica; Malenović, Anđelija; Medenica, Mirjana

    2015-03-20

    The aim of this study was to examine the interaction of the chaotropic salts of different position in Hofmeister series (CF3COONa, NaClO4, NaPF6) added to the mobile phase with the stationary phases of different hydrophobicity (C8 and C18 XTerra(®) columns), as well as their common influence on the retention behavior of pramipexole and its structurally related impurities. The extended thermodynamic approach enabled the understanding of the underlying separation mechanism. Comparing six different column-salt systems it was observed that general system hydrophobicity presented by salt chaotropicity and column hydrophobicity favors stationary phase ion-pairing over the ion-pair formation in the eluent. Further, an attempt was made to describe the influence of analytes' nature on their retention behavior in such chromatographic systems. An analysis is performed in order to select and elucidate the molecular descriptors (electrostatical, quantum-chemical, geometrical, topological, and constitutional) that best explain the experimental evidence and findings obtained by the thermodynamic approach. The results of this analysis suggest that analytes' charge distribution and its complementarity to the structure of the electric double layer formed on the surface of the stationary phase upon the addition of chaotropic additives can be useful for understanding the differences in retention of structurally related analytes. These findings provide a novel understanding of the interactions between all the components of the chromatographic system containing chaotropic additive and a good basis for further investigations suggesting the development of generally applicable predictors in structure-retention relationship studies in related chromatographic systems. Copyright © 2015 Elsevier B.V. All rights reserved.

  11. Influence of a strong sample solvent on analyte dispersion in chromatographic columns.

    PubMed

    Mishra, Manoranjan; Rana, Chinar; De Wit, A; Martin, Michel

    2013-07-05

    In chromatographic columns, when the eluting strength of the sample solvent is larger than that of the carrier liquid, a deformation of the analyte zone occurs because its frontal part moves at a relatively high velocity due to a low retention factor in the sample solvent while the rear part of the analyte zone is more retained in the carrier liquid and hence moves at a lower velocity. The influence of this solvent strength effect on the separation of analytes is studied here theoretically using a mass balance model describing the spatio-temporal evolution of the eluent, the sample solvent and the analyte. The viscosity of the sample solvent and carrier fluid is supposed to be the same (i.e. no viscous fingering effects are taken into account). A linear isotherm adsorption with a retention factor depending upon the local concentration of the liquid phase is considered. The governing equations are numerically solved by using a Fourier spectral method and parametric studies are performed to analyze the effect of various governing parameters on the dispersion and skewness of the analyte zone. The distortion of this zone is found to depend strongly on the difference in eluting strength between the mobile phase and the sample solvent as well as on the sample volume. Copyright © 2013 Elsevier B.V. All rights reserved.

  12. Usefulness of Analytical Research: Rethinking Analytical R&D&T Strategies.

    PubMed

    Valcárcel, Miguel

    2017-11-07

    This Perspective is intended to help foster true innovation in Research & Development & Transfer (R&D&T) in Analytical Chemistry in the form of advances that are primarily useful for analytical purposes rather than solely for publishing. Devising effective means to strengthen the crucial contribution of Analytical Chemistry to progress in Chemistry, Science & Technology, and Society requires carefully examining the present status of our discipline and also identifying internal and external driving forces with a potential adverse impact on its development. The diagnostic process should be followed by administration of an effective therapy and supported by adoption of a theragnostic strategy if Analytical Chemistry is to enjoy a better future.

  13. Enantioselective Analytical- and Preparative-Scale Separation of Hexabromocyclododecane Stereoisomers Using Packed Column Supercritical Fluid Chromatography.

    PubMed

    Riddell, Nicole; Mullin, Lauren Gayle; van Bavel, Bert; Ericson Jogsten, Ingrid; McAlees, Alan; Brazeau, Allison; Synnott, Scott; Lough, Alan; McCrindle, Robert; Chittim, Brock

    2016-11-10

    Hexabromocyclododecane (HBCDD) is an additive brominated flame retardant which has been listed in Annex A of the Stockholm Convention for elimination of production and use. It has been reported to persist in the environment and has the potential for enantiomer-specific degradation, accumulation, or both, making enantioselective analyses increasingly important. The six main stereoisomers of technical HBCDD (i.e., the (+) and (-) enantiomers of α-, β-, and γ-HBCDD) were separated and isolated for the first time using enantioselective packed column supercritical fluid chromatography (pSFC) separation methods on a preparative scale. Characterization was completed using published chiral liquid chromatography (LC) methods and elution profiles, as well as X-ray crystallography, and the isolated fractions were definitively identified. Additionally, the resolution of the enantiomers, along with two minor components of the technical product (δ- and ε-HBCDD), was investigated on an analytical scale using both LC and pSFC separation techniques, and changes in elution order were highlighted. Baseline separation of all HBCDD enantiomers was achieved by pSFC on an analytical scale using a cellulose-based column. The described method emphasizes the potential associated with pSFC as a green method of isolating and analyzing environmental contaminants of concern.

  14. Seismic performance of interior precast concrete beam-column connections with T-section steel inserts under cyclic loading

    NASA Astrophysics Data System (ADS)

    Ketiyot, Rattapon; Hansapinyo, Chayanon

    2018-04-01

    An experimental investigation was conducted to study the performance of precast beam-column concrete connections using T-section steel inserts into the concrete beam and joint core, under reversed cyclic loading. Six 2/3-scale interior beam-column subassemblies, one monolithic concrete specimen and five precast concrete specimens were tested. One precast specimen was a simple connection for a gravity load resistant design. Other precast specimens were developed with different attributes to improve their seismic performance. The test results showed that the performance of the monolithic specimen M1 represented ductile seismic behavior. Failure of columns and joints could be prevented, and the failure of the frame occurred at the flexural plastic hinge formation at the beam ends, close to the column faces. For the precast specimens, the splitting crack along the longitudinal lapped splice was a major failure. The precast P5 specimen with double steel T-section inserts showed better seismic performance compared to the other precast models. However, the dowel bars connected to the steel inserts were too short to develop a bond. The design of the precast concrete beams with lap splice is needed for longer lap lengths and should be done at the beam mid span or at the low flexural stress region.

  15. Evaluation of Copper-1,3,5-benzenetricarboxylate Metal-organic Framework (Cu-MOF) as a Selective Sorbent for Lewis-base Analytes

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Harvey, Scott D.; Eckberg, Alison D.; Thallapally, Praveen K.

    2011-09-01

    The metal-organic framework Cu-BTC was evaluated for its ability to selectively interact with Lewis-base analytes, including explosives, by examining retention on GC columns packed with Chromosorb W HP that contained 3.0% SE-30 along with various loadings of Cu-BTC. SEM images of the support material showed the characteristic Cu-BTC crystals embedded in the SE-30 coating on the diatomaceous support. Results indicated that the Cu-BTC-containing stationary phase had limited thermal stability (220°C) and strong general retention for analytes. Kováts index calculations showed selective retention (amounting to about 300 Kováts units) relative to n-alkanes for many small Lewis-base analytes on a column thatmore » contained 0.75% Cu-BTC compared to an SE-30 control. Short columns that contained lower loadings of Cu-BTC (0.10%) were necessary to elute explosives and related analytes; however, selectivity was not observed for aromatic compounds (including nitroaromatics) or nitroalkanes. Observed retention characteristics are discussed.« less

  16. Separation of natural product using columns packed with Fused-Core particles.

    PubMed

    Yang, Peilin; Litwinski, George R; Pursch, Matthias; McCabe, Terry; Kuppannan, Krishna

    2009-06-01

    Three HPLC columns packed with 3 microm, sub-2 microm, and 2.7 microm Fused-Core (superficially porous) particles were compared in separation performance using two natural product mixtures containing 15 structurally related components. The Ascentis Express C18 column packed with Fused-Core particles showed an 18% increase in column efficiency (theoretical plates), a 76% increase in plate number per meter, a 65% enhancement in separation speed and a 19% increase in back pressure compared to the Atlantis T3 C18 column packed with 3 microm particles. Column lot-to-lot variability for critical pairs in the natural product mixture was observed with both columns, with the Atlantis T3 column exhibiting a higher degree of variability. The Ascentis Express column was also compared with the Acquity BEH column packed with sub-2 microm particles. Although the peak efficiencies obtained by the Ascentis Express column were only about 74% of those obtained by the Acquity BEH column, the 50% lower back pressure and comparable separation speed allowed high-efficiency and high-speed separation to be performed using conventional HPLC instrumentation.

  17. [Study for the revision of analytical method for tris (2,3-dibromopropyl) phosphate with restriction in textiles].

    PubMed

    Mimura, Mayumi; Nakashima, Harunobu; Yoshida, Jin; Yoshida, Toshiaki; Kawakami, Tsuyoshi; Isama, Kazuo

    2014-01-01

    The official analytical method for tris(2,3-dibromopropyl)phosphate (TDBPP), which is banned from use in textile products by the "Act on Control of Household Products Containing Harmful Substances", requires revision. This study examined an analytical method for TDBPP by GC/MS using a capillary column. Thermal decomposition of TDBPP was observed by GC/MS measurement using capillary column, unlike in the case of gas chromatography/flame photometric detector (GC/FPD) measurement based on a direct injection method using a capillary megabore column. A quadratic curve, Y=2572X(1.416), was obtained for the calibration curve of GC/FPD in the concentration range 2.0-100 μg/mL. The detection limit was 1.0 μg/mL under S/N=3. The reproducibility for repetitive injections was satisfactory. A pretreatment method was established using methanol extraction, followed by liquid-liquid partition and purification with a florisil cartridge column. The recovery rate of this method was ~100%. TDBPP was not detected in any of the five commercial products that this study analyzed. To understand the cause of TDBPP decomposition during GC/MS (electron ionization; EI) measurement using capillary column, GC/MS (chemical ionization; CI), GC/FPD, and gas chromatography/flame ionization detector (GC/FID) measurements were conducted. It was suggested that TDBPP might thermally decompose both during GC injection, especially through a splitless injection method, and in the column or ion sources. To attempt GC/MS measurement, an injection part comprising quartz liner was used and the column length was halved (15 m); thus, only one peak could be obtained.

  18. Biosensor for the enantioselective analysis of the thyroid hormones (+)-3,3',5-triiodo-L-thyronine (T3) and (+)-3,3',5,5'-tetraiodo-L-thyronine (T4).

    PubMed

    Aboul-Enein, Hassan V; Stefan, Raluca-Ioana; Litescu, Simona; Radu, Gabriel Lucian

    2002-01-01

    An amperometric biosensor based on L-aminoacid oxidase is proposed for enantioselective assay of (+)-3,3',5-triiodo-L-thyronine (L-T3) and (+)-3,3',5,5'-tetraiodo-L-thyronine (L-T4), due to the fact that only the L enantiomer has the hormonal activity. The construction of the amperometric biosensor is simple and reproducible. The analytical information obtained from enantioselective analysis are reliable. The RSD <1% assured by using the amperometric biosensors for L enantiomers assay as raw materials, and from tablets, demonstrated their suitability for the analysis of T3 and T4 at ppb concentration levels.

  19. Signal Enhancement in HPLC/Micro-Coil NMR Using Automated Column Trapping

    PubMed Central

    Djukovic, Danijel; Liu, Shuhui; Henry, Ian; Tobias, Brian; Raftery, Daniel

    2008-01-01

    A new HPLC-NMR system is described that performs analytical separation, pre-concentration, and NMR spectroscopy in rapid succession. The central component of our method is the online pre-concentration sequence that improves the match between post-column analyte peak volume and the micro-coil NMR detection volume. Separated samples are collected on to a C18 guard column with a mobile phase composed of 90% D2O/10% acetonitrile-D3, and back-flashed to the NMR micro-coil probe with 90% acetonitrile-D3/10% D2O. In order to assess the performance of our unit, we separated a standard mixture of 1 mM ibuprofen, naproxen, and phenylbutazone using a commercially available C18 analytical column. The S/N measurements from the NMR acquisitions indicated that we achieved signal enhancement factors up to 10.4 (±1.2)-fold. Furthermore, we observed that pre-concentration factors increased as the injected amount of analyte decreased. The highest concentration enrichment of 14.7 (±2.2)-fold was attained injecting 100 μL solution of 0.2 mM (~4 μg) ibuprofen. PMID:17037915

  20. A novel approach to the simultaneous extraction and non-targeted analysis of the small molecules metabolome and lipidome using 96-well solid phase extraction plates with column-switching technology.

    PubMed

    Li, Yubo; Zhang, Zhenzhu; Liu, Xinyu; Li, Aizhu; Hou, Zhiguo; Wang, Yuming; Zhang, Yanjun

    2015-08-28

    This study combines solid phase extraction (SPE) using 96-well plates with column-switching technology to construct a rapid and high-throughput method for the simultaneous extraction and non-targeted analysis of small molecules metabolome and lipidome based on ultra-performance liquid chromatography quadrupole time-of-flight mass spectrometry. This study first investigated the columns and analytical conditions for small molecules metabolome and lipidome, separated by an HSS T3 and BEH C18 columns, respectively. Next, the loading capacity and actuation duration of SPE were further optimized. Subsequently, SPE and column switching were used together to rapidly and comprehensively analyze the biological samples. The experimental results showed that the new analytical procedure had good precision and maintained sample stability (RSD<15%). The method was then satisfactorily applied to more widely analyze the small molecules metabolome and lipidome to test the throughput. The resulting method represents a new analytical approach for biological samples, and a highly useful tool for researches in metabolomics and lipidomics. Copyright © 2015 Elsevier B.V. All rights reserved.

  1. Quantifying the condition of eruption column collapse during explosive volcanic eruptions

    NASA Astrophysics Data System (ADS)

    Koyaguchi, Takehiro; Suzuki, Yujiro

    2016-04-01

    During an explosive eruption, a mixture of pyroclasts and volcanic gas forms a buoyant eruption column or a pyroclastic flow. Generation of a pyroclastic flow caused by eruption column collapse is one of the most hazardous phenomena during explosive volcanic eruptions. The quantification of column collapse condition (CCC) is, therefore, highly desired for volcanic hazard assessment. Previously the CCC was roughly predicted by a simple relationship between magma discharge rate and water content (e.g., Carazzo et al., 2008). When a crater is present above the conduit, because of decompression/compression process inside/above the crater, the CCC based on this relationship can be strongly modified (Woods and Bower, 1995; Koyaguchi et al., 2010); however, the effects of the crater on CCC has not been fully understood in a quantitative fashion. Here, we have derived a semi-analytical expression of CCC, in which the effects of the crater is taken into account. The CCC depends on magma properties, crater shape (radius, depth and opening angle) as well as the flow rate at the base of crater. Our semi-analytical CCC expresses all these dependencies by a single surface in a parameter space of the dimensionless magma discharge rate, the dimensionless magma flow rate (per unit area) and the ratio of the cross-sectional areas at the top and the base of crater. We have performed a systematic parameter study of three-dimensional (3D) numerical simulations of eruption column dynamics to confirm the semi-analytical CCC. The results of the 3D simulations are consistent with the semi-analytical CCC, while they show some additional fluid dynamical features in the transitional state (e.g., partial column collapse). Because the CCC depends on such many parameters, the scenario towards the generation of pyroclastic flow during explosive eruptions is considered to be diverse. Nevertheless, our semi-analytical CCC together with the existing semi-analytical solution for the 1D conduit flow

  2. Analytical and Experimental Assessment of Seismic Vulnerability of Beam-Column Joints without Transverse Reinforcement in Concrete Buildings

    NASA Astrophysics Data System (ADS)

    Hassan, Wael Mohammed

    Beam-column joints in concrete buildings are key components to ensure structural integrity of building performance under seismic loading. Earthquake reconnaissance has reported the substantial damage that can result from inadequate beam-column joints. In some cases, failure of older-type corner joints appears to have led to building collapse. Since the 1960s, many advances have been made to improve seismic performance of building components, including beam-column joints. New design and detailing approaches are expected to produce new construction that will perform satisfactorily during strong earthquake shaking. Much less attention has been focused on beam-column joints of older construction that may be seismically vulnerable. Concrete buildings constructed prior to developing details for ductility in the 1970s normally lack joint transverse reinforcement. The available literature concerning the performance of such joints is relatively limited, but concerns about performance exist. The current study aimed to improve understanding and assessment of seismic performance of unconfined exterior and corner beam-column joints in existing buildings. An extensive literature survey was performed, leading to development of a database of about a hundred tests. Study of the data enabled identification of the most important parameters and the effect of each parameter on the seismic performance. The available analytical models and guidelines for strength and deformability assessment of unconfined joints were surveyed and evaluated. In particular, The ASCE 41 existing building document proved to be substantially conservative in joint shear strength estimation. Upon identifying deficiencies in these models, two new joint shear strength models, a bond capacity model, and two axial capacity models designed and tailored specifically for unconfined beam-column joints were developed. The proposed models strongly correlated with previous test results. In the laboratory testing phase of

  3. Temperature programmable microfabricated gas chromatography column

    DOEpatents

    Manginell, Ronald P.; Frye-Mason, Gregory C.

    2003-12-23

    A temperature programmable microfabricated gas chromatography column enables more efficient chemical separation of chemical analytes in a gas mixture by the integration of a resistive heating element and temperature sensing on the microfabricated column. Additionally, means are provided to thermally isolate the heated column from their surroundings. The small heat capacity and thermal isolation of the microfabricated column improves the thermal time response and power consumption, both important factors for portable microanalytical systems.

  4. Liquid-chromatographic analysis for cyclosporine with use of a microbore column and small sample volume.

    PubMed

    Annesley, T; Matz, K; Balogh, L; Clayton, L; Giacherio, D

    1986-07-01

    This liquid-chromatographic assay requires 0.2 to 0.5 mL of whole blood, avoids the use of diethyl ether, and consumes only 10 to 20% of the solvents used in prior methods. Sample preparation involves an acidic extraction with methyl-t-butyl ether, performed in a 13 X 100 mm disposable glass tube, then a short second extraction of the organic phase with sodium hydroxide. After evaporation of the methyl-t-butyl ether, chromatography is performed on an "Astec" 2.0-mm (i.d.) octyl column. We compared results by this procedure with those by use of earlier larger-scale extractions and their respective 4.6-mm (i.d.) columns; analytical recoveries of cyclosporins A and D were comparable with previous findings and results for patients' specimens were equivalent, but the microbore columns provided greatly increased resolution and sensitivity.

  5. Enhanced capabilities of separation in Sequential Injection Chromatography--fused-core particle column and its comparison with narrow-bore monolithic column.

    PubMed

    Chocholouš, Petr; Kosařová, Lucie; Satínský, Dalibor; Sklenářová, Hana; Solich, Petr

    2011-08-15

    In the Sequential Injection Chromatography (SIC) only monolithic columns for chromatographic separations have been used so far. This article presents the first use of fused-core particle packed column in an attempt to extend of the chromatographic capabilities of the SIC system. A new fused-core particle column (2.7 μm) Ascentis(®) Express C18 (Supelco™ Analytical) 30 mm × 4.6 mm brings high separation efficiency within flow rates and pressures comparable to monolithic column Chromolith(®) Performance RP-18e 100-3 (Merck(®)) 100 mm × 3 mm. Both columns matches the conditions of the commercially produced SIC system - SIChrom™ (8-port high-pressure selection valve and medium-pressure Sapphire™ syringe pump with 4 mL reservoir - maximal work pressure 1000 PSI) (FIAlab(®), USA). The system was tested by the separation of four estrogens with similar structure and an internal standard - ethylparaben. The mobile phase composed of acetonitrile/water (40/60 (v/v)) was pumped isocratic at flow rate 0.48 mL min(-1). Spectrophotometric detection was performed at wavelength of 225 nm and injected volume of sample solutions was 10 μL. The chromatographic characteristics of both columns were compared. Obtained results and conclusions have shown that both fused-core particle column and longer narrow shaped monolithic column bring benefits into the SIC method. Copyright © 2011 Elsevier B.V. All rights reserved.

  6. Interdigitated Color- and Disparity-Selective Columns within Human Visual Cortical Areas V2 and V3

    PubMed Central

    Polimeni, Jonathan R.; Tootell, Roger B.H.

    2016-01-01

    In nonhuman primates (NHPs), secondary visual cortex (V2) is composed of repeating columnar stripes, which are evident in histological variations of cytochrome oxidase (CO) levels. Distinctive “thin” and “thick” stripes of dark CO staining reportedly respond selectively to stimulus variations in color and binocular disparity, respectively. Here, we first tested whether similar color-selective or disparity-selective stripes exist in human V2. If so, available evidence predicts that such stripes should (1) radiate “outward” from the V1–V2 border, (2) interdigitate, (3) differ from each other in both thickness and length, (4) be spaced ∼3.5–4 mm apart (center-to-center), and, perhaps, (5) have segregated functional connections. Second, we tested whether analogous segregated columns exist in a “next-higher” tier area, V3. To answer these questions, we used high-resolution fMRI (1 × 1 × 1 mm3) at high field (7 T), presenting color-selective or disparity-selective stimuli, plus extensive signal averaging across multiple scan sessions and cortical surface-based analysis. All hypotheses were confirmed. V2 stripes and V3 columns were reliably localized in all subjects. The two stripe/column types were largely interdigitated (e.g., nonoverlapping) in both V2 and V3. Color-selective stripes differed from disparity-selective stripes in both width (thickness) and length. Analysis of resting-state functional connections (eyes closed) showed a stronger correlation between functionally alike (compared with functionally unlike) stripes/columns in V2 and V3. These results revealed a fine-scale segregation of color-selective or disparity-selective streams within human areas V2 and V3. Together with prior evidence from NHPs, this suggests that two parallel processing streams extend from visual subcortical regions through V1, V2, and V3. SIGNIFICANCE STATEMENT In current textbooks and reviews, diagrams of cortical visual processing highlight two distinct neural

  7. Repeatability of the efficiency of columns packed with sub-3μm core-shell particles: Part III. 2.7μm Poroshell 120 EC-C18 particles in 4.6mm and 2.1mm × 100mm column formats.

    PubMed

    Gritti, Fabrice; Guiochon, Georges

    2012-08-24

    As part of an investigation of the column-to-column repeatability of the efficiency of columns packed with sub-3μm shell particles, the parameters of the mass transfer kinetics of twelve columns packed with the same batch of 2.7μm Poroshell 120 EC-C(18) particles (Agilent Technologies, Little Fall, DE, USA) were sequentially measured, using columns provided by the manufacturers that were representative of the efficiency distribution given by the quality test control. The reduced longitudinal diffusion term (B) was measured using the peak parking (PP) method; the reduced solid-liquid mass transfer resistance term (C) was given by a combination of the PP results and the most accurate model of effective diffusion in ternary composite materials. The overall eddy diffusion term (A) was obtained by subtraction of these two HETP terms from the overall reduced HETP derived from the peak moments measured by numerical integration of the entire peak profiles. The results demonstrate that the dispersion of the column efficiencies is a result of the random nature of the packing process and the eddy diffusion term resulting from the lack of homogeneity of the column bed. At the highest reduced velocity achieved for small analytes, the relative standard deviations (RSD) of the eddy diffusion term for the 2.1mm I.D. columns were ca. 3 and 11% (with average values h(eddy)= 2.5 and 13.5) for naphthalene (k=3) and uracil (k=0), respectively. For the 4.6mm I.D. columns, these RSDs were 5 and 13%, respectively, with average values h(eddy)= 1.4 and 2.9. For insulin at reduced velocities as high as 160, the RSDs of the total reduced plate heights were 3 and 8% for the 2.1 and 4.6mm I.D. columns, respectively. Copyright © 2012 Elsevier B.V. All rights reserved.

  8. The Effect of Column and Eluent Fluorination on the Retention and Separation of non-Fluorinated Amino Acids and Proteins by HPLC

    PubMed Central

    Joyner, Katherine; Wang, Weizhen; Yu, Yihua Bruce

    2011-01-01

    The effect of column and eluent fluorination on the retention and separation of non-fluorinated amino acids and proteins in HPLC is investigated. A side-by-side comparison of fluorocarbon column and eluents (F-column and F-eluents) with their hydrocarbon counterparts (H-column and H-eluents) in the separation of a group of 33 analytes, including 30 amino acids and 3 proteins, is conducted. The H-column and the F-column contain the n-C8H17 group and n-C8F17 group, respectively, in their stationary phases. The H-eluents include ethanol (EtOH) and isopropanol (ISP) while the F-eluents include trifluoroethanol (TFE) and hexafluorosopropanol (HFIP). The 2 columns and 4 eluents generated 8 (column, eluent) pairs that produce 264 retention time data points for the 33 analytes. A statistical analysis of the retention time data reveals that although the H-column is better than the F-column in analyte separation and H-eluents are better than F-eluents in analyte retention, the more critical factor is the proper pairing of column with eluent. Among the conditions explored in this project, optimal retention and separation is achieved when the fluorocarbon column is paired with ethanol, even though TFE is the most polar one among the 4 eluents. This result shows fluorocarbon columns have much potential in chromatographic analysis and separation of non-fluorinated amino acids and proteins. PMID:21318121

  9. Column Selection for Biomedical Analysis Supported by Column Classification Based on Four Test Parameters.

    PubMed

    Plenis, Alina; Rekowska, Natalia; Bączek, Tomasz

    2016-01-21

    This article focuses on correlating the column classification obtained from the method created at the Katholieke Universiteit Leuven (KUL), with the chromatographic resolution attained in biomedical separation. In the KUL system, each column is described with four parameters, which enables estimation of the FKUL value characterising similarity of those parameters to the selected reference stationary phase. Thus, a ranking list based on the FKUL value can be calculated for the chosen reference column, then correlated with the results of the column performance test. In this study, the column performance test was based on analysis of moclobemide and its two metabolites in human plasma by liquid chromatography (LC), using 18 columns. The comparative study was performed using traditional correlation of the FKUL values with the retention parameters of the analytes describing the column performance test. In order to deepen the comparative assessment of both data sets, factor analysis (FA) was also used. The obtained results indicated that the stationary phase classes, closely related according to the KUL method, yielded comparable separation for the target substances. Therefore, the column ranking system based on the FKUL-values could be considered supportive in the choice of the appropriate column for biomedical analysis.

  10. Fisheries Aspects of Seamounts and Taylor Columns

    DTIC Science & Technology

    1986-09-01

    the armorhead population. Due to a probable combination of overfishing and poor recruitment, the large fishery of the early 1970’s began a rapid...ACCESSION NO T I TLE (include Security Classification) FISHERIES ASPECTS OF SEAMOUNTS AND TAYLOR COLUMNS 2 PERSONAL AUTHOR(S) Brainard, Russell E. 13a...retention Seamount oceanography Taylor column Fisheries Nutrient enrichment 𔄃 3ASTRACT (Continue on reverse of necessary and identify by block number

  11. Sub-to super-ambient temperature programmable microfabricated gas chromatography column

    DOEpatents

    Robinson, Alex L.; Anderson, Lawrence F.

    2004-03-16

    A sub- to super-ambient temperature programmable microfabricated gas chromatography column enables more efficient chemical separation of chemical analytes in a gas mixture by combining a thermoelectric cooler and temperature sensing on the microfabricated column. Sub-ambient temperature programming enables the efficient separation of volatile organic compounds and super-ambient temperature programming enables the elution of less volatile analytes within a reasonable time. The small heat capacity and thermal isolation of the microfabricated column improves the thermal time response and power consumption, both important factors for portable microanalytical systems.

  12. Gas chromatographic column for the storage of sample profiles

    NASA Technical Reports Server (NTRS)

    Dimandja, J. M.; Valentin, J. R.; Phillips, J. B.

    1994-01-01

    The concept of a sample retention column that preserves the true time profile of an analyte of interest is studied. This storage system allows for the detection to be done at convenient times, as opposed to the nearly continuous monitoring that is required by other systems to preserve a sample time profile. The sample storage column is essentially a gas chromatography column, although its use is not the separation of sample components. The functions of the storage column are the selective isolation of the component of interest from the rest of the components present in the sample and the storage of this component as a function of time. Using octane as a test substance, the sample storage system was optimized with respect to such parameters as storage and readout temperature, flow rate through the storage column, column efficiency and storage time. A 3-h sample profile was collected and stored at 30 degrees C for 20 h. The profile was then retrieved, essentially intact, in 5 min at 130 degrees C.

  13. Column Selection for Biomedical Analysis Supported by Column Classification Based on Four Test Parameters

    PubMed Central

    Plenis, Alina; Rekowska, Natalia; Bączek, Tomasz

    2016-01-01

    This article focuses on correlating the column classification obtained from the method created at the Katholieke Universiteit Leuven (KUL), with the chromatographic resolution attained in biomedical separation. In the KUL system, each column is described with four parameters, which enables estimation of the FKUL value characterising similarity of those parameters to the selected reference stationary phase. Thus, a ranking list based on the FKUL value can be calculated for the chosen reference column, then correlated with the results of the column performance test. In this study, the column performance test was based on analysis of moclobemide and its two metabolites in human plasma by liquid chromatography (LC), using 18 columns. The comparative study was performed using traditional correlation of the FKUL values with the retention parameters of the analytes describing the column performance test. In order to deepen the comparative assessment of both data sets, factor analysis (FA) was also used. The obtained results indicated that the stationary phase classes, closely related according to the KUL method, yielded comparable separation for the target substances. Therefore, the column ranking system based on the FKUL-values could be considered supportive in the choice of the appropriate column for biomedical analysis. PMID:26805819

  14. Ultra high pressure liquid chromatography. Column permeability and changes of the eluent properties.

    PubMed

    Gritti, Fabrice; Guiochon, Georges

    2008-04-11

    The behavior of four similar liquid chromatography columns (2.1mm i.d. x 30, 50, 100, and 150 mm, all packed with fine particles, average d(p) approximately 1.7 microm, of bridged ethylsiloxane/silica hybrid-C(18), named BEH-C(18)) was studied in wide ranges of temperature and pressure. The pressure and the temperature dependencies of the viscosity and the density of the eluent (pure acetonitrile) along the columns were also derived, using the column permeabilities and applying the Kozeny-Carman and the heat balance equations. The heat lost through the external surface area of the chromatographic column was directly derived from the wall temperature of the stainless steel tube measured with a precision of +/-0.2 degrees C in still air and +/-0.1 degrees C in the oven compartment. The variations of the density and viscosity of pure acetonitrile as a function of the temperature and pressure was derived from empirical correlations based on precise experimental data acquired between 298 and 373 K and at pressures up to 1.5 kbar. The measurements were made with the Acquity UPLC chromatograph that can deliver a maximum flow rate of 2 mL/min and apply a maximum column inlet pressure of 1038 bar. The average Kozeny-Carman permeability constant of the columns was 144+/-3.5%. The temperature hence the viscosity and the density profiles of the eluent along the column deviate significantly from linear behavior under high-pressure gradients. For a 1000 bar pressure drop, we measured DeltaT=25-30 K, (Deltaeta/eta) approximately 100%, and (Deltarho/rho) approximately 10%. These results show that the radial temperature profiles are never fully developed within 1% for any of the columns, even under still-air conditions. This represents a practical advantage regarding the apparent column efficiency at high flow rates, since the impact of the differential analyte velocity between the column center and the column wall is not maximum. The interpretation of the peak profiles recorded in

  15. Chromatographic selectivity of poly(alkyl methacrylate-co-divinylbenzene) monolithic columns for polar aromatic compounds by pressure-driven capillary liquid chromatography.

    PubMed

    Lin, Shu-Ling; Wang, Chih-Chieh; Fuh, Ming-Ren

    2016-10-05

    In this study, divinylbenzene (DVB) was used as the cross-linker to prepare alkyl methacrylate (AlMA) monoliths for incorporating π-π interactions between the aromatic analytes and AlMA-DVB monolithic stationary phases in capillary LC analysis. Various AlMA/DVB ratios were investigated to prepare a series of 30% AlMA-DVB monolithic stationary phases in fused-silica capillaries (250-μm i.d.). The physical properties (such as porosity, permeability, and column efficiency) of the synthesized AlMA-DVB monolithic columns were investigated for characterization. Isocratic elution of phenol derivatives was first employed to evaluate the suitability of the prepared AlMA-DVB columns for small molecule separation. The run-to-run (0.16-1.20%, RSD; n = 3) and column-to-column (0.26-2.95%, RSD; n = 3) repeatabilities on retention times were also examined using the selected AlMA-DVB monolithic columns. The π-π interactions between the aromatic ring and the DVB-based stationary phase offered better recognition on polar analytes with aromatic moieties, which resulted in better separation resolution of aromatic analytes on the AlMA-DVB monolithic columns. In order to demonstrate the capability of potential environmental and/or food safety applications, eight phenylurea herbicides with single benzene ring and seven sulfonamide antibiotics with polyaromatic moieties were analyzed using the selected AlMA-DVB monolithic columns. Copyright © 2016. Published by Elsevier B.V.

  16. Quantitation of promethazine and metabolites in urine samples using on-line solid-phase extraction and column-switching

    NASA Technical Reports Server (NTRS)

    Song, Q.; Putcha, L.; Harm, D. L. (Principal Investigator)

    2001-01-01

    A chromatographic method for the quantitation of promethazine (PMZ) and its three metabolites in urine employing on-line solid-phase extraction and column-switching has been developed. The column-switching system described here uses an extraction column for the purification of PMZ and its metabolites from a urine matrix. The extraneous matrix interference was removed by flushing the extraction column with a gradient elution. The analytes of interest were then eluted onto an analytical column for further chromatographic separation using a mobile phase of greater solvent strength. This method is specific and sensitive with a range of 3.75-1400 ng/ml for PMZ and 2.5-1400 ng/ml for the metabolites promethazine sulfoxide, monodesmethyl promethazine sulfoxide and monodesmethyl promethazine. The lower limits of quantitation (LLOQ) were 3.75 ng/ml with less than 6.2% C.V. for PMZ and 2.50 ng/ml with less than 11.5% C.V. for metabolites based on a signal-to-noise ratio of 10:1 or greater. The accuracy and precision were within +/- 11.8% in bias and not greater than 5.5% C.V. in intra- and inter-assay precision for PMZ and metabolites. Method robustness was investigated using a Plackett-Burman experimental design. The applicability of the analytical method for pharmacokinetic studies in humans is illustrated.

  17. T.Rex Visual Analytics for Transactional Exploration

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    None

    2014-07-01

    T.Rex is PNNL's visual analytics tool that specializes in tabular structured data, like you might open with Excel. It's a client-server application, allowing the server to do a lot of the heavy lifting and the client to open spreadsheets with millions of rows. With datasets of that size, especially if you're unfamiliar with the contents, it's very hard to get a good grasp of what's in it using traditional tools. With T.Rex, the multiple views allow you to see categorical, temporal, numerical, relational, and summary data. The interactivity lets you look across your data and see how things relate tomore » each other.« less

  18. T.Rex Visual Analytics for Transactional Exploration

    ScienceCinema

    None

    2018-01-16

    T.Rex is PNNL's visual analytics tool that specializes in tabular structured data, like you might open with Excel. It's a client-server application, allowing the server to do a lot of the heavy lifting and the client to open spreadsheets with millions of rows. With datasets of that size, especially if you're unfamiliar with the contents, it's very hard to get a good grasp of what's in it using traditional tools. With T.Rex, the multiple views allow you to see categorical, temporal, numerical, relational, and summary data. The interactivity lets you look across your data and see how things relate to each other.

  19. Pathways of Methylmercury Transfer to the Water Column Across Multiple Estuaries

    NASA Astrophysics Data System (ADS)

    Schartup, A. T.; Balcom, P. H.; Mason, R. P.; Chen, C.

    2014-12-01

    Estuarine water column methylmercury (MeHg) is an important driver of bioaccumulation in pelagic organisms so it is important to understand the sources and cycling of MeHg. As MeHg biomagnifies in food webs, increased water column concentrations can be transferred to fish consumed by humans. Few studies have taken a multi-estuary approach to look at MeHg cycling in the water column of these important MeHg producing areas. We examined the distributions and partitioning of sediment and water column MeHg across a geographic range of estuaries. In 2008 we sampled 10 shallow-water estuarine sites from Maine to New Jersey, sampled 11 sites in 4 estuaries in 2009, and sampled at 3 estuarine turbidity maximum (ETM) sites in 1 estuary in 2012. Sediment measurements included both solid phase and pore water MeHg and total mercury (HgT). Water column parameters included dissolved and particulate MeHg and HgT, total suspended solids, nutrients, and dissolved organic carbon. Average suspended particle MeHg was highest at Wells (ME; 6 to 11.5 pmol/g; 4.5 to 7% of HgT) and lowest at Portsmouth (NH) and in Long Island Sound (CT-NY; 0.2 to 5.5 pmol/g; 0.25 to 3.75% of HgT). Average water column dissolved MeHg was highest in the Delaware River ETM (0.5 to 0.7 pM; 16 to 24% of HgT) and lowest at Portsmouth (0.06 to 0.12 pM; 1 to 2% of HgT). Significant positive correlations were found between MeHg and HgT across multiple estuaries in both sediment and the water column in 2008 and 2009. In contrast, water column dissolved and suspended particle MeHg do not correlate well with sediment MeHg or HgT, pore water MeHg or methylation rates in sediment across estuaries, indicating that sediment is often not a good predictor of water MeHg levels. However, ratios of average dissolved:pore water MeHg and suspended particle:sediment MeHg are close to 1 in the Delaware River ETM, suggesting that sediment supplies MeHg to the water column in this turbulent region, but average pore water MeHg was

  20. Tank 241-T-204, core 188 analytical results for the final report

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Nuzum, J.L.

    TANK 241-T-204, CORE 188, ANALYTICAL RESULTS FOR THE FINAL REPORT. This document is the final laboratory report for Tank 241 -T-204. Push mode core segments were removed from Riser 3 between March 27, 1997, and April 11, 1997. Segments were received and extruded at 222-8 Laboratory. Analyses were performed in accordance with Tank 241-T-204 Push Mode Core Sampling and analysis Plan (TRAP) (Winkleman, 1997), Letter of instruction for Core Sample Analysis of Tanks 241-T-201, 241- T-202, 241-T-203, and 241-T-204 (LAY) (Bell, 1997), and Safety Screening Data Qual@ Objective (DO) ODukelow, et al., 1995). None of the subsamples submitted for totalmore » alpha activity (AT) or differential scanning calorimetry (DC) analyses exceeded the notification limits stated in DO. The statistical results of the 95% confidence interval on the mean calculations are provided by the Tank Waste Remediation Systems Technical Basis Group and are not considered in this report.« less

  1. Ideal versus real automated twin column recycling chromatography process.

    PubMed

    Gritti, Fabrice; Leal, Mike; McDonald, Thomas; Gilar, Martin

    2017-07-28

    The full baseline separation of two compounds (selectivity factors α<1.03) is either impractical (too long analysis times) or even impossible when using a single column of any length given the pressure limitations of current LC instruments. The maximum efficiency is that of an infinitely long column operated at infinitely small flow rates. It is determined by the maximum allowable system pressure, the column permeability (particle size), the viscosity of the eluent, and the intensity of the effective diffusivity of the analytes along the column. Alternatively, the twin-column recycling separation process (TCRSP) can overcome the efficiency limit of the single-column approach. In the TCRSP, the sample mixture may be transferred from one to a second (twin) column until its band has spread over one column length. Basic theory of chromatography is used to confirm that the speed-resolution performance of the TCRSP is intrinsically superior to that of the single-column process. This advantage is illustrated in this work by developing an automated TCRSP for the challenging separation of two polycyclic aromatic hydrocarbon (PAH) isomers (benzo[a]anthracene and chrysene) in the reversed-phase retention mode at pressure smaller than 5000psi. The columns used are the 3.0mm×150mm column packed with 3.5μm XBridge BEH-C 18 material (α=1.010) and the 3.0mm or 4.6mm×150mm columns packed with the same 3.5μm XSelect HSST 3 material (α=1.025). The isocratic mobile phase is an acetonitrile-water mixture (80/20, v/v). Remarkably, significant differences are observed between the predicted retention times and efficiencies of the ideal TCRSP (given by the number of cycles multiplied by the retention time and efficiency of one column) and those of the real TCRSP. The fundamental explanation lies in the pressure-dependent retention of these PAHs or in the change of their partial molar volume as they are transferred from the mobile to the stationary phase. A revisited retention and

  2. The Application of TD/GC/NICI-MS with an Al2O3-PLOT-S Column for the Determination of Perfluoroalkylcycloalkanes in the Atmosphere.

    PubMed

    Ren, Yu; Schlager, Hans; Martin, Damien

    2014-01-01

    A modified method for the quantitative determination of atmospheric perfluoroalkylcycloalkanes (PFCs) using thermal desorption coupled with gas chromatography and detection by negative ion chemical ionization-mass spectrometry was developed. Using an optimized analytical system, a commercially available Al 2 O 3 porous layer open tubular (PLOT) capillary column (30 m × 0.25 mm) deactivated with Na 2 SO 4 was used for separation of PFCs. Improvements in the separation of PFCs, the corresponding identification and the limit of detection of PFCs using this method and column are presented. The method was successfully applied to determine the atmospheric background concentrations of a range of PFCs from a number of samples collected at a rural site in Germany. The results of this study suggest that the method outlined using the Al 2 O 3 -PLOT-S capillary column has good sensitivity and selectivity, and that it can be deployed in a routine laboratory process for the analysis of PFCs in the future research work. In addition, the ability of this column to separate the isomers of one of the lower boiling PFCs (perfluorodimethylcyclobutane) and its ability to resolve perfluoroethylcyclohexane offer the opportunity for single-column analysis for multiple PFCs.

  3. Local buckling of composite channel columns

    NASA Astrophysics Data System (ADS)

    Szymczak, Czesław; Kujawa, Marcin

    2018-05-01

    The investigation concerns local buckling of compressed flanges of axially compressed composite channel columns. Cooperation of the member flange and web is taken into account here. The buckling mode of the member flange is defined by rotation angle a flange about the line of its connection with the web. The channel column under investigation is made of unidirectional fibre-reinforced laminate. Two approaches to member orthotropic material modelling are performed: the homogenization with the aid of theory of mixture and periodicity cell or homogenization upon the Voigt-Reuss hypothesis. The fundamental differential equation of local buckling is derived with the aid of the stationary total potential energy principle. The critical buckling stress corresponding to a number of buckling half-waves is assumed to be a minimum eigenvalue of the equation. Some numerical examples dealing with columns are given here. The analytical results are compared with the finite element stability analysis carried out by means of ABAQUS software. The paper is focused on a close analytical solution of the critical buckling stress and the associated buckling mode while the web-flange cooperation is assumed.

  4. Simple column-switching ion chromatography method for determining eight monosaccharides and oligosaccharides in honeydew and nectar.

    PubMed

    Ni, Chengzhu; Zhu, Binhe; Wang, Nani; Wang, Muhua; Chen, Suqing; Zhang, Jiajie; Zhu, Yan

    2016-03-01

    Honeydew is excreted by aphids as a sweet waste and nectar is floral honey. Honeydew and nectar are complicated samples which consist of various sugars and amino acids. In this work, a simple ion chromatography with column-switching method was developed for the simultaneous analysis of 8 monosaccharides and oligosaccharides in honeydew and nectar. A reversed-phase column was used as a pretreatment column to eliminate organics on-line and sugars were eluted from a collection loop to analytical column by using column-switching technique. This method showed good linearity (r⩾0.9994) and afforded low limits of detection ranging from 1.55 to 10.17μgL(-1) for all the analytes. Recoveries ranged from 95% to 105% and repeatability results were acceptable with relative standard deviation of less than 3.21% (n=6). This method was successfully applied to quantification of these sugars in honeydew and nectar. These results showed honeydew had much more oligosaccharides than nectar. Copyright © 2015 Elsevier Ltd. All rights reserved.

  5. The design of a new concept chromatography column.

    PubMed

    Camenzuli, Michelle; Ritchie, Harald J; Ladine, James R; Shalliker, R Andrew

    2011-12-21

    Active Flow Management is a new separation technique whereby the flow of mobile phase and the injection of sample are introduced to the column in a manner that allows migration according to the principles of the infinite diameter column. A segmented flow outlet fitting allows for the separation of solvent or solute that elutes along the central radial section of the column from that of the sample or solvent that elutes along the wall region of the column. Separation efficiency on the analytical scale is increased by 25% with an increase in sensitivity by as much as 52% compared to conventional separations.

  6. A design procedure for a tension-wire stiffened truss-column

    NASA Technical Reports Server (NTRS)

    Greene, W. H.

    1980-01-01

    A deployable, tension wire stiffened, truss column configuration was considered for space structure applications. An analytical procedure, developed for design of the truss column and exercised in numerical studies, was based on equivalent beam stiffness coefficients in the classical analysis for an initially imperfect beam column. Failure constraints were formulated to be used in a combined weight/strength and nonlinear mathematical programming automated design procedure to determine the minimum mass column for a particular combination of design load and length. Numerical studies gave the mass characteristics of the truss column for broad ranges of load and length. Comparisons of the truss column with a baseline tubular column used a special structural efficiency parameter for this class of columns.

  7. Long-range attraction of an ultrarelativistic electron beam by a column of neutral plasma

    NASA Astrophysics Data System (ADS)

    Adli, E.; Lindstrøm, C. A.; Allen, J.; Clarke, C. I.; Frederico, J.; Gessner, S. J.; Green, S. Z.; Hogan, M. J.; Litos, M. D.; O'Shea, B.; Yakimenko, V.; An, W.; Clayton, C. E.; Marsh, K. A.; Mori, W. B.; Joshi, C.; Vafaei-Najafabadi, N.; Corde, S.; Lu, W.

    2016-10-01

    We report on the experimental observation of the attraction of a beam of ultrarelativistic electrons towards a column of neutral plasma. In experiments performed at the FACET test facility at SLAC we observe that an electron beam moving parallel to a neutral plasma column, at an initial distance of many plasma column radii, is attracted into the column. Once the beam enters the plasma it drives a plasma wake similar to that of an electron beam entering the plasma column head-on. A simple analytical model is developed in order to capture the essential physics of the attractive force. The attraction is further studied by 3D particle-in-cell numerical simulations. The results are an important step towards better understanding of particle beam-plasma interactions in general and plasma wakefield accelerator technology in particular.

  8. Rapid and sensitive analytical method for monitoring of 12 organotin compounds in natural waters.

    PubMed

    Vahčič, Mitja; Milačič, Radmila; Sčančar, Janez

    2011-03-01

    A rapid analytical method for the simultaneous determination of 12 different organotin compounds (OTC): methyl-, butyl-, phenyl- and octyl-tins in natural water samples was developed. It comprises of in situ derivatisation (by using NaBEt4) of OTC in salty or fresh water sample matrix adjusted to pH 6 with Tris-citrate buffer, extraction of ethylated OTC into hexane, separation of OTC in organic phase on 15 m GC column and subsequent quantitative determination of separated OTC by ICP-MS. To optimise the pH of ethylation, phosphate, carbonate and Tris-citrate buffer were investigated alternatively to commonly applied sodium acetate - acetic acid buffer. The ethylation yields in Tris-citrate buffer were found to be better for TBT, MOcT and DOcT in comparison to commonly used acetate buffer. Iso-octane and hexane were examined as organic phase for extraction of ethylated OTC. The advantage of hexane was in its ability for quantitative determination of TMeT. GC column of 15 m in length was used for separation of studied OTC under the optimised separation conditions and its performances compared to 30 m column. The analytical method developed enables sensitive simultaneous determination of 12 different OTC and appreciably shortened analysis time in larger series of water samples. LOD's obtained for the newly developed method ranged from 0.05-0.06 ng Sn L-1 for methyl-, 0.11-0.45 ng Sn L-1 for butyl-, 0.11-0.16 ng Sn L-1 for phenyl-, and 0.07-0.10 ng Sn L-1 for octyl-tins. By applying the developed analytical method, marine water samples from the Northern Adriatic Sea containing mainly butyl- and methyl-tin species were analysed to confirm the proposed method's applicability.

  9. Solid-phase extraction of polar pesticides from environmental water samples on graphitized carbon and Empore-activated carbon disks and on-line coupling to octadecyl-bonded silica analytical columns.

    PubMed

    Slobodník, J; Oztezkizan, O; Lingeman, H; Brinkman, U A

    1996-10-25

    The suitability of Empore-activated carbon disks (EACD), Envi-Carb graphitized carbon black (GCB) and CPP-50 graphitized carbon for the trace enrichment of polar pesticides from water samples was studied by means of off-line and on-line solid-phase extraction (SPE). In the off-line procedure, 0.5-2 l samples spiked with a test mixture of oxamyl, methomyl and aldicarb sulfoxide were enriched on EnviCarb SPE cartridges or 47 mm diameter EACD and eluted with dichloromethane-methanol. After evaporation, a sample was injected onto a C18-bonded silica column and analysed by liquid chromatography with ultraviolet (LC-UV) detection. EACD performed better than EnviCarb cartridges in terms of breakthrough volumes (> 2 l for all test analytes), reproducibility (R.S.D. of recoveries, 4-8%, n = 3) and sampling speed (100 ml/min); detection limits in drinking water were 0.05-0.16 microgram/l. In the on-line experiments, 4.6 mm diameter pieces cut from original EACD and stacked onto each other in a 9 mm long precolumn, and EnviCarb and CPP-50 packed in 10 x 2.0 mm I.D. precolumn, were tested, and 50-200 ml spiked water samples were preconcentrated. Because of the peak broadening caused by the strong sorption of the analytes on carbon, the carbon-packed precolumns were eluted by a separate stream of 0.1 ml/min acetonitrile which was mixed with the gradient LC eluent in front of the C18 analytical column. The final on-line procedure was also applied for the less polar propoxur, carbaryl and methiocarb. EnviCarb could not be used due to its poor pressure resistance. CPP-50 provided less peak broadening than EACD: peak widths were 0.1-0.3 min and R.S.D. of peak heights 4-14% (n = 3). In terms of analyte trapping efficiency on-line SPE-LC-UV with a CPP-50 precolumn also showed better performance than when Bondesil C18/OH or polymeric PLRP-S was used, but chromatographic resolution was similar. With the CPP-50-based system, detection limits of the test compounds were 0.05-1 microgram

  10. Monolithic column modified with bifunctional ionic liquid and styrene stationary phases for capillary electrochromatography.

    PubMed

    Mao, Zhenkun; Chen, Zilin

    2017-01-13

    A novel monolithic column with ionic liquid and styrene-modified bifunctional group was prepared for capillary electrochromatography (CEC) by in situ copolymerization in a ternary porogenic solvent. Ionic liquid (1-allyl-methylimidazolium chloride, AlMeIm + Cl - ) and styrene served as the bifunctional monomer, while ethylene dimethacrylate (EDMA) was used as the cross-linker. The monomer of AlMeIm + Cl - was introduced as anion-exchange group, while styrene as hydrophobic and aromatic group; the similar conjugated structure in AlMeIm + Cl - and styrene was beneficial for offeing obvious synergistic effect. The bifunctional stationary phase possessed powerful selectivity for the separation of neutral compounds, acidic analytes and phenols. The highest column efficiency was 2.70×10 5 platesm -1 (theoretical plates, N) for toluene. A relatively strong electroosmotic flow (EOF) was obtained in a wide range of pH values from 2.0 to 12.0, which could successfully achieve the rapid separation of the analytes within 10min. The proposed monolithic column was characterized by scanning electron microscopy (SEM) and Fourier transform infrared (FT-IR). The results indicated that the resultant monolithic column had good permeability and excellent mechanical stability. Good reproducibility was obtained with relative standard deviations (RSDs) of the retention time in the range of 0.24-0.47% and 0.81-2.17% for run-to-run (n=5) and day-to-day (n=5), while 1.09-2.70% and 0.98-1.70% for column-to-column (n=3) and batch-to-batch (n=3), respectively. The combination of AlMeIm + Cl - and styrene was a promising option in the fabrication of the organic polymer monolithic column. Copyright © 2016 Elsevier B.V. All rights reserved.

  11. Long-range attraction of an ultrarelativistic electron beam by a column of neutral plasma

    DOE PAGES

    Adli, Erik; Lindstrom, C. A.; Allen, J.; ...

    2016-10-12

    Here, we report on the experimental observation of the attraction of a beam of ultrarelativistic electrons towards a column of neutral plasma. In experiments performed at the FACET test facility at SLAC we observe that an electron beam moving parallel to a neutral plasma column, at an initial distance of many plasma column radii, is attracted into the column. Once the beam enters the plasma it drives a plasma wake similar to that of an electron beam entering the plasma column head-on. A simple analytical model is developed in order to capture the essential physics of the attractive force. Themore » attraction is further studied by 3D particle-in-cell numerical simulations. The results are an important step towards better understanding of particle beam–plasma interactions in general and plasma wakefield accelerator technology in particular.« less

  12. Long-range attraction of an ultrarelativistic electron beam by a column of neutral plasma

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Adli, Erik; Lindstrom, C. A.; Allen, J.

    Here, we report on the experimental observation of the attraction of a beam of ultrarelativistic electrons towards a column of neutral plasma. In experiments performed at the FACET test facility at SLAC we observe that an electron beam moving parallel to a neutral plasma column, at an initial distance of many plasma column radii, is attracted into the column. Once the beam enters the plasma it drives a plasma wake similar to that of an electron beam entering the plasma column head-on. A simple analytical model is developed in order to capture the essential physics of the attractive force. Themore » attraction is further studied by 3D particle-in-cell numerical simulations. The results are an important step towards better understanding of particle beam–plasma interactions in general and plasma wakefield accelerator technology in particular.« less

  13. Analysis of packing microstructure and wall effects in a narrow-bore ultrahigh pressure liquid chromatography column using focused ion-beam scanning electron microscopy.

    PubMed

    Reising, Arved E; Schlabach, Sabine; Baranau, Vasili; Stoeckel, Daniela; Tallarek, Ulrich

    2017-09-01

    Column wall effects are well recognized as major limiting factor in achieving high separation efficiency in HPLC. This is especially important for modern analytical columns packed with small particles, where wall effects dominate the band broadening. Detailed knowledge about the packing microstructure of packed analytical columns has so far not been acquired. Here, we present the first three-dimensional reconstruction protocol for these columns utilizing focused ion-beam scanning electron microscopy (FIB-SEM) on a commercial 2.1mm inner diameter×50mm length narrow-bore analytical column packed with 1.7μm bridged-ethyl hybrid silica particles. Two sections from the packed bed are chosen for reconstruction by FIB-SEM: one from the bulk packing region of the column and one from its critical wall region. This allows quantification of structural differences between the wall region and the center of the bed due to effects induced by the hard, confining column wall. Consequences of these effects on local flow velocity in the column are analyzed with flow simulations utilizing the lattice-Boltzmann method. The reconstructions of the bed structures reveal significant structural differences in the wall region (extending radially over approximately 62 particle diameters) compared to the center of the column. It includes the local reduction of the external porosity by up to 10% and an increase of the mean particle diameter by up to 3%, resulting in a decrease of the local flow velocity by up to 23%. In addition, four (more ordered) layers of particles in the direct vicinity of the column wall induce local velocity fluctuations by up to a factor of three regarding the involved velocity amplitudes. These observations highlight the impact of radial variations in packing microstructure on band migration and column performance. This knowledge on morphological peculiarities of column wall effects helps guiding us towards further optimization of the packing process for analytical

  14. 3D-Printing for Analytical Ultracentrifugation

    PubMed Central

    Desai, Abhiksha; Krynitsky, Jonathan; Pohida, Thomas J.; Zhao, Huaying

    2016-01-01

    Analytical ultracentrifugation (AUC) is a classical technique of physical biochemistry providing information on size, shape, and interactions of macromolecules from the analysis of their migration in centrifugal fields while free in solution. A key mechanical element in AUC is the centerpiece, a component of the sample cell assembly that is mounted between the optical windows to allow imaging and to seal the sample solution column against high vacuum while exposed to gravitational forces in excess of 300,000 g. For sedimentation velocity it needs to be precisely sector-shaped to allow unimpeded radial macromolecular migration. During the history of AUC a great variety of centerpiece designs have been developed for different types of experiments. Here, we report that centerpieces can now be readily fabricated by 3D printing at low cost, from a variety of materials, and with customized designs. The new centerpieces can exhibit sufficient mechanical stability to withstand the gravitational forces at the highest rotor speeds and be sufficiently precise for sedimentation equilibrium and sedimentation velocity experiments. Sedimentation velocity experiments with bovine serum albumin as a reference molecule in 3D printed centerpieces with standard double-sector design result in sedimentation boundaries virtually indistinguishable from those in commercial double-sector epoxy centerpieces, with sedimentation coefficients well within the range of published values. The statistical error of the measurement is slightly above that obtained with commercial epoxy, but still below 1%. Facilitated by modern open-source design and fabrication paradigms, we believe 3D printed centerpieces and AUC accessories can spawn a variety of improvements in AUC experimental design, efficiency and resource allocation. PMID:27525659

  15. The fractionation of t-RNA on N,N′-bis(3-aminopropyl)-piperazine substituted-Sepharose

    PubMed Central

    Leberman, Reuben; Giovanelli, Ruth; Acosta, Zenobio

    1974-01-01

    An anion exchange agarose has been prepared by modifying sepharose 6B with N,N′-bis (-3-aminopropyl) piperazine. This material (BAPP-Sepharose) has been used for the fractionation of t-RNA from E.coli by column chromatography. The results obtained with gram quantities of crude t-RNA at pH 4.6 and pH 8.0 as measured by the elution patterns of alanyl, arginyl, aspartyl, leucyl, lysyl, methionyl, phenylalanyl, prolyl, seryl, tyrosyl, and valyl t-RNA are described. PMID:10793731

  16. The non-modulated transfer of total effluent for serially coupled columns in gas chromatography.

    PubMed

    Krupcík, Ján; Mydlová-Memersheimerová, Janka; Májek, Pavel; Zapadlo, Michal; Sandra, Pat

    2010-03-12

    The non-modulated transfer (NMT) of the total effluent of the separation of polychlorinated biphenyls (PCBs) on two columns coupled in series has been studied. A non-polar poly(5%-phenyl-95%-methyl)siloxane column (40 m x 100 microm x 0.1 microm) and a polar 70%-cyanopropyl-polysilphenylene-siloxane column (4 m x 0.1 mm x 0.1 microm) were used as (1)D and (2)D columns, respectively. The effluents from both the (1)D column and the (1)D+(2)D column series were monitored independently by two FIDs. Data from the (1)D and (1)D+(2)D integration reports were used to evaluate the NMT experiment. (1)D retention times, t(R,i,D1), were directly accessible from (1)D integration report while (2)D retention times, t(R,i,B), were calculated for all corresponding peak pairs from (1)D and (1)D+(2)D integration reports as a difference t(R,i,D2)=t(R,i,D1+D2)-t(R,i,D1). Search for corresponding peaks of PCB congeners in the (1)D and (1)D+(2)D chromatograms is elucidated in detail on standard PCB samples and on PCB congeners present in the technical formulation Arochlor 1242. Both retention times (t(R,i,D1) and t(R,i,D2)) as well as peak widths at half height (w(h,i)) and peak heights (h(i)) obtained from integration reports were used to construct 2D and 3D images for PCB NMT separations on serially coupled columns. The performance of the NMT procedure is illustrated by the separation of (i) standard PCB solutions, (ii) a mixture of the 209 PCBs, and (iii) a mixture of Arochlor 1242 and hydrocarbons on the DB-5+BPX-70 column series. Copyright (c) 2010 Elsevier B.V. All rights reserved.

  17. Peak distortion effects in analytical ion chromatography.

    PubMed

    Wahab, M Farooq; Anderson, Jordan K; Abdelrady, Mohamed; Lucy, Charles A

    2014-01-07

    The elution profile of chromatographic peaks provides fundamental understanding of the processes that occur in the mobile phase and the stationary phase. Major advances have been made in the column chemistry and suppressor technology in ion chromatography (IC) to handle a variety of sample matrices and ions. However, if the samples contain high concentrations of matrix ions, the overloaded peak elution profile is distorted. Consequently, the trace peaks shift their positions in the chromatogram in a manner that depends on the peak shape of the overloading analyte. In this work, the peak shapes in IC are examined from a fundamental perspective. Three commercial IC columns AS16, AS18, and AS23 were studied with borate, hydroxide and carbonate as suppressible eluents. Monovalent ions (chloride, bromide, and nitrate) are used as model analytes under analytical (0.1 mM) to overload conditions (10-500 mM). Both peak fronting and tailing are observed. On the basis of competitive Langmuir isotherms, if the eluent anion is more strongly retained than the analyte ion on an ion exchanger, the analyte peak is fronting. If the eluent is more weakly retained on the stationary phase, the analyte peak always tails under overload conditions regardless of the stationary phase capacity. If the charge of the analyte and eluent anions are different (e.g., Br(-) vs CO3(2-)), the analyte peak shapes depend on the eluent concentration in a more complex pattern. It was shown that there are interesting similarities with peak distortions due to strongly retained mobile phase components in other modes of liquid chromatography.

  18. Cyclodextrins as a chiral mobile phase additive in nano-liquid chromatography: comparison of reversed-phase silica monolithic and particulate capillary columns.

    PubMed

    Rocco, Anna; Maruška, Audrius; Fanali, Salvatore

    2012-03-01

    Enantioseparations of racemic nonsteroidal anti-inflammatory drugs (naproxen, ibuprofen, ketoprofen, flurbiprofen, suprofen, indoprofen, cicloprofen, and carprofen) were performed by nano-liquid chromatography, employing achiral capillary columns and heptakis(2,3,6-tri-O-methyl)-β-cyclodextrin (TM-β-CD) or hydroxylpropyl-β-cyclodextrin (HP-β-CD) as a chiral mobile phase additive (CMPA). Working under the same experimental conditions (in terms of mobile phase and linear velocity), the performance of a RP-C18 monolithic column was compared with that of a RP-C18 packed column of the same dimensions (100 μm i.d. × 10 cm). Utilizing a mobile phase composed of 30% ACN (v/v) buffered with 50 mM sodium acetate at pH 3, and containing 30 mM TM-β-CD, the monolithic column provided faster analysis but lower resolution than the packed column. This behavior was ascribed to the high permeability of the monolithic column, as well as to its minor selectivity. HP-β-CD was chosen as an alternative to TM-β-CD. Employing the monolithic column, the effects of different parameters such as HP-β-CD concentration, mobile phase composition, and pH on the retention factor and the chiral resolution of the analytes were studied. For the most of the analytes, enantioresolution (which ranged from R(s) = 1.80 for naproxen to R(s) = 0.86 for flurbiprofen) was obtained with a mobile phase consisting of sodium acetate buffer (25 mM, pH 3), 10% MeOH, and 15 mM HP-β-CD. When the same experimental conditions were used with the packed column, no compound eluted within 1 h. Upon increasing the percentage of organic modifier to favor analyte elution, only suprofen eluted within 30 min, with an R(s) value of 1.14 (20% MeOH). Replacing MeOH with ACN resulted in a loss of enantioresolution, except for naproxen (R(s) = 0.89).

  19. Desulfurization of coal by microbial column flotation.

    PubMed

    Ohmura, N; Saiki, H

    1994-06-05

    Twenty-three strains capable of oxidizing iron were isolated from coal and ore storage sites as well as coal and ore mines, volcanic areas, and hot spring. Four strains were found to have high iron-oxidizing activity. One strain (T-4) was selected for this experiment since the strain showed the fastest leaching rate of iron and sulfate from pyrite among the four strains. The T-4 strain was assigned for Thiobacillus ferrooxidans from its cultural and morphological characteristics.Bacterial treatment was applied to column flotation. An increase of cell density in the microbial column flotation resulted in the increase of pyrite removal from a coal-pyrite mixture (high sulfur imitated coal) with corresponding decrease of coal recovery. The addition of kerosene into the microbial column flotation increased the recovery of the imitated coal from 55% (without kerosene) to 81% (with 50 microL/L kerosene) with the reduction of pyrite sulfur content from 11% (feed coal) to 3.9% (product coal). The kerosene addition could reduce the pyritic sulfur content by collecting the coal in the recovery. However, the addition could not enhance separation of pyrite from the coal-pyrite mixture, since pyrite rejection was not affected by the increase of the kerosene addition. An excellent separation was obtained by the microbial flotation using a long column which had a length-diameter (L/D) ratio of 12.7. The long column flotation reduced the pyritic sulfur content from 11% (feed coal) to 1.8% (product coal) when 80% of the feed coal was recovered without the kerosene addition. The long column flotation not only attained an excellent separation but also reduced the amount of cells for desulfurization to as little as one-tenth of the reported amount.

  20. SU-D-213AB-05: Commissioning a CT Compatible LDR T&O Applicator Using Analytical Calculation with ID and 3D Dosimetry.

    PubMed

    Adamson, J; Newton, J; Steffey, B; Cai, J; Adamovics, J; Oldham, M; Chino, J; Craciunescu, O

    2012-06-01

    To determine the characteristics of a new commercially available CT-compatible LDR Tandem and Ovoid (T&O) applicator using 3D dosimetry. We characterized source attenuation through the asymmetric gold shielding in the buckets by measuring dose with diode and 3D dosimetry and compared to an analytical line integral calculation. For 3D dosimetry, a cylindrical PRESAGE dosimeter (9.5cm diameter, 9.2cm height) with a central 6mm channel bored for source placement was scanned with the Duke Large field of view Optical CT-Scanner (DLOS) before and after delivering a nominal 7.7Gy at a distance of 1 cm using a Cs-137 source loaded in the bucket. The optical CT scan time lasted approximately 15 minutes during which 720 projections were acquired at 0.5° increments, anda 3D dose distribution was reconstructed with a 0.5mm 3 isotropic voxel size. The 3D dose distribution was applied to a CT-based T&O implant to determine effect of ovoid shielding on the dose delivered to ICRU 38 Point A as well as D2cc of the bladder, rectum, bowel, and sigmoid. Dose transmission through the gold shielding at a radial distance of 1-3cm from midplane of the source was 86.6%, 86.1, and 87.0% for analytical calculation, diode, and 3D dosimetry, respectively. For the gold shielding of the bucket, dose transmission calculated using the 3D dosimetrymeasurement was found to be lowest at oblique angles from the bucket witha minimum of ∼51%. For the patient case, attenuation from the buckets leadto a decrease in average Point A dose of ∼4% and decrease in D2cc to bladder, rectum, sigmoid, and bowel of 2%, 15%, 2%, and 7%, respectively. The measured 3D dose distribution provided unique insight to the dosimetry and shielding characteristics of the investigated applicator, the technique for which can be applied to commissioning of other brachytherapy applicators. John Adamovics is the owner of Heuris Pharma LLC. Partially supported by NIH Grant R01 CA100835-01. © 2012 American Association of

  1. 3-D discrete analytical ridgelet transform.

    PubMed

    Helbert, David; Carré, Philippe; Andres, Eric

    2006-12-01

    In this paper, we propose an implementation of the 3-D Ridgelet transform: the 3-D discrete analytical Ridgelet transform (3-D DART). This transform uses the Fourier strategy for the computation of the associated 3-D discrete Radon transform. The innovative step is the definition of a discrete 3-D transform with the discrete analytical geometry theory by the construction of 3-D discrete analytical lines in the Fourier domain. We propose two types of 3-D discrete lines: 3-D discrete radial lines going through the origin defined from their orthogonal projections and 3-D planes covered with 2-D discrete line segments. These discrete analytical lines have a parameter called arithmetical thickness, allowing us to define a 3-D DART adapted to a specific application. Indeed, the 3-D DART representation is not orthogonal, It is associated with a flexible redundancy factor. The 3-D DART has a very simple forward/inverse algorithm that provides an exact reconstruction without any iterative method. In order to illustrate the potentiality of this new discrete transform, we apply the 3-D DART and its extension to the Local-DART (with smooth windowing) to the denoising of 3-D image and color video. These experimental results show that the simple thresholding of the 3-D DART coefficients is efficient.

  2. Analytical evaluation of point of care cTnT and clinical performances in an unselected population as compared with central laboratory highly sensitive cTnT.

    PubMed

    Dupuy, Anne Marie; Sebbane, Mustapha; Roubille, François; Coste, Thibault; Bargnoux, Anne Sophie; Badiou, Stéphanie; Kuster, Nils; Cristol, Jean Paul

    2015-03-01

    To report the analytical performances of the Radiometer AQT90 FLEX® cTnT assay (Neuilly-Plaisance, France) and to evaluate the concordance with hs-cTnT results from central laboratory for the diagnosis of acute myocardial infarction (AMI) at baseline and during a short follow-up among unselected patients admitted in emergency room or cardiology department. Analytical performances of AQT90 FLEX® cTnT immunoassay included imprecision study with determination of a coefficient of variation at 10% and 20%, linearity, and limit of detection. The concordance study was based on samples obtained from 170 consecutive patients with chest pain suggestive of acute coronary syndrome (ACS) admitted in the emergency room or cardiology department. The kinetic study (within 62 additional samples 3h later) was based on absolute delta criterion and the combination of relative change of 30% with absolute change of 7ng/L. The cTnT assay from Radiometer was evaluated as clinically usable, although less sensitive than the Roche hs-cTnT assay as demonstrated by the concordance and the kinetic studies. In non-selected population, the cTnT AQT Flex© assay on AQT90© with kinetic change at 3h, provides similar clinical classification of patients, particularly for AMI group as compared to central laboratory hs-cTnT assay and could be suitable for clinical use. Copyright © 2014 The Canadian Society of Clinical Chemists. Published by Elsevier Inc. All rights reserved.

  3. Continuous electrophoretic purification of individual analytes from multicomponent mixtures.

    PubMed

    McLaren, David G; Chen, David D Y

    2004-04-15

    Individual analytes can be isolated from multicomponent mixtures and collected in the outlet vial by carrying out electrophoretic purification through a capillary column. Desired analytes are allowed to migrate continuously through the column under the electric field while undesired analytes are confined to the inlet vial by application of a hydrodynamic counter pressure. Using pressure ramping and buffer replenishment techniques, 18% of the total amount present in a bulk sample can be purified when the resolution to the adjacent peak is approximately 3. With a higher resolution, the yield could be further improved. Additionally, by periodically introducing fresh buffer into the sample, changes in pH and conductivity can be mediated, allowing higher purity (>or=99.5%) to be preserved in the collected fractions. With an additional reversed cycle of flow counterbalanced capillary electrophoresis, any individual component in a sample mixture can be purified providing it can be separated in an electrophoresis system.

  4. Ensuring repeatability and robustness of poly(glycidyl methacrylate-co-ethylene dimethacrylate) HPLC monolithic columns of 3 mm id through covalent bonding to the column wall.

    PubMed

    Laaniste, Asko; Kruve, Anneli; Leito, Ivo

    2013-08-01

    Two different methods to reinforce the poly(glycidyl methacrylate-co-ethylene dimethacrylate) HPLC monolithic columns of 3 mm id in a glass column reservoir were studied: composite columns with polymeric particles in the monolith and surface treatment of the reservoir wall. Of the two methods used to counter the mechanical instability and formation of flow channels (composite columns and column wall surface treatment), we demonstrated that proper column wall surface treatment was sufficient to solve both problems. Our study also indicated that no surface treatment is efficient, and of the methods studied silanization in acidified ethanol solution and constant renewal of the reaction mixture (dynamic mode) proved to be the most effective. As a result of this study, we have been able to prepare repeatable and durable methacrylate HPLC columns with good efficiencies. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Study on Predicting Axial Load Capacity of CFST Columns

    NASA Astrophysics Data System (ADS)

    Ravi Kumar, H.; Muthu, K. U.; Kumar, N. S.

    2017-11-01

    This work presents an analytical study and experimental study on the behaviour and ultimate load carrying capacity of axially compressed self-compacting concrete-filled steel tubular columns. Results of tests conducted by various researchers on 213 samples concrete-filled steel tubular columns are reported and present authors experimental data are reported. Two theoretical equations were derived for the prediction of the ultimate axial load strength of concrete-filled steel tubular columns. The results from prediction were compared with the experimental data. Validation to the experimental results was made.

  6. 3. DRAINING & DRYING BUILDING, REINFORCED CONCRETE MUSHROOM COLUMNS WITH ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    3. DRAINING & DRYING BUILDING, REINFORCED CONCRETE MUSHROOM COLUMNS WITH DROP PANELS SUPPORTING DRAINING BINS (IRON VALVES OF DRAINING BINS ARE EMBEDDED IN THE CEILING), VIEW LOOKING WEST - Mill "C" Complex, Sand Draining & Drying Building, South of Dee Bennet Road, near Illinois River, Ottawa, La Salle County, IL

  7. Analytic model for washout of HCl(g) from dispersing rocket exhaust clouds

    NASA Technical Reports Server (NTRS)

    Pellett, G. L.

    1981-01-01

    The potential is investigated that precipitation scavenging of HCl from large solid rocket exhaust clouds may result in unacceptably acidic rain in the Cape Canaveral, Florida, area before atmospheric dispersion reduces HCl concentrations to safe limits. Several analytic expressions for HCl(g) and HCl(g + aq) washout are derived; a geometric mean washout coefficient is recommended. A previous HCl washout model is refined and applied to a space shuttle case (70 t HCl exhausted up to 4 km) and eight Titan 3 (60 percent less exhaust) dispersion cases. The vertical column density (sigma) decays were deduced by application of a multilayer Gaussian diffusion model to seven standard meteorological regimes for overland advection. The Titan 3 decays of sigma and initial rain pH differed greatly among regimes; e.g., a range of 2 pH units was spanned at x 100 km downwind and t = 2 hr. Environmentally significant pH's .5 for infrequent exposures were shown possible at X = 50 km and t 5 hr for the two least dispersive Titan 3 cases. Representative examples of downwind rainwater pH and G(X) are analyzed. Factors affecting the validity of the results are discussed.

  8. Comparison of adjoint and analytical Bayesian inversion methods for constraining Asian sources of carbon monoxide using satellite (MOPITT) measurements of CO columns

    NASA Astrophysics Data System (ADS)

    Kopacz, Monika; Jacob, Daniel J.; Henze, Daven K.; Heald, Colette L.; Streets, David G.; Zhang, Qiang

    2009-02-01

    We apply the adjoint of an atmospheric chemical transport model (GEOS-Chem CTM) to constrain Asian sources of carbon monoxide (CO) with 2° × 2.5° spatial resolution using Measurement of Pollution in the Troposphere (MOPITT) satellite observations of CO columns in February-April 2001. Results are compared to the more common analytical method for solving the same Bayesian inverse problem and applied to the same data set. The analytical method is more exact but because of computational limitations it can only constrain emissions over coarse regions. We find that the correction factors to the a priori CO emission inventory from the adjoint inversion are generally consistent with those of the analytical inversion when averaged over the large regions of the latter. The adjoint solution reveals fine-scale variability (cities, political boundaries) that the analytical inversion cannot resolve, for example, in the Indian subcontinent or between Korea and Japan, and some of that variability is of opposite sign which points to large aggregation errors in the analytical solution. Upward correction factors to Chinese emissions from the prior inventory are largest in central and eastern China, consistent with a recent bottom-up revision of that inventory, although the revised inventory also sees the need for upward corrections in southern China where the adjoint and analytical inversions call for downward correction. Correction factors for biomass burning emissions derived from the adjoint and analytical inversions are consistent with a recent bottom-up inventory on the basis of MODIS satellite fire data.

  9. An investigation of transient pressures and plasma properties in a pinched plasma column. M.S. Thesis

    NASA Technical Reports Server (NTRS)

    Stover, E. K.; York, T. M.

    1971-01-01

    The transient pinched plasma column generated in a linear Z-pinch was studied experimentally and analytically. The plasma column was investigated experimentally with several plasma diagnostics; they were: a rapid response pressure transducer, a magnetic field probe, a voltage probe, and discharge luminosity. Axial pressure profiles on the discharge chamber axis were used to identify three characteristic regions of plasma column behavior: (1) strong axial pressure asymmetry noted early in plasma column lifetime, (2) followed by plasma heating in which there is a rapid rise in static pressure, and (3) a slight decrease static pressure before plasma column breakup. Plasma column lifetime was approximately 5 microseconds. The axial pressure asymmetry was attributed to nonsimultaneous pinching of the imploding current sheet along the discharge chamber axis. The rapid heating could be attributed in part to viscous effects introduced by radial gradients in the axial streaming velocity.

  10. Empirical Approach for Determining Axial Strength of Circular Concrete Filled Steel Tubular Columns

    NASA Astrophysics Data System (ADS)

    Jayalekshmi, S.; Jegadesh, J. S. Sankar; Goel, Abhishek

    2018-06-01

    The concrete filled steel tubular (CFST) columns are highly regarded in recent years as an interesting option in the construction field by designers and structural engineers, due to their exquisite structural performance, with enhanced load bearing capacity and energy absorption capacity. This study presents a new approach to simulate the capacity of circular CFST columns under axial loading condition, using a large database of experimental results by applying artificial neural network (ANN). A well trained network is established and is used to simulate the axial capacity of CFST columns. The validation and testing of the ANN is carried out. The current study is focused on proposing a simplified equation that can predict the ultimate strength of the axially loaded columns with high level of accuracy. The predicted results are compared with five existing analytical models which estimate the strength of the CFST column. The ANN-based equation has good prediction with experimental data, when compared with the analytical models.

  11. Empirical Approach for Determining Axial Strength of Circular Concrete Filled Steel Tubular Columns

    NASA Astrophysics Data System (ADS)

    Jayalekshmi, S.; Jegadesh, J. S. Sankar; Goel, Abhishek

    2018-03-01

    The concrete filled steel tubular (CFST) columns are highly regarded in recent years as an interesting option in the construction field by designers and structural engineers, due to their exquisite structural performance, with enhanced load bearing capacity and energy absorption capacity. This study presents a new approach to simulate the capacity of circular CFST columns under axial loading condition, using a large database of experimental results by applying artificial neural network (ANN). A well trained network is established and is used to simulate the axial capacity of CFST columns. The validation and testing of the ANN is carried out. The current study is focused on proposing a simplified equation that can predict the ultimate strength of the axially loaded columns with high level of accuracy. The predicted results are compared with five existing analytical models which estimate the strength of the CFST column. The ANN-based equation has good prediction with experimental data, when compared with the analytical models.

  12. Significance of Iron(II,III) Hydroxycarbonate Green Rust in Arsenic Remediation Using Zerovalent Iron in Laboratory Column Tests

    EPA Science Inventory

    We examined the corrosion products of zerovalent iron used in three column tests for removing arsenic from water under dynamic flow conditions. Each column test lasted three- to four-months using columns consisting of a 10.3-cm depth of 50 : 50 (w : w, Peerless iron : sand) in t...

  13. Sequential injection system with in-line solid phase extraction and soil mini-column for determination of zinc and copper in soil leachates.

    PubMed

    Paluch, Justyna; Mesquita, Raquel B R; Cerdà, Víctor; Kozak, Joanna; Wieczorek, Marcin; Rangel, António O S S

    2018-08-01

    A sequential injection (SI) system equipped with in-line solid phase extraction column and in-line soil mini-column is proposed for determination of zinc and copper in soil leachates. The spectrophotometric determination (560 nm) is based on the reaction of both analytes with 1-(2-Pyridylazo)-2-naphthol (PAN). Zinc is determined after retaining copper on a cationic resin (Chelex100) whereas copper is determined from the difference of the absorbance measured for both analytes, introduced into the system with the use of a different channel, and zinc absorbance. The influence of several potential interferences was studied. Using the developed method, zinc and copper were determined within the concentration ranges of 0.005-0.300 and 0.011-0.200 mg L -1 , and with a relative standard deviation lower than 6.0% and 5.1%, respectively. The detection limits are 1.4 and 3.0 µg/L for determination of zinc and copper, respectively. The developed SI method was verified by the determination of both analytes in synthetic and certified reference materials of water samples, and applied to the determination of the analytes in rain water and soil leachates from laboratory scale soil core column and in-line soil mini-column. Copyright © 2018 Elsevier B.V. All rights reserved.

  14. Pressure, temperature and density drops along supercritical fluid chromatography columns. I. Experimental results for neat carbon dioxide and columns packed with 3- and 5-micron particles.

    PubMed

    Poe, Donald P; Veit, Devon; Ranger, Megan; Kaczmarski, Krzysztof; Tarafder, Abhijit; Guiochon, Georges

    2012-08-10

    The pressure drop and temperature drop on columns packed with 3- and 5-micron particles were measured using neat CO(2) at a flow rate of 5 mL/min, at temperatures from 20°C to 100°C, and outlet pressures from 80 to 300 bar. The density drop was calculated based on the temperature and pressure at the column inlet and outlet. The columns were suspended in a circulating air bath either bare or covered with foam insulation. The results show that the pressure drop depends on the outlet pressure, the operating temperature, and the thermal environment. A temperature drop was observed for all conditions studied. The temperature drop was relatively small (less than 3°C) for combinations of low temperature and high pressure. Larger temperature drops and density drops occurred at higher temperatures and low to moderate pressures. Covering the column with thermal insulation resulted in larger temperature drops and corresponding smaller density drops. At 20°C the temperature drop was never more than a few degrees. The largest temperature drops occurred for both columns when insulated at 80°C and 80 bar, reaching a maximum value of 21°C for the 5-micron column, and 26°C for the 3-micron column. For an adiabatic column, the temperature drop depends on the pressure drop, the thermal expansion coefficient, and the density and the heat capacity of the mobile phase fluid, and can be described by a simple mathematical relationship. For a fixed operating temperature and outlet pressure, the temperature drop increases monotonically with the pressure drop. Copyright © 2012 Elsevier B.V. All rights reserved.

  15. Abdominal girth and vertebral column length can adjust spinal anesthesia for lower limb surgery, a prospective, observational study.

    PubMed

    Zhou, Qing-he; Zhu, Bo; Wei, Chang-na; Yan, Min

    2016-03-24

    Studies have shown that abdominal girth and vertebral column length have high predictive value for spinal spread after administering a dose of plain bupivacaine. we designed a study to identify the specific correlations between abdominal girth, vertebral column length and a 0.5% dosage of plain bupivacaine, which should provide a minimum upper block level (T12) and a suitable upper block level (T10) for lower limb surgeries. A suitable dose of 0.5% plain bupivacaine was administered intrathecally between the L3 and L4 vertebrae for lower limb surgeries. If the upper cephalad spread of the patient by loss of pinprick discrimination was T12 or T10, the patient was enrolled in this study. Five patient variables and intrathecal plain bupivacaine dose were recorded. Linear regression and multiple regression analyses were performed. Totals of 111 patients and 121 patients who lost pinprick discrimination at T12 and T10, respectively, were analyzed in this study. Linear regression analysis showed that only abdominal girth and plain bupivacaine dose were strongly correlated (r =-0.827 for T12, r = -0.806 for T10; both p < 0.0001). Multiple linear regression analysis showed that both abdominal girth and vertebral column length were the key determinants of plain bupivacaine dose (both p < 0.0001). R(2) was 0.874 and 0.860 for the loss of pinprick discrimination at T12 and T10, respectively. Our data indicated that vertebral column length and abdominal girth were strongly correlated with the dosage of intrathecal plain bupivacaine for the loss of pinprick discrimination at T12 and T10. The two regression equations were YT12 = 3.547 + 0.045X1-0.044X2 and YT10 = 3.848 + 0.047X1- 0.046X2 (Y, 0.5% plain bupivacaine volume; X1, vertebral column length;and X 2, abdominal girth), which can accurately predict the minimum and suitable intrathecal bupivacaine dose for lower limb surgery to a great extent, separately.

  16. Nano-amylose-2,3-bis(3,5-dimethylphenylcarbamate)-silica hybrid sol immobilized on open tubular capillary column for capillary electrochromatography enantioseparation.

    PubMed

    Sun, Yaming; Wu, Qi; Shi, Xiaofeng; Gao, Jie; Dong, Shuqing; Zhao, Liang

    2018-04-01

    The chiral organic-inorganic hybrid materials can exhibit a high loading, and the chiral selector nanoparticles can create efficient stationary phases for open-tubular capillary electrochromatography (OT-CEC). Hence, a novel protocol for the preparation of an OT column coated with nano-amylose-2,3-bis(3,5-dimethylphenylcarbamate) (nano-ABDMPC)-silica hybrid sol through in situ layer-by-layer self-assembly method was developed for CEC enantioseparation. By controlling the assembly cycle number of nano-ABDMPC-silica hybrid sol, a homogeneous, dense and stable coating was successfully prepared, which was confirmed by SEM and elemental analysis. As the main parameter influencing the chiral separating effect, the nano-ABDMPC bearing 3-(triethoxysilyl)propyl residues concentration was investigated. The experimental results showed that 10.0 mg/mL nano-ABDMPC bearing 3-(triethoxysilyl)propyl residues coated OT capillary column possessed chiral recognition ability toward the six enantiomers (phenylalanine, tyrosine, tryptophan, phenethyl alcohol, 1-phenyl-2-propanol, and Tröger's base) at some of the different conditions tested. Additionally, the coated OT column revealed adequate repeatability concerning run-to-run, day-to-day and column-to-column. These results demonstrated the promising applicability of nano-ABDMPC-silica hybrid sol coated OT column in CEC enantioseparations. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. Design Through Simulation of a Molecular Sieve Column for Treatment of MON-3

    NASA Technical Reports Server (NTRS)

    Swartz, A. Ben; Wilson, D. B.

    1999-01-01

    The presence of water in propellant-grade MON-3 is a concern in the Aerospace Industry. NASA Johnson Space Center (JSC), White Sands Test Facility (WSTF) Propulsion Department has evaluated many types of molecular sieves for control of iron, the corrosion product of water in Mixed Oxides of Nitrogen (MON-3). In 1995, WSTF initiated laboratory and pilot-scale testing of molecular sieve type 3A for removal of water and iron. These tests showed sufficient promise that a series of continuous recycle tests were conducted at WSTF. Periodic samples of the circulating MON-3 solution were analyzed for water (wt %) and iron (ppm, wt). This test column was modeled as a series of transfer units; i. e., each unit represented the height equivalent of a theoretical plate. Such a model assumes there is equilibrium between the adsorbent material and the effluent stream from the unit. Operational and design parameters were derived based on the simulation results. These parameters were used to predict the design characteristics of a proposed molecular sieve column for removal of water and iron from MON-3 at the NASA Kennedy Space Center (KSC). In addition, these parameters were used to simulate a small, single-pass operation column at KSC currently used for treating MON-3. The results of this work indicated that molecular sieve type 3A in 1/16 in. diameter pellets, in a column 2.5 ft. in diameter, 18 ft. in height, and operated at 25 gpm is adequate for the required removal of water and iron from MON-3.

  18. Buckling analysis of non-prismatic columns based on modified vibration modes

    NASA Astrophysics Data System (ADS)

    Rahai, A. R.; Kazemi, S.

    2008-10-01

    In this paper, a new procedure is formulated for the buckling analysis of tapered column members. The calculation of the buckling loads was carried out by using modified vibrational mode shape (MVM) and energy method. The change of stiffness within a column is characterized by introducing a tapering index. It is shown that, the changes in the vibrational mode shapes of a tapered column can be represented by considering a linear combination of various modes of uniform-section columns. As a result, by making use of these modified mode shapes (MVM) and applying the principle of stationary total potential energy, the buckling load of tapered columns can be obtained. Several numerical examples on tapered columns demonstrate the accuracy and efficiency of the proposed analytical method.

  19. Distribution-centric 3-parameter thermodynamic models of partition gas chromatography.

    PubMed

    Blumberg, Leonid M

    2017-03-31

    If both parameters (the entropy, ΔS, and the enthalpy, ΔH) of the classic van't Hoff model of dependence of distribution coefficients (K) of analytes on temperature (T) are treated as the temperature-independent constants then the accuracy of the model is known to be insufficient for the needed accuracy of retention time prediction. A more accurate 3-parameter Clarke-Glew model offers a way to treat ΔS and ΔH as functions, ΔS(T) and ΔH(T), of T. A known T-centric construction of these functions is based on relating them to the reference values (ΔS ref and ΔH ref ) corresponding to a predetermined reference temperature (T ref ). Choosing a single T ref for all analytes in a complex sample or in a large database might lead to practically irrelevant values of ΔS ref and ΔH ref for those analytes that have too small or too large retention factors at T ref . Breaking all analytes in several subsets each with its own T ref leads to discontinuities in the analyte parameters. These problems are avoided in the K-centric modeling where ΔS(T) and ΔS(T) and other analyte parameters are described in relation to their values corresponding to a predetermined reference distribution coefficient (K Ref ) - the same for all analytes. In this report, the mathematics of the K-centric modeling are described and the properties of several types of K-centric parameters are discussed. It has been shown that the earlier introduced characteristic parameters of the analyte-column interaction (the characteristic temperature, T char , and the characteristic thermal constant, θ char ) are a special chromatographically convenient case of the K-centric parameters. Transformations of T-centric parameters into K-centric ones and vice-versa as well as the transformations of one set of K-centric parameters into another set and vice-versa are described. Copyright © 2017 Elsevier B.V. All rights reserved.

  20. Analysis of amino acid composition in proteins of animal tissues and foods as pre-column o-phthaldialdehyde derivatives by HPLC with fluorescence detection.

    PubMed

    Dai, Zhaolai; Wu, Zhenlong; Jia, Sichao; Wu, Guoyao

    2014-08-01

    Studies of protein nutrition and biochemistry require reliable methods for analysis of amino acid (AA) composition in polypeptides of animal tissues and foods. Proteins are hydrolyzed by 6M HCl (110°C for 24h), 4.2M NaOH (105°C for 20 h), or proteases. Analytical techniques that require high-performance liquid chromatography (HPLC) include pre-column derivatization with 4-chloro-7-nitrobenzofurazan, 9-fluorenyl methylchloroformate, phenylisothiocyanate, naphthalene-2,3-dicarboxaldehyde, 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate, and o-phthaldialdehyde (OPA). OPA reacts with primary AA (except cysteine or cystine) in the presence of 2-mercaptoethanol or 3-mercaptopropionic acid to form a highly fluorescent adduct. OPA also reacts with 4-amino-1-butanol and 4-aminobutane-1,3-diol produced from oxidation of proline and 4-hydroxyproline, respectively, in the presence of chloramine-T plus sodium borohydride at 60°C, or with S-carboxymethyl-cysteine formed from cysteine and iodoacetic acid at 25°C. Fluorescence of OPA derivatives is monitored at excitation and emission wavelengths of 340 and 455 nm, respectively. Detection limits are 50 fmol for AA. This technique offers the following advantages: simple procedures for preparation of samples, reagents, and mobile-phase solutions; rapid pre-column formation of OPA-AA derivatives and their efficient separation at room temperature (e.g., 20-25°C); high sensitivity of detection; easy automation on the HPLC apparatus; few interfering side reactions; a stable chromatography baseline for accurate integration of peak areas; and rapid regeneration of guard and analytical columns. Thus, the OPA method provides a useful tool to determine AA composition in proteins of animal tissues (e.g., skeletal muscle, liver, intestine, placenta, brain, and body homogenates) and foods (e.g., milk, corn grain, meat, and soybean meal). Copyright © 2014 Elsevier B.V. All rights reserved.

  1. Analysis of underivatised low volatility compounds by comprehensive two-dimensional gas chromatography with a short primary column.

    PubMed

    Novaes, Fábio Junior Moreira; Kulsing, Chadin; Bizzo, Humberto Ribeiro; de Aquino Neto, Francisco Radler; Rezende, Claudia Moraes; Marriott, Philip John

    2018-02-09

    Comprehensive two-dimensional gas chromatography (GC×GC) approaches with cryogenic modulation were developed for the qualitative analysis of selected low volatility compounds in raw coffee bean extracts, without derivatisation. The approaches employed short first ( 1 D) and second ( 2 D) dimension columns, specifically a 1 D 65% phenyl methyl siloxane column (11m) and a 2 D 5% phenyl methyl siloxane column (1m), which allowed elution of high molar mass compounds (e.g.>600Da). Solutes included hydrocarbons, fatty acids, diterpenes, tocopherols, sterols, diterpene esters, and di- and triacylglycerides. An oven temperature program up to 370°C was employed. The effects of experimental conditions were investigated, revealing that the GC×GC results strongly depended on the cryogenic trap T, and oven T program. An appropriate condition was selected and further applied for group type analysis of low volatility compounds in green Arabica coffee beans. Retention indices were compiled for 1D GC analysis and were similar for the composite column data in GC×GC. The elution of some compounds was confirmed by use of authentic standards. The approach allowed direct analysis of coffee extract in ethyl acetate solution, with improved analyte peak capacity (approximately 200 compounds were detected) without prior fractionation or pre-treatment of the sample. This avoided potential hydrolysis of high molar mass conjugate esters as well as degradation of thermally labile compounds such as the derivatives of the diterpenes cafestol and kahweol. Copyright © 2017 Elsevier B.V. All rights reserved.

  2. Non-planar microfabricated gas chromatography column

    DOEpatents

    Lewis, Patrick R.; Wheeler, David R.

    2007-09-25

    A non-planar microfabricated gas chromatography column comprises a planar substrate having a plurality of through holes, a top lid and a bottom lid bonded to opposite surfaces of the planar substrate, and inlet and outlet ports for injection of a sample gas and elution of separated analytes. A plurality of such planar substrates can be aligned and stacked to provide a longer column length having a small footprint. Furthermore, two or more separate channels can enable multi-channel or multi-dimensional gas chromatography. The through holes preferably have a circular cross section and can be coated with a stationary phase material or packed with a porous packing material. Importantly, uniform stationary phase coatings can be obtained and band broadening can be minimized with the circular channels. A heating or cooling element can be disposed on at least one of the lids to enable temperature programming of the column.

  3. Preparation and Characterization of a Polymeric Monolithic Column for Use in High-Performance Liquid Chromatography (HPLC)

    ERIC Educational Resources Information Center

    Bindis, Michael P.; Bretz, Stacey Lowery; Danielson, Neil D.

    2011-01-01

    The high-performance liquid chromatography (HPLC) experiment, most often done in the undergraduate analytical instrumentation laboratory course, generally illustrates reversed-phase chromatography using a commercial C[subscript]18 silica column. To avoid the expense of periodic column replacement and introduce a choice of columns with different…

  4. Rapid, direct determination of polyphenols in tea by reversed-phase column liquid chromatography.

    PubMed

    Ding, M; Yang, H; Xiao, S

    1999-07-23

    Column liquid chromatography on a C18-bonded silica column with water-methanol-acetic acid as eluent was used to determine polyphenols and caffeine in tea. Without any pretreatment, catechin, epicatechin gallate, epigallocatechin gallate, epigallocatechin, epicatechin and caffeine were separated successfully within 15 min. The detection limits (S/N = 3) of polyphenols studied were 1.8-24 mg/l at a detection wavelength 270 nm. The linear range of the peak area calibration curves for the analytes were over two orders of magnitude with a correlation coefficient of 0.996-0.999. Using this method, some Chinese tea samples were analyzed with a good reproducibility (RSD are below 5%).

  5. Automated metal-free multiple-column nanoLC for improved phosphopeptide analysis sensitivity and throughput

    PubMed Central

    Zhao, Rui; Ding, Shi-Jian; Shen, Yufeng; Camp, David G.; Livesay, Eric A.; Udseth, Harold; Smith, Richard D.

    2009-01-01

    We report on the development and characterization of automated metal-free multiple-column nanoLC instrumentation for sensitive and high-throughput analysis of phosphopeptides with mass spectrometry analysis. The system implements a multiple-column capillary LC fluidic design developed for high-throughput analysis of peptides (Anal. Chem. 2001, 73, 3011–3021), incorporating modifications to achieve broad and sensitive analysis of phosphopeptides. The integrated nanoLC columns (50 µm i.d. × 30 cm containing 5 µm C18 particles) and the on-line solid phase extraction columns (150 µm i.d. × 4 cm containing 5 µm C18 particles) were connected to automatic switching valves with non-metal chromatographic accessories, and other modifications to avoid the exposure of the analyte to any metal surfaces during handling, separation, and electrospray ionization. The nanoLC developed provided a separation peak capacity of ∼250 for phosphopeptides (and ∼400 for normal peptides). A detection limit of 0.4 fmol was obtained when a linear ion trap tandem mass spectrometer (Finnegan LTQ) was coupled to a 50-µm i.d. column of the nanoLC. The separation power and sensitivity provided by the nanoLC-LTQ enabled identification of ∼4600 phosphopeptide candidates from ∼60 µg COS-7 cell tryptic digest followed by IMAC enrichment and ∼520 tyrosine phosphopeptides from ∼2 mg of human T cells digests followed by phosphotyrosine peptide immunoprecipitation. PMID:19217835

  6. Determination of alpidem, an imidazopyridine anxiolytic, and its metabolites by column-switching high-performance liquid chromatography with fluorescence detection.

    PubMed

    Flaminio, L; Ripamonti, M; Ascalone, V

    1994-05-13

    Alpidem, 6-chloro-2-(4-chlorophenyl)-N,N-dipropylimidazo[1,2-a]pyridine- 3-acetamide, is an anxiolytic imidazopyridine that undergoes a first-pass elimination after oral administration to humans; it is actively metabolized and three circulating metabolites have been identified in plasma due to N-dealkylation, oxidation or a combination of both processes. For the determination of the unchanged drug and its metabolites in human plasma, a column-switching HPLC method was developed. The method, based on solid-phase extraction (performed on-line), involves the automatic injection of plasma samples (200 microliters) on to a precolumn filled with C18 material, clean-up of the sample with water in order to remove protein and salts and transfer of the analytes to the analytical column (after valve switching) by means of the mobile phase. All the processes were performed in the presence of an internal standard, a compound chemically related to alpidem. During the analytical chromatography, the precolumn was flushed with different solvents and after regeneration with water, it was ready for further injections. The analytical column was a C8 type and the mobile phase was acetonitrile-methanol-phosphate buffer solution (45:15:45, v/v/v) at a flow-rate of 1.5 ml min-1. The column was connected to a fluorimetric detector operating at excitation and emission wavelengths of 255 and 423 nm, respectively. The limits of quantitation of alpidem and three metabolites were 2.5 and 1.5 ng ml-1, respectively, in human plasma.

  7. Separation of cannabinoids on three different mixed-mode columns containing carbon/nanodiamond/amine-polymer superficially porous particles.

    PubMed

    Hung, Chuan-Hsi; Zukowski, Janusz; Jensen, David S; Miles, Andrew J; Sulak, Clayton; Dadson, Andrew E; Linford, Matthew R

    2015-09-01

    Three mixed-mode high-performance liquid chromatography columns packed with superficially porous carbon/nanodiamond/amine-polymer particles were used to separate mixtures of cannabinoids. Columns evaluated included: (i) reversed phase (C18 ), weak anion exchange, 4.6 × 33 mm, 3.6 μm, and 4.6 × 100 mm, 3.6 μm, (ii) reversed phase, strong anion exchange (quaternary amine), 4.6×33 mm, 3.6 μm, and (iii) hydrophilic interaction liquid chromatography, 4.6 × 150 mm, 3.6 μm. Different selectivities were achieved under various mobile phase and stationary phase conditions. Efficiencies and peak capacities were as high as 54 000 N/m and 56, respectively. The reversed phase mixed-mode column (C18 ) retained tetrahydrocannabinolic acid strongly under acidic conditions and weakly under basic conditions. Tetrahydrocannabinolic acid was retained strongly on the reversed phase, strong anion exchange mixed-mode column under basic polar organic mobile phase conditions. The hydrophilic interaction liquid chromatography column retained polar cannabinoids better than the (more) neutral ones under basic conditions. A longer reversed phase (C18 ) mixed-mode column (4.6 × 100 mm) showed better resolution for analytes (and a contaminant) than a shorter column. Fast separations were achieved in less than 5 min and sometimes 2 min. A real world sample (bubble hash extract) was also analyzed by gradient elution. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Lateral column length in adult flatfoot deformity.

    PubMed

    Kang, Steve; Charlton, Timothy P; Thordarson, David B

    2013-03-01

    In adult acquired flatfoot deformity, it is unclear whether the lateral column length shortens with progression of the deformity, whether it is short to begin with, or whether it is short at all. To our knowledge, no previous study has examined the lateral column length of patients with adult acquired flatfoot deformity compared to a control population. The purpose of our study was to compare the lateral column length in patients with and without adult acquired flatfoot deformity to see if there was a significant difference. The study was a retrospective radiographic review of 2 foot and ankle fellowship-trained orthopaedic surgeons' patients with adult flatfoot deformity. Our study population consisted of 75 patients, 85 feet (28 male, 57 female) with adult flatfoot deformity with a mean age of 64 (range, 23-93). Our control population consisted of 57 patients and 70 feet (23 male, 47 female) without flatfoot deformity with a mean age of 61 (range, 40-86 years). Weightbearing anteroposterior (AP) and lateral foot radiographs were analyzed for each patient, and the following measurements were made: medial and lateral column lengths, talonavicular uncoverage angle, talus-first metatarsal angle, calcaneal pitch angle, and medial and lateral column heights. An unpaired t test was used to analyze the measurements between the groups. Ten patients' radiographs were remeasured, and correlation coefficients were obtained to assess the reliability of the measuring techniques. For the flatfoot group, the mean medial and lateral column lengths on the AP radiograph were 108.6 mm and 95.8 mm, respectively; the mean talo-navicular uncoverage angle was 26.2 degrees; and the mean talus-first metatarsal angle was 20.0 degrees. In the control group, the mean medial and lateral column lengths on the AP radiograph were 108.8 mm and 96.5 mm, respectively; the mean talo-navicular uncoverage angle was 8.2 degrees; and the mean talus-first metatarsal angle was 7.7 degrees. On the lateral

  9. Quantification of 3-nitrobenzanthrone-DNA adducts using online column-switching HPLC-electrospray tandem mass spectrometry.

    PubMed

    Gamboa da Costa, Gonçalo; Singh, Rajinder; Arlt, Volker M; Mirza, Amin; Richards, Meirion; Takamura-Enya, Takeji; Schmeiser, Heinz H; Farmer, Peter B; Phillips, David H

    2009-11-01

    The aromatic nitroketone 3-nitrobenzanthrone (3-nitro-7H-benz[de]anthracen-7-one; 3-NBA) is an extremely potent mutagen and a suspected human carcinogen detected in the exhaust of diesel engines and in airborne particulate matter. 3-NBA is metabolically activated via reduction of the nitro group to the hydroxylamine (N-OH-3-ABA) to form covalent DNA adducts. Thus far, the detection and quantification of covalent 3-NBA-DNA adducts has relied solely on (32)P-postlabeling methodologies. In order to expand the range of available techniques for the detection and improved quantification of 3-NBA-DNA adducts, we have developed a method based upon online column-switching HPLC coupled to electrospray tandem mass spectrometry, with isotopic dilution of (15)N-labeled internal standards. This methodology was applied to the determination of three 3-NBA-derived adducts: 2-(2'-deoxyguanosin-N(2)-yl)-3-aminobenzanthrone (dG-N(2)-3-ABA), N-(2'-deoxyguanosin-8-yl)-3-aminobenzanthrone (dG-C8-N-3-ABA) and 2-(2'-deoxyguanosine-8-yl)-3-aminobenzanthrone (dG-C8-C2-3-ABA). Dose-dependent increases were observed for all three adducts when salmon testis DNA was reacted with N-acetoxy-3-aminobenzanthrone (N-AcO-3-ABA). dG-C8-C2-3-ABA was detected at much lower levels (overall 1%) than the other two adducts. DNA samples isolated from tissues of rats treated either intratracheally with 3-NBA or intraperitoneally with N-OH-3-ABA were analyzed by mass spectrometry, and the results compared to those obtained by (32)P-postlabeling. The method required 50 microg of hydrolyzed animal DNA on column and the limit of detection was 2.0 fmol for each adduct. dG-C8-C2-3-ABA was not observed in any of the samples providing confirmation that it is not formed in vivo. Linear regression analysis of the levels of dG-N(2)-3-ABA and dG-C8-N-3-ABA in the rat DNA showed a reasonable correlation between the two methods (R(2) = 0.88 and 0.93, respectively). In summary, the mass spectrometric method is a faster, more

  10. Demonstration of motionless Knudsen pump based micro-gas chromatography featuring micro-fabricated columns and on-column detectors.

    PubMed

    Liu, Jing; Gupta, Naveen K; Wise, Kensall D; Gianchandani, Yogesh B; Fan, Xudong

    2011-10-21

    This paper reports the investigation of a micro-gas chromatography (μGC) system that utilizes an array of miniaturized motionless Knudsen pumps (KPs) as well as microfabricated separation columns and optical detectors. A prototype system was built to achieve a flow rate of 1 mL min(-1) and 0.26 mL min(-1) for helium and dry air, respectively, when they were used as carrier gas. This system was then employed to evaluate GC performance compromises and demonstrate the ability to separate and detect gas mixtures containing analytes of different volatilities and polarities. Furthermore, the use of pressure programming of the KP array was demonstrated to significantly shorten the analysis time while maintaining a high detection resolution. Using this method, we obtained a high resolution detection of 5 alkanes of different volatilities within 5 min. Finally, we successfully detected gas mixtures of various polarities using a tandem-column μGC configuration by installing two on-column optical detectors to obtain complementary chromatograms.

  11. Preparation and evaluation of a novel hybrid monolithic column based on pentafluorobenzyl imidazolium bromide ionic liquid.

    PubMed

    Shan, Yuanhong; Qiao, Lizhen; Shi, Xianzhe; Xu, Guowang

    2015-01-02

    To develop a novel hybrid monolithic column based on pentafluorobenzyl imidazolium bromide ionic liquid, a new ionic liquid monomer was synthesized from 1-vinylimidazole and pentafluorobenzyl bromide. By employing a facile one-step copolymerization of polyhedral-oligomeric-silsesquioxane-type (POSS) cross-linking agent and the home-made ionic liquid monomer, the hybrid monolithic columns were in situ fabricated in fused-silica capillary. The morphology of monolithic column was characterized by scanning electron microscope (SEM) and the chemical composition was confirmed by Fourier-transform infrared spectroscopy (FT-IR) and elemental analysis. Excellent mechanical stability and slight swelling propensity were exhibited which was ascribed to the rigid hybrid monolithic skeleton. Reproducibility results of run-to-run, column-to-column, batch-to-batch and day-to-day were investigated and the RSDs were less than 0.46%, 1.84%, 3.96% and 3.17%, respectively. The mixed-mode retention mechanism with hydrophobic interaction, π-π stacking, ion-exchange, electrostatic interaction and dipole-dipole interaction was explored systematically using analytes with different structure types. Satisfied separation capability and column efficiency were achieved for the analysis of small molecular compounds such as alkylbenzenes, polycyclic aromatic hydrocarbons, nucleosides and halogenated compounds. Copyright © 2014 Elsevier B.V. All rights reserved.

  12. Liquid chromatography determination of 10-hydroxycamptothecin in human serum by a column-switching system containing a pre-column with restricted access media and its application to a clinical pharmacokinetic study.

    PubMed

    Ma, Jun; Jia, Zheng-Ping; Zhang, Qiang; Fan, Jun-Jie; Jiang, Ning-Xi; Wang, Rong; Xie, Hua; Wang, Juan

    2003-10-25

    A simple, rapid, sensitive column-switching HPLC method is described for the analysis of the 10-hydroxycamptothecin (HCPT) in human serum. A pre-column containing restricted access media (RAM) is used for the sample clean-up and trace enrichment and is combined with a C18 column for the final separation. The analytical time is 8 min. The HCPT is monitored with fluorescence detector, excitation and emission wavelengths being 385 and 539 nm, respectively. There is a linear response range of 1-1000 ng/ml with correlation coefficient of 0.998 while the limit of quantification is 0.1 ng/ml. The intra-day and inter-day variations are less than 5%. This analytic procedure has been applied to a pharmacokinetic study of HCPT in clinical patients and the pharmacokinetic parameters of one-compartment model are calculated.

  13. Laboratory-Scale Column Testing Using IONSIV IE-911 for Removing Cesium from Acidic Tank Waste Simulant. 2: Determination of Cesium Exchange Capacity and Effective Mass Transfer Coefficient from a 500-cm3 Column Experiement

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    T.J. Tranter; R.D. Tillotson; T.A. Todd

    2005-04-01

    A semi-scale column test was performed using a commercial form of crystalline silicotitanate (CST) for removing radio-cesium from a surrogate acidic tank solution, which represents liquid waste stored at the Idaho National Engineering and Environmental Laboratory (INEEL). The engineered form of CST ion exchanger, known as IONSIVtmIE-911 (UOP, Mt. Laurel,NJ, USA), was tested in a 500-cm3 column to obtain a cesium breakthrough curve. The cesium exchange capacity of this column matched that obtained from previous testing with a 15-mc3 column. A numerical algorithm using implicit finite difference approximations was developed to solve the governing mass transport equations for the CSTmore » columns. An effective mass transfer coefficient was derived from solving these equations for previously reported 15 cm3 tests. The effective mass transfer coefficient was then used to predict the cesium breakthrough curve for the 500-cm3 column and compared to the experimental data reported in this paper. The calculated breakthrough curve showed excellent agreement with the data from the 500-cm3 column even though the interstitial velocity was a factor of two greater. Thus, this approach should provide a reasonable method for scale up to larger columns for treating actual tank waste.« less

  14. Axisymmetric collapses of granular columns

    NASA Astrophysics Data System (ADS)

    Lube, Gert; Huppert, Herbert E.; Sparks, R. Stephen J.; Hallworth, Mark A.

    2004-06-01

    Experimental observations of the collapse of initially vertical columns of small grains are presented. The experiments were performed mainly with dry grains of salt or sand, with some additional experiments using couscous, sugar or rice. Some of the experimental flows were analysed using high-speed video. There are three different flow regimes, dependent on the value of the aspect ratio a {=} h_i/r_i, where h_i and r_i are the initial height and radius of the granular column respectively. The differing forms of flow behaviour are described for each regime. In all cases a central, conically sided region of angle approximately 59(°) , corresponding to an aspect ratio of 1.7, remains undisturbed throughout the motion. The main experimental results for the final extent of the deposit and the time for emplacement are systematically collapsed in a quantitative way independent of any friction coefficients. Along with the kinematic data for the rate of spread of the front of the collapsing column, this is interpreted as indicating that frictional effects between individual grains in the bulk of the moving flow only play a role in the last instant of the flow, as it comes to an abrupt halt. For a {<} 1.7, the measured final runout radius, r_infty, is related to the initial radius by r_infty {=} r_i(1 {+} 1.24a); while for 1.7 {<} a the corresponding relationship is r_infty {=} r_i(1 {+} 1.6a(1/2) ). The time, t_infty, taken for the grains to reach r_infty is given by t_infty {=} 3(h_i/g)(1/2} {=} 3(r_i/g)({1/2}a^{1/2)) , where g is the gravitational acceleration. The insights and conclusions gained from these experiments can be applied to a wide range of industrial and natural flows of concentrated particles. For example, the observation of the rapid deposition of the grains can help explain details of the emplacement of pyroclastic flows resulting from the explosive eruption of volcanoes.

  15. Preparation and evaluation of open-tubular capillary columns modified with metal-organic framework incorporated polymeric porous layer for liquid chromatography.

    PubMed

    Zhu, Manman; Zhang, Lingyi; Chu, Zhanying; Wang, Shulei; Chen, Kai; Zhang, Weibing; Liu, Fan

    2018-07-01

    An open tubular capillary liquid phase chromatographic column (1 m × 25 µm i.d.× 375 µm o.d.) was prepared by incorporating metal organic framework particles modified with vancomycin directly into zwitterionic polymer coating synthesized by the copolymerization of [2-(methacryloyloxy)ethyl]dimethyl-(3-sulfopropyl) ammonium hydroxide and N,N'-methylenebisacrylamide. The incorporation of IRMOF-3 (isoreticular metal organic framework-3) particles improved selectivity of zwitterionic polymer coating with absolute column efficiency reaching 79900 plates for p-xylene. Besides strong hydrophilic interaction, the separation of neutral, basic, and acidic compounds demonstrates that π-π stacking interaction and the coordination effect of unsaturated Zn 2+ of MOF also contribute to separation of various analytes. The RSD values (run-to-run, day-to-day, column-to-column, n = 3) of retention time of neutral compounds were less than 0.71%, 0.69% and 3.08% respectively, suggesting good repeatability. In addition, the column was applied to the analysis of the trypsin digest of bovine serum albumin, revealing the potential in separating biological samples. Copyright © 2018 Elsevier B.V. All rights reserved.

  16. Changes in Vertebral Column Height (VCH) at Different Distance Intervals During a 3-Mile Walk.

    PubMed

    Roush, J R; Kee, M; Toeppe, J

    2008-08-01

    The purpose of this study was to determine the changes in vertebral column height (VCH) of males and females, at every one-half mile, for a total walking distance of 3 miles. Twenty males and twenty females between the ages of 21 and 40 years walked 3 miles on a treadmill maintaining a walking speed that the subject rated between 12 and 14 on Borg's rate of perceived exertion scale. Blood pressure, heart rate, and VCH measurements were taken initially and at each half-mile interval throughout the three-mile walk. Vertebral column height (VCH) was measured from the spinous process of C7 to S2 using a standard tape measure. Significant differences existed in vertebral column height according to sex (F = 16.18; p < .05) and significant differences in vertebral column height at the different distances (F = 65.02: p < .0001). Significant changes occurred in the VCH between half-mile intervals only between 0.5 miles and 1.0 mile and between 1.0 mile and 1.5 miles during the walk. As found with a regression analysis, curvilinear relationship exists between the distance walked and VCH; with VCH decreasing throughout the distance of the walk. Vertebral column height decreased in a curvilinear relationship throughout the distance of walking 3 miles in both males and females.

  17. Changes in Vertebral Column Height (VCH) at Different Distance Intervals During a 3-Mile Walk

    PubMed Central

    Kee, M; Toeppe, J

    2008-01-01

    Background The purpose of this study was to determine the changes in vertebral column height (VCH) of males and females, at every one-half mile, for a total walking distance of 3 miles. Methods Twenty males and twenty females between the ages of 21 and 40 years walked 3 miles on a treadmill maintaining a walking speed that the subject rated between 12 and 14 on Borg's rate of perceived exertion scale. Blood pressure, heart rate, and VCH measurements were taken initially and at each half-mile interval throughout the three-mile walk. Vertebral column height (VCH) was measured from the spinous process of C7 to S2 using a standard tape measure. Results Significant differences existed in vertebral column height according to sex (F = 16.18; p < .05) and significant differences in vertebral column height at the different distances (F = 65.02: p < .0001). Significant changes occurred in the VCH between half-mile intervals only between 0.5 miles and 1.0 mile and between 1.0 mile and 1.5 miles during the walk. As found with a regression analysis, curvilinear relationship exists between the distance walked and VCH; with VCH decreasing throughout the distance of the walk. Conclusions Vertebral column height decreased in a curvilinear relationship throughout the distance of walking 3 miles in both males and females. PMID:21509126

  18. Oak Ridge Bio-surveillance Toolkit (ORBiT): Integrating Big-Data Analytics with Visual Analysis for Public Health Dynamics

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Ramanathan, Arvind; Pullum, Laura L; Steed, Chad A

    In this position paper, we describe the design and implementation of the Oak Ridge Bio-surveillance Toolkit (ORBiT): a collection of novel statistical and machine learning tools implemented for (1) integrating heterogeneous traditional (e.g. emergency room visits, prescription sales data, etc.) and non-traditional (social media such as Twitter and Instagram) data sources, (2) analyzing large-scale datasets and (3) presenting the results from the analytics as a visual interface for the end-user to interact and provide feedback. We present examples of how ORBiT can be used to summarize ex- tremely large-scale datasets effectively and how user interactions can translate into the datamore » analytics process for bio-surveillance. We also present a strategy to estimate parameters relevant to dis- ease spread models from near real time data feeds and show how these estimates can be integrated with disease spread models for large-scale populations. We conclude with a perspective on how integrating data and visual analytics could lead to better forecasting and prediction of disease spread as well as improved awareness of disease susceptible regions.« less

  19. Preparative liquid column electrophoresis of T and B lymphocytes at gravity = 1

    NASA Technical Reports Server (NTRS)

    Van Oss, C. J.; Bigazzi, P. E.; Gillman, C. F.; Allen, R. E.

    1974-01-01

    Vertical liquid columns containing low-molecular-weight dextran density gradients can be used for preparative lymphocyte electrophoresis on earth, in simulation of zero gravity conditions. Another method that has been tested at 1 g, is the electrophoresis of lymphocytes in an upward direction in vertical columns. By both methods up to 100 million lymphocytes can be separated at one time in a 30-cm glass column of 8-mm inside diameter, at 12 V/cm, in two hours. Due to convection and sedimentation problems, the separation at 1 g is less than ideal, but it is expected that at zero gravity electrophoresis will probe to be a uniquely powerful cell separation tool.

  20. HPLC determination of cefprozil in tablets using monolithic and C18 silica columns.

    PubMed

    Can, Nafiz O

    2011-08-01

    Cefprozil (CPZ) is a second-generation semi-synthetic cephalosporin antibiotic that commonly exists as the mixture of Z and E diastereoisomers, at the ratio of approximately 9:1. A novel reversed-phase HPLC method for the determination of CPZ in tablets was described. The separation of CPZ diastereoisomers and caffeine (internal standard) was carried out by applying the same analytical and instrumental conditions on two stationary phases, which have different surface chemistries. The columns used in the study were monolithic silica Merck Chromolith Performance RP-18e and conventional C18 silica Phenomenex Synergi Hydro RP columns. In total, 10 μL aliquots of samples were injected into the system and eluted using water-acetonitrile (90:10, v/v) solution, which was pumped through the column at a flow rate of 1.0 mL/min. The analyte peaks were detected at 200 nm using diode array detector with high specificity. CPZ diastereoisomers and caffeine were measured within 13 min using the C18 column, whereas <5 min was required for the monolithic one. Validation studies were performed according to official recommendations. Value of a monolithic column for the assay of diastereoisomers in pharmaceutical tablets was evaluated for the first time and found as a powerful alternative to highly efficient C18 columns. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Analytical general solutions for static wormholes in f(R,T) gravity

    NASA Astrophysics Data System (ADS)

    Moraes, P. H. R. S.; Correa, R. A. C.; Lobato, R. V.

    2017-07-01

    Originally proposed as a tool for teaching the general theory of relativity, wormholes are today approached in many different ways and are seeing as an efficient alternative for interstellar and time travel. Attempts to achieve observational signatures of wormholes have been growing as the subject has become more and more popular. In this article we investigate some f(R,T) theoretical predictions for static wormholes, i.e., wormholes whose throat radius can be considered a constant. Since the T-dependence in f(R,T) gravity is due to the consideration of quantum effects, a further investigation of wormholes in such a theory is well motivated. We obtain the energy conditions of static wormholes in f(R,T) gravity and apply an analytical approach to find their physical and geometrical solutions. We highlight that our results are in agreement with previous solutions and assumptions presented in the literature.

  2. Growth and Brilliant Photo-Emission of Crystalline Hexagonal Column of Alq3 Microwires

    PubMed Central

    Kim, Seokho; Kim, Do Hyoung; Choi, Jinho; Lee, Hojin; Kim, Sun-Young; Park, Jung Woon; Park, Dong Hyuk

    2018-01-01

    We report the growth and nanoscale luminescence characteristics of 8-hydroxyquinolinato aluminum (Alq3) with a crystalline hexagonal column morphology. Pristine Alq3 nanoparticles (NPs) were prepared using a conventional reprecipitation method. Crystal hexagonal columns of Alq3 were grown by using a surfactant-assisted self-assembly technique as an adjunct to the aforementioned reprecipitation method. The formation and structural properties of the crystalline and non-crystalline Alq3 NPs were analyzed with scanning electron microscopy and X-ray diffraction. The nanoscale photoluminescence (PL) characteristics and the luminescence color of the Alq3 single NPs and their crystal microwires (MWs) were evaluated from color charge-coupled device images acquired using a high-resolution laser confocal microscope. In comparison with the Alq3 NPs, the crystalline MWs exhibited a very bright and sharp emission. This enhanced and sharp emission from the crystalline Alq3 single MWs originated from effective π-π stacking of the Alq3 molecules due to strong interactions in the crystalline structure. PMID:29565306

  3. Determination of 3-hydroxypropylmercapturic acid in urine by three column-switching high-performance liquid chromatography with electrochemical detection using a diamond electrode.

    PubMed

    Higashi, Kyohei; Shibasaki, Mana; Kuni, Kyoshiro; Uemura, Takeshi; Waragai, Masaaki; Uemura, Kenichi; Igarashi, Kazuei; Toida, Toshihiko

    2017-09-29

    A three column-switching high-performance liquid chromatography (HPLC) using an electrochemical detector (ECD) equipped with a diamond electrode was established to determine 3-hydroxypropylmercapturic acid (3-HPMA) in urine. An extracted urine sample was consecutively fractionated using a strong anion-exchange column (first column) and a C8 column (second column) via a switching valve before application on an Octa Decyl Silyl (ODS) column (third column), followed by ECD analysis. The% recovery of 3-HPMA standard throughout the three-column process and limit of detection (LOD) were 94±1% and 0.1pmol, respectively. A solid phase extraction step is required for the sensitive analysis of 3-HPMA in urine by column-switching HPLC-ECD despite a decreased% recovery (55%) of urine sample spiked with 100pmol of 3-HPMA. To test the utility of our column-switching HPLC-ECD method, 3-HPMA levels of 27 urine samples were determined, and the correlation between HPLC-ECD and LC-Electrospray ionization (ESI)-MS/MS method was examined. As a result, the median values of μmol 3-HPMA/g Creatinine (Cre) in urine obtained by column-switching HPLC-ECD and LC-MS/MS were 2.19±2.12μmol/g Cre and 2.13±3.38μmol/g Cre, respectively, and the calibration curve (y=1.5171x-1.007) exhibited good linearity within a defined range (r 2 =0.907). These results indicate that the combination of column-switching HPLC and ECD is a powerful tool for the specific, reliable detection of 3-HPMA in urine. Copyright © 2017 Elsevier B.V. All rights reserved.

  4. Simultaneous determination of nandrolone, testosterone, and methyltestosterone by multi-immunoaffinity column and capillary electrophoresis.

    PubMed

    Qi, Xiao-Hua; Zhang, Li-Wei; Zhang, Xin-Xiang

    2008-08-01

    A multitarget antibody immunoaffinity column was proposed for the purification and enrichment of nandrolone, testosterone, and methyltestosterone from urine. Nandrolone-3-site substituted antigen was designed and synthesized and the polyclonal antibody was prepared with immunizing rabbits. The stationary phase of the immunoaffinity column was synthesized by covalently bonding the antibodies specific to nandrolone, testosterone, and methyltestosterone onto CNBr-actived Sepharose 4B. The analytes of interest were extracted with a methanol/water mixture in one step. The immunoaffinity column showed high affinity and high selectivity to a class of structurally related compounds. The elution was then transferred to a micellar electrokinetic CE system with a running buffer of sodium borate and sodium cholate for separation and determination. Recoveries of the three steroids from complex matrix were 88-94% with RSD values less than 5.2%. Optimization of the immunoaffinity column purification was achieved and the feasibility of the technique for the analysis of steroid hormone was discussed. The results indicated that the combination of multi-immunoaffinity column and CE was an effective technique, which was rapid, simple, and sensitive for the assay of steroids.

  5. Mechanisms for Development and Function of Foxp3+ Regulatory T Cells

    DTIC Science & Technology

    2008-04-04

    of the immunological synapse (studies by our group - Thomas et al, 2003); Cholesterol 9 synthesis and thereby the cholesterol amount in CD4 T-cells...precursor of cholesterol synthesis (studies by our group - Brumeanu et al, 2007). At present, it is generally accepted that lipid rafts play a...mice induces a fulminate diabetes within 10-14 days. T-regs and diabetogenic T-cells were isolated on CD4 columns followed by CD25 Ab-magnetic

  6. Simultaneous determination of byak-angelicin and oxypeucedanin hydrate in rat plasma by column-switching high-performance liquid chromatography with ultraviolet detection.

    PubMed

    Ishihara, K; Fukutake, M; Asano, T; Mizuhara, Y; Wakui, Y; Yanagisawa, T; Kamei, H; Ohmori, S; Kitada, M

    2001-04-05

    A simple and sensitive column-switching HPLC method was developed for the simultaneous determination of two furocoumarin compounds, byak-angelicin and oxypeucedanin hydrate, which are the main components of hot water extract of Angelica dahurica root (AE), in rat plasma. Plasma sample was simply deproteinated with perchloric acid. After centrifugation, the supernatant was injected into a column-switching HPLC system consisting of a clean-up column (Symmetry Shield RP 8, 20x3.9 mm I.D.) and analytical column (Symmetry C18, 75x4.6 mm I.D.) which were connected with a six-port switching valve. The flow-rate of the mobile phase (acetonitrile-water, 20:80) was maintained at 1 ml/min. Detection was carried out at wavelength 260 nm with a UV detector. The column temperature was maintained at 40 degrees C. The calibration curves of byak-angelicin and oxypeucedanin hydrate were linear over the ranges 19.6 to 980 ng/ml (r2>0.997). The accuracy of these analytes was less than 4.4%. The intra- and inter-day relative standard deviations of byak-angelicin and oxypeucedanin hydrate were within 12.0% and 12.7%, respectively. The present method was applied for the analysis of plasma concentration from rats after administration of AE.

  7. [Rapid determination of trace iodate using monolithic column ion-pair chromatography coupled with direct conductivity detection].

    PubMed

    Liu, Yuzhen; Yu, Hong; Li, Siwen

    2011-10-01

    A method was developed on a monolithic column for the fast determination of trace iodate (IO(3)- ) by ion-pair chromatography with direct conductivity detection. The analytes were separated using a mobile phase of tetrabutylammonium hydroxide (TBA)-phthalic acid-acetonitrile on a reversed-phase silica-based monolithic column. The effects of eluent, flow rate and column temperature on the retention of iodate were investigated. The optimized chromatographic conditions for the determination of the anion were as follows: 0. 25 mmol/L TBA-0. 18 mmol/L phthalic acid-3% acetonitrile (pH 5.5) as mobile phase, a flow rate of 4.0 mL/min and a column temperature of 30 degrees C. Under the optimal conditions, retention time of iodate was less than 0. 5 min and the baseline separation of iodate was achieved without any interference by other anions (Cl-, NO , SO4(2)-, I- ). The detection limit (S/N= 3) was 0.36 mg/L for IO(3)- . Relative standard deviation (RSD, n = 5) of chromatographic peak area and retention time were 0. 35% and 0. 28%, respectively. The proposed method was applied to the determination of trace iodate in iodized medicine. The spiked recovery of iodate was 96. 4%. The method is rapid, simple, accurate, reliable, and practical.

  8. On the Origin of the High Column Density Turnover in the HI Column Density Distribution

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Erkal, Denis; Gnedin, Nickolay Y.; Kravtsov, Andrey V.

    We study the high column density regime of the HI column density distribution function and argue that there are two distinct features: a turnover at NHI ~ 10^21 cm^-2 which is present at both z=0 and z ~ 3, and a lack of systems above NHI ~ 10^22 cm^-2 at z=0. Using observations of the column density distribution, we argue that the HI-H2 transition does not cause the turnover at NHI ~ 10^21 cm^-2, but can plausibly explain the turnover at NHI > 10^22 cm^-2. We compute the HI column density distribution of individual galaxies in the THINGS sample andmore » show that the turnover column density depends only weakly on metallicity. Furthermore, we show that the column density distribution of galaxies, corrected for inclination, is insensitive to the resolution of the HI map or to averaging in radial shells. Our results indicate that the similarity of HI column density distributions at z=3 and z=0 is due to the similarity of the maximum HI surface densities of high-z and low-z disks, set presumably by universal processes that shape properties of the gaseous disks of galaxies. Using fully cosmological simulations, we explore other candidate physical mechanisms that could produce a turnover in the column density distribution. We show that while turbulence within GMCs cannot affect the DLA column density distribution, stellar feedback can affect it significantly if the feedback is sufficiently effective in removing gas from the central 2-3 kpc of high-redshift galaxies. Finally, we argue that it is meaningful to compare column densities averaged over ~ kpc scales with those estimated from quasar spectra which probe sub-pc scales due to the steep power spectrum of HI column density fluctuations observed in nearby galaxies.« less

  9. The three-dimensional model for helical columns on type-J synchronous counter-current chromatography.

    PubMed

    Guan, Y H; van den Heuvel, Remco

    2011-08-05

    Unlike the existing 2-D pseudo-ring model for helical columns undergoing synchronous type-J planetary motion of counter-current chromatograph (CCC), the 3-D "helix" model developed in this work shows that there is a second normal force (i.e. the binormal force) applied virtually in the axial direction of the helical column. This force alternates in the two opposite directions and intensifies phase mixing with increasing the helix angle. On the contrary, the 2-D spiral column operated on the same CCC device lacks this third-dimensional mixing force. The (principal) normal force quantified by this "helix" model has been the same as that by the pseudo-ring model. With β>0.25, this normal centrifugal force has been one-directional and fluctuates cyclically. Different to the spiral column, this "helix" model shows that the centrifugal force (i.e. the hydrostatic force) does not contribute to stationary phase retention in the helical column. Between the popular helical columns and the emerging spiral columns for type-J synchronous CCC, this work has thus illustrated that the former is associated with better phase mixing yet poor retention for the stationary phase whereas the latter has potential for better retention for the stationary phase yet poor phase mixing. The methodology developed in this work may be regarded as a new platform for designing optimised CCC columns for analytical and engineering applications. Copyright © 2011 Elsevier B.V. All rights reserved.

  10. Analytical general solutions for static wormholes in f ( R , T ) gravity

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Moraes, P.H.R.S.; Correa, R.A.C.; Lobato, R.V., E-mail: moraes.phrs@gmail.com, E-mail: fis04132@gmail.com, E-mail: ronaldo.lobato@icranet.org

    Originally proposed as a tool for teaching the general theory of relativity, wormholes are today approached in many different ways and are seeing as an efficient alternative for interstellar and time travel. Attempts to achieve observational signatures of wormholes have been growing as the subject has become more and more popular. In this article we investigate some f ( R , T ) theoretical predictions for static wormholes, i.e., wormholes whose throat radius can be considered a constant. Since the T -dependence in f ( R , T ) gravity is due to the consideration of quantum effects, a furthermore » investigation of wormholes in such a theory is well motivated. We obtain the energy conditions of static wormholes in f ( R , T ) gravity and apply an analytical approach to find their physical and geometrical solutions. We highlight that our results are in agreement with previous solutions and assumptions presented in the literature.« less

  11. The application of multiple analyte adduct formation in the LC-MS3 analysis of valproic acid in human serum.

    PubMed

    Dziadosz, Marek

    2017-01-01

    LC-MS using electrospray ionisation (negative ion mode) and low-energy collision-induced dissociation tandem mass spectrometric (CID-MS/MS) analysis, together with the multiple analyte adduct formation with the components of the mobile phase, were applied to analyse valproic acid in human serum with LC-MS 3 . The CID-fragmentation of the precursor analyte adduct [M+2CH 3 COONa-H] - was applied in the method validation (307.1/225.1/143.0). Chromatographic separation was performed with a Luna 5μm C18 (2) 100A, 150mm×2mm column and the elution with a mobile phase consisting of A (H 2 O/methanol=95/5, v/v) and B (H 2 O/methanol=3/97, v/v), both with 10mM ammonium acetate and 0.1% acetic acid. A binary flow pumping mode with a total flow rate of 0.400mL/min was used. The calculated limit of detection/quantification of the method calibrated in the range of 10-200μg/mL was 0.31/1.0μg/mL. The sample preparation based on protein precipitation with 1mL of H 2 O/methanol solution (3/97, v/v) with 10mM sodium acetate and 100mM acetic acid. On the basis of the experiments performed could be demonstrated, that multiple analyte adduct formation can be applied to generate MS 3 quantitation of analytes with problematic fragmentation. The presented new strategy makes the analysis of small drugs, which do not produce any stable product ions at all, on the basis of LC-MS 3 possible. Copyright © 2016 Elsevier B.V. All rights reserved.

  12. Analytical interference of 4-hydroxy-3-methoxymethamphetamine with the measurement of plasma free normetanephrine by ultra-high pressure liquid chromatography-tandem mass spectrometry.

    PubMed

    Dunand, Marielle; Donzelli, Massimiliano; Rickli, Anna; Hysek, Cédric M; Liechti, Matthias E; Grouzmann, Eric

    2014-08-01

    The diagnosis of pheochromocytoma relies on the measurement of plasma free metanephrines assay whose reliability has been considerably improved by ultra-high pressure liquid chromatography tandem mass spectrometry (UHPLC-MS/MS). Here we report an analytical interference occurring between 4-hydroxy-3-methoxymethamphetamine (HMMA), a metabolite of 3,4-methylenedioxymethamphetamine (MDMA, "Ecstasy"), and normetanephrine (NMN) since they share a common pharmacophore resulting in the same product ion after fragmentation. Synthetic HMMA was spiked into plasma samples containing various concentrations of NMN and the intensity of the interference was determined by UPLC-MS/MS before and after improvement of the analytical method. Using a careful adjustment of chromatographic conditions including the change of the UPLC analytical column, we were able to distinguish both compounds. HMMA interference for NMN determination should be seriously considered since MDMA activates the sympathetic nervous system and if confounded with NMN may lead to false-positive tests when performing a differential diagnostic of pheochromocytoma. Copyright © 2014 The Canadian Society of Clinical Chemists. Published by Elsevier Inc. All rights reserved.

  13. Kinetic investigation of narrow-bore columns packed with prototype sub-2 μm superficially porous particles with various shell thickness.

    PubMed

    Gritti, Fabrice; Omamogho, Jesse; Guiochon, Georges

    2011-10-07

    The recent successful breakthrough of sub-3 μm shell particles in HPLC has triggered considerable research efforts toward the design of new brands of core-shell particles. We investigated the mass transfer mechanism of a few analytes in narrow-bore columns packed with prototype 1.7 μm shell particles, made of 1.0, 1.2, and 1.4 μm solid nonporous cores surrounded by porous shells 350, 250, and 150 nm thick, respectively. Three probe solutes, uracil, naphthalene, and insulin, were chosen to assess the kinetic performance of these columns. Inverse size exclusion chromatography, peak parking experiments, and the numerical integration of the experimental peak profiles were carried out in order to measure the external, internal, and total column porosities, the true bulk diffusion coefficients of these analytes, the height equivalent to a theoretical plate, the longitudinal diffusion term, and the trans-particle mass transfer resistance term. The residual eddy diffusion term was measured by difference. The results show the existence of important trans-column velocity biases (7%) possibly due to the presence of particle multiplets in the slurry mixture used during the packing process. Our results illustrates some of the difficulties encountered by scientists preparing and packing shell particles into narrow-bore columns. Copyright © 2011 Elsevier B.V. All rights reserved.

  14. The impact of column connection on band broadening in very high pressure liquid chromatography.

    PubMed

    Stankovich, Joseph J; Gritti, Fabrice; Stevenson, Paul G; Guiochon, Georges

    2013-09-01

    A series of experiments was conducted to evaluate the degree of band broadening in very high pressure LC due to column connections. Different column manufacturers use slightly different designs for their column fittings. If the same column connections are repeatedly used to attach columns of different origins, different void volumes form between capillary tubes and column inlets. An Agilent Ultra Low Dispersion Kit (tubing id 75 μm) was installed on an Agilent Infinity 1290 ultra HPLC and used to connect successively an Agilent, a Phenomenex, and a Waters column. A series of uracil (unretained) samples were injected and eluted at a wide range of flow rates with a water/acetonitrile mixture as eluent. In order to determine the variance contribution from column connections as accurately as possible a nonretained probe compound was selected because the variance contribution from the column is the smallest for analytes, which have very low k values. Yet, this effect still has an impact on the resolution for moderately retained compounds (k > 2) for narrow-bore columns packed with fine particles, since variance contributions are additive for linear chromatographic systems. Each injection was replicated five times under the same experimental conditions. Then NanoViper column connections (tubing id 75 μm) were used and the same injections were made. This system was designed to minimize connection void volumes for any column. Band variances were calculated as the second central moment of elution peaks and used to assess the degree of band broadening due to the column connections. Band broadening may increase from 3.8 to 53.9% when conventional metal ferrules were used to join columns to connection sites. The results show that the variance contribution from improper connections can generate as much as 60.5% of the total variance observed. This demonstrates that column connections can play a larger role than the column packing with respect to band dispersion. © 2013 WILEY

  15. [Examples for using capillary gas chromatography with wide bore columns in occupational health].

    PubMed

    Frank, H; Senf, L; Welsch, T

    1990-12-01

    Wide bore capillary columns (0.4-0.75 mm ID) can be easily and inexpensively installed in packed column GCs. The analytical advantages cause an expanding market for such capillaries and interconverting hardware kits. It is illustrated with some examples that often individual exposition levels can be determined exactly only by using capillary columns: ethylbenzene may be separated from the C8-isomers also in complex mixtures, the marker PBN for rubber smoke expositions can be determined with 30 min sampling time, the detection sensitivity of the FID is sufficient also for chlorinated pesticides and the analyses of high-boiling compounds profit by the high phase ratio of wide bore capillary columns. A single capillary column substitutes a variety of different packed columns, so saving time and money and protecting the analyst from failures and frustrating compromises.

  16. IoT Big-Data Centred Knowledge Granule Analytic and Cluster Framework for BI Applications: A Case Base Analysis.

    PubMed

    Chang, Hsien-Tsung; Mishra, Nilamadhab; Lin, Chung-Chih

    2015-01-01

    The current rapid growth of Internet of Things (IoT) in various commercial and non-commercial sectors has led to the deposition of large-scale IoT data, of which the time-critical analytic and clustering of knowledge granules represent highly thought-provoking application possibilities. The objective of the present work is to inspect the structural analysis and clustering of complex knowledge granules in an IoT big-data environment. In this work, we propose a knowledge granule analytic and clustering (KGAC) framework that explores and assembles knowledge granules from IoT big-data arrays for a business intelligence (BI) application. Our work implements neuro-fuzzy analytic architecture rather than a standard fuzzified approach to discover the complex knowledge granules. Furthermore, we implement an enhanced knowledge granule clustering (e-KGC) mechanism that is more elastic than previous techniques when assembling the tactical and explicit complex knowledge granules from IoT big-data arrays. The analysis and discussion presented here show that the proposed framework and mechanism can be implemented to extract knowledge granules from an IoT big-data array in such a way as to present knowledge of strategic value to executives and enable knowledge users to perform further BI actions.

  17. IoT Big-Data Centred Knowledge Granule Analytic and Cluster Framework for BI Applications: A Case Base Analysis

    PubMed Central

    Chang, Hsien-Tsung; Mishra, Nilamadhab; Lin, Chung-Chih

    2015-01-01

    The current rapid growth of Internet of Things (IoT) in various commercial and non-commercial sectors has led to the deposition of large-scale IoT data, of which the time-critical analytic and clustering of knowledge granules represent highly thought-provoking application possibilities. The objective of the present work is to inspect the structural analysis and clustering of complex knowledge granules in an IoT big-data environment. In this work, we propose a knowledge granule analytic and clustering (KGAC) framework that explores and assembles knowledge granules from IoT big-data arrays for a business intelligence (BI) application. Our work implements neuro-fuzzy analytic architecture rather than a standard fuzzified approach to discover the complex knowledge granules. Furthermore, we implement an enhanced knowledge granule clustering (e-KGC) mechanism that is more elastic than previous techniques when assembling the tactical and explicit complex knowledge granules from IoT big-data arrays. The analysis and discussion presented here show that the proposed framework and mechanism can be implemented to extract knowledge granules from an IoT big-data array in such a way as to present knowledge of strategic value to executives and enable knowledge users to perform further BI actions. PMID:26600156

  18. Particle size distribution and column efficiency. An ongoing debate revived with 1.9μm Titan-C18 particles.

    PubMed

    Gritti, Fabrice; Bell, David S; Guiochon, Georges

    2014-08-15

    The mass transfer mechanism in four prototype columns (2.1 and 3.0×50mm, 2.1 and 3.0×100mm) packed with 1.9μm fully porous Titan-C18 particles was investigated by using two previously reported home-made protocols. The first one was used to measure the eddy dispersion HETP of these new columns, the second one to estimate their intrinsic (corrected for HPLC system contribution) HETPs. Titan particles are fully porous particles with a narrow particle size distribution (RSD of 9.2%). The mean Sauter diameter (dSauter=2.04μm) was determined from Coulter counter measurements on the raw silica material (before C18 derivatization) and in the absence of a dispersant agent (Triton X-100) in a 2% NaCl electrolyte solution. The results show that these RPLC Titan columns have intrinsic minimum reduced HETPs ranging from 1.7 to 1.9 and generate up to 290,000 plates per meter. The 3.0mm i.d. columns are more efficient than the 2.1mm i.d. ones and short columns are preferred to minimize efficiency losses due to frictional heating at high speeds. This work also revealed that (1) the lowest h values of the Titan columns are observed at low reduced velocities (νopt=5); (2) this is due to the unusually small diffusivity of analytes across the porous Titan-C18 particles; and (3) the Titan columns are not packed more uniformly than conventional columns packed with fully porous particles. Earlier and recent findings showing that the PSD has no direct physical impact on eddy dispersion and column efficiency are confirmed by these results. Copyright © 2014 Elsevier B.V. All rights reserved.

  19. Optimization of post-column reactor radius in capillary high performance liquid chromatography Effect of chromatographic column diameter and particle diameter

    PubMed Central

    Xu, Hongjuan; Weber, Stephen G.

    2006-01-01

    A post-column reactor consisting of a simple open tube (Capillary Taylor Reactor) affects the performance of a capillary LC in two ways: stealing pressure from the column and adding band spreading. The former is a problem for very small radius reactors, while the latter shows itself for large reactor diameters. We derived an equation that defines the observed number of theoretical plates (Nobs) taking into account the two effects stated above. Making some assumptions and asserting certain conditions led to a final equation with a limited number of variables, namely chromatographic column radius, reactor radius and chromatographic particle diameter. The assumptions and conditions are that the van Deemter equation applies, the mass transfer limitation is for intraparticle diffusion in spherical particles, the velocity is at the optimum, the analyte’s retention factor, k′, is zero, the post-column reactor is only long enough to allow complete mixing of reagents and analytes and the maximum operating pressure of the pumping system is used. Optimal ranges of the reactor radius (ar) are obtained by comparing the number of observed theoretical plates (and theoretical plates per time) with and without a reactor. Results show that the acceptable reactor radii depend on column diameter, particle diameter, and maximum available pressure. Optimal ranges of ar become narrower as column diameter increases, particle diameter decreases or the maximum pressure is decreased. When the available pressure is 4000 psi, a Capillary Taylor Reactor with 12 μm radius is suitable for all columns smaller than 150 μm (radius) packed with 2–5 μm particles. For 1 μm packing particles, only columns smaller than 42.5 μm (radius) can be used and the reactor radius needs to be 5 μm. PMID:16494886

  20. HPLC column-switching technique for sample preparation and fluorescence determination of propranolol in urine using fused-core columns in both dimensions.

    PubMed

    Satínský, Dalibor; Havlíková, Lucie; Solich, Petr

    2013-08-01

    A new and fast high-performance liquid chromatography (HPLC) column-switching method using fused-core columns in both dimensions for sample preconcentration and determination of propranolol in human urine has been developed. On-line sample pretreatment and propranolol preconcentration were performed on an Ascentis Express RP-C-18 guard column (5 × 4.6 mm), particle size, 2.7 μm, with mobile phase acetonitrile/water (5:95, v/v) at a flow rate of 2.0 mL min(-1) and at a temperature of 50 °C. Valve switch from pretreatment column to analytical column was set at 4.0 min in a back-flush mode. Separation of propranolol from other endogenous urine compounds was achieved on the fused-core column Ascentis Express RP-Amide (100 × 4.6 mm), particle size, 2.7 μm, with mobile phase acetonitrile/water solution of 0.5% triethylamine, pH adjusted to 4.5 by means of glacial acetic acid (25:75, v/v), at a flow rate of 1.0 mL min(-1) and at a temperature of 50 °C. Fluorescence excitation/emission detection wavelengths were set at 229/338 nm. A volume of 1,500 μL of filtered urine sample solution was injected directly into the column-switching HPLC system. The total analysis time including on-line sample pretreatment was less than 8 min. The experimentally determined limit of detection of the method was found to be 0.015 ng mL(-1).

  1. SPEEDUP{trademark} ion exchange column model

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Hang, T.

    2000-03-06

    A transient model to describe the process of loading a solute onto the granular fixed bed in an ion exchange (IX) column has been developed using the SpeedUp{trademark} software package. SpeedUp offers the advantage of smooth integration into other existing SpeedUp flowsheet models. The mathematical algorithm of a porous particle diffusion model was adopted to account for convection, axial dispersion, film mass transfer, and pore diffusion. The method of orthogonal collocation on finite elements was employed to solve the governing transport equations. The model allows the use of a non-linear Langmuir isotherm based on an effective binary ionic exchange process.more » The SpeedUp column model was tested by comparing to the analytical solutions of three transport problems from the ion exchange literature. In addition, a sample calculation of a train of three crystalline silicotitanate (CST) IX columns in series was made using both the SpeedUp model and Purdue University's VERSE-LC code. All test cases showed excellent agreement between the SpeedUp model results and the test data. The model can be readily used for SuperLig{trademark} ion exchange resins, once the experimental data are complete.« less

  2. On N. Park's Analytical solution for steady state density- and mixing regime—dependent solute transport in a vertical soil column

    NASA Astrophysics Data System (ADS)

    Thiele, Michael

    1998-04-01

    Recently, Park [1996] presented an analytical solution for stationary one-dimensional solute transport in a variable-density fluid flow through a vertical soil column. He used the widespread Bear-Scheidegger dispersion model describing solute mixing as a sum of molecular diffusion and velocity-proportional mechanical dispersion effects. His closed-form implicit concentration and pressure distributions thus allow for a discussion of the combined impact of molecular diffusion and mechanical dispersion in a variable-density environment. Whereas Park only considered the example of vanishing molecular diffusion in detail, both phenomena are taken into account simultaneously in the present study in order to elucidate their different influences on concentration distribution characteristics. The boundary value problem dealt with herein is based on an upward inflow of high-density fluid of constant solute concentration and corresponding outflow of a lower constant concentration fluid at the upper end of the column when dispersivity does not change along the flow path. The thickness of the transition zone between the two fluids appeared to strongly depend on the prevailing share of the molecular diffusion and mechanical dispersion mechanisms. The latter can be characterized by a molecular Peclet number Pe, which here is defined as the ratio of the column outflow velocity multiplied by a characteristic pore size and the molecular diffusion coefficient. For very small values of Pe, when molecular diffusion represents the exclusive mixing process, density differences have no impact on transition zone thicknesses. A relative density-;dependent thickness increases with flow velocities (increasing Pe values) very rapidly compared to the density-independent case, and after having passed a maximum decreases asymptotically to a constant value for the large Peclet number limit when mechanical dispersion is the only mixing mechanism. Hence the special transport problem analyzed gives

  3. Enantiomeric resolution of five chiral pesticides on a Chiralpak IB-H column by SFC.

    PubMed

    Jin, Lixia; Gao, Weiliang; Yang, Huayun; Lin, Chunmian; Liu, Weiping

    2011-10-01

    The enantiomeric separations of five chiral pesticides, diclofopmethyl, 1; benalaxy, 2; acetofenate, 3; myclobutanil, 4; and difenoconazole, 5, were conducted on a Chiralpak IB-H column by a packed-column supercritical fluid chromatography (p-SFC). All compounds, except difenoconazole and myclobutanil, were well resolved within 10 min. As the mobile phase polarity decreased through changing the percentage and the type of alcohol modifiers in the supercritical carbon dioxide (CO(2)), the retention time, the separation factors, and the resolution increased. However, based on the retention time and the resolution, the optimized separations were obtained with the mobile phase containing 10% 2-propanol for diclofop-methyl 1; benalaxy, 2; myclobutanil, 4; difenoconazole, 5; and containing 3% 2-propanol for acetofenate, 3. The optimized separation temperature was at 35°C under the supercritical fluid condition. The π-π interactions and the hydrogen bonding interactions between Chiralpak IB-H CSP and the analytes might be the main chiral discriminations on enantioseparation of these five pesticides.

  4. Simultaneous determination of 3-monochloropropane-1,2-diol and acrylamide in food by gas chromatography-triple quadrupole mass spectrometry with coupled column separation.

    PubMed

    Xu, Xiao-min; He, Hua-li; Zhu, Yan; Feng, Liang; Ying, Ying; Huang, Bai-fen; Shen, Hai-tao; Han, Jian-long; Ren, Yi-ping

    2013-01-14

    Both 3-monochloropropane-1,2-diol (3-MCPD) and acrylamide are contaminants found in heat-processed foods and their related products. A quantitative method was developed for the simultaneous determination of both contaminants in food by gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS). The analytes were purified and extracted by the matrix solid-phase dispersion extraction (MSPDE) technique with Extrelut NT. A coupled column (a 3 m Innowax combined with a 30 m DB-5 ms) was developed to separate both compounds efficiently without derivatization. Triple quadrupole mass spectrometry in multiple reaction monitoring mode (MRM) was applied to suppress matrix interference and obtain good sensitivity in the determination of both analytes. The limit of detection (LOD) in the sample matrix was 5 μg kg(-1) for 3-MCPD or acrylamide. The average recoveries for 3-MCPD and acrylamide in different food matrices were 90.5-107% and 81.9-95.7%, respectively, with the intraday relative standard deviations (RSDs) of 5.6-13.5% and 5.3-13.4%, respectively. The interday RSDs were 6.1-12.6% for 3-MCPD and were 5.0-12.8% for acrylamide. Both contaminants were found in samples of bread, fried chips, fried instant noodles, soy sauce, and instant noodle flavoring. Neither 3-MCPD nor acrylamide was detected in the samples of dairy products (solid or liquid samples) and non-fried instant noodles. Copyright © 2012 Elsevier B.V. All rights reserved.

  5. Evaluation of chromatographic columns packed with semi- and fully porous particles for benzimidazoles separation.

    PubMed

    Gonzalo-Lumbreras, Raquel; Sanz-Landaluze, Jon; Cámara, Carmen

    2015-07-01

    The behavior of 15 benzimidazoles, including their main metabolites, using several C18 columns with standard or narrow-bore diameters and different particle size and type were evaluated. These commercial columns were selected because their differences could affect separation of benzimidazoles, and so they can be used as alternative columns. A simple screening method for the analysis of benzimidazole residues and their main metabolites was developed. First, the separation of benzimidazoles was optimized using a Kinetex C18 column; later, analytical performances of other columns using the above optimized conditions were compared and then individually re-optimized. Critical pairs resolution, analysis run time, column type and characteristics, and selectivity were considered for chromatographic columns comparison. Kinetex XB was selected because it provides the shortest analysis time and the best resolution of critical pairs. Using this column, the separation conditions were re-optimized using a factorial design. Separations obtained with the different columns tested can be applied to the analysis of specific benzimidazoles residues or other applications. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. The cat vertebral column: stance configuration and range of motion

    NASA Technical Reports Server (NTRS)

    Macpherson, J. M.; Ye, Y.; Peterson, B. W. (Principal Investigator)

    1998-01-01

    This study examined the configuration of the vertebral column of the cat during independent stance and in various flexed positions. The range of motion in the sagittal plane is similar across most thoracic and lumbar joints, with the exception of a lesser range at the transition region from thoracic-type to lumbar-type vertebrae. The upper thoracic column exhibits most of its range in dorsiflexion and the lower thoracic and lumbar in ventroflexion. Lateral flexion is limited to less than 5 degrees at all segments. The range in torsion is almost 180 degrees and occurs primarily in the midthoracic region, T4-T11. Contrary to the depiction in most atlases, the standing cat exhibits several curvatures, including a mild dorsiflexion in the lower lumbar segments, a marked ventroflexion in the lower thoracic and upper lumbar segments, and a profound dorsiflexion in the upper thoracic (above T9) and cervical segments. The curvatures are not significantly changed by altering stance distance but are affected by head posture. During stance, the top of the scapula lies well above the spines of the thoracic vertebrae, and the glenohumeral joint is just below the bodies of vertebrae T3-T5. Using a simple static model of the vertebral column in the sagittal plane, it was estimated that the bending moment due to gravity is bimodal with a dorsiflexion moment in the lower thoracic and lumbar region and a ventroflexion moment in the upper thoracic and cervical region. Given the bending moments and the position of the scapula during stance, it is proposed that two groups of scapular muscles provide the major antigravity support for the head and anterior trunk. Levator scapulae and serratus ventralis form the lateral group, inserting on the lateral processes of cervical vertebrae and on the ribs. The major and minor rhomboids form the medial group, inserting on the spinous tips of vertebrae from C4 to T4. It is also proposed that the hypaxial muscles, psoas major, minor, and quadratus

  7. Automation of nanoflow liquid chromatography-tandem mass spectrometry for proteome analysis by using a strong cation exchange trap column.

    PubMed

    Jiang, Xiaogang; Feng, Shun; Tian, Ruijun; Han, Guanghui; Jiang, Xinning; Ye, Mingliang; Zou, Hanfa

    2007-02-01

    An approach was developed to automate sample introduction for nanoflow LC-MS/MS (microLC-MS/MS) analysis using a strong cation exchange (SCX) trap column. The system consisted of a 100 microm id x 2 cm SCX trap column and a 75 microm id x 12 cm C18 RP analytical column. During the sample loading step, the flow passing through the SCX trap column was directed to waste for loading a large volume of sample at high flow rate. Then the peptides bound on the SCX trap column were eluted onto the RP analytical column by a high salt buffer followed by RP chromatographic separation of the peptides at nanoliter flow rate. It was observed that higher performance of separation could be achieved with the system using SCX trap column than with the system using C18 trap column. The high proteomic coverage using this approach was demonstrated in the analysis of tryptic digest of BSA and yeast cell lysate. In addition, this system was also applied to two-dimensional separation of tryptic digest of human hepatocellular carcinoma cell line SMMC-7721 for large scale proteome analysis. This system was fully automated and required minimum changes on current microLC-MS/MS system. This system represented a promising platform for routine proteome analysis.

  8. Hemifield columns co-opt ocular dominance column structure in human achiasma.

    PubMed

    Olman, Cheryl A; Bao, Pinglei; Engel, Stephen A; Grant, Andrea N; Purington, Chris; Qiu, Cheng; Schallmo, Michael-Paul; Tjan, Bosco S

    2018-01-01

    In the absence of an optic chiasm, visual input to the right eye is represented in primary visual cortex (V1) in the right hemisphere, while visual input to the left eye activates V1 in the left hemisphere. Retinotopic mapping In V1 reveals that in each hemisphere left and right visual hemifield representations are overlaid (Hoffmann et al., 2012). To explain how overlapping hemifield representations in V1 do not impair vision, we tested the hypothesis that visual projections from nasal and temporal retina create interdigitated left and right visual hemifield representations in V1, similar to the ocular dominance columns observed in neurotypical subjects (Victor et al., 2000). We used high-resolution fMRI at 7T to measure the spatial distribution of responses to left- and right-hemifield stimulation in one achiasmic subject. T 2 -weighted 2D Spin Echo images were acquired at 0.8mm isotropic resolution. The left eye was occluded. To the right eye, a presentation of flickering checkerboards alternated between the left and right visual fields in a blocked stimulus design. The participant performed a demanding orientation-discrimination task at fixation. A general linear model was used to estimate the preference of voxels in V1 to left- and right-hemifield stimulation. The spatial distribution of voxels with significant preference for each hemifield showed interdigitated clusters which densely packed V1 in the right hemisphere. The spatial distribution of hemifield-preference voxels in the achiasmic subject was stable between two days of testing and comparable in scale to that of human ocular dominance columns. These results are the first in vivo evidence showing that visual hemifield representations interdigitate in achiasmic V1 following a similar developmental course to that of ocular dominance columns in V1 with intact optic chiasm. Copyright © 2017 Elsevier Inc. All rights reserved.

  9. Core-Shell Columns in High-Performance Liquid Chromatography: Food Analysis Applications

    PubMed Central

    Preti, Raffaella

    2016-01-01

    The increased separation efficiency provided by the new technology of column packed with core-shell particles in high-performance liquid chromatography (HPLC) has resulted in their widespread diffusion in several analytical fields: from pharmaceutical, biological, environmental, and toxicological. The present paper presents their most recent applications in food analysis. Their use has proved to be particularly advantageous for the determination of compounds at trace levels or when a large amount of samples must be analyzed fast using reliable and solvent-saving apparatus. The literature hereby described shows how the outstanding performances provided by core-shell particles column on a traditional HPLC instruments are comparable to those obtained with a costly UHPLC instrumentation, making this novel column a promising key tool in food analysis. PMID:27143972

  10. Determination of T-2 toxin, HT-2 toxin, and three other type A trichothecenes in layer feed by high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS)--comparison of two sample preparation methods.

    PubMed

    Bernhardt, Katrin; Valenta, Hana; Kersten, Susanne; Humpf, Hans-Ulrich; Dänicke, Sven

    2016-05-01

    A sensitive method for the simultaneous determination of T-2 toxin, HT-2 toxin, neosolaniol, T-2 triol, and T-2 tetraol in layer feed using high-performance liquid chromatography coupled to triple quadrupole mass spectrometry in the positive ionization mode (LC-ESI-MS/MS) is described. Two fast and easy clean-up methods-with BondElut Mycotoxin and MycoSep 227 columns, respectively-were tested. The separation of the toxins was conducted on a Pursuit XRs Ultra 2.8 HPLC column using 0.13 mM ammonium acetate as eluent A and methanol as eluent B. Detection of the mycotoxins was carried out in the multiple reaction monitoring (MRM) mode using ammonium adducts as precursor ions. Quantification of all analytes was performed with d3-T-2 toxin as an internal standard. The clean-up method with MycoSep 227 columns gave slightly better results for layer feed compared to the method using BondElut Mycotoxin columns (MycoSep 227: recovery between 50 and 63%, BondElut Mycotoxin: recovery between 32 and 67%) and was therefore chosen as the final method. The limits of detection ranged between 0.9 and 7.5 ng/g depending on the mycotoxin. The method was developed for the analysis of layer feed used at carry-over experiments with T-2 toxin in laying hens. For carry-over experiments, it is necessary that the method includes not only T-2 toxin but also the potential metabolites in animal tissues HT-2 toxin, neosolaniol, T-2 triol, and T-2 tetraol which could naturally occur in cereals used as feed stuff as well.

  11. MHD Instabilities and Toroidal Field Effects on Plasma Column Behavior in Tokamak

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Khorshid, Pejman; Plasma Physics Research Center, Islamic Azad University, 14665-678, Tehran; Wang, L.

    2006-12-04

    In the edge plasma of the CT-6B and IRAN-T1 tokamaks the shape of plasma column based on MHD behavior has been studied. The bulk of plasma behavior during plasma column rotation as non-rigid body plasma has been investigated. We found that mode number and rotation frequency of plasma column are different in angle position, so that the mode number detected from Mirnov coils array located in poloidal angle on the inner side of chamber is more than outer side which it can be because of toroidal magnetic field effects. The results of IR-T1 and CT-6B tokamaks compared with each other,more » so that in the CT-6B because of its coils number must be less, but because of its Iron core the effect of toroidal magnetic field became more effective with respect to IR-T1. In addition, it is shown that the plasma column behaves as non-Rigid body plasma so that the poloidal rotation velocity variation in CT-6B is more than IR-T1. A relative correction for island rotation frequency has been suggested in connection with IRAN-T1 and CT-6B tokamak results, which can be considered for optical measurement purposes and also for future advanced tokamak control design.« less

  12. Two-column sequential injection chromatography--new approach for fast and effective analysis and its comparison with gradient elution chromatography.

    PubMed

    Chocholous, Petr; Satínský, Dalibor; Sklenárová, Hana; Solich, Petr

    2010-05-23

    This work presents novel approach in low-pressure chromatography flow systems--two-column Sequential Injection Chromatography (2-C SIC) and its comparison with gradient elution chromatography on the same instrument. The system was equipped with two different chromatographic columns (connected to selection valve in parallel design) for isocratic separation and determination of all components in composed anti-inflammatory pharmaceutical preparation (tablets). The sample was first injected on the first column of length 30 mm where less retained analytes were separated and then the sample was injected on the second column of length 10 mm where more retained analytes were separated. The SIC system was based on a commercial SIChrom manifold (8-port high-pressure selection valve and medium-pressure syringe pump with 4 mL reservoir) (FIAlab, USA) with two commercially available monolithic columns the "first column" Chromolith Flash RP-18e (25 mm x 4.6 mm i.d. with guard column 5 mm x 4.6 mm i.d.) and the "second column" Chromolith RP-18e (10 mm x 4.6 mm i.d.) and CCD UV-vis detector USB 4000 with micro-volume 1.0 cm Z flow cell. Two mobile phases were used for analysis (one for each column). The mobile phase 1 used for elution of paracetamol, caffeine and salicylic acid (internal standard) was acetonitrile/water (10:90, v/v, the water part of pH 3.5 adjusted with acetic acid), flow rate was 0.9 mL min(-1) (volume 3.0 mL of mobile phase per analysis). The mobile phase 2 used for elution of propyphenazone was acetonitrile/water (30:70, v/v); flow rate was 1.2 mL min(-1) (volume 1.5 mL of mobile phase per analysis). Absorbance was monitored at 210 nm. Samples were prepared by dissolving of one tablet in 30% acetonitrile and 10 microL of filtered supernatant was injected on each column (2 x 10 microL). The chromatographic resolution between all compounds was >1.45 and analysis time was 5.5 min under the optimal conditions. Limits of detection were determined at 0.4 microg m

  13. Effect of extra-column volume on practical chromatographic parameters of sub-2-μm particle-packed columns in ultra-high pressure liquid chromatography.

    PubMed

    Wu, Naijun; Bradley, Ashley C; Welch, Christopher J; Zhang, Li

    2012-08-01

    Effects of extra-column volume on apparent separation parameters were studied in ultra-high pressure liquid chromatography with columns and inlet connection tubings of various internal diameters (id) using 50-mm long columns packed with 1.8-μm particles under isocratic conditions. The results showed that apparent retention factors were on average 5, 11, 18, and 41% lower than those corrected with extra-column volumes for 4.6-, 3.0-, 2.1-, and 1.0-mm id columns, respectively, when the extra-column volume (11.3 μL) was kept constant. Also, apparent pressures were 31, 16, 12, and 10% higher than those corrected with pressures from extra-column volumes for 4.6-, 3.0-, 2.1-, and 1.0-mm id columns at the respective optimum flow rate for a typical ultra-high pressure liquid chromatography system. The loss in apparent efficiency increased dramatically from 4.6- to 3.0- to 2.1- to 1.0-mm id columns, less significantly as retention factors increased. The column efficiency was significantly improved as the inlet tubing id was decreased for a given column. The results suggest that maximum ratio of extra-column volume to column void volume should be approximately 1:10 for column porosity more than 0.6 and a retention factor more than 5, where 80% or higher of theoretically predicted efficiency could be achieved. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Green approach using monolithic column for simultaneous determination of coformulated drugs.

    PubMed

    Yehia, Ali M; Mohamed, Heba M

    2016-06-01

    Green chemistry and sustainability is now entirely encompassed across the majority of pharmaceutical companies and research labs. Researchers' attention is careworn toward implementing the green analytical chemistry principles for more eco-friendly analytical methodologies. Solvents play a dominant role in determining the greenness of the analytical procedure. Using safer solvents, the greenness profile of the methodology could be increased remarkably. In this context, a green chromatographic method has been developed and validated for the simultaneous determination of phenylephrine, paracetamol, and guaifenesin in their ternary pharmaceutical mixture. The chromatographic separation was carried out using monolithic column and green solvents as mobile phase. The use of monolithic column allows efficient separation protocols at higher flow rates, which results in short time of analysis. Two-factor three-level experimental design was used to optimize the chromatographic conditions. The greenness profile of the proposed methodology was assessed using eco-scale as a green metrics and was found to be an excellent green method with regard to the usage and production of hazardous chemicals and solvents, energy consumption, and amount of produced waste. The proposed method improved the environmental impact without compromising the analytical performance criteria and could be used as a safer alternate for the routine analysis of the studied drugs. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. A surrogate analyte method to determine D-serine in mouse brain using liquid chromatography-tandem mass spectrometry.

    PubMed

    Kinoshita, Kohnosuke; Jingu, Shigeji; Yamaguchi, Jun-ichi

    2013-01-15

    A bioanalytical method for determining endogenous d-serine levels in the mouse brain using a surrogate analyte and liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed. [2,3,3-(2)H]D-serine and [(15)N]D-serine were used as a surrogate analyte and an internal standard, respectively. The surrogate analyte was spiked into brain homogenate to yield calibration standards and quality control (QC) samples. Both endogenous and surrogate analytes were extracted using protein precipitation followed by solid phase extraction. Enantiomeric separation was achieved on a chiral crown ether column with an analysis time of only 6 min without any derivatization. The column eluent was introduced into an electrospray interface of a triple-quadrupole mass spectrometer. The calibration range was 1.00 to 300 nmol/g, and the method showed acceptable accuracy and precision at all QC concentration levels from a validation point of view. In addition, the brain d-serine levels of normal mice determined using this method were the same as those obtained by a standard addition method, which is time-consuming but is often used for the accurate measurement of endogenous substances. Thus, this surrogate analyte method should be applicable to the measurement of d-serine levels as a potential biomarker for monitoring certain effects of drug candidates on the central nervous system. Copyright © 2012 Elsevier Inc. All rights reserved.

  16. T-phase and tsunami pressure waveforms recorded by near-source IMS water-column hydrophone triplets during the 2015 Chile earthquake

    NASA Astrophysics Data System (ADS)

    Matsumoto, H.; Haralabus, G.; Zampolli, M.; Özel, N. M.

    2016-12-01

    Underwater acoustic signal waveforms recorded during the 2015 Chile earthquake (Mw 8.3) by the hydrophones of hydroacoustic station HA03, located at the Juan Fernandez Islands, are analyzed. HA03 is part of the Comprehensive Nuclear-Test-Ban Treaty International Monitoring System. The interest in the particular data set stems from the fact that HA03 is located only approximately 700 km SW from the epicenter of the earthquake. This makes it possible to study aspects of the signal associated with the tsunamigenic earthquake, which would be more difficult to detect had the hydrophones been located far from the source. The analysis shows that the direction of arrival of the T phase can be estimated by means of a three-step preprocessing technique which circumvents spatial aliasing caused by the hydrophone spacing, the latter being large compared to the wavelength. Following this preprocessing step, standard frequency-wave number analysis (F-K analysis) can accurately estimate back azimuth and slowness of T-phase signals. The data analysis also shows that the dispersive tsunami signals can be identified by the water-column hydrophones at the time when the tsunami surface gravity wave reaches the station.

  17. The CH2O column as a possible constraint on methane oxidation

    NASA Astrophysics Data System (ADS)

    Valin, L. C.; Fiore, A. M.; Lin, M.

    2013-12-01

    We explore the potential for space-based measurements of the CH2O column to quantify variations of methane oxidation in the remote atmosphere due to changes in climate (e.g., T, H2O, stratospheric O3) and atmospheric composition (e.g., NOxO, O3, CO, CH4). We investigate the variability of methane oxidation and the formaldehyde column using available global simulations (MOZART-2 chemistry-transport model, GFDL AM3 climate-chemistry model). Over a large region (135° - 175° W; 0° - 16° S), the rate of methane oxidation simulated in the models varies intraseasonally (×10%), seasonally (×20%) and interannually (×5%), and is well correlated with the simulated variability of the CH2O column (R2 = 0.75; ~1x1015 molecules cm-2). The precision of a single space-based measurement is approximately 1×1016 molecules cm-2, an order of magnitude larger than the simulated variability of the CH2O column. However, in a large region such as the tropical Pacific, UV/Vis spectrometers are capable of making thousands of measurements daily, enough sampling to theoretically increase the precision by √N, such that variations on the order of 1×1015 molecules cm-2 should be observable on intraseasonal and interannual timescales.

  18. A new method for rapid determination of indole-3-carbinol and its condensation products in nutraceuticals using core-shell column chromatography method.

    PubMed

    Fibigr, Jakub; Šatínský, Dalibor; Havlíková, Lucie; Solich, Petr

    2016-02-20

    Indole-3-carbinol is a natural glucosinolate known for prevention of human breast, prostate and other types of cancer and it started to be used in commercial preparations, as food supplements. However no analytical method has been proposed for quality control of nutraceuticals with this substance yet. In this paper a new high-performance liquid chromatography (HPLC) method using core-shell column for separation of indole-3-carbinol and its condensation/degradation products was developed and used for the quantitative determination of indole-3-carbinol in nutraceuticals. Separation of indole-3-carbinol, its condensation/degradation products and internal standard ethylparaben was performed on the core-shell column Kinetex 5μ XB-C18 100A (100×4.6mm), particle size 5.0μm, with mobile phase acetonitrile/water according to the gradient program at a flow rate of 1.25mLmin(-1) and at temperature 50°C. The detection wavelength was set at 270nm. Under the optimal chromatographic conditions good linearity of determination was achieved. Available commercial samples of nutraceuticals were extracted with 100% methanol using ultrasound bath. A 5-μL sample volume of the supernatant was directly injected into the HPLC system. The developed method provided rapid and accurate tool for quality control of nutraceuticals based on cruciferous vegetable extracts with indole-3-carbinol content. The presented study showed that the declared content of indole-3-carbinol significantly varied in the different nutraceuticals available on the market. Two analyzed preparations showed the presence of condensation/degradation products of indole-3-carbinol which were not officially declared by the manufacturer. Moreover, further two analyzed nutraceutical preparations showed absolutely no content of declared amount of indole-3-carbinol. Copyright © 2015 Elsevier B.V. All rights reserved.

  19. Comprehensive data resources and analytical tools for pathological association of aminoacyl tRNA synthetases with cancer

    PubMed Central

    Lee, Ji-Hyun; You, Sungyong; Hyeon, Do Young; Kang, Byeongsoo; Kim, Hyerim; Park, Kyoung Mii; Han, Byungwoo; Hwang, Daehee; Kim, Sunghoon

    2015-01-01

    Mammalian cells have cytoplasmic and mitochondrial aminoacyl-tRNA synthetases (ARSs) that catalyze aminoacylation of tRNAs during protein synthesis. Despite their housekeeping functions in protein synthesis, recently, ARSs and ARS-interacting multifunctional proteins (AIMPs) have been shown to play important roles in disease pathogenesis through their interactions with disease-related molecules. However, there are lacks of data resources and analytical tools that can be used to examine disease associations of ARS/AIMPs. Here, we developed an Integrated Database for ARSs (IDA), a resource database including cancer genomic/proteomic and interaction data of ARS/AIMPs. IDA includes mRNA expression, somatic mutation, copy number variation and phosphorylation data of ARS/AIMPs and their interacting proteins in various cancers. IDA further includes an array of analytical tools for exploration of disease association of ARS/AIMPs, identification of disease-associated ARS/AIMP interactors and reconstruction of ARS-dependent disease-perturbed network models. Therefore, IDA provides both comprehensive data resources and analytical tools for understanding potential roles of ARS/AIMPs in cancers. Database URL: http://ida.biocon.re.kr/, http://ars.biocon.re.kr/ PMID:25824651

  20. Semi-micro high-performance liquid chromatographic analysis of tiropramide in human plasma using column-switching.

    PubMed

    Baek, Soo Kyoung; Lee, Seung Seok; Park, Eun Jeon; Sohn, Dong Hwan; Lee, Hye Suk

    2003-02-05

    A rapid and sensitive column-switching semi-micro high-performance liquid chromatography method was developed for the direct analysis of tiropramide in human plasma. The plasma sample (100 microl) was directly injected onto Capcell Pak MF Ph-1 precolumn where deproteinization and analyte fractionation occurred. Tiropramide was then eluted into an enrichment column (Capcell Pak UG C(18)) using acetonitrile-potassium phosphate (pH 7.0, 50 mM) (12:88, v/v) and was analyzed on a semi-micro C(18) analytical column using acetonitrile-potassium phosphate (pH 7.0, 10 mM) (50:50, v/v). The method showed excellent sensitivity (limit of quantification 5 ng/ml), and good precision (C.V.

  1. Tank 241-B-108, cores 172 and 173 analytical results for the final report

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Nuzum, J.L., Fluoro Daniel Hanford

    1997-03-04

    The Data Summary Table (Table 3) included in this report compiles analytical results in compliance with all applicable DQOS. Liquid subsamples that were prepared for analysis by an acid adjustment of the direct subsample are indicated by a `D` in the A column in Table 3. Solid subsamples that were prepared for analysis by performing a fusion digest are indicated by an `F` in the A column in Table 3. Solid subsamples that were prepared for analysis by performing a water digest are indicated by a I.wl. or an `I` in the A column of Table 3. Due to poormore » precision and accuracy in original analysis of both Lower Half Segment 2 of Core 173 and the core composite of Core 173, fusion and water digests were performed for a second time. Precision and accuracy improved with the repreparation of Core 173 Composite. Analyses with the repreparation of Lower Half Segment 2 of Core 173 did not show improvement and suggest sample heterogeneity. Results from both preparations are included in Table 3.« less

  2. Approximate transient and long time limit solutions for the band broadening induced by the thin sidewall-layer in liquid chromatography columns.

    PubMed

    Broeckhoven, Ken; Desmet, Gert

    2007-11-16

    Using a combination of both analytical and numerical techniques, approximate analytical expressions have been established for the transient and long time limit band broadening, originating from the presence of a thin disturbed sidewall layer in liquid chromatography columns, including packed, monolithic as well as microfabricated columns. The established expressions can be used to compare the importance of a thin disturbed sidewall layer with that of other radial heterogeneity effects (such as transcolumn packing density variations due to the relief of packing stresses). The expressions are independent of the actual velocity profile inside the layer as long as the disturbed sidewall layer occupies less than 2.5% of the column width.

  3. Comparison of post-contrast 3D-T1-MPRAGE, 3D-T1-SPACE and 3D-T2-FLAIR MR images in evaluation of meningeal abnormalities at 3-T MRI.

    PubMed

    Jeevanandham, Balaji; Kalyanpur, Tejas; Gupta, Prashant; Cherian, Mathew

    2017-06-01

    This study was to assess the usefulness of newer three-dimensional (3D)-T 1 sampling perfection with application optimized contrast using different flip-angle evolutions (SPACE) and 3D-T 2 fluid-attenuated inversion recovery (FLAIR) sequences in evaluation of meningeal abnormalities. 78 patients who presented with high suspicion of meningeal abnormalities were evaluated using post-contrast 3D-T 2 -FLAIR, 3D-T 1 magnetization-prepared rapid gradient-echo (MPRAGE) and 3D-T 1 -SPACE sequences. The images were evaluated independently by two radiologists for cortical gyral, sulcal space, basal cisterns and dural enhancement. The diagnoses were confirmed by further investigations including histopathology. Post-contrast 3D-T 1 -SPACE and 3D-T 2 -FLAIR images yielded significantly more information than MPRAGE images (p < 0.05 for both SPACE and FLAIR images) in detection of meningeal abnormalities. SPACE images best demonstrated abnormalities in dural and sulcal spaces, whereas FLAIR was useful for basal cisterns enhancement. Both SPACE and FLAIR performed equally well in detection of gyral enhancement. In all 10 patients, where both SPACE and T 2 -FLAIR images failed to demonstrate any abnormality, further analysis was also negative. The 3D-T 1 -SPACE sequence best demonstrated abnormalities in dural and sulcal spaces, whereas FLAIR was useful for abnormalities in basal cisterns. Both SPACE and FLAIR performed holds good for detection of gyral enhancement. Post-contrast SPACE and FLAIR sequences are superior to the MPRAGE sequence for evaluation of meningeal abnormalities and when used in combination have the maximum sensitivity for leptomeningeal abnormalities. The negative-predictive value is nearly 100%, where no leptomeningeal abnormality was detected on these sequences. Advances in knowledge: Post-contrast 3D-T 1 -SPACE and 3D-T 2 -FLAIR images are more useful than 3D-T 1 -MPRAGE images in evaluation of meningeal abnormalities.

  4. Ab Initio and Analytic Intermolecular Potentials for Ar–CH3OH

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Tasic, Uros; Alexeev, Yuri; Vayner, Grigoriy

    2006-09-20

    Ab initio calculations at the CCSD(T)/aug-cc-pVTZ level of theory were used to characterize the Ar–CH₃y6tOH intermolecular potential energy surface (PES). Potential energy curves were calculated for four different Ar + CH₃OH orientations and used to derive an analytic function for the intermolecular PES. A sum of Ar–C, Ar–O, Ar–H(C), and Ar–H(O) two-body potentials gives an excellent fit to these potential energy curves up to 100 kcal mol¯¹, and adding an additional r¯¹n term to the Buckingham two-body potential results in only a minor improvement in the fit. Three Ar–CH₃OH van der Waals minima were found from the CCSD(T)/aug-cc-pVTZ//MP2/aug-cc-pVTZ calculations. Themore » structure of the global minimum is in overall good agreement with experiment (X.-C. Tan, L. Sun and R. L. Kuczkowski, J. Mol. Spectrosc., 1995, 171, 248). It is T-shaped with the hydroxyl H-atom syn with respect to Ar. Extrapolated to the complete basis set (CBS) limit, the global minimum has a well depth of 0.72 kcal mol¯¹ with basis set superposition error (BSSE) correction. The aug-cc-pVTZ basis set gives a well depth only 0.10 kcal mol¯¹ smaller than this value. The well depths of the other two minima are within 0.16 kcal mol¯¹ of the global minimum. The analytic Ar–CH₃OH intermolecular potential also identifies these three minima as the only van der Waals minima and the structures predicted by the analytic potential are similar to the ab initio structures. The analytic potential identifies the same global minimum and the predicted well depths for the minima are within 0.05 kcal mol¯1 of the ab initio values. Combining this Ar–CH₃OH intermolecular potential with a potential for a OH-terminated alkylthiolate self-assembled monolayer surface (i.e., HO-SAM) provides a potential to model Ar + HO-SAM collisions.« less

  5. Recovery of 1,3-, 2,3-dichloropropenes, 1,2-dibromo-3-chloropropane, and o-, p-dichlorobenzenes from fatty and non-fat foodstuffs by liquid extraction technique.

    PubMed

    Daft, J L

    1990-01-01

    Food samples including fatty, non-fatty, grain-based, and nongrain-based types were fortified with the following five nematocides and fumigants: 1,3-dichloropropene, 2,3-dichloropropene, 1,2-dibromo-3-chloropropane, o-dichlorobenzene, and p-dichlorobenzene. Then, depending on sample consistency and type, the samples were diluted in, or extracted with organic solvent such as isooctane. A few of the high-fat extracts were passed through Florisil to remove excess fat or endogenous interferences. Analysis of the initial or cleaned up extracts was done by gas chromatography (GC) at 90 degrees C. The dichloropropenes were determined on 20% OV-101 columns with electron-capture and Hall electroconductivity detectors. The dichlorobenzenes and 1,2-dibromo-3-chloropropane, which elute beyond 30 min on the above columns, were determined on 5%-loaded columns using the same detectors. All five analytes were recovered from these techniques. Mean analyte recovery following a direct dilution or extraction was 83%, and following the Florisil cleanup step, was 52%. In 1986, a fumigant survey of about 200 foodstuffs by using this overall technique gave no findings of the five compounds studied here.

  6. Design and Performance of a 1 ms High-Speed Vision Chip with 3D-Stacked 140 GOPS Column-Parallel PEs †.

    PubMed

    Nose, Atsushi; Yamazaki, Tomohiro; Katayama, Hironobu; Uehara, Shuji; Kobayashi, Masatsugu; Shida, Sayaka; Odahara, Masaki; Takamiya, Kenichi; Matsumoto, Shizunori; Miyashita, Leo; Watanabe, Yoshihiro; Izawa, Takashi; Muramatsu, Yoshinori; Nitta, Yoshikazu; Ishikawa, Masatoshi

    2018-04-24

    We have developed a high-speed vision chip using 3D stacking technology to address the increasing demand for high-speed vision chips in diverse applications. The chip comprises a 1/3.2-inch, 1.27 Mpixel, 500 fps (0.31 Mpixel, 1000 fps, 2 × 2 binning) vision chip with 3D-stacked column-parallel Analog-to-Digital Converters (ADCs) and 140 Giga Operation per Second (GOPS) programmable Single Instruction Multiple Data (SIMD) column-parallel PEs for new sensing applications. The 3D-stacked structure and column parallel processing architecture achieve high sensitivity, high resolution, and high-accuracy object positioning.

  7. A rapid HPLC column switching method for sample preparation and determination of β-carotene in food supplements.

    PubMed

    Brabcová, Ivana; Hlaváčková, Markéta; Satínský, Dalibor; Solich, Petr

    2013-11-15

    A simple and automated HPLC column-switching method with rapid sample pretreatment has been developed for quantitative determination of β-carotene in food supplements. Commercially samples of food supplements were dissolved in chloroform with help of saponification with 1M solution of sodium hydroxide in ultrasound bath. A 20-min sample dissolution/extraction step was necessary before chromatography analysis to transfer β-carotene from solid state of food supplements preparations (capsules,tablets) to chloroform solution. Sample volume - 3μL of chloroform phase was directly injected into the HPLC system. Next on-line sample clean-up was achieved on the pretreatment precolumn Chromolith Guard Cartridge RP-18e (Merck), 10×4.6mm, with a washing mobile phase (methanol:water, 92:8, (v/v)) at a flow rate of 1.5mL/min. Valve switch to analytical column was set at 2.5min in a back-flush mode. After column switching to the analytical column Ascentis Express C-18, 30×4.6mm, particle size 2.7μm (Sigma Aldrich), the separation and determination of β-carotene in food supplements was performed using a mobile phase consisting of 100% methanol, column temperature at 60°C and flow rate 1.5mL/min. The detector was set at 450nm. Under the optimum chromatographic conditions standard calibration curve was measured with good linearity - correlation coefficient for β-carotene (r(2)=0.999014; n=6) between the peak areas and concentration of β-carotene 20-200μg/mL. Accuracy of the method defined as a mean recovery was in the range 96.66-102.40%. The intraday method precision was satisfactory at three concentration levels 20, 125 and 200μg/mL and relative standard deviations were in the range 0.90-1.02%. The chromatography method has shown high sample throughput during column-switching pretreatment process and analysis in one step in short time (6min) of the whole chromatographic analysis. Copyright © 2013 Elsevier Ltd. All rights reserved.

  8. On-column nitrosation of amines observed in liquid chromatography impurity separations employing ammonium hydroxide and acetonitrile as mobile phase.

    PubMed

    Myers, David P; Hetrick, Evan M; Liang, Zhongming; Hadden, Chad E; Bandy, Steven; Kemp, Craig A; Harris, Thomas M; Baertschi, Steven W

    2013-12-06

    The availability of high performance liquid chromatography (HPLC) columns capable of operation at pH values up to 12 has allowed a greater selectivity space to be explored for method development in pharmaceutical analysis. Ammonium hydroxide is of particular value in the mobile phase because it is compatible with direct interfacing to electrospray mass spectrometers. This paper reports an unexpected N-nitrosation reaction that occurs with analytes containing primary and secondary amines when ammonium hydroxide is used to achieve the high pH and acetonitrile is used as the organic modifier. The nitrosation reaction has generality. It has been observed on multiple columns from different vendors and with multiple amine-containing analytes. Ammonia was established to be the source of the nitroso nitrogen. The stainless steel column frit and metal ablated from the frit have been shown to be the sites of the reactions. The process is initiated by removal of the chromium oxide protective film from the stainless steel by acetonitrile. It is hypothesized that the highly active, freshly exposed metals catalyze room temperature oxidation of ammonia to NO but that the actual nitrosating agent is likely N(2)O(3). Copyright © 2013 Elsevier B.V. All rights reserved.

  9. Fiber-based monolithic columns for liquid chromatography.

    PubMed

    Ladisch, Michael; Zhang, Leyu

    2016-10-01

    Fiber-based monoliths for use in liquid chromatographic separations are defined by columns packed with aligned fibers, woven matrices, or contiguous fiber structures capable of achieving rapid separations of proteins, macromolecules, and low molecular weight components. A common denominator and motivating driver for this approach, first initiated 25 years ago, was reducing the cost of bioseparations in a manner that also reduced residence time of retained components while achieving a high ratio of mass to momentum transfer. This type of medium, when packed into a liquid chromatography column, minimized the fraction of stagnant liquid and resulted in a constant plate height for non-adsorbing species. The uncoupling of dispersion from eluent flow rate enabled the surface chemistry of the stationary phase to be considered separately from fluid transport phenomena and pointed to new ways to apply chemistry for the engineering of rapid bioseparations. This paper addresses developments and current research on fiber-based monoliths and explains how the various forms of this type of chromatographic stationary phase have potential to provide new tools for analytical and preparative scale separations. The different stationary phases are discussed, and a model that captures the observed constant plate height as a function of mobile phase velocity is reviewed. Methods that enable hydrodynamically stable fiber columns to be packed and operated over a range of mobile phase flow rates, together with the development of new fiber chemistries, are shown to provide columns that extend the versatility of liquid chromatography using monoliths, particularly at the preparative scale. Graphical Abstract Schematic representation of a sample mixture being separated by a rolled-stationary phase column, resulting separated peaks shown in the chromatogram.

  10. KM3NeT

    NASA Astrophysics Data System (ADS)

    de Jong, M.

    2015-07-01

    KM3NeT is a large research infrastructure, that will consist of a network of deep-sea neutrino telescopes in the Mediterranean Sea. The main objective of KM3NeT is the discovery and subsequent observation of high-energy neutrino sources in the Universe. A further physics perspective is the measurement of the mass hierarchy of neutrinos. A corresponding study, ORCA, is ongoing within KM3NeT. A cost effective technology for (very) large water Cherenkov detectors has been developed based on a new generation of low price 3-inch photo-multiplier tubes. Following the successful deployment and operation of two prototypes, the construction of the KM3NeT research infrastructure has started. The prospects of the different phases of the implementation of KM3NeT are summarised.

  11. Stochastic Accumulation by Cortical Columns May Explain the Scalar Property of Multistable Perception

    NASA Astrophysics Data System (ADS)

    Cao, Robin; Braun, Jochen; Mattia, Maurizio

    2014-08-01

    The timing of certain mental events is thought to reflect random walks performed by underlying neural dynamics. One class of such events—stochastic reversals of multistable perceptions—exhibits a unique scalar property: even though timing densities vary widely, higher moments stay in particular proportions to the mean. We show that stochastic accumulation of activity in a finite number of idealized cortical columns—realizing a generalized Ehrenfest urn model—may explain these observations. Modeling stochastic reversals as the first-passage time of a threshold number of active columns, we obtain higher moments of the first-passage time density. We derive analytical expressions for noninteracting columns and generalize the results to interacting columns in simulations. The scalar property of multistable perception is reproduced by a dynamic regime with a fixed, low threshold, in which the activation of a few additional columns suffices for a reversal.

  12. Radial distribution of the flow velocity, efficiency and concentration in a wide HPLC column

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Farkas, T.; Sepaniak, M.J.; Guiochon, G.

    1997-08-01

    The use of optical fibers in a fluorescence-detection scheme permits the accurate determination of the radial distribution of the transit time, the column efficiency, and the analyte concentration at the exit of a chromatographic axial-compression column (50 mmID). The results obtained demonstrate that the column is not homogeneous, but suggest a nearly cylindrical distribution of the packing density. The average velocity close to the column wall is 7% lower than along its axis and the HETP 25% higher. The lack of homogeneity of the column packing is another source of band broadening not taken into account in chromatography so far.more » It causes the apparent HETP derived from the conventional elution chromatogram recorded on the bulk eluent to be larger than the local HETP and the band profile to be unsymmetrical with a slight tail reminiscent of kinetic tailing.« less

  13. Characterization of retentivity of reversed phase liquid chromatography columns.

    PubMed

    Ying, P T; Dorsey, J G

    1991-03-01

    There are dozens of commercially available reversed phase columns, most marketed as C-8 or C-18 materials, but with no useful way of classifying their retentivity. A useful way of ranking these columns in terms of column "strength" or retentivity is presented. The method utilizes a value for ln k'(w), the estimated retention of a solute from a mobile phase of 100% water, and the slope of the plot of ln k' vsE(T)(30), the solvent polarity. The method is validated with 26 solutes varying in ln k'(w) from about 2 to over 20, on 14 different reversed phase columns. In agreement with previous work, it is found that the phase volume ratio of the column is the most important parameter in determining retentivity. It is strongly suggested that manufacturers adopt a uniform method of calculating this value and that it be made available in advertising, rather than the uninterpretable "% carbon".

  14. Modeling Stone Columns.

    PubMed

    Castro, Jorge

    2017-07-11

    This paper reviews the main modeling techniques for stone columns, both ordinary stone columns and geosynthetic-encased stone columns. The paper tries to encompass the more recent advances and recommendations in the topic. Regarding the geometrical model, the main options are the "unit cell", longitudinal gravel trenches in plane strain conditions, cylindrical rings of gravel in axial symmetry conditions, equivalent homogeneous soil with improved properties and three-dimensional models, either a full three-dimensional model or just a three-dimensional row or slice of columns. Some guidelines for obtaining these simplified geometrical models are provided and the particular case of groups of columns under footings is also analyzed. For the latter case, there is a column critical length that is around twice the footing width for non-encased columns in a homogeneous soft soil. In the literature, the column critical length is sometimes given as a function of the column length, which leads to some disparities in its value. Here it is shown that the column critical length mainly depends on the footing dimensions. Some other features related with column modeling are also briefly presented, such as the influence of column installation. Finally, some guidance and recommendations are provided on parameter selection for the study of stone columns.

  15. Modeling Stone Columns

    PubMed Central

    2017-01-01

    This paper reviews the main modeling techniques for stone columns, both ordinary stone columns and geosynthetic-encased stone columns. The paper tries to encompass the more recent advances and recommendations in the topic. Regarding the geometrical model, the main options are the “unit cell”, longitudinal gravel trenches in plane strain conditions, cylindrical rings of gravel in axial symmetry conditions, equivalent homogeneous soil with improved properties and three-dimensional models, either a full three-dimensional model or just a three-dimensional row or slice of columns. Some guidelines for obtaining these simplified geometrical models are provided and the particular case of groups of columns under footings is also analyzed. For the latter case, there is a column critical length that is around twice the footing width for non-encased columns in a homogeneous soft soil. In the literature, the column critical length is sometimes given as a function of the column length, which leads to some disparities in its value. Here it is shown that the column critical length mainly depends on the footing dimensions. Some other features related with column modeling are also briefly presented, such as the influence of column installation. Finally, some guidance and recommendations are provided on parameter selection for the study of stone columns. PMID:28773146

  16. KM3NeT

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Jong, M. de; Leiden Institute of Physics, Leiden University, Leiden; Collaboration: KM3NeT Collaboration

    2015-07-15

    KM3NeT is a large research infrastructure, that will consist of a network of deep-sea neutrino telescopes in the Mediterranean Sea. The main objective of KM3NeT is the discovery and subsequent observation of high-energy neutrino sources in the Universe. A further physics perspective is the measurement of the mass hierarchy of neutrinos. A corresponding study, ORCA, is ongoing within KM3NeT. A cost effective technology for (very) large water Cherenkov detectors has been developed based on a new generation of low price 3-inch photo-multiplier tubes. Following the successful deployment and operation of two prototypes, the construction of the KM3NeT research infrastructure hasmore » started. The prospects of the different phases of the implementation of KM3NeT are summarised.« less

  17. Simultaneous determination of acetylsalicylic acid and salicylic acid in human plasma by isocratic high-pressure liquid chromatography with post-column hydrolysis and fluorescence detection.

    PubMed

    Hobl, Eva-Luise; Jilma, Bernd; Ebner, Josef; Schmid, Rainer W

    2013-06-01

    A selective, sensitive and rapid high-performance liquid chromatography method with post-column hydrolysis and fluorescence detection was developed for the simultaneous quantification of acetylsalicylic acid and its metabolite salicylic acid in human plasma. Following the addition of 2-hydroxy-3-methoxybenzoic acid as internal standard and simple protein precipitation with acetonitrile, the analytes were separated on a ProntoSIL 120 C18 ace-EPS column (150 × 2 mm, 3 µm) protected by a C8 guard column (5 µm). The mobile phase, 10 mm formic acid in water (pH 2.9) and acetonitrile (70:30, v/v), was used at a flow rate of 0.35 mL/min. After on-line post-column hydrolysis of acetylsalicylic acid (ASA) to salicylic acid (SA) by addition of alkaline solution, the analytes were measured at 290 nm (λex ) and 400 nm (λem ). The method was linear in the concentration ranges between 0.05 and 20 ng/μL for both ASA and SA with a lower limit of quantification of 25 pg/μL for SA and 50 pg/μL for ASA. The limit of detection was 15 pg/μL for SA and 32.5 pg/μL for ASA. The analysis of ASA and SA can be carried out within 8 min; therefore this method is suitable for measuring plasma concentrations of salicylates in clinical routine. Copyright © 2012 John Wiley & Sons, Ltd.

  18. Column on column’ structures as indicators of lava/ice interaction, Ruapehu andesite volcano, New Zealand

    NASA Astrophysics Data System (ADS)

    Spörli, K. B.; Rowland, J. V.

    2006-10-01

    Lava flows of the Mangawhero Formation (ca. 15-60 ka) on Ruapehu volcano erupted during the last glaciation. In a distal flow lobe at Tukino, on the east side of the mountain, small secondary columns (10-20 cm thick) have formed on the sides of large, rectangular, primary (0.5-3 m thick) cooling columns. Thick (10 m+) zones of such small columns form a lateral and basal outer rind of the lobe. As they do not mark glassy zones of quenching, these secondary columns are interpreted as being formed by a second cooling event at temperatures below the boundary between the low creep and elastic regimes (˜ 600 °C) by rapid influx of copious amounts of water. Temperature drops deduced from extensional strains of the two sets of columns were used to gauge the viability of such a two-stage process. Absence of reliable data on andesite contraction coefficients was overcome by using a sliding scale to assess a large range of values. The estimates indicate that two-stage chilling is feasible. After flowing across relatively ice-poor terrain, the lava flow must have interacted with a valley glacier that provided water for further chilling the already formed primary columns and formation of the outer rind small columns. Given this evidence for lava/ice interaction, it is likely that prominent, thick flows elsewhere in the Mangawhero Formation may have been constrained to their ridge-top locations by ice conditions similar to those described by Lescinsky and Sisson [Lescinsky, D.T., Sisson, T.W., 1998. Ridge-forming, ice-bounded lava flows at Mount Rainier, Washington. Geology, 26, 351-354].

  19. 3D printed titanium micro-bore columns containing polymer monoliths for reversed-phase liquid chromatography.

    PubMed

    Gupta, Vipul; Talebi, Mohammad; Deverell, Jeremy; Sandron, Sara; Nesterenko, Pavel N; Heery, Brendan; Thompson, Fletcher; Beirne, Stephen; Wallace, Gordon G; Paull, Brett

    2016-03-03

    The potential of 3D selective laser melting (SLM) technology to produce compact, temperature and pressure stable titanium alloy chromatographic columns is explored. A micro bore channel (0.9 mm I.D. × 600 mm long) was produced within a 5 × 30 × 30 mm titanium alloy (Ti-6Al-4V) cuboid, in form of a double handed spiral. A poly(butyl methacrylate-co-ethyleneglycoldimethacrylate) (BuMA-co-EDMA) monolithic stationary phase was thermally polymerised within the channel for application in reversed-phase high-performance liquid chromatography. The prepared monolithic column was applied to the liquid chromatographic separation of intact proteins and peptides. Peak capacities of 69-76 (for 6-8 proteins respectively) were observed during isothermal separation of proteins at 44 °C which were further increased to 73-77 using a thermal step gradient with programmed temperature from 60 °C to 35 °C using an in-house built direct-contact heater/cooler platform based upon matching sized Peltier thermoelectric modules. Rapid temperature gradients were possible due to direct-contact between the planar metal column and the Peltier module, and the high thermal conductivity of the titanium column as compared to a similar stainless steel printed column. The separation of peptides released from a digestion of E.coli was also achieved in less than 35 min with ca. 40 distinguishable peaks at 210 nm. Copyright © 2016 Elsevier B.V. All rights reserved.

  20. Experimental Research of FRP Composite Tube Confined Steel-reinforced Concrete Stub Columns Under Axial Compression

    NASA Astrophysics Data System (ADS)

    Wang, Ji Zhong; Cheng, Lu; Wang, Xin Pei

    2018-06-01

    A new column of FRP composite tube confined steel-reinforced concrete (FTCSRC) column was proposed. This paper elaborates on laboratorial and analytical studies on the behavior of FCTSRC columns subjected to axial compressive load. Eight circular FTCSRC stub columns and one circular steel tube confined concrete (STCC) stub column were tested to investigate the failure mode and axial compression performance of circular FTCRSC columns. Parametric analysis was implemented to inquire the influence of confinement material (CFRP-steel tube or CFRP-GFRP tube), internal steel and CFRP layers on the ultimate load capacity. CFRP-steel composite tube was composed of steel tube and CFRP layer which was wrapped outside the steel tube, while CFRP-GFRP composite tube was composite of GFRP tube and CFRP layer. The test results indicate that the confinement effect of CFRP-steel tube is greatly superior to CFRP-GFRP tube. The ductility performance of steel tube confined high-strength concrete column can be improved obviously by encasing steel in the core concrete. Furthermore, with the increase in the layers of FRP wraps, the axial load capacity increases greatly.

  1. Constraining the H2 column density distribution at z ˜ 3 from composite DLA spectra

    NASA Astrophysics Data System (ADS)

    Balashev, S. A.; Noterdaeme, P.

    2018-07-01

    We present the detection of the average H2 absorption signal in the overall population of neutral gas absorption systems at z˜ 3 using composite absorption spectra built from the Sloan Digital Sky Survey-III damped Lyman α catalogue. We present a new technique to directly measure the H2 column density distribution function f_H_2(N) from the average H2 absorption signal. Assuming a power-law column density distribution, we obtain a slope β = -1.29 ± 0.06(stat) ± 0.10 (sys) and an incidence rate of strong H2 absorptions [with N(H2) ≳ 1018 cm-2] to be 4.0 ± 0.5(stat) ± 1.0 (sys) per cent in H I absorption systems with N(H I) ≥1020 cm-2. Assuming the same inflexion point where f_H_2(N) steepens as at z = 0, we estimate that the cosmological density of H2 in the column density range log N(H_2) (cm^{-2})= 18{-}22 is {˜ } 15 per cent of the total. We find one order of magnitude higher H2 incident rate in a sub-sample of extremely strong damped Lyman α absorption systems (DLAs) [log N(H I) (cm^{-2}) ≥ 21.7], which, together with the derived shape of f_H_2(N), suggests that the typical H I-H2 transition column density in DLAs is log N(H)(cm-2) ≳ 22.3 in agreement with theoretical expectations for the average (low) metallicity of DLAs at high-z.

  2. Constraining the H2 column density distribution at z˜3 from composite DLA spectra

    NASA Astrophysics Data System (ADS)

    Balashev, S. A.; Noterdaeme, P.

    2018-04-01

    We present the detection of the average H2 absorption signal in the overall population of neutral gas absorption systems at z ˜ 3 using composite absorption spectra built from the Sloan Digital Sky Survey-III damped Lyman-α catalogue. We present a new technique to directly measure the H2 column density distribution function f_H_2(N) from the average H2 absorption signal. Assuming a power-law column density distribution, we obtain a slope β = -1.29 ± 0.06(stat) ± 0.10 (sys) and an incidence rate of strong H2 absorptions (with N(H2) ≳ 1018 cm-2) to be 4.0 ± 0.5(stat) ± 1.0 (sys) % in H I absorption systems with N(H I)≥1020 cm-2. Assuming the same inflexion point where f_H_2(N) steepens as at z = 0, we estimate that the cosmological density of H2 in the column density range log N(H_2) (cm^{-2})= 18-22 is ˜15% of the total. We find one order of magnitude higher H2 incident rate in a sub-sample of extremely strong DLAs (log N(H I) (cm^{-2}) ≥ 21.7), which, together with the the derived shape of f_H_2(N), suggests that the typical H I-H2 transition column density in DLAs is log N(H)(cm-2) ≳ 22.3 in agreement with theoretical expectations for the average (low) metallicity of DLAs at high-z.

  3. Reconstruction of 7T-Like Images From 3T MRI

    PubMed Central

    Bahrami, Khosro; Shi, Feng; Zong, Xiaopeng; Shin, Hae Won; An, Hongyu

    2016-01-01

    In the recent MRI scanning, ultra-high-field (7T) MR imaging provides higher resolution and better tissue contrast compared to routine 3T MRI, which may help in more accurate and early brain diseases diagnosis. However, currently, 7T MRI scanners are more expensive and less available at clinical and research centers. These motivate us to propose a method for the reconstruction of images close to the quality of 7T MRI, called 7T-like images, from 3T MRI, to improve the quality in terms of resolution and contrast. By doing so, the post-processing tasks, such as tissue segmentation, can be done more accurately and brain tissues details can be seen with higher resolution and contrast. To do this, we have acquired a unique dataset which includes paired 3T and 7T images scanned from same subjects, and then propose a hierarchical reconstruction based on group sparsity in a novel multi-level Canonical Correlation Analysis (CCA) space, to improve the quality of 3T MR image to be 7T-like MRI. First, overlapping patches are extracted from the input 3T MR image. Then, by extracting the most similar patches from all the aligned 3T and 7T images in the training set, the paired 3T and 7T dictionaries are constructed for each patch. It is worth noting that, for the training, we use pairs of 3T and 7T MR images from each training subject. Then, we propose multi-level CCA to map the paired 3T and 7T patch sets to a common space to increase their correlations. In such space, each input 3T MRI patch is sparsely represented by the 3T dictionary and then the obtained sparse coefficients are used together with the corresponding 7T dictionary to reconstruct the 7T-like patch. Also, to have the structural consistency between adjacent patches, the group sparsity is employed. This reconstruction is performed with changing patch sizes in a hierarchical framework. Experiments have been done using 13 subjects with both 3T and 7T MR images. The results show that our method outperforms previous

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

    PubMed

    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.

  5. Longitudinal On-Column Thermal Modulation for Comprehensive Two-Dimensional Liquid Chromatography.

    PubMed

    Creese, Mari E; Creese, Mathew J; Foley, Joe P; Cortes, Hernan J; Hilder, Emily F; Shellie, Robert A; Breadmore, Michael C

    2017-01-17

    Longitudinal on-column thermal modulation for comprehensive two-dimensional liquid chromatography is introduced. Modulation optimization involved a systematic investigation of heat transfer, analyte retention, and migration velocity at a range of temperatures. Longitudinal on-column thermal modulation was realized using a set of alkylphenones and compared to a conventional valve-modulator employing sample loops. The thermal modulator showed a reduced modulation-induced pressure impact than valve modulation, resulting in reduced baseline perturbation by a factor of 6; yielding a 6-14-fold improvement in signal-to-noise. A red wine sample was analyzed to demonstrate the potential of the longitudinal on-column thermal modulator for separation of a complex sample. Discrete peaks in the second dimension using the thermal modulator were 30-55% narrower than with the valve modulator. The results shown herein demonstrate the benefits of an active focusing modulator, such as reduced detection limits and increased total peak capacity.

  6. Sol-gel chemistry-based Ucon-coated columns for capillary electrophoresis.

    PubMed

    Hayes, J D; Malik, A

    1997-07-18

    A sol-gel chemistry-based novel approach for the preparation of a Ucon-coated fused-silica capillary column in capillary electrophoresis is presented. In this approach the sol-gel process is carried out inside 25 microm I.D. fused-silica capillaries. The sol solution contained appropriate quantities of an alkoxide-based sol-gel precursor, a polymeric coating material (Ucon), a crosslinking reagent, a surface derivatizing reagent, controlled amounts of water and a catalyst dissolved in a suitable solvent system. The coating procedure involves filling a capillary with the sol solution and allowing the sol-gel process to proceed for an optimum period. Hydrolysis of the alkoxide precursor and polycondensation of the hydrolyzed products with the surface silanol groups and the hydroxy-terminated Ucon molecules lead to the formation of a surface-bonded sol-gel coating on the inner walls of the capillary. The thickness of the coated film can be controlled by varying the reaction time, coating solution composition and experimental conditions. Commercial availability of high purity sol-gel precursors (e.g., TEOS 99.999%), the ease of coating, run-to-run and column-to-column reproducibility, and long column lifetimes make sol-gel coating chemistry very much suitable for being applied in analytical microseparations column technology. Test samples of basic proteins and nucleotides were used to evaluate the column performance. These results show that the sol-gel coating scheme has allowed for the generation of bio-compatible surfaces characterized by high separation efficiencies in CE. For different types of solutes, the sol-gel coated Ucon column consistently provided migration time R.S.D. values of the order of 0.5%.

  7. Evaluation of analytical errors in a clinical chemistry laboratory: a 3 year experience.

    PubMed

    Sakyi, As; Laing, Ef; Ephraim, Rk; Asibey, Of; Sadique, Ok

    2015-01-01

    Proficient laboratory service is the cornerstone of modern healthcare systems and has an impact on over 70% of medical decisions on admission, discharge, and medications. In recent years, there is an increasing awareness of the importance of errors in laboratory practice and their possible negative impact on patient outcomes. We retrospectively analyzed data spanning a period of 3 years on analytical errors observed in our laboratory. The data covered errors over the whole testing cycle including pre-, intra-, and post-analytical phases and discussed strategies pertinent to our settings to minimize their occurrence. We described the occurrence of pre-analytical, analytical and post-analytical errors observed at the Komfo Anokye Teaching Hospital clinical biochemistry laboratory during a 3-year period from January, 2010 to December, 2012. Data were analyzed with Graph Pad Prism 5(GraphPad Software Inc. CA USA). A total of 589,510 tests was performed on 188,503 outpatients and hospitalized patients. The overall error rate for the 3 years was 4.7% (27,520/58,950). Pre-analytical, analytical and post-analytical errors contributed 3.7% (2210/58,950), 0.1% (108/58,950), and 0.9% (512/58,950), respectively. The number of tests reduced significantly over the 3-year period, but this did not correspond with a reduction in the overall error rate (P = 0.90) along with the years. Analytical errors are embedded within our total process setup especially pre-analytical and post-analytical phases. Strategic measures including quality assessment programs for staff involved in pre-analytical processes should be intensified.

  8. An investigation of transient pressure and plasma properties in a pinched plasma column. M.S. Thesis

    NASA Technical Reports Server (NTRS)

    Stover, E. K.; York, T. M.

    1971-01-01

    The transient pinched plasma column generated in a linear Z-pinch was studied experimentally and analytically. The plasma column was investigated experimentally with the following plasma diagnostics: a special rapid response pressure transducer, a magnetic field probe, a voltage probe and discharge luminosity. Axial pressure profiles on the discharge chamber axis were used to identify three characteristic regions of plasma column behavior; they were in temporal sequence: strong axial pressure asymmetry noted early in plasma column lifetime followed by plasma heating in which there is a rapid rise in static pressure and a slight decrease static pressure before plasma column breakup. Plasma column lifetime was approximately 5 microseconds. The axial pressure asymmetry was attributed to nonsimultaneous pinching of the imploding current sheet along the discharge chamber axis. The rapid heating is attributed in part to viscous effects introduced by radial gradients in the axial streaming velocity. Turbulent heating arising from discharge current excitation of the ion acoustic wave instability is also considered a possible heating mechanism.

  9. Diagnosing the radiative and chemical contributions to future changes in tropical column ozone with the UM-UKCA chemistry-climate model

    NASA Astrophysics Data System (ADS)

    Keeble, James; Bednarz, Ewa M.; Banerjee, Antara; Abraham, N. Luke; Harris, Neil R. P.; Maycock, Amanda C.; Pyle, John A.

    2017-11-01

    Chemical and dynamical drivers of trends in tropical total-column ozone (TCO3) for the recent past and future periods are explored using the UM-UKCA (Unified Model HadGEM3-A (Hewitt et al., 2011) coupled with the United Kingdom Chemistry and Aerosol scheme) chemistry-climate model. A transient 1960-2100 simulation is analysed which follows the representative concentration pathway 6.0 (RCP6.0) emissions scenario for the future. Tropical averaged (10° S-10° N) TCO3 values decrease from the 1970s, reach a minimum around 2000 and return to their 1980 values around 2040, consistent with the use and emission of halogenated ozone-depleting substances (ODSs), and their later controls under the Montreal Protocol. However, when the ozone column is subdivided into three partial columns (PCO3) that cover the upper stratosphere (PCO3US), lower stratosphere (PCO3LS) and troposphere (PCO3T), significant differences in the temporal behaviour of the partial columns are seen. Modelled PCO3T values under the RCP6.0 emissions scenario increase from 1960 to 2000 before remaining approximately constant throughout the 21st century. PCO3LS values decrease rapidly from 1960 to 2000 and remain constant from 2000 to 2050, before gradually decreasing further from 2050 to 2100 and never returning to their 1980s values. In contrast, PCO3US values decrease from 1960 to 2000, before increasing rapidly throughout the 21st century and returning to 1980s values by ˜ 2020, and reach significantly higher values by 2100. Using a series of idealised UM-UKCA time-slice simulations with concentrations of well-mixed greenhouse gases (GHGs) and halogenated ODS species set to either year 2000 or 2100 levels, we examine the main processes that drive the PCO3 responses in the three regions and assess how these processes change under different emission scenarios. Finally, we present a simple, linearised model to describe the future evolution of tropical stratospheric column ozone values based on terms

  10. Cytosolic T3-binding protein modulates dynamic alteration of T3-mediated gene expression in cells.

    PubMed

    Takeshige, Keiko; Sekido, Takashi; Kitahara, Jun-ichirou; Ohkubo, Yousuke; Hiwatashi, Dai; Ishii, Hiroaki; Nishio, Shin-ichi; Takeda, Teiji; Komatsu, Mitsuhisa; Suzuki, Satoru

    2014-01-01

    μ-Crystallin (CRYM) is also known as NADPH-dependent cytosolic T3-binding protein. A study using CRYM-null mice suggested that CRYM stores triiodothyronine (T3) in tissues. We previously established CRYM-expressing cells derived from parental GH3 cells. To examine the precise regulation of T3-responsive genes in the presence of CRYM, we evaluated serial alterations of T3-responsive gene expression by changing pericellular T3 concentrations in the media. We estimated the constitutive expression of three T3-responsive genes, growth hormone (GH), deiodinase 1 (Dio1), and deiodinase 2 (Dio2), in two cell lines. Subsequently, we measured the responsiveness of these three genes at 4, 8, 16, and 24 h after adding various concentrations of T3. We also estimated the levels of these mRNAs 24 and 48 h after removing T3. The levels of constitutive expression of GH and Dio1 were low and high in C8 cells, respectively, while Dio2 expression was not significantly different between GH3 and C8 cells. When treated with T3, Dio2 expression was significantly enhanced in C8 cells, while there were no differences in GH or Dio1 expression between GH3 and C8 cell lines. In contrast, removal of T3 retained the mRNA expression of GH and Dio2 in C8 cells. These results suggest that CRYM expression increases and sustains the T3 responsiveness of genes in cells, especially with alteration of the pericellular T3 concentration. The heterogeneity of T3-related gene expression is dependent on cellular CRYM expression in cases of dynamic changes in pericellular T3 concentration.

  11. Dog erythrocyte antigens 1.1, 1.2, 3, 4, 7, and Dal blood typing and cross-matching by gel column technique.

    PubMed

    Kessler, Rebecca J; Reese, Jessica; Chang, Denise; Seth, Mayank; Hale, Anne S; Giger, Urs

    2010-09-01

    Testing for canine blood types other than dog erythrocyte antigen 1.1 (DEA 1.1) is controversial and complicated by reagent availability and methodology. The objectives of this study were to use available gel column technology to develop an extended blood-typing method using polyclonal reagents for DEA 1.1, 1.2, 3, 4, 7, and Dal and to assess the use of gel columns for cross-matching. Dogs (43-75) were typed for DEA 1.1, 1.2, 3, 4, 7, and Dal. METHODS included tube agglutination (Tube) using polyclonal reagents, a commercially available DEA 1.1 gel column test kit (Standard-Gel) using monoclonal reagent, and multiple gel columns (Extended-Gel) using polyclonal reagents. Blood from 10 recipient and 15 donor dogs was typed as described above and cross-matched using the gel column technique. Of 43 dogs typed for DEA 1.1, 23, 25, and 20 dogs were positive using Standard-Gel, Extended-Gel, and Tube, respectively. Typing for DEA 1.2 was not achievable with Extended-Gel. For 75 dogs typed for DEA 3, 4, and 7, concordance of Extended-Gel with Tube was 94.7%, 100%, and 84%, respectively. Dal, determined only by Extended-Gel, was positive for all dogs. Post-transfusion major cross-matches were incompatible in 10 of 14 pairings, but none were associated with demonstrable blood type incompatibilities. Gel column methodology can be adapted for use with polyclonal reagents for detecting DEA 1.1, 3, 4, 7, and Dal. Agglutination reactions are similar between Extended-Gel and Tube, but are more easily interpreted with Extended-Gel. When using gel columns for cross-matching, incompatible blood cross-matches can be detected following sensitization by transfusion, although in this study incompatibilities associated with any tested DEA or Dal antigens were not found. ©2010 American Society for Veterinary Clinical Pathology.

  12. Experimental investigation and numerical simulation of 3He gas diffusion in simple geometries: implications for analytical models of 3He MR lung morphometry.

    PubMed

    Parra-Robles, J; Ajraoui, S; Deppe, M H; Parnell, S R; Wild, J M

    2010-06-01

    Models of lung acinar geometry have been proposed to analytically describe the diffusion of (3)He in the lung (as measured with pulsed gradient spin echo (PGSE) methods) as a possible means of characterizing lung microstructure from measurement of the (3)He ADC. In this work, major limitations in these analytical models are highlighted in simple diffusion weighted experiments with (3)He in cylindrical models of known geometry. The findings are substantiated with numerical simulations based on the same geometry using finite difference representation of the Bloch-Torrey equation. The validity of the existing "cylinder model" is discussed in terms of the physical diffusion regimes experienced and the basic reliance of the cylinder model and other ADC-based approaches on a Gaussian diffusion behaviour is highlighted. The results presented here demonstrate that physical assumptions of the cylinder model are not valid for large diffusion gradient strengths (above approximately 15 mT/m), which are commonly used for (3)He ADC measurements in human lungs. (c) 2010 Elsevier Inc. All rights reserved.

  13. The effects of carbide column to swelling potential and Atterberg limit on expansive soil with column to soil drainage

    NASA Astrophysics Data System (ADS)

    Muamar Rifa'i, Alfian; Setiawan, Bambang; Djarwanti, Noegroho

    2017-12-01

    The expansive soil is soil that has a potential for swelling-shrinking due to changes in water content. Such behavior can exert enough force on building above to cause damage. The use of columns filled with additives such as Calcium Carbide is done to reduce the negative impact of expansive soil behavior. This study aims to determine the effect of carbide columns on expansive soil. Observations were made on swelling and spreading of carbides in the soil. 7 Carbide columns with 5 cm diameter and 20 cm height were installed into the soil with an inter-column spacing of 8.75 cm. Wetting is done through a pipe at the center of the carbide column for 20 days. Observations were conducted on expansive soil without carbide columns and expansive soil with carbide columns. The results showed that the addition of carbide column could reduce the percentage of swelling by 4.42%. Wetting through the center of the carbide column can help spread the carbide into the soil. The use of carbide columns can also decrease the rate of soil expansivity. After the addition of carbide column, the plasticity index value decreased from 71.76% to 4.3% and the shrinkage index decreased from 95.72% to 9.2%.

  14. Time-Fractional Advection-Dispersion Equation (tFADE) to Quantify Aqueous Phase Contaminant Elution from a Trichloroethene (TCE) NAPL Source Zone in Sand Columns

    NASA Astrophysics Data System (ADS)

    Tick, G. R.; Wei, S.; Sun, H.; Zhang, Y.

    2016-12-01

    Pore-scale heterogeneity, NAPL distribution, and sorption/desorption processes can significantly affect aqueous phase elution and mass flux in porous media systems. The application of a scale-independent fractional derivative model (tFADE) was used to simulate elution curves for a series of columns (5 cm, 7 cm, 15 cm, 25 cm, and 80 cm) homogeneously packed with 20/30-mesh sand and distributed with uniform saturations (7-24%) of NAPL phase trichloroethene (TCE). An additional set of columns (7 cm and 25 cm) were packed with a heterogeneous distribution of quartz sand upon which TCE was emplaced by imbibing the immiscible liquid, under stable displacement conditions, to simulate a spill-type process. The tFADE model was able to better represent experimental elution behavior for systems that exhibited extensive long-term concentration tailing requiring much less parameters compared to typical multi-rate mass transfer models (MRMT). However, the tFADE model was not able to effectively simulate the entire elution curve for such systems with short concentration tailing periods since it assumes a power-law distribution for the dissolution rate for TCE. Such limitations may be solved using the tempered fractional derivative model, which can capture the single-rate mass transfer process and therefore the short elution concentration tailing behavior. Numerical solution for the tempered fractional-derivative model in bounded domains however remains a challenge and therefore requires further study. However, the tFADE model shows excellent promise for understanding impacts on concentration elution behavior for systems in which physical heterogeneity, non-uniform NAPL distribution, and pronounced sorption-desorption effects dominate or are present.

  15. Evaluation of Analytical Errors in a Clinical Chemistry Laboratory: A 3 Year Experience

    PubMed Central

    Sakyi, AS; Laing, EF; Ephraim, RK; Asibey, OF; Sadique, OK

    2015-01-01

    Background: Proficient laboratory service is the cornerstone of modern healthcare systems and has an impact on over 70% of medical decisions on admission, discharge, and medications. In recent years, there is an increasing awareness of the importance of errors in laboratory practice and their possible negative impact on patient outcomes. Aim: We retrospectively analyzed data spanning a period of 3 years on analytical errors observed in our laboratory. The data covered errors over the whole testing cycle including pre-, intra-, and post-analytical phases and discussed strategies pertinent to our settings to minimize their occurrence. Materials and Methods: We described the occurrence of pre-analytical, analytical and post-analytical errors observed at the Komfo Anokye Teaching Hospital clinical biochemistry laboratory during a 3-year period from January, 2010 to December, 2012. Data were analyzed with Graph Pad Prism 5(GraphPad Software Inc. CA USA). Results: A total of 589,510 tests was performed on 188,503 outpatients and hospitalized patients. The overall error rate for the 3 years was 4.7% (27,520/58,950). Pre-analytical, analytical and post-analytical errors contributed 3.7% (2210/58,950), 0.1% (108/58,950), and 0.9% (512/58,950), respectively. The number of tests reduced significantly over the 3-year period, but this did not correspond with a reduction in the overall error rate (P = 0.90) along with the years. Conclusion: Analytical errors are embedded within our total process setup especially pre-analytical and post-analytical phases. Strategic measures including quality assessment programs for staff involved in pre-analytical processes should be intensified. PMID:25745569

  16. Ion mobility based on column leaching of South African gold tailings dam with chemometric evaluation.

    PubMed

    Cukrowska, Ewa M; Govender, Koovila; Viljoen, Morris

    2004-07-01

    New column leaching experiments were designed and used as an alternative rapid screening approach to element mobility assessment. In these experiments, field-moist material was treated with an extracting solution to assess the effects of acidification on element mobility in mine tailings. The main advantage of this version of column leaching experiments with partitioned segments is that they give quick information on current element mobility in conditions closely simulating field conditions to compare with common unrepresentative air-dried, sieved samples used for column leaching experiments. Layers from the tailings dump material were sampled and packed into columns. The design of columns allows extracting leachates from each layer. The extracting solutions used were natural (pH 6.8) and acidified (pH 4.2) rainwater. Metals and anions were determined in the leachates. The concentrations of metals (Ca, Mg, Fe, Mn, Al, Cr, Ni, Co, Zn, and Cu) in sample leachates were determined using ICP OES. The most important anions (NO3-, Cl-, and SO4(2)-) were determined using the closed system izotacophoresis ITP analyser. The chemical analytical data from tailings leaching and physico-chemical data from field measurements (including pH, conductivity, redox potential, temperature) were used for chemometric evaluation of element mobility. Principal factor analysis (PFA) was used to evaluate ions mobility from different layers of tailings dump arising from varied pH and redox conditions. It was found that the results from the partitioned column leaching illustrate much better complex processes of metals mobility from tailings dump than the total column. The chemometric data analysis (PFA) proofed the differences in the various layers leachability that are arising from physico-chemical processes due to chemical composition of tailings dump deposit. Copyright 2004 Elsevier Ltd.

  17. Liquid chromatography-tandem mass spectrometry detection of the quaternary ammonium compound mebezonium as an active ingredient in t61.

    PubMed

    Kirschbaum, Katrin M; Grellner, Wolfgang; Rochholz, Gertrud; Musshoff, Frank; Madea, Burkhard

    2011-03-01

    Quaternary ammonium compounds pose an analytical challenge. Mebezonium, a muscle-relaxing agent contained in veterinary euthanasia solution T61, was analyzed in body fluids, organs, and injection sites of a veterinarian by liquid chromatography-tandem mass spectrometry (LC-MS-MS) method. Additionally, embutramide and tetracaine, which are two other active ingredients contained in T61, methadone, xylazine, and analgesics were detected by LC-MS-MS and high-performance liquid chromatography-ultraviolet detection methods. For detection of mebezonium a solid-phase extraction (SPE) combined with ionpairing reagent heptafluorobutyric acid was developed. Separation was achieved on Phenomenex Synergi Hydro RP C(18) column combined with ammonium formate buffer and acetonitrile (pH 3.5). To enrich other drugs, liquid-liquid extraction procedures were used. Most of these drugs were separated on a Restek Allure PFP Propyl column using the mentioned mobile phase. Mebezonium and embutramide were detected in femoral vein serum in concentrations of 10.9 and 2.0 mg/L, respectively. The concentration of xylazine and methadone in serum was 2.0 and 0.4 mg/L, respectively. The LC-MS-MS method with SPE combined with an ion-pairing reagent allowed the quantitation of mebezonium. Methadone was detected in toxic concentrations and was, in combination with xylazine and T61, considered to be the cause of death.

  18. Analytical validation and establishment of reference intervals for a 'high-sensitivity' cardiac troponin-T assay in horses.

    PubMed

    Shields, E; Seiden-Long, I; Massie, S; Passante, S; Leguillette, R

    2016-06-13

    Cardiac troponin-I assays have been validated in horses.'High-sensitivity' cardiac troponin assays are now the standard in human cardiology. Appropriately validate the'high-sensitivity' cardiac Troponin-T (hscTnT) assay for clinical use in horses, establish reference intervals, determine the biological variation, and demonstrate assay utility in selected clinical cases. Analytical validation of the Roche hscTnT assay included within- and between-run precision, linear dose response, limit of quantitation (LoQ), stability, and comparison with cTn-I (iSTAT). Reference intervals and biological variation were determined using adult, healthy, Non-Competition Horses (N = 125) and Racing-Thoroughbreds (N = 178). HscTnT levels were measured in two horses with cardiac pathology. The hscTnT demonstrates acceptable within-run (L1 = 6.5 ng/L, CV 14.9 %, L2 = 10.1 ng/L, CV 8.7 %, L3 = 15.3 ng/L, CV 5.4 %) and between-run precision (L1 = 12.2 ng/L, CV 8.4 %, L2 = 57.0 ng/L, CV 8.4 %, L3 = 256.0 ng/L, CV 9.0 %). The assay was linear from 3 to 391 ng/L. The LoQ was validated at 3 ng/L. Samples demonstrated insignificant decay over freeze-thaw cycle. Comparison with cTnI assay showed excellent correlation (range: 8.0-3535.0 ng/L, R(2) = 0.9996). Reference intervals: The upper 95(th) and 99(th) percentile of the hscTnT population distribution were 6.8 and 16.2 ng/L in Non-Competition Horses, and 14.0 and 23.2 ng/L in Racing-Thoroughbreds. Between-breed, diurnal effect, and between-day variation was below LoQ. Two clinical cases with presumed cardiac pathology had hscTnT levels of 220.9 ng/L and 5723.0 ng/L. This benchmark study is the first to comply with CLSI guidelines, thus further establishing the performance characteristics of the hscTnT assay, and reference intervals in healthy horses. Two clinical cases demonstrated further the clinical utility of the assay.

  19. Gas Chromatograph Method Optimization Trade Study for RESOLVE: 20-meter Column v. 8-meter Column

    NASA Technical Reports Server (NTRS)

    Huz, Kateryna

    2014-01-01

    RESOLVE is the payload on a Class D mission, Resource Prospector, which will prospect for water and other volatile resources at a lunar pole. The RESOLVE payload's primary scientific purpose includes determining the presence of water on the moon in the lunar regolith. In order to detect the water, a gas chromatograph (GC) will be used in conjunction with a mass spectrometer (MS). The goal of the experiment was to compare two GC column lengths and recommend which would be best for RESOLVE's purposes. Throughout the experiment, an Inficon Fusion GC and an Inficon Micro GC 3000 were used. The Fusion had a 20m long column with 0.25mm internal diameter (Id). The Micro GC 3000 had an 8m long column with a 0.32mm Id. By varying the column temperature and column pressure while holding all other parameters constant, the ideal conditions for testing with each column length in their individual instrument configurations were determined. The criteria used for determining the optimal method parameters included (in no particular order) (1) quickest run time, (2) peak sharpness, and (3) peak separation. After testing numerous combinations of temperature and pressure, the parameters for each column length that resulted in the most optimal data given my three criteria were selected. The ideal temperature and pressure for the 20m column were 95 C and 50psig. At this temperature and pressure, the peaks were separated and the retention times were shorter compared to other combinations. The Inficon Micro GC 3000 operated better at lower temperature mainly due to the shorter 8m column. The optimal column temperature and pressure were 70 C and 30psig. The Inficon Micro GC 3000 8m column had worse separation than the Inficon Fusion 20m column, but was able to separate water within a shorter run time. Therefore, the most significant tradeoff between the two column lengths was peak separation of the sample versus run time. After performing several tests, it was concluded that better

  20. Novel hybrid columns made of ultra-high performance concrete and fiber reinforced polymers

    NASA Astrophysics Data System (ADS)

    Zohrevand, Pedram

    The application of advanced materials in infrastructure has grown rapidly in recent years mainly because of their potential to ease the construction, extend the service life, and improve the performance of structures. Ultra-high performance concrete (UHPC) is one such material considered as a novel alternative to conventional concrete. The material microstructure in UHPC is optimized to significantly improve its material properties including compressive and tensile strength, modulus of elasticity, durability, and damage tolerance. Fiber-reinforced polymer (FRP) composite is another novel construction material with excellent properties such as high strength-to-weight and stiffness-to-weight ratios and good corrosion resistance. Considering the exceptional properties of UHPC and FRP, many advantages can result from the combined application of these two advanced materials, which is the subject of this research. The confinement behavior of UHPC was studied for the first time in this research. The stress-strain behavior of a series of UHPC-filled fiber-reinforced polymer (FRP) tubes with different fiber types and thicknesses were tested under uniaxial compression. The FRP confinement was shown to significantly enhance both the ultimate strength and strain of UHPC. It was also shown that existing confinement models are incapable of predicting the behavior of FRP-confined UHPC. Therefore, new stress-strain models for FRP-confined UHPC were developed through an analytical study. In the other part of this research, a novel steel-free UHPC-filled FRP tube (UHPCFFT) column system was developed and its cyclic behavior was studied. The proposed steel-free UHPCFFT column showed much higher strength and stiffness, with a reasonable ductility, as compared to its conventional reinforced concrete (RC) counterpart. Using the results of the first phase of column tests, a second series of UHPCFFT columns were made and studied under pseudo-static loading to study the effect of column

  1. Abdominal girth and vertebral column length aid in predicting intrathecal hyperbaric bupivacaine dose for elective cesarean section

    PubMed Central

    Wei, Chang-Na; Zhou, Qing-He; Wang, Li-Zhong

    2017-01-01

    Abstract Currently, there is no consensus on how to determine the optimal dose of intrathecal bupivacaine for an individual undergoing an elective cesarean section. In this study, we developed a regression equation between intrathecal 0.5% hyperbaric bupivacaine volume and abdominal girth and vertebral column length, to determine a suitable block level (T5) for elective cesarean section patients. In phase I, we analyzed 374 parturients undergoing an elective cesarean section that received a suitable dose of intrathecal 0.5% hyperbaric bupivacaine after a combined spinal-epidural (CSE) was performed at the L3/4 interspace. Parturients with T5 blockade to pinprick were selected for establishing the regression equation between 0.5% hyperbaric bupivacaine volume and vertebral column length and abdominal girth. Six parturient and neonatal variables, intrathecal 0.5% hyperbaric bupivacaine volume, and spinal anesthesia spread were recorded. Bivariate line correlation analyses, multiple line regression analyses, and 2-tailed t tests or chi-square test were performed, as appropriate. In phase II, another 200 parturients with CSE for elective cesarean section were enrolled to verify the accuracy of the regression equation. In phase I, a total of 143 parturients were selected to establish the following regression equation: YT5 = 0.074X1 − 0.022X2 − 0.017 (YT5 = 0.5% hyperbaric bupivacaine volume for T5 block level; X1 = vertebral column length; and X2 = abdominal girth). In phase II, a total of 189 participants were enrolled in the study to verify the accuracy of the regression equation, and 155 parturients with T5 blockade were deemed eligible, which accounted for 82.01% of all participants. This study evaluated parturients with T5 blockade to pinprick after a CSE for elective cesarean section to establish a regression equation between parturient vertebral column length and abdominal girth and 0.5% hyperbaric intrathecal bupivacaine volume. This equation

  2. Abdominal girth and vertebral column length aid in predicting intrathecal hyperbaric bupivacaine dose for elective cesarean section.

    PubMed

    Wei, Chang-Na; Zhou, Qing-He; Wang, Li-Zhong

    2017-08-01

    Currently, there is no consensus on how to determine the optimal dose of intrathecal bupivacaine for an individual undergoing an elective cesarean section. In this study, we developed a regression equation between intrathecal 0.5% hyperbaric bupivacaine volume and abdominal girth and vertebral column length, to determine a suitable block level (T5) for elective cesarean section patients.In phase I, we analyzed 374 parturients undergoing an elective cesarean section that received a suitable dose of intrathecal 0.5% hyperbaric bupivacaine after a combined spinal-epidural (CSE) was performed at the L3/4 interspace. Parturients with T5 blockade to pinprick were selected for establishing the regression equation between 0.5% hyperbaric bupivacaine volume and vertebral column length and abdominal girth. Six parturient and neonatal variables, intrathecal 0.5% hyperbaric bupivacaine volume, and spinal anesthesia spread were recorded. Bivariate line correlation analyses, multiple line regression analyses, and 2-tailed t tests or chi-square test were performed, as appropriate. In phase II, another 200 parturients with CSE for elective cesarean section were enrolled to verify the accuracy of the regression equation.In phase I, a total of 143 parturients were selected to establish the following regression equation: YT5 = 0.074X1 - 0.022X2 - 0.017 (YT5 = 0.5% hyperbaric bupivacaine volume for T5 block level; X1 = vertebral column length; and X2 = abdominal girth). In phase II, a total of 189 participants were enrolled in the study to verify the accuracy of the regression equation, and 155 parturients with T5 blockade were deemed eligible, which accounted for 82.01% of all participants.This study evaluated parturients with T5 blockade to pinprick after a CSE for elective cesarean section to establish a regression equation between parturient vertebral column length and abdominal girth and 0.5% hyperbaric intrathecal bupivacaine volume. This equation can accurately

  3. Hydrodynamic flow in capillary-channel fiber columns for liquid chromatography.

    PubMed

    Stanelle, Rayman D; Sander, Lane C; Marcus, R Kenneth

    2005-12-23

    The flow characteristics of capillary-channel polymer (C-CP) fiber liquid chromatographic (LC) columns have been investigated. The C-CP fibers are manufactured with eight longitudinal grooves (capillary channels) extending the length of the fibers. Three C-CP fiber examples were studied, with fiber dimensions ranging from approximately 35 microm to 65 microm, and capillary-channel dimensions ranging from approximately 6 microm to 35 microm. The influence of fiber packing density and column inner diameter on peak asymmetry, peak width, and run-to-run reproducibility have been studied for stainless steel LC columns packed with polyester (PET) and polypropylene (PP) C-CP fibers. The van Deemter A-term was evaluated as a function of fiber packing density (approximately 0.3 g/cm(3)-0.75 g/cm(3)) for columns of 4.6 mm inner diameter (i.d.) and at constant packing densities for 1.5 mm, 3.2 mm, 4.6 mm, and 7.7 mm i.d. columns. Although column diameter had little influence on the eluting peak widths, peak asymmetry increased with increasing column diameter. The A-terms for the C-CP fiber packed columns are somewhat larger than current commercial, microparticulate-packed columns, and means for improvement are discussed. Applications in the area of protein (macromolecule) separations appear the most promising at this stage of the system development.

  4. A high-throughput, simultaneous analysis of carotenoids, chlorophylls and tocopherol using sub two micron core shell technology columns.

    PubMed

    Chebrolu, Kranthi K; Yousef, Gad G; Park, Ryan; Tanimura, Yoshinori; Brown, Allan F

    2015-09-15

    A high-throughput, robust and reliable method for simultaneous analysis of five carotenoids, four chlorophylls and one tocopherol was developed for rapid screening large sample populations to facilitate molecular biology and plant breeding. Separation was achieved for 10 known analytes and four unknown carotenoids in a significantly reduced run time of 10min. Identity of the 10 analytes was confirmed by their UV-Vis absorption spectras. Quantification of tocopherol, carotenoids and chlorophylls was performed at 290nm, 460nm and 650nm respectively. In this report, two sub two micron particle core-shell columns, Kinetex from Phenomenex (1.7μm particle size, 12% carbon load) and Cortecs from Waters (1.6μm particle size, 6.6% carbon load) were investigated and their separation efficiencies were evaluated. The peak resolutions were >1.5 for all analytes except for chlorophyll-a' with Cortecs column. The ruggedness of this method was evaluated in two identical but separate instruments that produced CV<2 in peak retentions for nine out of 10 analytes separated. Copyright © 2015 Elsevier B.V. All rights reserved.

  5. A novel in situ strategy for the preparation of a β-cyclodextrin/polydopamine-coated capillary column for capillary electrochromatography enantioseparations.

    PubMed

    Guo, Heying; Niu, Xiaoying; Pan, Congjie; Yi, Tao; Chen, Hongli; Chen, Xingguo

    2017-06-01

    Inspired by the chiral recognition ability of β-cyclodextrin and the natural adhesive properties of polydopamine under alkaline conditions, in this study, a rapid and in situ modification strategy was developed to fabricate β-cyclodextrin/polydopamine composite material coated-capillary columns for open tubular capillary electrochromatography. The results of scanning electron microscopy, FTIR spectroscopy, streaming potential, and electro-osmotic flow studies indicated that β-cyclodextrin/polydopamine was successfully fixed on the inner wall of the capillary column. This coating can be achieved within 1 h affording a greatly reduced capillary preparation time. The performance of the β-cyclodextrin/polydopamine-coated capillary was validated by the analysis of seven pairs of chiral analytes, namely epinephrine, norepinephrine, isoprenaline, terbutaline, verapamil, tryptophane, carvedilol. Good enantioseparation efficiencies were achieved for all. For three consecutive runs, the relative standard deviations for the migration times of the analytes for intraday, interday, and column-to-column repeatability were in the range of 0.41-1.74, 1.03-4.18, and 1.66-8.24%, respectively. Moreover, the separation efficiency of the β-cyclodextrin/polydopamine-coated capillary column did not decrease obviously over 90 runs. The strategy should also be feasible to introduce and immobilize other chiral selectors on the inner walls surface of capillary columns. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Comparison of only T3 and T3T4 sympathectomy for axillary hyperhidrosis regarding treatment effect and compensatory sweating

    PubMed Central

    Yuncu, Gökhan; Turk, Figen; Ozturk, Gökhan; Atinkaya, Cansel

    2013-01-01

    OBJECTIVES Patients diagnosed with axillary hyperhidrosis can face psychosocial issues that can ultimately hinder their quality of life both privately and socially. The routine treatment for axillary hyperhidrosis is T3T4 sympathectomy, but compensatory sweating is a serious side effect that is commonly seen with this approach. This study was designed to evaluate whether a T3 sympathectomy was effective for the treatment of axillary hyperhidrosis and whether this treatment led to less compensatory sweating than T3T4 sympathectomies among our 60-patient population. METHODS One hundred and twenty endoscopic thoracic sympathectomies were performed on 60 patients who had axillary hyperhidrosis. The sympathectomies were accomplished by means of a single-lumen endotracheal tube and a single port. The axillary hyperhidrosis patients were randomly divided into two groups with 17 patients in Group 1 undergoing T3T4 sympathectomies and 43 in Group 2 undergoing only T3 sympathectomies. We analysed the data associated with the resolution of axillary hyperhidrosis, the degree of patient satisfaction with the surgical outcome and the quality of life in parallel with compensatory sweating after the procedure as reported by the patient and confirmed by the examiner. Moreover, the results were compared statistically. RESULTS No statistically significant difference was observed between the groups based on age (P = 0.56), gender (P = 0.81), duration of the surgery (P = 0.35) or postoperative satisfaction levels (P = 0.45). However, the incidence and degree of compensatory sweating were lower in the T3 group than the T3T4 group at the 1-year follow-up (P = 0.008). CONCLUSIONS T3 sympathectomy was as effective as T3T4 sympathectomy for the treatment of axillary hyperhidrosis based on the patients’ reported postoperative satisfaction, and the T3 group demonstrated lower compensatory sweating at the 1-year follow-up. PMID:23644731

  7. Anion-exchange behavior of several alkylsilica reversed-phase columns.

    PubMed

    Marchand, D H; Snyder, L R

    2008-10-31

    Some alkylsilica columns carry a positive charge at low pH, as determined by anion-exchange with nitrate ion. In the present study, the relative positive charge for 14 alkylsilica columns was measured for a mobile-phase pH 3.0. All but 3 of these columns were found to carry a significant positive charge under these conditions. The relative positive charge on these columns was found to correlate approximately with two other column characteristics: relative cation-exchange behavior as measured by the hydrophobic-subtraction model (values of C-2.8), and slow equilibration of the column to changes in the mobile-phase-as evidenced by a slow change in the retention of anionic and cationic solutes with time. The origin of this positive charge may arise from the bonding process, with incorporation of some cationic entity into the stationary phase.

  8. Hydrodynamic chromatography of macromolecules using polymer monolithic columns.

    PubMed

    Edam, Rob; Eeltink, Sebastiaan; Vanhoutte, Dominique J D; Kok, Wim Th; Schoenmakers, Peter J

    2011-12-02

    The selectivity window of size-based separations of macromolecules was tailored by tuning the macropore size of polymer monolithic columns. Monolithic materials with pore sizes ranging between 75 nm and 1.2 μm were prepared in situ in large I.D. columns. The dominant separation mechanism was hydrodynamic chromatography in the flow-through pores. The calibration curves for synthetic polymers matched with the elution behavior by HDC separations in packed columns with 'analyte-to-pore' aspect ratios (λ) up to 0.2. For large-macropore monoliths, a deviation in retention behavior was observed for small polystyrene polymers (M(r)<20 kDa), which may be explained by a combined HDC-SEC mechanism for λ<0.02. The availability of monoliths with very narrow pore sizes allowed investigation of separations at high λ values. For high-molecular weight polymers (M(r)>300,000 Da) confined in narrow channels, the separation strongly depended on flow rate. Flow-rate dependent elution behavior was evaluated by calculation of Deborah numbers and confirmed to be outside the scope of classic shear deformation or slalom chromatography. Shear-induced forces acting on the periphery of coiled polymers in solution may be responsible for flow-rate dependent elution. Copyright © 2011 Elsevier B.V. All rights reserved.

  9. Simultaneous determination of 1- and 2-naphthol in human urine using on-line clean-up column-switching liquid chromatography-fluorescence detection.

    PubMed

    Preuss, Ralf; Angerer, Jürgen

    2004-03-05

    We developed a new 3-D HPLC method for on-line clean-up and simultaneous quantification of two important naphthalene metabolites, 1-naphthol and 2-naphthol, in human urine. Except an enzymatic hydrolysis no further sample pre-treatment is necessary. The metabolites are stripped from urinary matrix by on-line extraction on a restricted access material pre-column (RAM RP-8), transferred in backflush mode onto a silica-based CN-(cyano)phase column for further purification from interfering substances. By another successive column switching step both analytes are transferred with a minimum of overlapping interferences onto a C12 bonded reversed phase column with trimethylsilyl endcapping where the final separation is carried out. The entire arrangement is software controlled. Eluting analytes are quantified by fluorescence detection (227/430 nm) after an external calibration. Within a total run time of 40 min we can selectively quantify both naphthols with detection limits in the lower ppb range (1.5 and 0.5 microg/l for 1- and 2-naphthol, respectively) with excellent reliability (ensured by precision, accuracy, matrix-independency and FIOH quality assurance program participation). First results on a collective of 53 occupationally non exposed subjects showed mean levels of 11.0 microg/l (1-naphthol) and 12.9 microg/l (2-naphthol). Among smokers (n=21) a significantly elevated mean level of urinary naphthols was determined (1-naphthol: 19.2 microg/l and 2-naphthol: 23.7 microg/l) in comparison to non smokers (n=32; 1-naphthol: 5.6 microg/l, 2-naphthol: 5.6 microg/l).

  10. High-field fMRI unveils orientation columns in humans.

    PubMed

    Yacoub, Essa; Harel, Noam; Ugurbil, Kâmil

    2008-07-29

    Functional (f)MRI has revolutionized the field of human brain research. fMRI can noninvasively map the spatial architecture of brain function via localized increases in blood flow after sensory or cognitive stimulation. Recent advances in fMRI have led to enhanced sensitivity and spatial accuracy of the measured signals, indicating the possibility of detecting small neuronal ensembles that constitute fundamental computational units in the brain, such as cortical columns. Orientation columns in visual cortex are perhaps the best known example of such a functional organization in the brain. They cannot be discerned via anatomical characteristics, as with ocular dominance columns. Instead, the elucidation of their organization requires functional imaging methods. However, because of insufficient sensitivity, spatial accuracy, and image resolution of the available mapping techniques, thus far, they have not been detected in humans. Here, we demonstrate, by using high-field (7-T) fMRI, the existence and spatial features of orientation- selective columns in humans. Striking similarities were found with the known spatial features of these columns in monkeys. In addition, we found that a larger number of orientation columns are devoted to processing orientations around 90 degrees (vertical stimuli with horizontal motion), whereas relatively similar fMRI signal changes were observed across any given active column. With the current proliferation of high-field MRI systems and constant evolution of fMRI techniques, this study heralds the exciting prospect of exploring unmapped and/or unknown columnar level functional organizations in the human brain.

  11. Spatio-temporal interpolation of soil moisture in 3D+T using automated sensor network data

    NASA Astrophysics Data System (ADS)

    Gasch, C.; Hengl, T.; Magney, T. S.; Brown, D. J.; Gräler, B.

    2014-12-01

    Soil sensor networks provide frequent in situ measurements of dynamic soil properties at fixed locations, producing data in 2- or 3-dimensions and through time (2D+T and 3D+T). Spatio-temporal interpolation of 3D+T point data produces continuous estimates that can then be used for prediction at unsampled times and locations, as input for process models, and can simply aid in visualization of properties through space and time. Regression-kriging with 3D and 2D+T data has successfully been implemented, but currently the field of geostatistics lacks an analytical framework for modeling 3D+T data. Our objective is to develop robust 3D+T models for mapping dynamic soil data that has been collected with high spatial and temporal resolution. For this analysis, we use data collected from a sensor network installed on the R.J. Cook Agronomy Farm (CAF), a 37-ha Long-Term Agro-Ecosystem Research (LTAR) site in Pullman, WA. For five years, the sensors have collected hourly measurements of soil volumetric water content at 42 locations and five depths. The CAF dataset also includes a digital elevation model and derivatives, a soil unit description map, crop rotations, electromagnetic induction surveys, daily meteorological data, and seasonal satellite imagery. The soil-water sensor data, combined with the spatial and temporal covariates, provide an ideal dataset for developing 3D+T models. The presentation will include preliminary results and address main implementation strategies.

  12. Exogenous factors contributing to column bed heterogeneity: Part 1: Consequences of 'air' injections in liquid chromatography.

    PubMed

    Samuelsson, Jörgen; Fornstedt, Torgny; Shalliker, Andrew

    2015-08-07

    It has been shown that not only the packing homogeneity, but also factors external to the column bed, such as, frits and distributors can have important effects on the column performance. This current communication is the first in a series focusing on the impact of exogenous factors on the column bed heterogeneity. This study is based on several observations by us and others that chromatographic runs often, for technical reasons, include more or less portions of air in the injections. It is therefore extremely important to find out the impact of air on the column performance, the reliability of the results derived from analyses where air was injected, and the effect on the column homogeneity. We used a photographic approach for visualising the air transport phenomena, and found that the air transport through the column is comprised of many different types of transport phenomena, such as laminal flow, viscous fingering like flows, channels and bulbs, and pulsations. More particularly, the air clouds within the column definitely interact in the adsorption, i.e. mobile phase adsorbed to the column surface is displaced. In addition, irrespective of the type of air transport phenomena, the air does not penetrate the column homogeneously. This process is strongly flow dependent. In this work we study air transport both in an analytical scale and a semi-prep column. Copyright © 2015. Published by Elsevier B.V.

  13. Inelastic column behavior

    NASA Technical Reports Server (NTRS)

    Duberg, John E; Wilder, Thomas W , III

    1952-01-01

    The significant findings of a theoretical study of column behavior in the plastic stress range are presented. When the behavior of a straight column is regarded as the limiting behavior of an imperfect column as the initial imperfection (lack of straightness) approaches zero, the departure from the straight configuration occurs at the tangent-modulus load. Without such a concept of the behavior of a straight column, one is led to the unrealistic conclusion that lateral deflection of the column can begin at any load between the tangent-modulus value and the Euler load, based on the original elastic modulus. A family of curves showing load against lateral deflection is presented for idealized h-section columns of various lengths and of various materials that have a systematic variation of their stress-strain curves.

  14. Repeatability of the efficiency of columns packed with sub-3μm core-shell particles: Part I. 2.6μm Kinetex-C(18) particles in 4.6mm and 2.1mm×100mm column formats.

    PubMed

    Gritti, Fabrice; Guiochon, Georges

    2012-08-24

    The column-to-column repeatability of the mass transfer mechanism in columns packed with sub-3μm shell particles was investigated. The parameters of this mechanism were measured for twelve columns (six 2.1mm×100mm and six 4.6mm×100mm) packed with the same batch of 2.6μm Kinetex-C(18) particles (Phenomenex, CA, USA). For both series, the manufacturer provided columns at different positions in the efficiency distribution given by the quality test control. Three compounds were used, uracil, naphthalene and insulin. The reduced longitudinal diffusion term was measured with the peak parking (PP) method, the reduced solid-liquid mass transfer resistance term was given by a combination of the PP results and a model of effective diffusion in ternary composite materials (non-porous cores, concentric porous shell, and eluent matrix), validated previously. The overall eddy diffusion term was obtained by subtraction of these two HETP terms from the overall reduced HETP measured by numerical integration of the entire peak profiles. The results demonstrate that the dispersion of the column efficiencies is only due to the random nature of the packing process. At the highest reduced velocity achieved, the relative standard deviations (RSDs) of the eddy diffusion term for the 2.1mm I.D. columns were ca. 7% and 3% for the low molecular weight compounds and for insulin, respectively. For the 4.6mm I.D. columns, these RSDs were 15% and 5%, respectively. The larger RSDs for the 4.6mm I.D. columns is explained by the exceptionally low value of the eddy diffusion term. Copyright © 2012 Elsevier B.V. All rights reserved.

  15. High performance liquid chromatography column efficiency enhancement by zero dead volume recycling and practical approach using park and recycle arrangement.

    PubMed

    Minarik, Marek; Franc, Martin; Minarik, Milan

    2018-06-15

    A new instrumental approach to recycling HPLC is described. The concept is based on fast reintroduction of incremental peak sections back onto the separation column. The re-circulation is performed within a closed loop containing only the column and two synchronized switching valves. By having HPLC pump out of the cycle, the method minimizes peak broadening due to dead volume. As a result the efficiency is dramatically increased allowing for the most demanding analytical applications. In addition, a parking loop is employed for temporary storage of analytes from the middle section of the separated mixture prior to their recycling. Copyright © 2018 Elsevier B.V. All rights reserved.

  16. Steady-State Serum T3 Concentrations for 48 Hours Following the Oral Administration of a Single Dose of 3,5,3'-Triiodothyronine Sulfate (T3S).

    PubMed

    Santini, Ferruccio; Giannetti, Monica; Ricco, Ilaria; Querci, Giorgia; Saponati, Giorgio; Bokor, Daniela; Rivolta, Giovanni; Bussi, Simona; Braverman, Lewis E; Vitti, Paolo; Pinchera, Aldo

    2014-07-01

    Sulfate conjugation of thyroid hormones is an alternate metabolic pathway that facilitates the biliary and urinary excretion of iodothyronines and enhances their deiodination rate, leading to the generation of inactive metabolites. A desulfating pathway reverses this process, and thyromimetic effects have been observed following the parenteral administration of 3,5,3'-triiodothyronine (T3) sulfate (T3S) in rats. The present study investigated whether T3S is absorbed after oral administration in humans and if it represents a source of T3. Twenty-eight hypothyroid patients (7 men and 21 women; mean age, 44 ± 11 years) who had a thyroidectomy for thyroid carcinoma were enrolled. Replacement thyroid hormone therapy was withdrawn (42 days for thyroxine, 14 days for T3) prior to 131I remnant ablation. A single oral dose of 20, 40, 80 (4 patients/group), or 160 μg (16 patients/group) of T3S was administered 3 days before the planned administration of 131I. Blood samples for serum T3S and total T3 (TT3) concentrations were obtained at various times up to 48 hours after T3S administration. At all T3S doses, serum T3S concentrations increased, reaching a peak at 2 to 4 hours and progressively returning to basal levels within 8 to 24 hours. The T3S maximum concentration (Cmax) and area under the 0- to 48-hour concentration-time curve (AUC0-48h) were directly and significantly related to the administered dose. An increase in serum TT3 concentration was observed (significant after 1 hour), and the concentration increased further at 2 and 4 hours and then remained steady up to 48 hours after T3S administration. There was a significant direct correlation between the TT3 AUC0-48h and the administered dose of T3S. No changes in serum free thyroxine (T4) concentrations during the entire study period were observed, whereas serum thyroid-stimulating hormone levels increased slightly at 48 hours, but this was not related to the dose of T3S. No adverse events were reported. (1) T3S is

  17. On-line hyphenation of solid-phase extraction to chromatographic separation of sulfonamides with fused-core columns in sequential injection chromatography.

    PubMed

    Batista, Alex D; Chocholouš, Petr; Satínský, Dalibor; Solich, Petr; Rocha, Fábio R P

    2015-02-01

    On-line sample pretreatment (clean-up and analyte preconcentration) is for the first time coupled to sequential injection chromatography. The approach combines anion-exchange solid-phase extraction and the highly effective pentafluorophenylpropyl (F5) fused-core particle column for separation of eight sulfonamide antibiotics with similar structures (sulfathiazole, sulfanilamide, sulfacetamide, sulfadiazine, sulfamerazine, sulfadimidine, sulfamethoxazole and sulfadimethoxine). The stationary phase was selected after a critical comparison of the performance achieved by three fused-core reversed phase columns (Ascentis(®) Express RP-Amide, Phenyl-Hexyl, and F5) and two monolithic columns (Chromolith(®) High Resolution RP-18 and CN). Acetonitrile and acetate buffer pH 5.0 at 0.60 mL min(-1) were used as mobile phase to perform the separations before spectrophotometric detection. The first mobile phase was successfully used as eluent from SPE column ensuring transfer of a narrow zone to the chromatographic column. Enrichment factors up to 39.2 were achieved with a 500 µL sample volume. The developed procedure showed analysis time <10.5 min, resolutions >1.83 with peak symmetry ≤1.52, LODs between 4.9 and 27 µg L(-1), linear response ranges from 30.0 to 1000.0 µg L(-1) (r(2)>0.996) and RSDs of peak heights <2.9% (n=6) at a 100 µg L(-1) level and enabled the screening control of freshwater samples contaminated at the 100 µg L(-1) level. The proposed approach expanded the analytical potentiality of SIC and avoided the time-consuming batch sample pretreatment step, thus minimizing risks of sample contamination and analyte losses. Copyright © 2014 Elsevier B.V. All rights reserved.

  18. Direct and simultaneous analysis of loxoprofen and its diastereometric alcohol metabolites in human serum by on-line column switching liquid chromatography and its application to a pharmacokinetic study.

    PubMed

    Cho, Hea-Young; Park, Chan-Ho; Lee, Yong-Bok

    2006-05-01

    A simple, rapid, and accurate column-switching liquid chromatography method was developed and validated for direct and simultaneous analysis of loxoprofen and its metabolites (trans- and cis-alcohol metabolites) in human serum. After direct serum injection into the system, deproteinization and trace enrichment occurred on a Shim-pack MAYI-ODS pretreatment column (10 mm x 4.6 mm i.d.) by an eluent consisting of 20 mM phosphate buffer (pH 6.9)/acetonitrile (95/5, v/v) and 0.1% formic acid. The drug trapped by the pretreatment column was introduced to the Shim-pack VP-ODS analytical column (150 mm x 4.6 mm i.d.) using acetonitrile/water (45/55, v/v) containing 0.1% formic acid when the 6-port valve status was switched. Ketoprofen was used as the internal standard. The analysis was monitored on a UV detector at 225 nm. The chromatograms showed good resolution, sensitivity, and no interference by human serum. Coefficients of variations (CV%) and recoveries for loxoprofen and its metabolites were below 15 and over 95%, respectively, in the concentration range of 0.1-20 microg/ml. With UV detection, the limit of quantitation was 0.1 microg/ml, and good linearity (r = 0.999) was observed for all the compounds with 50 microl serum samples. The mean absolute recoveries of loxoprofen, trans- and cis-alcohol for human serum were 89.6 +/- 3.9, 93.5 +/- 3.2, and 93.7 +/- 4.3%, respectively. Stability studies showed that loxoprofen and its metabolites in human serum were stable during storage and the assay procedure. This analytical method showed excellent sensitivity with small sample volume (50 microl), good precision, accuracy, and speed (total analytical time 18 min), without any loss in chromatographic efficiency. This method was successfully applied to the pharmacokinetic study of loxoprofen in human volunteers following a single oral administration of loxoprofen sodium (60 mg, anhydrate) tablet.

  19. JCE Feature Columns

    NASA Astrophysics Data System (ADS)

    Holmes, Jon L.

    1999-05-01

    The Features area of JCE Online is now readily accessible through a single click from our home page. In the Features area each column is linked to its own home page. These column home pages also have links to them from the online Journal Table of Contents pages or from any article published as part of that feature column. Using these links you can easily find abstracts of additional articles that are related by topic. Of course, JCE Online+ subscribers are then just one click away from the entire article. Finding related articles is easy because each feature column "site" contains links to the online abstracts of all the articles that have appeared in the column. In addition, you can find the mission statement for the column and the email link to the column editor that I mentioned above. At the discretion of its editor, a feature column site may contain additional resources. As an example, the Chemical Information Instructor column edited by Arleen Somerville will have a periodically updated bibliography of resources for teaching and using chemical information. Due to the increase in the number of these resources available on the WWW, it only makes sense to publish this information online so that you can get to these resources with a simple click of the mouse. We expect that there will soon be additional information and resources at several other feature column sites. Following in the footsteps of the Chemical Information Instructor, up-to-date bibliographies and links to related online resources can be made available. We hope to extend the online component of our feature columns with moderated online discussion forums. If you have a suggestion for an online resource you would like to see included, let the feature editor or JCE Online (jceonline@chem.wisc.edu) know about it. JCE Internet Features JCE Internet also has several feature columns: Chemical Education Resource Shelf, Conceptual Questions and Challenge Problems, Equipment Buyers Guide, Hal's Picks, Mathcad

  20. Column Liquid Chromatography.

    ERIC Educational Resources Information Center

    Majors, Ronald E.; And Others

    1984-01-01

    Reviews literature covering developments of column liquid chromatography during 1982-83. Areas considered include: books and reviews; general theory; columns; instrumentation; detectors; automation and data handling; multidimensional chromatographic and column switching techniques; liquid-solid chromatography; normal bonded-phase, reversed-phase,…

  1. Evaluation of punching shear strength of flat slabs supported on rectangular columns

    NASA Astrophysics Data System (ADS)

    Filatov, Valery

    2018-03-01

    The article presents the methodology and results of an analytical study of structural parameters influence on the value of punching force for the joint of columns and flat reinforced concrete slab. This design solution is typical for monolithic reinforced concrete girderless frames, which have a wide application in the construction of high-rise buildings. As the results of earlier studies show the punching shear strength of slabs at rectangular columns can be lower than at square columns with a similar length of the control perimeter. The influence of two structural parameters on the punching strength of the plate is investigated - the ratio of the side of the column cross-section to the effective depth of slab C/d and the ratio of the sides of the rectangular column Cmax/Cmin. According to the results of the study, graphs of reduction the control perimeter depending on the structural parameters are presented for columns square and rectangular cross-sections. Comparison of results obtained by proposed approach and MC2010 simplified method are shown, that proposed approach gives a more conservative estimate of the influence of the structural parameters. A significant influence of the considered structural parameters on punching shear strength of reinforced concrete slabs is confirmed by the results of experimental studies. The results of the study confirm the necessity of taking into account the considered structural parameters when calculating the punching shear strength of flat reinforced concrete slabs and further development of code design methods.

  2. Capacity for cooperative binding of thyroid hormone (T3) receptor dimers defines wild type T3 response elements.

    PubMed

    Brent, G A; Williams, G R; Harney, J W; Forman, B M; Samuels, H H; Moore, D D; Larsen, P R

    1992-04-01

    Thyroid hormone response elements (T3REs) have been identified in a variety of promoters including those directing expression of rat GH (rGH), alpha-myosin heavy chain (rMHC), and malic enzyme (rME). A detailed biochemical and genetic analysis of the rGH element has shown that it consists of three hexamers related to the consensus [(A/G)GGT(C/A)A]. We have extended this analysis to the rMHC and rME elements. Binding of highly purified thyroid hormone receptor (T3R) to T3REs was determined using the gel shift assay, and thyroid hormone (T3) induction was measured in transient tranfections. We show that the wild type version of each of the three elements binds T3R dimers cooperatively. Mutational analysis of the rMHC and rME elements identified domains important for binding T3R dimers and allowed a direct determination of the relationship between T3R binding and function. In each element two hexamers are required for dimer binding, and mutations that interfere with dimer formation significantly reduce T3 induction. Similar to the rGH element, the rMHC T3RE contains three hexameric domains arranged as a direct repeat followed by an inverted copy, although the third domain is weaker than in rGH. All three are required for full function and T3R binding. The rME T3RE is a two-hexamer direct repeat T3RE, which also binds T3R monomer and dimer. Across a series of mutant elements, there was a strong correlation between dimer binding in vitro and function in vivo for rMHC (r = 0.99, P less than 0.01) and rME (r = 0.67, P less than 0.05) T3REs. Our results demonstrate a similar pattern of T3R dimer binding to a diverse array of hexameric sequences and arrangements in three wild type T3REs. Addition of nuclear protein enhanced T3R binding but did not alter the specificity of binding to wild type or mutant elements. Binding of purified T3R to T3REs was highly correlated with function, both with and without the addition of nuclear protein. T3R dimer formation is the common

  3. Relationship Between Column-Density and Surface Mixing Ratio: Statistical Analysis of O3 and NO2 Data from the July 2011 Maryland DISCOVER-AQ Mission

    NASA Technical Reports Server (NTRS)

    Flynn, Clare; Pickering, Kenneth E.; Crawford, James H.; Lamsol, Lok; Krotkov, Nickolay; Herman, Jay; Weinheimer, Andrew; Chen, Gao; Liu, Xiong; Szykman, James; hide

    2014-01-01

    To investigate the ability of column (or partial column) information to represent surface air quality, results of linear regression analyses between surface mixing ratio data and column abundances for O3 and NO2 are presented for the July 2011 Maryland deployment of the DISCOVER-AQ mission. Data collected by the P-3B aircraft, ground-based Pandora spectrometers, Aura/OMI satellite instrument, and simulations for July 2011 from the CMAQ air quality model during this deployment provide a large and varied data set, allowing this problem to be approached from multiple perspectives. O3 columns typically exhibited a statistically significant and high degree of correlation with surface data (R(sup 2) > 0.64) in the P- 3B data set, a moderate degree of correlation (0.16 < R(sup 2) < 0.64) in the CMAQ data set, and a low degree of correlation (R(sup 2) < 0.16) in the Pandora and OMI data sets. NO2 columns typically exhibited a low to moderate degree of correlation with surface data in each data set. The results of linear regression analyses for O3 exhibited smaller errors relative to the observations than NO2 regressions. These results suggest that O3 partial column observations from future satellite instruments with sufficient sensitivity to the lower troposphere can be meaningful for surface air quality analysis.

  4. Gradient HPLC of antibiotics in urine, ground water, chicken muscle, hospital wastewater, and pharmaceutical samples using C-18 and RP-amide columns.

    PubMed

    Kumar, Ashwini; Kumar Malik, Ashok; Kumar Tewary, Dhananjay; Singh, Baldev

    2008-02-01

    A simple and highly sensitive high pressure liquid chromatographic (HPLC-UV) method has been developed for the determination of ofloxacin, lomefloxacin, cinoxacin, and nalidixic acid, in mobile phase citrate buffer (0.001 M) of pH 4.5 prepared in water (X), methanol (Y), and ACN (Z) using gradient at a flow rate of 1.0 mL/min by direct UV absorbance detection at lambda = 280 nm. Separation of analytes was studied on the C-18 and RP-amide columns and best results were observed on the RP-amide column with LODs (3.3 x S/m) 0.89, 0.55, 0.67, and 1.41 ng/mL for ofloxacin, lomefloxacin, cinoxacin, and nalidixic acid, respectively, and better RSD than the C-18 column. The recovery of Fluoroquinolones (FQs) in urine, ground water, hospital wastewater, and chicken muscle using this method is more than 90%. The method was successfully applied to the analysis of ofloxacin, lomefloxacin, cinoxacin, and nalidixic acid in urine, ground water, pharmaceutical dosage forms, hospital wastewater, and chicken muscle.

  5. [Monitoring method for macroporous resin column chromatography process of salvianolic acids based on near infrared spectroscopy].

    PubMed

    Hou, Xiang-Mei; Zhang, Lei; Yue, Hong-Shui; Ju, Ai-Chun; Ye, Zheng-Liang

    2016-07-01

    To study and establish a monitoring method for macroporous resin column chromatography process of salvianolic acids by using near infrared spectroscopy (NIR) as a process analytical technology (PAT).The multivariate statistical process control (MSPC) model was developed based on 7 normal operation batches, and 2 test batches (including one normal operation batch and one abnormal operation batch) were used to verify the monitoring performance of this model. The results showed that MSPC model had a good monitoring ability for the column chromatography process. Meanwhile, NIR quantitative calibration model was established for three key quality indexes (rosmarinic acid, lithospermic acid and salvianolic acid B) by using partial least squares (PLS) algorithm. The verification results demonstrated that this model had satisfactory prediction performance. The combined application of the above two models could effectively achieve real-time monitoring for macroporous resin column chromatography process of salvianolic acids, and can be used to conduct on-line analysis of key quality indexes. This established process monitoring method could provide reference for the development of process analytical technology for traditional Chinese medicines manufacturing. Copyright© by the Chinese Pharmaceutical Association.

  6. New method for evaluating irreversible adsorption and stationary phase bleed in gas chromatographic capillary columns.

    PubMed

    Wright, Bob W; Wright, Cherylyn W

    2012-10-26

    A novel method is described for the evaluation of irreversible adsorption and column bleed in gas chromatographic (GC) columns using a tandem GC approach. This work specifically determined the degree of irreversible adsorption behavior of specific sulfur and phosphorous containing test probe compounds at levels ranging from approximately 50 picograms (pg) to 1 nanogram (ng) on selected gas chromatographic columns. This method does not replace existing evaluation methods that characterize reversible adsorption but provides an additional tool. The test compounds were selected due to their ease of adsorption and their importance in the specific trace analytical detection methodology being developed. Replicate chromatographic columns with 5% phenylmethylpolysiloxane (PMS), polyethylene glycol (wax), trifluoropropylpolysiloxane (TFP), or 78% cyanopropylpolysiloxane stationary phases from a variety of vendors were evaluated. As expected, the results demonstrate that the different chromatographic phases exhibit differing degrees of irreversible adsorption behavior. The results also indicate that all manufacturers do not produce equally inert columns nor are columns from a given manufacturer identical. The wax-coated columns for the test probes used were more inert as a group than 5% PMS coated columns, and they were more reproducibly manufactured. Both TFP and 78% cyanopropylpolysiloxane columns displayed superior inertness to the test compounds compared to either 5% PMS- or wax-coated columns. Irreversible adsorption behavior was characterized for a limited range of stationary phase film thicknesses. In addition, the method was shown effective for characterizing column bleed and methods to remove bleed components. This method is useful in screening columns for demanding applications and to obtain diagnostic information related to improved preparation methods. Copyright © 2012 Elsevier B.V. All rights reserved.

  7. TCE degradation in groundwater by chelators-assisted Fenton-like reaction of magnetite: Sand columns demonstration.

    PubMed

    Jia, Daqing; Sun, Sheng-Peng; Wu, Zhangxiong; Wang, Na; Jin, Yaoyao; Dong, Weiyang; Chen, Xiao Dong; Ke, Qiang

    2018-03-15

    Trichloroethylene (TCE) degradation in sand columns has been investigated to evaluate the potential of chelates-enhanced Fenton-like reaction with magnetite as iron source for in situ treatment of TCE-contaminated groundwater. The results showed that successful degradation of TCE in sand columns was obtained by nitrilotriacetic acid (NTA)-assisted Fenton-like reaction of magnetite. Addition of ethylenediaminedisuccinic acid (EDDS) resulted in an inhibitory effect on TCE degradation in sand columns. Similar to EDDS, addition of ethylenediaminetetraacetic acid (EDTA) also led to an inhibition of TCE degradation in sand column with small content of magnetite (0.5 w.t.%), but enhanced TCE degradation in sand column with high content of magnetite (7.0 w.t.%). Additionally, the presence of NTA, EDDS and EDTA greatly decreased H 2 O 2 uptake in sand columns due to the competition between chelates and H 2 O 2 for surface sites on magnetite (and sand). Furthermore, the presented results show that magnetite in sand columns remained stable in a long period operation of 230 days without significant loss of performance in terms of TCE degradation and H 2 O 2 uptake. Moreover, it was found that TCE was degraded mainly to formic acid and chloride ion, and the formation of chlorinated organic intermediates was minimal by this process. Copyright © 2017 Elsevier B.V. All rights reserved.

  8. Investigation of the short argon arc with hot anode. II. Analytical model

    NASA Astrophysics Data System (ADS)

    Khrabry, A.; Kaganovich, I. D.; Nemchinsky, V.; Khodak, A.

    2018-01-01

    A short atmospheric pressure argon arc is studied numerically and analytically. In a short arc with an inter-electrode gap of several millimeters, non-equilibrium effects in plasma play an important role in operation of the arc. High anode temperature leads to electron emission and intensive radiation from its surface. A complete, self-consistent analytical model of the whole arc comprising of models for near-electrode regions, arc column, and a model of heat transfer in cylindrical electrodes was developed. The model predicts the width of non-equilibrium layers and arc column, voltages and plasma profiles in these regions, and heat and ion fluxes to the electrodes. Parametric studies of the arc have been performed for a range of the arc current densities, inter-electrode gap widths, and gas pressures. The model was validated against experimental data and verified by comparison with numerical solution. Good agreement between the analytical model and simulations and reasonable agreement with experimental data were obtained.

  9. Investigation of the short argon arc with hot anode. II. Analytical model

    DOE PAGES

    Khrabry, A.; Kaganovich, I. D.; Nemchinsky, V.; ...

    2018-01-22

    A short atmospheric pressure argon arc is studied numerically and analytically. In a short arc with an inter-electrode gap of several millimeters, non-equilibrium effects in plasma play an important role in operation of the arc. High anode temperature leads to electron emission and intensive radiation from its surface. A complete, self-consistent analytical model of the whole arc comprising of models for near-electrode regions, arc column, and a model of heat transfer in cylindrical electrodes was developed. The model predicts the width of non-equilibrium layers and arc column, voltages and plasma profiles in these regions, and heat and ion fluxes tomore » the electrodes. Parametric studies of the arc have been performed for a range of the arc current densities, inter-electrode gap widths, and gas pressures. The model was validated against experimental data and verified by comparison with numerical solution. In conclusion, good agreement between the analytical model and simulations and reasonable agreement with experimental data were obtained.« less

  10. Investigation of the short argon arc with hot anode. II. Analytical model

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Khrabry, A.; Kaganovich, I. D.; Nemchinsky, V.

    A short atmospheric pressure argon arc is studied numerically and analytically. In a short arc with an inter-electrode gap of several millimeters, non-equilibrium effects in plasma play an important role in operation of the arc. High anode temperature leads to electron emission and intensive radiation from its surface. A complete, self-consistent analytical model of the whole arc comprising of models for near-electrode regions, arc column, and a model of heat transfer in cylindrical electrodes was developed. The model predicts the width of non-equilibrium layers and arc column, voltages and plasma profiles in these regions, and heat and ion fluxes tomore » the electrodes. Parametric studies of the arc have been performed for a range of the arc current densities, inter-electrode gap widths, and gas pressures. The model was validated against experimental data and verified by comparison with numerical solution. In conclusion, good agreement between the analytical model and simulations and reasonable agreement with experimental data were obtained.« less

  11. FIELD ANALYTICAL SCREENING PROGRAM: PCP METHOD - INNOVATIVE TECHNOLOGY EVALUATION REPORT

    EPA Science Inventory

    The Field Analytical Screening Program (FASP) pentachlorophenol (PCP) method uses a gas chromatograph (GC) equipped with a megabore capillary column and flame ionization detector (FID) and electron capture detector (ECD) to identify and quantify PCP. The FASP PCP method is design...

  12. Post-analytical stability of 23 common chemistry and immunochemistry analytes in incurred samples.

    PubMed

    Nielsen, Betina Klint; Frederiksen, Tina; Friis-Hansen, Lennart; Larsen, Pia Bükmann

    2017-12-01

    Storage of blood samples after centrifugation, decapping and initial sampling allows ordering of additional blood tests. The pre-analytic stability of biochemistry and immunochemistry analytes has been studied in detail, but little is known about the post-analytical stability in incurred samples. We examined the stability of 23 routine analytes on the Dimension Vista® (Siemens Healthineers, Denmark): 42-60 routine samples in lithium-heparin gel tubes (Vacutainer, BD, USA) were centrifuged at 3000×g for 10min. Immediately after centrifugation, initial concentration of analytes were measured in duplicate (t=0). The tubes were stored decapped at room temperature and re-analyzed after 2, 4, 6, 8 and 10h in singletons. The concentration from reanalysis were normalized to initial concentration (t=0). Internal acceptance criteria for bias and total error were used to determine stability of each analyte. Additionally, evaporation from the decapped blood collection tubes and the residual platelet count in the plasma after centrifugation were quantified. We report a post-analytical stability of most routine analytes of ≥8h and do therefore - with few exceptions - suggest a standard 8hour-time limit for reordering and reanalysis of analytes in incurred samples. Copyright © 2017 The Canadian Society of Clinical Chemists. Published by Elsevier Inc. All rights reserved.

  13. Analytical balance-based Faraday magnetometer

    NASA Astrophysics Data System (ADS)

    Riminucci, Alberto; Uhlarz, Marc; De Santis, Roberto; Herrmannsdörfer, Thomas

    2017-03-01

    We introduce a Faraday magnetometer based on an analytical balance in which we were able to apply magnetic fields up to 0.14 T. We calibrated it with a 1 mm Ni sphere previously characterized in a superconducting quantum interference device (SQUID) magnetometer. The proposed magnetometer reached a theoretical sensitivity of 3 × 10-8 A m2. We demonstrated its operation on magnetic composite scaffolds made of poly(ɛ-caprolactone)/iron-doped hydroxyapatite. To confirm the validity of the method, we measured the same scaffold properties in a SQUID magnetometer. The agreement between the two measurements was within 5% at 0.127 T and 12% at 24 mT. With the addition, for a small cost, of a permanent magnet and computer controlled linear translators, we were thus able to assemble a Faraday magnetometer based on an analytical balance, which is a virtually ubiquitous instrument. This will make simple but effective magnetometry easily accessible to most laboratories, in particular, to life sciences ones, which are increasingly interested in magnetic materials.

  14. Analytical investigations of seismic responses for reinforced concrete bridge columns subjected to strong near-fault ground motion

    NASA Astrophysics Data System (ADS)

    Su, Chin-Kuo; Sung, Yu-Chi; Chang, Shuenn-Yih; Huang, Chao-Hsun

    2007-09-01

    Strong near-fault ground motion, usually caused by the fault-rupture and characterized by a pulse-like velocity-wave form, often causes dramatic instantaneous seismic energy (Jadhav and Jangid 2006). Some reinforced concrete (RC) bridge columns, even those built according to ductile design principles, were damaged in the 1999 Chi-Chi earthquake. Thus, it is very important to evaluate the seismic response of a RC bridge column to improve its seismic design and prevent future damage. Nonlinear time history analysis using step-by-step integration is capable of tracing the dynamic response of a structure during the entire vibration period and is able to accommodate the pulsing wave form. However, the accuracy of the numerical results is very sensitive to the modeling of the nonlinear load-deformation relationship of the structural member. FEMA 273 and ATC-40 provide the modeling parameters for structural nonlinear analyses of RC beams and RC columns. They use three parameters to define the plastic rotation angles and a residual strength ratio to describe the nonlinear load-deformation relationship of an RC member. Structural nonlinear analyses are performed based on these parameters. This method provides a convenient way to obtain the nonlinear seismic responses of RC structures. However, the accuracy of the numerical solutions might be further improved. For this purpose, results from a previous study on modeling of the static pushover analyses for RC bridge columns (Sung et al. 2005) is adopted for the nonlinear time history analysis presented herein to evaluate the structural responses excited by a near-fault ground motion. To ensure the reliability of this approach, the numerical results were compared to experimental results. The results confirm that the proposed approach is valid.

  15. HPLC separation of triacylglycerol positional isomers on a polymeric ODS column.

    PubMed

    Kuroda, Ikuma; Nagai, Toshiharu; Mizobe, Hoyo; Yoshimura, Nobuhito; Gotoh, Naohiro; Wada, Shun

    2008-07-01

    A polymeric ODS column was applied to the resolution of triacylglycerol positional isomers (TAG-PI), i.e. 1,3-dioleoyl-2-palmitoyl-glycerol (OPO) and 1,2-dioleoyl-3-palmitoyl-rac-glycerol (OOP), with a recycle HPLC system. To investigate the ODS column species and the column temperatures for the resolution of a TAG-PI pair, a mixture of OPO and OOP was subjected to an HPLC system equipped with a non-endcapped polymeric, endcapped monomeric, endcapped intermediate, or non-endcapped monomeric ODS column at three different column temperatures (40, 25, or 10 degrees C). Only the non-endcapped polymeric ODS column achieved the separation of OPO and OOP, and the lowest column temperature (10 degrees C) showed the best resolution for them. The other pair of TAG-PI, a mixture of 1,3-dipalmitoyl-2-oleoyl-glycerol (POP) and 1,2-dipalmitoyl-3-oleoyl-rac-glycerol (PPO) was also subjected to the system equipped with a non-endcapped polymeric or monomeric ODS column at five different column temperatures (40, 32, 25, 17, and 10 degrees C). Thus, POP and PPO were also separated on only the non-endcapped polymeric ODS column at 25 degrees C. However, no clear peak appeared at 10 degrees C. These results would indicate that the polymeric ODS stationary phase has an ability to recognize the structural differences between TAG-PI pairs. Also, the column temperature is a very important factor for separating the TAG-PI pair, and the optimal temperature would relate to the solubility of TAG-PI in the mobile phase. Furthermore, the recycle HPLC system provided measurements for the separation and analysis of TAG-PI pairs.

  16. Repeatability of the efficiency of columns packed with sub-3μm core-shell particles: Part II. 2.7 μm Halo-ES-Peptide-C18 particles in 4.6mm and 2.1mm×100mm column formats.

    PubMed

    Gritti, Fabrice; Guiochon, Georges

    2012-08-24

    The column-to-column repeatability of the mass transfer kinetics in columns packed with sub-3μm shell particles was investigated. The parameters of this kinetics were measured for twelve columns (six 2.1mm×100mm and six 4.6mm×100mm) packed with the same batch of 2.7μm Halo-ES-Peptide-C(18) particles (Advanced Material Technologies, Wilmington, DE, USA). For both series, the manufacturer provided columns at different positions in the efficiency distribution given by the quality test control. Three compounds were used, uracil, naphthalene and insulin. The reduced longitudinal diffusion term was measured with the peak parking (PP) method; the reduced solid-liquid mass transfer resistance term was given by a combination of the PP results and the most accurate model of effective diffusion in ternary composite materials (non-porous cores, concentric porous shell, and eluent matrix), validated previously. The overall eddy diffusion term was obtained by subtraction of these two HETP terms from the overall reduced HETP measured by numerical integration of the entire peak profiles. The results demonstrate that the dispersion of the column efficiencies is mostly due to the random nature of the packing process and the associated eddy diffusion term. At the highest reduced velocity achieved, the relative standard deviations (RSDs) of the eddy diffusion term for the 2.1mm I.D. columns were ca. 5 and 10% (with average values A(ν)=2.3 and 8.5) for naphthalene and uracil, respectively. For the 4.6mm I.D. columns, these RSDs were 3 and 5%, respectively, with average values A(ν)=1.5 and 2.7. Copyright © 2012 Elsevier B.V. All rights reserved.

  17. Bernstein modes in a non-neutral plasma column

    NASA Astrophysics Data System (ADS)

    Walsh, Daniel; Dubin, Daniel H. E.

    2018-05-01

    This paper presents theory and numerical calculations of electrostatic Bernstein modes in an inhomogeneous cylindrical plasma column. These modes rely on finite Larmor radius effects to propagate radially across the column until they are reflected when their frequency matches the upper hybrid frequency. This reflection sets up an internal normal mode on the column and also mode-couples to the electrostatic surface cyclotron wave (which allows the normal mode to be excited and observed using external electrodes). Numerical results predicting the mode spectra, using a novel linear Vlasov code on a cylindrical grid, are presented and compared to an analytical Wentzel Kramers Brillouin (WKB) theory. A previous version of the theory [D. H. E. Dubin, Phys. Plasmas 20(4), 042120 (2013)] expanded the plasma response in powers of 1/B, approximating the local upper hybrid frequency, and consequently, its frequency predictions are spuriously shifted with respect to the numerical results presented here. A new version of the WKB theory avoids this approximation using the exact cold fluid plasma response and does a better job of reproducing the numerical frequency spectrum. The effect of multiple ion species on the mode spectrum is also considered, to make contact with experiments that observe cyclotron modes in a multi-species pure ion plasma [M. Affolter et al., Phys. Plasmas 22(5), 055701 (2015)].

  18. 3.0 T plaque imaging.

    PubMed

    Hinton-Yates, Denise P; Cury, Ricardo C; Wald, Lawrence L; Wiggins, Graham C; Keil, Boris; Seethmaraju, Ravi; Gangadharamurthy, Dakshinamurthy; Ogilvy, Christopher S; Dai, Guangping; Houser, Stuart L; Stone, James R; Furie, Karen L

    2007-10-01

    The aim of this article is to evaluate 3.0 T magnetic resonance imaging for characterization of vessel morphology and plaque composition. Emphasis is placed on early and moderate stages of carotid atherosclerosis, where increases in signal-to-noise (SNR) and contrast-to-noise (CNR) ratios compared with 1.5 T are sought. Comparison of in vivo 3.0 T imaging to histopathology is performed for validation. Parallel acceleration methods applied with an 8-channel carotid array are investigated as well as higher field ex vivo imaging to explore even further gains. The overall endeavor is to improve prospective assessment of atherosclerosis stage and stability for reduction of atherothrombotic event risk. A total of 10 male and female subjects ranging in age from 22 to 72 years (5 healthy and 5 with cardiovascular disease) participated. Custom-built array coils were used with endogenous and exogenous multicontrast bright and black-blood protocols for 3.0 T carotid imaging. Comparisons were performed to 1.5 T, and ex vivo plaque was stained with hematoxylin and eosin for histology. Imaging (9.4 T) was also performed on intact specimens. The factor of 2 gain in signal-to-noise SNR is realized compared with 1.5 T along with improved wall-lumen and plaque component CNR. Post-contrast black-blood imaging within 5-10 minutes of gadolinium injection is optimal for detection of the necrotic lipid component. In a preliminary 18-month follow-up study, this method provided measurement of a 50% reduction in lipid content with minimal change in plaque size in a subject receiving aggressive statin therapy. Parallel imaging applied with signal averaging further improves 3.0 T black-blood vessel wall imaging. The use of 3.0 T for carotid plaque imaging has demonstrated increases in SNR and CNR compared with 1.5 T. Quantitative prospective studies of moderate and early plaques are feasible at 3.0 T. Continued improvements in coil arrays, 3-dimensional pulse sequences, and the use of novel

  19. Advantages of core-shell particle columns in Sequential Injection Chromatography for determination of phenolic acids.

    PubMed

    Chocholouš, Petr; Vacková, Jana; Srámková, Ivana; Satínský, Dalibor; Solich, Petr

    2013-01-15

    Currently, for Sequential Injection Chromatography (SIC), only reversed phase C18 columns have been used for chromatographic separations. This article presents the first use of three different stationary phases: three core-shell particle-packed reversed phase columns in flow systems. The aim of this work was to extend the chromatographic capabilities of the SIC system. Despite the particle-packed columns reaching system pressures of ≤ 610 PSI, their conditions matched those of a commercially produced and optimised SIC system (SIChrom™ (FIAlab(®), USA)) with a 8-port high-pressure selection valve and medium-pressure Sapphire™ syringe pump with a 4 mL reservoir and maximum system pressure of ≤ 1000 PSI. The selectivity of each of the tested columns, Ascentis(®) Express RP-Amide, Ascentis(®) Express Phenyl-Hexyl and Ascentis(®) Express C18 (30 mm × 4.6mm, core-shell particle size 2.7 μm), was compared by their ability to separate seven phenolic acids that are secondary metabolite substances widely distributed in plants. The separations of all of the components were performed by isocratic elution using binary mobile phases composed of acetonitrile and 0.065% phosphoric acid at pH 2.4 (a specific ratio was used for each column) at a flow-rate of 0.60 mL/min. The volume of the mobile phase was 3.8 mL for each separation. The injection volume of the sample was 10 μL for each separation. The UV detection wavelengths were set to 250, 280 and 325 nm. The RP-Amide column provided the highest chromatographic resolution and allowed for complete baseline separation of protocatechuic, syringic, vanillic, ferulic, sinapinic, p-coumaric and o-coumaric acids. The Phenyl-Hexyl and C18 columns were unable to completely separate the tested mixture, syringic and vanillic acid and ferulic and sinapinic acids could not be separated from one another. The analytical parameters were a LOD of 0.3 mg L(-1), a LOQ of 1.0 mg L(-1), a calibration range of 1.0-50.0 (100.0) mg L(-1

  20. Effect of 3,5,3'-Triiodothyronine (T3) administration on dio1 gene expression and T3 metabolism in normal and type 1 deiodinase-deficient mice.

    PubMed

    Maia, A L; Kieffer, J D; Harney, J W; Larsen, P R

    1995-11-01

    The type 1 deiodinase (D1) catalyzes the monodeiodination of T4 to produce T3, the active thyroid hormone. In the C3H mouse, hepatic D1 and the dio1 messenger RNA (mRNA) are only 10% that in the C57 strain, the common phenotype. Low activity cosegregated with a series of five GCT repeats located in the 5'-flanking region of the C3H dio1 gene that impaired C3H promoter potency and provided a partial explanation for the lower D1. The present studies were performed to search for additional explanations for low D1 activity in C3H mice. Previous studies have shown that T3 up-regulates the dio1 gene. Therefore, loss of the capacity to respond to endogenous T3 is a possible additional cause of the lower D1 levels in the C3H mice. The hepatic C3H dio1 mRNA increases 10- to 20 fold after T3 administration. The t3 effect occurs at a transplantation level and T3 does not alter the dio1 mRNA half-life. Despite the transcriptional response to T3, no functional thyroid response elements were identified in the 1.5-kilobase 5'-flanking region of either the C57 or C3H dio1 gene. After the same dose of exogenous T3, both dio1 mRNA and D1 of the C3H mouse respond to a greater extent than those of the C57 strain. This can be explained in part by the reduction in T3 clearance due to the lower D1 levels in C3H mice in which higher concentrations of circulating T3 are maintained. The decrease in serum T3 levels and T3 production observed in fasting and systemic illness in both human and experimental animals has been attributed in part to a decrease in hepatic D1. In contrast, despite markedly lower hepatic and renal D1 levels, serum T3 concentrations remain normal in C3H mice. The present studies suggest that the absence of stress-induced hypothalamic-pituitary suppression that allows T4 production to be maintained together with the reduced clearance of T3 and T4 via inner ring deiodination compensate for the D1 deficiency.

  1. Iptycene-based stationary phase with three-dimensional aromatic structure for highly selective separation of H-bonding analytes and aromatic isomers.

    PubMed

    Yang, Xiaohong; Han, Ying; Qi, Meiling; Chen, Chuanfeng

    2016-05-06

    Unique structures and molecular recognition ability endow iptycene derivatives with great potential as stationary phases in chromatography, which, however, has not been explored yet. Herein, we report the first example of utilizing a pentiptycene quinone (PQ) for gas chromatographic (GC) separations. Remarkably, the statically coated capillary column with the stationary phase achieved extremely high column efficiency of 4800 plates/m. It exhibited preferential retention and high resolving capability for H-bonding and aromatic analytes and positional isomers, showing advantages over the ordinary polysiloxane phase. Moreover, the fabricated iptycene column showed excellent separation repeatability with RSD values of 0.02-0.06% for intra-day, 0.20-0.35% for inter-day and 3.1-5.5% for between-column, respectively. In conclusion, iptycene derivatives as a new class of stationary phases show promising future for their use in GC separations. Copyright © 2016 Elsevier B.V. All rights reserved.

  2. Microchip-based Integration of Cell Immobilization, Electrophoresis, Post-column Derivatization, and Fluorescence Detection for Monitoring the Release of Dopamine from PC 12 Cells

    PubMed Central

    Li, Michelle W.; Martin, R. Scott

    2008-01-01

    In this paper, we describe the fabrication and evaluation of a multilayer microchip device that can be used to quantitatively measure the amount of catecholamines released from PC 12 cells immobilized within the same device. This approach allows immobilized cells to be stimulated on-chip and, through rapid actuation of integrated microvalves, the products released from the cells are repeatedly injected into the electrophoresis portion of the microchip, where the analytes are separated based upon mass and charge and detected through post-column derivatization and fluorescence detection. Following optimization of the post-column derivatization detection scheme (using naphthalene-2,3-dicarboxaldehyde and 2-β-mercaptoethanol), off-chip cell stimulation experiments were performed to demonstrate the ability of this device to detect dopamine from a population of PC 12 cells. The final 3-dimensional device that integrates an immobilized PC 12 cell reactor with the bilayer continuous flow sampling/electrophoresis microchip was used to continuously monitor the on-chip stimulated release of dopamine from PC 12 cells. Similar dopamine release was seen when stimulating on-chip versus off-chip yet the on-chip immobilization studies could be carried out with 500 times fewer cells in a much reduced volume. While this paper is focused on PC 12 cells and neurotransmitter analysis, the final device is a general analytical tool that is amenable to immobilization of a variety of cell lines and analysis of various released analytes by electrophoretic means. PMID:18810283

  3. Sequential Injection Chromatography with an Ultra-short Monolithic Column for the Low-Pressure Separation of α-Tocopherol and γ-Oryzanol in Vegetable Oils and Nutrition Supplements.

    PubMed

    Thaithet, Sujitra; Kradtap Hartwell, Supaporn; Lapanantnoppakhun, Somchai

    2017-01-01

    A low-pressure separation procedure of α-tocopherol and γ-oryzanol was developed based on a sequential injection chromatography (SIC) system coupled with an ultra-short (5 mm) C-18 monolithic column, as a lower cost and more compact alternative to the HPLC system. A green sample preparation, dilution with a small amount of hexane followed by liquid-liquid extraction with 80% ethanol, was proposed. Very good separation resolution (R s = 3.26), a satisfactory separation time (10 min) and a total run time including column equilibration (16 min) were achieved. The linear working range was found to be 0.4 - 40 μg with R 2 being more than 0.99. The detection limits of both analytes were 0.28 μg with the repeatability within 5% RSD (n = 7). Quantitative analyses of the two analytes in vegetable oil and nutrition supplement samples, using the proposed SIC method, agree well with the results from HPLC.

  4. Effects of potassium iodide in concentrations of TSH, tT3 and tT4 in serum of subjects with sporotrichosis.

    PubMed

    Ramírez Soto, Max Carlos

    2014-08-01

    The saturated potassium iodide solution (SSKI) as treatment for sporotrichosis may cause hypothyroidism by suppressing the synthesis of thyroid hormones (tT3 and tT4 ) and the iodine excess could lead to thyrotoxicosis. Evaluating the changes in serum levels of TSH, tT3 and tT4 in euthyroid patients with sporotrichosis treated with SSKI. For the selection of euthyroid patients, TSH, tT3 and tT4 concentrations were measured for those adults and children diagnosed with sporotrichosis. Each paediatric patient was administered SSKI orally in increasing doses of 2-20 drops/3 times/day and 4-40 drops/3 times/day in adults. Serum concentrations of TSH, tT3 and tT4 were measured 20 days after started the treatment and 15 days posttreatment. Eight euthyroid patients aged between 2 to 65 years old were included. After 20 days of treatment, two suffered subclinical hypothyroidism, one developed subclinical hyperthyroidism, and one hyperthyroxinaemia euthyroid. At 15 days posttreatment only four patients were evaluated and all serum levels of TSH, tT3 and tT4 were normal. Some euthyroid patients with sporotrichosis can develop hyperthyroidism or subclinical iodine-induced hypothyroidism, during the administration of 3 or 6 g SSKI/day. © 2014 Blackwell Verlag GmbH.

  5. Glass-silicon column

    DOEpatents

    Yu, Conrad M.

    2003-12-30

    A glass-silicon column that can operate in temperature variations between room temperature and about 450.degree. C. The glass-silicon column includes large area glass, such as a thin Corning 7740 boron-silicate glass bonded to a silicon wafer, with an electrode embedded in or mounted on glass of the column, and with a self alignment silicon post/glass hole structure. The glass/silicon components are bonded, for example be anodic bonding. In one embodiment, the column includes two outer layers of silicon each bonded to an inner layer of glass, with an electrode imbedded between the layers of glass, and with at least one self alignment hole and post arrangement. The electrode functions as a column heater, and one glass/silicon component is provided with a number of flow channels adjacent the bonded surfaces.

  6. Systems for column-based separations, methods of forming packed columns, and methods of purifying sample components

    DOEpatents

    Egorov, Oleg B.; O'Hara, Matthew J.; Grate, Jay W.; Chandler, Darrell P.; Brockman, Fred J.; Bruckner-Lea, Cynthia J.

    2000-01-01

    The invention encompasses systems for column-based separations, methods of packing and unpacking columns and methods of separating components of samples. In one aspect, the invention includes a method of packing and unpacking a column chamber, comprising: a) packing a matrix material within a column chamber to form a packed column; and b) after the packing, unpacking the matrix material from the column chamber without moving the column chamber. In another aspect, the invention includes a system for column-based separations, comprising: a) a fluid passageway, the fluid passageway comprising a column chamber and a flow path in fluid communication with the column chamber, the flow path being obstructed by a retaining material permeable to a carrier fluid and impermeable to a column matrix material suspended in the carrier fluid, the flow path extending through the column chamber and through the retaining material, the flow path being configured to form a packed column within the column chamber when a suspension of the fluid and the column matrix material is flowed along the flow path; and b) the fluid passageway extending through a valve intermediate the column chamber and the retaining material.

  7. Systems For Column-Based Separations, Methods Of Forming Packed Columns, And Methods Of Purifying Sample Components

    DOEpatents

    Egorov, Oleg B.; O'Hara, Matthew J.; Grate, Jay W.; Chandler, Darrell P.; Brockman, Fred J.; Bruckner-Lea, Cynthia J.

    2006-02-21

    The invention encompasses systems for column-based separations, methods of packing and unpacking columns and methods of separating components of samples. In one aspect, the invention includes a method of packing and unpacking a column chamber, comprising: a) packing a matrix material within a column chamber to form a packed column; and b) after the packing, unpacking the matrix material from the column chamber without moving the column chamber. In another aspect, the invention includes a system for column-based separations, comprising: a) a fluid passageway, the fluid passageway comprising a column chamber and a flow path in fluid communication with the column chamber, the flow path being obstructed by a retaining material permeable to a carrier fluid and impermeable to a column matrix material suspended in the carrier fluid, the flow path extending through the column chamber and through the retaining material, the flow path being configured to form a packed column within the column chamber when a suspension of the fluid and the column matrix material is flowed along the flow path; and b) the fluid passageway extending through a valve intermediate the column chamber and the retaining material.

  8. Systems For Column-Based Separations, Methods Of Forming Packed Columns, And Methods Of Purifying Sample Components.

    DOEpatents

    Egorov, Oleg B.; O'Hara, Matthew J.; Grate, Jay W.; Chandler, Darrell P.; Brockman, Fred J.; Bruckner-Lea, Cynthia J.

    2004-08-24

    The invention encompasses systems for column-based separations, methods of packing and unpacking columns and methods of separating components of samples. In one aspect, the invention includes a method of packing and unpacking a column chamber, comprising: a) packing a matrix material within a column chamber to form a packed column; and b) after the packing, unpacking the matrix material from the column chamber without moving the column chamber. In another aspect, the invention includes a system for column-based separations, comprising: a) a fluid passageway, the fluid passageway comprising a column chamber and a flow path in fluid communication with the column chamber, the flow path being obstructed by a retaining material permeable to a carrier fluid and impermeable to a column matrix material suspended in the carrier fluid, the flow path extending through the column chamber and through the retaining material, the flow path being configured to form a packed column within the column chamber when a suspension of the fluid and the column matrix material is flowed along the flow path; and b) the fluid passageway extending through a valve intermediate the column chamber and the retaining material.

  9. Analytical Application of Flow Immunosensor in Detection of Thyroxine and Triiodothyronine in Serum.

    PubMed

    Wani, Tanveer A; Zargar, Seema; Majid, Salma; Darwish, Ibrahim A

    2016-11-01

    In this study, an immunosensor based on kinetic exclusion analysis (KinExA) was used for thyroxine (T4) and triiodothyronine (T3) estimation. A KinExA™ 3200 instrument was used for this analysis, which is an automated flow fluorimeter designed to separate free unbound antibody binding sites in reaction mixtures of antibody, antigen, and antibody-antigen complex. A T3-BSA- and T4-BSA-coated polymethyl methacrylate (PMMA) bead microcolumn is generated inside the flow cell of the instrument. A sample mixture containing T3 and T4 with their respective monoclonal antibodies and their complexes are drawn past the microbead column. The unbound T3 or T4 monoclonal antibody binding sites are captured by their respective T3 and T4 antigens coated on the PMMA beads as bovine serum albumin conjugates. Fluorescently labeled secondary antibodies bind to the T3 or T4 antigen-antibody complex to generate fluorescence intensity for analysis. The limit of detection for the T3 and T4 assays was found to be 0.06 and 1.9 ng mL -1 with acceptable precision values. The convenience of the automated KinExA format may be valuable in medical diagnostic laboratories.

  10. Enhanced reductive dechlorination in columns treated with edible oil emulsion

    NASA Astrophysics Data System (ADS)

    Long, Cameron M.; Borden, Robert C.

    2006-09-01

    The effect of edible oil emulsion treatment on enhanced reductive dechlorination was evaluated in a 14 month laboratory column study. Experimental treatments included: (1) emulsified soybean oil and dilute HCl to inhibit biological activity; (2) emulsified oil only; (3) emulsified oil and anaerobic digester sludge; and (4) continuously feeding soluble substrate. A single application of emulsified oil was effective in generating strongly reducing, anaerobic conditions for over 14 months. PCE was rapidly reduced to cis-DCE in all three live columns. Bioaugmentation with a halorespiring enrichment culture resulted in complete dechlorination of PCE to ethene in the soluble substrate column (yeast extract and lactate). However, an additional treatment with a pulse of yeast extract and bioaugmentation culture was required to stimulate complete dechlorination in the emulsion treated columns. Once the dechlorinating population was established, the emulsion only column degraded PCE from 90-120 μM to below detection with concurrent ethene production in a 33 day contact time. The lower biodegradation rates in the emulsion treated columns compared to the soluble substrate column suggest that emulsified oil barriers may require a somewhat longer contact time for effective treatment. In the HCl inhibited column, partitioning of PCE to the retained oil substantially delayed PCE breakthrough. However, reduction of PCE to more soluble degradation products ( cis-DCE, VC and ethene) greatly reduced the impact of oil-water partitioning in live columns. There was only a small decline in the hydraulic conductivity ( K) of column #1 (low pH + emulsion, Kfinal/ Kinitial = 0.57) and column #2 (live + emulsion, Kfinal/ Kinitial = 0.73) indicating emulsion injection did not result in appreciable clogging of the clayey sand. However, K loss was greater in column #3 (sludge +emulsion, Kfinal/ Kinitial = 0.12) and column #4 (soluble substrate, Kfinal/ Kinitial = 0.03) indicating clogging due

  11. Bacterial diversity in permanently cold and alkaline ikaite columns from Greenland.

    PubMed

    Schmidt, Mariane; Priemé, Anders; Stougaard, Peter

    2006-12-01

    Bacterial diversity in alkaline (pH 10.4) and permanently cold (4 degrees C) ikaite tufa columns from the Ikka Fjord, SW Greenland, was investigated using growth characterization of cultured bacterial isolates with Terminal-restriction fragment length polymorphism (T-RFLP) and sequence analysis of bacterial 16S rRNA gene fragments. More than 200 bacterial isolates were characterized with respect to pH and temperature tolerance, and it was shown that the majority were cold-active alkaliphiles. T-RFLP analysis revealed distinct bacterial communities in different fractions of three ikaite columns, and, along with sequence analysis, it showed the presence of rich and diverse bacterial communities. Rarefaction analysis showed that the 109 sequenced clones in the 16S rRNA gene library represented between 25 and 65% of the predicted species richness in the three ikaite columns investigated. Phylogenetic analysis of the 16S rRNA gene sequences revealed many sequences with similarity to alkaliphilic or psychrophilic bacteria, and showed that 33% of the cloned sequences and 33% of the cultured bacteria showed less than 97% sequence identity to known sequences in databases, and may therefore represent yet unknown species.

  12. Family of columns isospectral to gravity-loaded columns with tip force: A discrete approach

    NASA Astrophysics Data System (ADS)

    Ramachandran, Nirmal; Ganguli, Ranjan

    2018-06-01

    A discrete model is introduced to analyze transverse vibration of straight, clamped-free (CF) columns of variable cross-sectional geometry under the influence of gravity and a constant axial force at the tip. The discrete model is used to determine critical combinations of loading parameters - a gravity parameter and a tip force parameter - that cause onset of dynamic instability in the CF column. A methodology, based on matrix-factorization, is described to transform the discrete model into a family of models corresponding to weightless and unloaded clamped-free (WUCF) columns, each with a transverse vibration spectrum isospectral to the original model. Characteristics of models in this isospectral family are dependent on three transformation parameters. A procedure is discussed to convert the isospectral discrete model description into geometric description of realistic columns i.e. from the discrete model, we construct isospectral WUCF columns with rectangular cross-sections varying in width and depth. As part of numerical studies to demonstrate efficacy of techniques presented, frequency parameters of a uniform column and three types of tapered CF columns under different combinations of loading parameters are obtained from the discrete model. Critical combinations of these parameters for a typical tapered column are derived. These results match with published results. Example CF columns, under arbitrarily-chosen combinations of loading parameters are considered and for each combination, isospectral WUCF columns are constructed. Role of transformation parameters in determining characteristics of isospectral columns is discussed and optimum values are deduced. Natural frequencies of these WUCF columns computed using Finite Element Method (FEM) match well with those of the given gravity-loaded CF column with tip force, hence confirming isospectrality.

  13. Acylhydrazone bond dynamic covalent polymer gel monolithic column online coupling to high-performance liquid chromatography for analysis of sulfonamides and fluorescent whitening agents in food.

    PubMed

    Zhang, Chengjiang; Luo, Xialin; Wei, Tianfu; Hu, Yufei; Li, Gongke; Zhang, Zhuomin

    2017-10-13

    A new dynamic covalent polymer (DCP) gel was well designed and constructed based on imine chemistry. Polycondensation of 4,4'-biphenyldicarboxaldehyde and 1,3,5-benzenetricarbohydrazide via Schiff-base reaction resulted in an acylhydrazone bond gel (AB-gel) DCP. AB-gel DCP had three-dimensional network of interconnected nanoparticles with hierarchically porous structure. AB-gel DCP was successfully fabricated as a monolithic column by an in-situ chemical bonding method for online enrichment and separation purpose with excellent permeability. AB-gel DCP based monolithic column showed remarkable adsorption affinity towards target analytes including sulfonamides (SAs) and fluorescent whitening agents (FWAs) due to its strong π-π affinity, hydrophobic effect and hydrogen bonding interaction. Then, AB-gel DCP based monolithic column was applied for online separation and analysis of trace SAs and FWAs in food samples coupled with high-performance liquid chromatography (HPLC). Sulfathiazole (ST) and sulfadimidine (SM2) in one positive weever sample were actually found and determined with concentrations of 273.8 and 286.3μg/kg, respectively. 2,5-Bis(5-tert-butyl-2-benzoxazolyl) thiophene (FWA184) was actually quantified in one tea infusion sample with the concentration of 268.5ng/L. The spiked experiments suggested the good recoveries in range of 74.5-110% for SAs in weever and shrimp samples with relative standard deviations (RSDs) less than 9.7% and in range of 74.0-113% for FWAs in milk and tea infusion samples with RSDs less than 9.0%. AB-gel DCP monolithic column was proved to be a promising sample preparation medium for online separation and analysis of trace analytes in food samples with complex matrices. Copyright © 2017 Elsevier B.V. All rights reserved.

  14. Distillation Column Flooding Predictor

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    George E. Dzyacky

    2010-11-23

    The Flooding Predictor™ is a patented advanced control technology proven in research at the Separations Research Program, University of Texas at Austin, to increase distillation column throughput by over 6%, while also increasing energy efficiency by 10%. The research was conducted under a U. S. Department of Energy Cooperative Agreement awarded to George Dzyacky of 2ndpoint, LLC. The Flooding Predictor™ works by detecting the incipient flood point and controlling the column closer to its actual hydraulic limit than historical practices have allowed. Further, the technology uses existing column instrumentation, meaning no additional refining infrastructure is required. Refiners often push distillationmore » columns to maximize throughput, improve separation, or simply to achieve day-to-day optimization. Attempting to achieve such operating objectives is a tricky undertaking that can result in flooding. Operators and advanced control strategies alike rely on the conventional use of delta-pressure instrumentation to approximate the column’s approach to flood. But column delta-pressure is more an inference of the column’s approach to flood than it is an actual measurement of it. As a consequence, delta pressure limits are established conservatively in order to operate in a regime where the column is never expected to flood. As a result, there is much “left on the table” when operating in such a regime, i.e. the capacity difference between controlling the column to an upper delta-pressure limit and controlling it to the actual hydraulic limit. The Flooding Predictor™, an innovative pattern recognition technology, controls columns at their actual hydraulic limit, which research shows leads to a throughput increase of over 6%. Controlling closer to the hydraulic limit also permits operation in a sweet spot of increased energy-efficiency. In this region of increased column loading, the Flooding Predictor is able to exploit the benefits of higher liquid

  15. Analytical sensitivity and specificity of a loop-mediated isothermal amplification (LAMP) kit prototype for detection of Trypanosoma cruzi DNA in human blood samples.

    PubMed

    Besuschio, Susana A; Llano Murcia, Mónica; Benatar, Alejandro F; Monnerat, Severine; Cruz, Israel; Picado, Albert; Curto, María de Los Ángeles; Kubota, Yutaka; Wehrendt, Diana P; Pavia, Paula; Mori, Yasuyoshi; Puerta, Concepción; Ndung'u, Joseph M; Schijman, Alejandro G

    2017-07-01

    This study aimed to assess analytical parameters of a prototype LAMP kit that was designed for detection of Trypanosoma cruzi DNA in human blood. The prototype is based on the amplification of the highly repetitive satellite sequence of T.cruzi in microtubes containing dried reagents on the inside of the caps. The reaction is carried out at 65°C during 40 minutes. Calcein allows direct detection of amplified products with the naked eye. Inclusivity and selectivity were tested in purified DNA from Trypanosoma cruzi stocks belonging to the six discrete typing units (DTUs), in DNA from other protozoan parasites and in human DNA. Analytical sensitivity was estimated in serial dilutions of DNA samples from Sylvio X10 (Tc I) and CL Brener (Tc VI) stocks, as well as from EDTA-treated or heparinized blood samples spiked with known amounts of cultured epimastigotes (CL Brener). LAMP sensitivity was compared after DNA extraction using commercial fiberglass columns or after "Boil & Spin" rapid preparation. Moreover, the same DNA and EDTA-blood spiked samples were subjected to standardized qPCR based on the satellite DNA sequence for comparative purposes. A panel of peripheral blood specimens belonging to Chagas disease patients, including acute, congenital, chronic and reactivated cases (N = 23), as well as seronegative controls (N = 10) were evaluated by LAMP in comparison to qPCR. LAMP was able to amplify DNAs from T. cruzi stocks representative of the six DTUs, whereas it did not amplify DNAs from Leishmania sp, T. brucei sp, T. rangeli KPN+ and KPN-, P. falciparum and non-infected human DNA. Analytical sensitivity was 1x10-2 fg/μL of both CL Brener and Sylvio X10 DNAs, whereas qPCR detected up to 1x 10-1 fg/μL of CL Brener DNA and 1 fg/μl of Sylvio X10 DNA. LAMP detected 1x10-2 parasite equivalents/mL in spiked EDTA blood and 1x10-1 par.eq/mL in spiked heparinized blood using fiberglass columns for DNA extraction, whereas qPCR detected 1x10-2 par.eq./mL in EDTA blood

  16. Accurate measurements of the true column efficiency and of the instrument band broadening contributions in the presence of a chromatographic column.

    PubMed

    Gritti, Fabrice; Guiochon, Georges

    2014-01-31

    A rapid and simple validated experimental protocol is proposed for the accurate determination of the true intrinsic column efficiency and for that of the variance of the extra-column volume of the instrument used, the latter being obtained without requiring the removal of the chromatographic column from the HPLC system. This protocol was applied to 2.1mm×100mm columns packed with sub-3 (2.7μm Halo Peptide ES-C18) and sub-2μm (1.6μm prototype) core-shell particles. It was validated by observing the linear behavior of the plot of the apparent column plate height versus the reciprocal of (1+k')(2) for at least three homologous compounds, with a linear regression coefficient R(2) larger than 0.999. Irrespective of the contribution of the several, different instruments used to the total band broadening, the same column HETP value was obtained within 5%. This new protocol outperform the classical one in which the chromatographic column is replaced with a zero dead volume (ZDV) union connector to measure the extra-column volume variance, which is subtracted from the variance measured with the column to measure the intrinsic HETP. This protocol fails because it significantly underestimates the system volume variance. Copyright © 2013 Elsevier B.V. All rights reserved.

  17. 4. TYPICAL COLUMN BASE (COLUMN #1 ON PHOTO ELEVATION PLAN) ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    4. TYPICAL COLUMN BASE (COLUMN #1 ON PHOTO ELEVATION PLAN) FACING SOUTH. - U.S. Naval Base, Pearl Harbor, Signal Tower, Corner of Seventh Street & Avenue D east of Drydock No. 1, Pearl City, Honolulu County, HI

  18. Pushover analysis of reinforced concrete frames considering shear failure at beam-column joints

    NASA Astrophysics Data System (ADS)

    Sung, Y. C.; Lin, T. K.; Hsiao, C. C.; Lai, M. C.

    2013-09-01

    Since most current seismic capacity evaluations of reinforced concrete (RC) frame structures are implemented by either static pushover analysis (PA) or dynamic time history analysis, with diverse settings of the plastic hinges (PHs) on such main structural components as columns, beams and walls, the complex behavior of shear failure at beam-column joints (BCJs) during major earthquakes is commonly neglected. This study proposes new nonlinear PA procedures that consider shear failure at BCJs and seek to assess the actual damage to RC structures. Based on the specifications of FEMA-356, a simplified joint model composed of two nonlinear cross struts placed diagonally over the location of the plastic hinge is established, allowing a sophisticated PA to be performed. To verify the validity of this method, the analytical results for the capacity curves and the failure mechanism derived from three different full-size RC frames are compared with the experimental measurements. By considering shear failure at BCJs, the proposed nonlinear analytical procedures can be used to estimate the structural behavior of RC frames, including seismic capacity and the progressive failure sequence of joints, in a precise and effective manner.

  19. Nuclear reactor control column

    DOEpatents

    Bachovchin, Dennis M.

    1982-01-01

    The nuclear reactor control column comprises a column disposed within the nuclear reactor core having a variable cross-section hollow channel and containing balls whose vertical location is determined by the flow of the reactor coolant through the column. The control column is divided into three basic sections wherein each of the sections has a different cross-sectional area. The uppermost section of the control column has the greatest cross-sectional area, the intermediate section of the control column has the smallest cross-sectional area, and the lowermost section of the control column has the intermediate cross-sectional area. In this manner, the area of the uppermost section can be established such that when the reactor coolant is flowing under normal conditions therethrough, the absorber balls will be lifted and suspended in a fluidized bed manner in the upper section. However, when the reactor coolant flow falls below a predetermined value, the absorber balls will fall through the intermediate section and into the lowermost section, thereby reducing the reactivity of the reactor core and shutting down the reactor.

  20. Constant pressure-assisted head-column field-amplified sample injection in combination with in-capillary derivatization for enhancing the sensitivity of capillary electrophoresis.

    PubMed

    Yan, Na; Zhou, Lei; Zhu, Zaifang; Zhang, Huige; Zhou, Ximin; Chen, Xingguo

    2009-05-15

    In this work, a novel method combining constant pressure-assisted head-column field-amplified sample injection (PA-HC-FASI) with in-capillary derivatization was developed for enhancing the sensitivity of capillary electrophoresis. PA-HC-FASI uses an appropriate positive pressure to counterbalance the electroosmotic flow in the capillary column during electrokinetic injection, while taking advantage of the field amplification in the sample matrix and the water of the "head column". Accordingly, the analytes were stacked at the stationary boundary between water and background electrolyte. After 600s PA-HC-FASI, 4-fluoro-7-nitro-2,1,3-benzoxadiazole as derivatization reagent was injected, followed by an electrokinetic step (5kV, 45s) to enhance the mixing efficiency of analytes and reagent plugs. Standing a specified time of 10min for derivatization reaction under 35 degrees C, then the capillary temperature was cooled to 25 degrees C and the derivatives were immediately separated and determined under 25 degrees C. By investigating the variables of the presented approach in detail, on-line preconcentration, derivatization and separation could be automatically operated in one run and required no modification of current CE commercial instrument. Moreover, the sensitivity enhancement factor of 520 and 800 together with the detection limits of 16.32 and 6.34pg/mL was achieved for model compounds: glufosinate and aminomethylphosphonic acid, demonstrating the high detection sensitivity of the presented method.

  1. Combination L-T3 and L-T4 therapy for hypothyroidism.

    PubMed

    Wartofsky, Leonard

    2013-10-01

    Because of the longstanding controversy regarding whether hypothyroid patients can be optimally replaced by treatment with levothyroxine (L-T4) alone, numerous studies have addressed potential benefits of combined therapy of triiodothyronine (T3) with L-T4. Results of these studies have failed to support a potential benefit of combined therapy. A strong argument for the addition of L-T3 to L-T4 monotherapy has been lacking until recent genetic studies indicated a rationale for such therapy among a small fraction of the hypothyroid patient population. Interest in this issue has focused on the importance of the deiodinases in maintaining the euthyroid state and the role of genetic polymorphisms in the deiodinase genes that would affect thyroid hormone concentrations in both blood and tissues. One such polymorphism in the D2 gene, Thr92Ala, is associated with reduced T4 to T3 activation in skeletal muscle and thyroid, linked to obesity and alterations in thyroid-pituitary feedback, and in responses to thyroid hormone treatment. Although our professional organizations continue to recommend L-T4 alone for the treatment of hypothyroidism, the possibility of a D2 gene polymorphism should be considered in patients on L-T4 monotherapy who continue to complain of fatigue in spite of dosage achieving low normal serum thyroid stimulating hormone levels. A suggestive clue to the presence of this polymorphism could be a higher than normal free T4/free T3 ratio. Clinicians could consider adding T3 as a therapeutic trial in selected patients. Future well controlled clinical trials will be required to more fully resolve the controversy.

  2. Programmable selectivity for GC with series-coupled columns using pulsed heating of the second column.

    PubMed

    Whiting, Joshua; Sacks, Richard

    2003-05-15

    A series-coupled ensemble of a nonpolar dimethyl polysiloxane column and a polar trifluoropropylmethyl polysiloxane column with independent at-column heating is used to obtain pulsed heating of the second column. For mixture component bands that are separated by the first column but coelute from the column ensemble, a temperature pulse is initiated after the first of the two components has crossed the column junction point and is in the second column, while the other component is still in the first column. This accelerates the band for the first component. If the second column cools sufficiently prior to the second component band crossing the junction, the second band experiences less acceleration, and increased separation is observed for the corresponding peaks in the ensemble chromatogram. High-speed at-column heating is obtained by wrapping the fused-silica capillary column with resistance heater wire and sensor wire. Rapid heating for a temperature pulse is obtained with a short-duration linear heating ramp of 1000 degrees C/min. During a pulse, the second-column temperature increases by 20-100 degrees C in a few seconds. Using a cold gas environment, cooling to a quiescent temperature of 30 degrees C can be obtained in approximately 25 s. The effects of temperature pulse initiation time and amplitude on ensemble peak separation and resolution are described. A series of appropriately timed temperature pulses is used to separate three coeluting pairs of components in a 13-component mixture.

  3. [Separation/preconcentration of trace rare earth elements in Tricholoma giganteum by micro-column with nanometer A1203 and their determination by ICP-AES].

    PubMed

    Liu, Hong-gao; Wang, Yuan-zhong

    2010-01-01

    Using a micro-column packed with immobilized 1-phenyl-3-methyl-4-bonzoil-5-pyrazone(PMBP) on nanometer Al2O3 powder as the adsorption material, the adsorption and elution behaviors of rare earth ions (Sc3+, Y3+ and La3+) on the above material under dynamic conditions were studied with inductively coupled plasma-atomic emission spectrometry. The conditions for preconcentration of rare earth ions were optimized, and the results show that the studied ions can be adsorbed quantitatively on the above material at pH 4.5 and the analytes adsorbed on the column can be eluted with 0.5 mol x L(-1) HCl solution. The detection limits of the method for Sc, Y and La were 0.15, 0.18 and 0.34 microg x L(-1), respectively, and the relative standard deviations were 2.5%, 3.0% and 1.7%, respectively (n=12, c = 0.5 mg x L(-1)). The proposed method was applied to the determination of trace amount of Sc, Y and La in Tricholoma giganteum with satisfactory results.

  4. Efficiency gain limits of the parallel segmented inlet and outlet flow concept in analytical liquid chromatography columns suffering from radial transcolumn packing density gradients.

    PubMed

    Broeckhoven, Ken; Desmet, Gert

    2012-10-05

    The maximal gain in efficiency that can be expected from the use of the segmented column end fittings that were recently introduced to alleviate the effect of transcolumn packing density gradients has been quantified and generalized using numerical computations of the band broadening process. It was found that, for an unretained compound in a column with a parabolic packing density gradient, the use of a segmented inlet or a segmented outlet allows to eliminate about 60-100% of the plate height contribution (H(tc)) originating from a parabolic transcolumn velocity gradient in a d(c)=4.6 mm column. In a d(c)=2.1 mm column, these percentages change from 10 to 100%. Using a combined segmented in- and outlet, H(tc) can be reduced by about 90-100% (d(c)=4.6 mm column) or 20-100% (d(c)=2.1 mm column). The strong variation of these gain percentages is due to fact that they depend very strongly on the column length and the flow rate. Dimensionless graphs have been established that allow to directly quantify the effect for each specific case. It was also found that, in agreement with one's physical intuition, trans-column velocity profiles that are more flat in the central region benefit more from the concept than sharp, parabolic-like profiles. The gain margins furthermore tend to become smaller with increasing retention and increasing diffusion coefficient. Copyright © 2012 Elsevier B.V. All rights reserved.

  5. Stability of column-supported embankments.

    DOT National Transportation Integrated Search

    2006-01-01

    Column-supported embankments have a great potential for application in the coastal regions of Virginia, where highway embankments are often constructed on soft ground. The columns can be driven piles, vibro-concrete columns, deep-mixing-method column...

  6. Relaxivity of Ferumoxytol at 1.5 T and 3.0 T.

    PubMed

    Knobloch, Gesine; Colgan, Timothy; Wiens, Curtis N; Wang, Xiaoke; Schubert, Tilman; Hernando, Diego; Sharma, Samir D; Reeder, Scott B

    2018-05-01

    The aim of this study was to determine the relaxation properties of ferumoxytol, an off-label alternative to gadolinium-based contrast agents, under physiological conditions at 1.5 T and 3.0 T. Ferumoxytol was diluted in gradually increasing concentrations (0.26-4.2 mM) in saline, human plasma, and human whole blood. Magnetic resonance relaxometry was performed at 37°C at 1.5 T and 3.0 T. Longitudinal and transverse relaxation rate constants (R1, R2, R2*) were measured as a function of ferumoxytol concentration, and relaxivities (r1, r2, r2*) were calculated. A linear dependence of R1, R2, and R2* on ferumoxytol concentration was found in saline and plasma with lower R1 values at 3.0 T and similar R2 and R2* values at 1.5 T and 3.0 T (1.5 T: r1saline = 19.9 ± 2.3 smM; r1plasma = 19.0 ± 1.7 smM; r2saline = 60.8 ± 3.8 smM; r2plasma = 64.9 ± 1.8 smM; r2*saline = 60.4 ± 4.7 smM; r2*plasma = 64.4 ± 2.5 smM; 3.0 T: r1saline = 10.0 ± 0.3 smM; r1plasma = 9.5 ± 0.2 smM; r2saline = 62.3 ± 3.7 smM; r2plasma = 65.2 ± 1.8 smM; r2*saline = 57.0 ± 4.7 smM; r2*plasma = 55.7 ± 4.4 smM). The dependence of relaxation rates on concentration in blood was nonlinear. Formulas from second-order polynomial fittings of the relaxation rates were calculated to characterize the relationship between R1blood and R2 blood with ferumoxytol. Ferumoxytol demonstrates strong longitudinal and transverse relaxivities. Awareness of the nonlinear relaxation behavior of ferumoxytol in blood is important for ferumoxytol-enhanced magnetic resonance imaging applications and for protocol optimization.

  7. Gas chromatography fractionation platform featuring parallel flame-ionization detection and continuous high-resolution analyte collection in 384-well plates.

    PubMed

    Jonker, Willem; Clarijs, Bas; de Witte, Susannah L; van Velzen, Martin; de Koning, Sjaak; Schaap, Jaap; Somsen, Govert W; Kool, Jeroen

    2016-09-02

    Gas chromatography (GC) is a superior separation technique for many compounds. However, fractionation of a GC eluate for analyte isolation and/or post-column off-line analysis is not straightforward, and existing platforms are limited in the number of fractions that can be collected. Moreover, aerosol formation may cause serious analyte losses. Previously, our group has developed a platform that resolved these limitations of GC fractionation by post-column infusion of a trap solvent prior to continuous small-volume fraction collection in a 96-wells plate (Pieke et al., 2013 [17]). Still, this GC fractionation set-up lacked a chemical detector for the on-line recording of chromatograms, and the introduction of trap solvent resulted in extensive peak broadening for late-eluting compounds. This paper reports advancements to the fractionation platform allowing flame ionization detection (FID) parallel to high-resolution collection of a full GC chromatograms in up to 384 nanofractions of 7s each. To this end, a post-column split was incorporated which directs part of the eluate towards FID. Furthermore, a solvent heating device was developed for stable delivery of preheated/vaporized trap solvent, which significantly reduced band broadening by post-column infusion. In order to achieve optimal analyte trapping, several solvents were tested at different flow rates. The repeatability of the optimized GC fraction collection process was assessed demonstrating the possibility of up-concentration of isolated analytes by repetitive analyses of the same sample. The feasibility of the improved GC fractionation platform for bioactivity screening of toxic compounds was studied by the analysis of a mixture of test pesticides, which after fractionation were subjected to a post-column acetylcholinesterase (AChE) assay. Fractions showing AChE inhibition could be unambiguously correlated with peaks from the parallel-recorded FID chromatogram. Copyright © 2016 Elsevier B.V. All rights

  8. Comparison between the intra-particle diffusivity in the hydrophilic interaction chromatography and reversed phase liquid chromatography modes. Impact on the column efficiency.

    PubMed

    Gritti, Fabrice; Guiochon, Georges

    2013-07-05

    The effective diffusion coefficients of five low molecular weigh compounds (naphthalene, uracil, uridine, adenosine, and cytosine) were measured at room temperature in a 4.6mm×100mm column packed with 3.5μm XBridge HILIC particles. The mobile phase was an acetonitrile-water mixture (92.5/7.5, v/v) containing 10mM ammonium acetate and 0.02% acetic acid. Using a physically reliable model of effective diffusion in binary composite media (Torquato's model), accurate estimates of the intra-particle diffusivities in the HILIC particles were obtained as a function of the retention of these analytes. The HILIC diffusion coefficients were compared to those previously obtained for endcapped RPLC-C18 particles (5.0μm Gemini-C18). The experimental results confirm that adsorption sites are not localized in RPLC whereas they are so in the HILIC mode. In contrast to RPLC columns, HILIC columns provide longitudinal diffusion B/u terms that increase very little with increasing retention factors. This confirms the absence of surface diffusion in HILIC. The impact of intra-particle diffusivity on the column efficiency was projected in HILIC and RPLC on the basis of the measured intra-particle diffusivities and on the well established theory of band broadening in particulate columns. Accordingly, RPLC columns generate short-range eddy dispersion and solid-liquid mass transfer resistance Cu terms that increase less than do HILIC column with increasing retention factors. The HETP contribution caused by the trans-column structure heterogeneity is smaller in the HILIC than in the RPLC modes because the transverse excursion length is smaller in HILIC. Even though the overall column efficiencies are comparable in HILIC and RPLC, this study shows that the individual mass transfer phenomena are inherently different in the HILIC and the RPLC retention modes. Copyright © 2013 Elsevier B.V. All rights reserved.

  9. Involvement of cell shape and flagella in the bacterial retention during percolation of contaminated water through soil columns in tropical region.

    PubMed

    Nola, Moise; Ewoti, Olive V Noah; Nougang, Mireille; Moungang, Marlyse L; Chihib, Nour-Eddine; Krier, Francois; Servais, Pierre; Hornez, Jean-Pierre; Njine, Thomas

    2010-09-01

    Microorganisms' retention in soil contributes to the natural purification of groundwater. Bacteria found in groundwater are generally of various shapes. The aim of this study was to assess the importance of cell shape and flagella in bacterial retention during polluted water percolation through two soil columns CA and CB, in the equatorial region in Central Africa. Percolation tests were carried out using different water loads samples which were contaminated by Escherichia coli (straight rods, peritrichous flagella), Vibrio parahaemolyticus (rods bacteria, polar flagella), and Staphylococcus saprophyticus (spherical, free-flagellum). It has been noted that showed that through soil column CA, the mean values of cells retention ratios (T(R)) varied with bacteria species considered, and from one applied water load sample to another. E. coli T(R) and that of S. saprophyticus were not significantly different (P> 0.05) for the two soil columns. V. parahaemolyticus T(R) significantly differed from that of E. coli and S. saprophyticus through soil column CA (P< 0.01) when the highest water load was applied, and through soil column CB (P< 0.05) for each of water load applied. A relative hierarchical arrangement of retained cells based on the T(R) showed that V. parahaemolyticus was less retained through the 2 soil columns. S. saprophyticus in most cases was more retained than others. The physical properties of the bacterial cell must be taken into consideration when evaluating the transfer of bacteriological pollutants towards groundwater.

  10. Practical comparison of LC columns packed with different superficially porous particles for the separation of small molecules and medium size natural products.

    PubMed

    Yang, Peilin; McCabe, Terry; Pursch, Matthias

    2011-11-01

    Commercial C(18) columns packed with superficially porous particles of different sizes and shell thicknesses (Ascentis Express, Kinetex, and Poroshell 120) or sub-2-μm totally porous particles (Acquity BEH) were systematically compared using a small molecule mixture and a complex natural product mixture as text probes. Significant efficiency loss was observed on 2.1-mm id columns even with a low dispersion ultra-high pressure liquid chromatography system. The Kinetex 4.6-mm id column packed with 2.6-μm particles exhibited the best overall efficiency for small molecule separations and the Poroshell 120 column showed better performance for mid-size natural product analytes. The Kinetex 2.1-mm id column packed with 1.7-μm particles did not deliver the expected performance and the possible reasons besides extra column effect have been proved to be frictional heating effect and poor column packing quality. Different column retentivities and selectivities have been observed on the four C(18) columns of different brands for the natural product separation. Column batch-to-batch variability that has been previously observed on the Ascentis Express column was also observed on the Kinetex and Poroshell 120 column. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Proline-coated column for the capillary electrochromatographic separation of amino acids by in-column derivatization.

    PubMed

    Lin, Chun-Chi; Liu, Chuen-Ying

    2004-10-01

    With 3-trimethoxysilylpropyl chloride as the spacer, a proline-coated capillary column was prepared for the capillary electrochromatographic (CEC) separation of amino acids by in-column derivatization. Nine standard mixtures, including aspartic acid, glutamic acid, valine, phenylalanine, alanine, isoleucine, leucine, tyrosine, and tryptophan, were injected. o-Phthalaldehyde (OPA), OPA/2-mercaptoethanol (2-ME) and OPA/N-acetylcysteine (NAC) in borate buffer were tested as the derivatizing agent. Among them, OPA (50 mM) in borate buffer (pH 9.5, 50 mM) gave the best performance. The formation of isoindole could be detected by UV detection. The sandwich-type injection was carried out in hydrostatic mode (10 cm) with the program R(10 s)S(10 s) R(10 s)W(10 min) with R, S, and W being the reagent, sample, and waiting times. Mesityl oxide, benzyl alcohol, and acetone showed some interaction with the column. A current monitoring method was used instead of the determination of the electroosmotic flow (EOF). The direction of EOF was from anode to cathode even under acidic condition lower than the pI value (6.31) of the bonded group due to some unreacted silanol groups. Some parameters including pH, nature, and concentration of the mobile phase and the effect of organic modifier with regard to the CEC separation were investigated. With the proline-coated column (75 (50) cm x 75 microm ID) the best separation was performed in phosphate buffer (pH 4.00, 100 mM) with an applied voltage of -15 kV. The established method was also compared with those precolumn derivatized prior to the separation with proline-coated column as well as with in-capillary derivatization and separation with a bare fused-silica column. Copyright 2004 WILEY-VCH Verlag GmbH & Co.

  12. Laboratory-Scale Column Testing Using IONSIV IE-911 for Removing Cesium from Acidic Tank Waste Simulant. 1: Cesium Exchange Capacity of a 15-cm3 Column and Dynamic Stability of the Exchange Media

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    T.J. Tranter; R.D. Tillotson; T.A. Todd

    2005-04-01

    Bench-scale column tests were performed using a commercial form of crystalline silicotitanate (CST) for removing radio-cesium from a surrogate acidic tank solution representative of liquid waste stored at the Idaho National Engineering and Environmental Laboratory (INEEL). An engineered form of CST ion exchanger, known as IONSIVtm IE-911 (UOP, Mt Laurel, NJ, USA), was tested in 15 cm3 columns at a flow rate of 5 bed volumes per hour. These experiments showed the ion exchange material to have reasonable selectivity and capacity for removing cesium from the complex chemical matrix of the solution. However, previous testing indicated that partial neutralization ofmore » the feed stream was necessary to increase the stability of the ion exchange media. Thus, in these studies, CST degradation was determined as a function of throughput in order to better assess the stability characteristics of the exchanger for potential future waste treatment applications. Results of these tests indicate that the degradation of the CST reaches a maximum very soon after the acidic feed is introduced to the column and then rapidly declines. Total dissolution of bed material did not exceed 3% under the experimental regime used.« less

  13. 7T MRI subthalamic nucleus atlas for use with 3T MRI.

    PubMed

    Milchenko, Mikhail; Norris, Scott A; Poston, Kathleen; Campbell, Meghan C; Ushe, Mwiza; Perlmutter, Joel S; Snyder, Abraham Z

    2018-01-01

    Deep brain stimulation (DBS) of the subthalamic nucleus (STN) reduces motor symptoms in most patients with Parkinson disease (PD), yet may produce untoward effects. Investigation of DBS effects requires accurate localization of the STN, which can be difficult to identify on magnetic resonance images collected with clinically available 3T scanners. The goal of this study is to develop a high-quality STN atlas that can be applied to standard 3T images. We created a high-definition STN atlas derived from seven older participants imaged at 7T. This atlas was nonlinearly registered to a standard template representing 56 patients with PD imaged at 3T. This process required development of methodology for nonlinear multimodal image registration. We demonstrate mm-scale STN localization accuracy by comparison of our 3T atlas with a publicly available 7T atlas. We also demonstrate less agreement with an earlier histological atlas. STN localization error in the 56 patients imaged at 3T was less than 1 mm on average. Our methodology enables accurate STN localization in individuals imaged at 3T. The STN atlas and underlying 3T average template in MNI space are freely available to the research community. The image registration methodology developed in the course of this work may be generally applicable to other datasets.

  14. A new method for the preparation of polymeric porous layer open tubular columns for GC application

    NASA Technical Reports Server (NTRS)

    Shen, T. C.; Wang, M. L.

    1995-01-01

    A new method to prepare polymeric PLOT columns by using in situ polymerization technology is described. The method involves a straightforward in situ polymerization of the monomer. The polymer produced is directly coated on the metal tubing. This eliminates many of the steps needed in conventional polymeric PLOT column preparation. Our method is easy to operate and produces very reproducible columns, as shown previously (T. C. Shen. J. Chromatogr. Sci. 30, 239, 1992). The effects of solvents, tubing pretreatments, initiators and reaction temperatures in the preparation of PLOT columns are studied. Several columns have been developed to separate (1) highly polar compounds, such as water and ammonia or water and HCN, and (2) hydrocarbons and inert gases. A recent improvement has allowed us to produce bonded polymeric PLOT columns. These were studied, and the results are included also.

  15. Analytic integrable systems: Analytic normalization and embedding flows

    NASA Astrophysics Data System (ADS)

    Zhang, Xiang

    In this paper we mainly study the existence of analytic normalization and the normal form of finite dimensional complete analytic integrable dynamical systems. More details, we will prove that any complete analytic integrable diffeomorphism F(x)=Bx+f(x) in (Cn,0) with B having eigenvalues not modulus 1 and f(x)=O(|) is locally analytically conjugate to its normal form. Meanwhile, we also prove that any complete analytic integrable differential system x˙=Ax+f(x) in (Cn,0) with A having nonzero eigenvalues and f(x)=O(|) is locally analytically conjugate to its normal form. Furthermore we will prove that any complete analytic integrable diffeomorphism defined on an analytic manifold can be embedded in a complete analytic integrable flow. We note that parts of our results are the improvement of Moser's one in J. Moser, The analytic invariants of an area-preserving mapping near a hyperbolic fixed point, Comm. Pure Appl. Math. 9 (1956) 673-692 and of Poincaré's one in H. Poincaré, Sur l'intégration des équations différentielles du premier order et du premier degré, II, Rend. Circ. Mat. Palermo 11 (1897) 193-239. These results also improve the ones in Xiang Zhang, Analytic normalization of analytic integrable systems and the embedding flows, J. Differential Equations 244 (2008) 1080-1092 in the sense that the linear part of the systems can be nonhyperbolic, and the one in N.T. Zung, Convergence versus integrability in Poincaré-Dulac normal form, Math. Res. Lett. 9 (2002) 217-228 in the way that our paper presents the concrete expression of the normal form in a restricted case.

  16. Hysteresis in column systems

    NASA Astrophysics Data System (ADS)

    Ivanyi, P.; Ivanyi, A.

    2015-02-01

    In this paper one column of a telescopic construction of a bell tower is investigated. The hinges at the support of the column and at the connecting joint between the upper and lower columns are modelled with rotational springs. The characteristics of the springs are assumed to be non-linear and the hysteresis property of them is represented with the Preisach hysteresis model. The mass of the columns and the bell with the fly are concentrated to the top of the column. The tolling process is simulated with a cycling load. The elements of the column are considered completely rigid. The time iteration of the non-linear equations of the motion is evaluated by the Crank-Nicolson schema and the implemented non-linear hysteresis is handled by the fix-point technique. The numerical simulation of the dynamic system is carried out under different combination of soft, medium and hard hysteresis properties of hinges.

  17. LIQUID-LIQUID EXTRACTION COLUMNS

    DOEpatents

    Thornton, J.D.

    1957-12-31

    This patent relates to liquid-liquid extraction columns having a means for pulsing the liquid in the column to give it an oscillatory up and down movement, and consists of a packed column, an inlet pipe for the dispersed liquid phase and an outlet pipe for the continuous liquid phase located in the direct communication with the liquid in the lower part of said column, an inlet pipe for the continuous liquid phase and an outlet pipe for the dispersed liquid phase located in direct communication with the liquid in the upper part of said column, a tube having one end communicating with liquid in the lower part of said column and having its upper end located above the level of said outlet pipe for the dispersed phase, and a piston and cylinder connected to the upper end of said tube for applying a pulsating pneumatic pressure to the surface of the liquid in said tube so that said surface rises and falls in said tube.

  18. Miniature Distillation Column for Producing LOX From Air

    NASA Technical Reports Server (NTRS)

    Rozzi, Jay C.

    2006-01-01

    The figure shows components of a distillation column intended for use as part of a system that produces high-purity liquid oxygen (LOX) from air by distillation. (The column could be easily modified to produce high-purity liquid nitrogen.) Whereas typical industrial distillation columns for producing high-purity liquid oxygen and/or nitrogen are hundreds of feet tall, this distillation column is less than 3 ft (less than about 0.9 m) tall. This column was developed to trickle-charge a LOX-based emergency oxygen system (EOS) for a large commercial aircraft. A description of the industrial production of liquid oxygen and liquid nitrogen by distillation is prerequisite to a meaningful description of the present miniaturized distillation column. Typically, such industrial production takes place in a chemical processing plant in which large quantities of high-pressure air are expanded in a turboexpander to (1) recover a portion of the electrical power required to compress the air and (2) partially liquefy the air. The resulting two-phase flow of air is sent to the middle of a distillation column. The liquid phase is oxygen-rich, and its oxygen purity increases as it flows down the column. The vapor phase is nitrogen-rich and its nitrogen purity increases as it flows up the column. A heater or heat exchanger, commonly denoted a reboiler, is at the bottom of the column. The reboiler is so named because its role is to reboil some of the liquid oxygen collected at the bottom of the column to provide a flow of oxygen-rich vapor. As the oxygen-rich vapor flows up the column, it absorbs the nitrogen in the down-flowing liquid by mass transfer. Once the vapor leaves the lower portion of the column, it interacts with down-flowing nitrogen liquid that has been condensed in a heat exchanger, commonly denoted a condenser, at the top of the column. Liquid oxygen and liquid nitrogen products are obtained by draining some of the purified product at the bottom and top of the column

  19. A silicone column for GC analysis of polar and nonpolar chemicals

    NASA Technical Reports Server (NTRS)

    Shen, T. C.

    1991-01-01

    The investigation of the Saturnian System is being proposed jointly by NASA and the European Space Agency (ESA). The mission is scheduled for a launch in 1996. The mission provides an opportunity for close observation and exploration of Saturn's atmosphere, the complex Saturnian System of satellites and rings, Titan (Saturn's planet-sized moon), and Saturn's magnetosphere. The mission gives special attention to Titan which is blanketed by a thick, opaque atmosphere. An atmospheric probe will be deposited into the Titan Atmosphere for in situ measurement during a slow, three hour descent to the surface. The results from this analysis may provide the information which is important to the research of chemical evolution, and the origin of life. An analytical system was developed as a part of the Titan Aerosol Gas Experiment (TAGEX), a proposed experiment for the Cassini Mission. This system will use two highly sensitive detectors, the Metastable Ionization Detector (MID) and the Ion Mobility Spectrometer (IMS). Unfortunately, when commercial columns are utilized with these highly sensitive detectors, volatile components continuously bleed from the column and interfere with the detector. In addition, light columns must be able to separate polar and nonpolar organic chemicals within 10-15 minutes under isothermal conditions for the Titan Mission. Therefore, a highly crosslinked silicone polymeric packed column was developed which is able to efficiently separate amines, alcohols, and hydrocarbons with retention times less that 15 minutes at 100 C isothermal condition.

  20. Experimental and Analytical Seismic Studies of a Four-Span Bridge System with Innovative Materials

    NASA Astrophysics Data System (ADS)

    Cruz Noguez, Carlos Alonso

    As part of a multi-university project utilizing the NSF Network for Earthquake Engineering Simulation (NEES), a quarter-scale model of a four-span bridge incorporating plastic hinges with different advanced materials was tested to failure on the three shake table system at the University of Nevada, Reno (UNR). The bridge was the second test model in a series of three 4-span bridges, with the first model being a conventional reinforced-concrete (RC) structure. The purpose of incorporating advanced materials was to improve the seismic performance of the bridge with respect to two damage indicators: (1) column damage and (2) permanent deformations. The goals of the study presented in this document were to (1) evaluate the seismic performance of a 4-span bridge system incorporating SMA/ECC and built-in rubber pad plastic hinges as well as post-tensioned piers, (2) quantify the relative merit of these advanced materials and details compared to each other and to conventional reinforced concrete plastic hinges, (3) determine the influence of abutment-superstructure interaction on the response, (4) examine the ability of available elaborate analytical modeling techniques to model the performance of advanced materials and details, and (5) conduct an extensive parametric study of different variations of the bridge model to study several important issues in bridge earthquake engineering. The bridge model included six columns, each pair of which utilized a different advanced detail at bottom plastic hinges: shape memory alloys (SMA), special engineered cementitious composites (ECC), elastomeric pads embedded into columns, and post-tensioning tendons. The design of the columns, location of the bents, and selection of the loading protocol were based on pre-test analyses conducted using computer program OpenSees. The bridge model was subjected to two-horizontal components of simulated earthquake records of the 1994 Northridge earthquake. Over 340 channels of data were collected

  1. Comparison of 7T and 3T MRI in patients with moyamoya disease.

    PubMed

    Oh, Byeong Ho; Moon, Hyeong Cheol; Baek, Hyeon Man; Lee, Youn Joo; Kim, Sang Woo; Jeon, Young Jai; Lee, Gun Seok; Kim, Hong Rae; Choi, Jai Ho; Min, Kyung Soo; Lee, Mou Seop; Kim, Young Gyu; Kim, Dong Ho; Kim, Won Seop; Park, Young Seok

    2017-04-01

    Magnetic resonance imaging and magnetic resonance angiography (MRI/MRA) are widely used for evaluating the moyamoya disease (MMD). This study compared the diagnostic accuracy of 7Tesla (T) and 3T MRI/MRA in MMD. In this case control study, 12 patients [median age: 34years; range (10-66years)] with MMD and 12 healthy controls [median age: 25years; range (22-59years)] underwent both 7T and 3T MRI/MRA. To evaluate the accuracy of MRI/MRA in MMD, five criteria were compared between imaging systems of 7T and 3T: Suzuki grading system, internal carotid artery (ICA) diameter, ivy sign, flow void of the basal ganglia on T2-weighted images, and high signal intensity areas of the basal ganglia on time-of-flight (TOF) source images. No difference was observed between 7T and 3T MRI/MRA in Suzuki stage, ICA diameter, and ivy sign score; while, 7T MRI/MRA showed a higher detection rate in the flow void on T2-weighted images and TOF source images (p<0.001). Receiver operating characteristic curves of both T2 and TOF criteria showed that 7T MRI/MRA had higher sensitivity and specificity than 3T MRI/MRA. Our findings indicate that 7T MRI/MRA is superior to 3T MRI/MRA for the diagnosis of MMD in point of detecting the flow void in basal ganglia by T2-weighted and TOF images. Copyright © 2016. Published by Elsevier Inc.

  2. 45. MAIN MEETING ROOM COLUMNS. Ends of gallery columns identified ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    45. MAIN MEETING ROOM COLUMNS. Ends of gallery columns identified at the time of removal for transfer to the George School for re-erection. The stamp reads, 'REMOVED FROM 12th ST. MTG HSE PHILA 1972'. - Twelfth Street Meeting House, 20 South Twelfth Street, Philadelphia, Philadelphia County, PA

  3. On the analytical modeling of the nonlinear vibrations of pretensioned space structures

    NASA Technical Reports Server (NTRS)

    Housner, J. M.; Belvin, W. K.

    1983-01-01

    Pretensioned structures are receiving considerable attention as candidate large space structures. A typical example is a hoop-column antenna. The large number of preloaded members requires efficient analytical methods for concept validation and design. Validation through analyses is especially important since ground testing may be limited due to gravity effects and structural size. The present investigation has the objective to present an examination of the analytical modeling of pretensioned members undergoing nonlinear vibrations. Two approximate nonlinear analysis are developed to model general structural arrangements which include beam-columns and pretensioned cables attached to a common nucleus, such as may occur at a joint of a pretensioned structure. Attention is given to structures undergoing nonlinear steady-state oscillations due to sinusoidal excitation forces. Three analyses, linear, quasi-linear, and nonlinear are conducted and applied to study the response of a relatively simple cable stiffened structure.

  4. Separating methane emissions from agricultural sources and natural gas: direct measurements of excess columns of CH4, C2H6 and NH3 in the Colorado Front Range

    NASA Astrophysics Data System (ADS)

    Kille, N.; Chiu, R.; Frey, M.; Hase, F.; Kumar Sha, M.; Blumenstock, T.; Hannigan, J. W.; Volkamer, R. M.

    2017-12-01

    Methane (CH4) is a major greenhouse gas emitted from biogenic, thermogenic, and pyrogenic sources. Here we demonstrate a novel approach to separate sources of CH4 emissions based on a network of small portable sensors performing column measurements in the Northern Colorado Front Range (NCFR). In the study area CH4 is emitted from biogenic sources such as concentrated animal feeding operations (CAFOs) and natural gas production and storage. In March 2015 we deployed a network of five Fourier Transform Spectrometers (FTS) to characterize the regional scale methane dome in Colorado's Denver-Julesburg Basin based on excess vertical column measurements (the column enhancement inside the dome over background). Three EM27sun FTS measured CH4, oxygen (O2) and water vapor (H2O) columns at Eaton, CO (inside the dome) and at two boundary sites; the CU mobile SOF (Solar Occultation Flux) measured ethane (C2H6), ammonia (NH3), and H2O at Eaton, CO. The column averaged dry air mole fractions XCH4, XC2H6, and XNH3 were determined using O2 columns for air mass factor normalization, and background column was subtracted to derive excess vertical columns of DXCH4, DXC2H6, DXNH3 at Eaton, CO. Eaton is located both near CAFOs and at the northern edge of oil and natural gas production wells. Our approach for source apportioning methane employs a linear regression analysis that explains DXCH4 in terms of DXC2H6 as tracer for natural gas sources, and DXNH3 as tracer for CAFO emissions. The results of the source apportionment are compared with literature values of the NH3/CH4 and C2H6/CH4 ratio to evaluate the method of excess columns, which is independent of boundary layer height.

  5. Use of a polar ionic liquid as second column for the comprehensive two-dimensional GC separation of PCBs.

    PubMed

    Zapadlo, Michal; Krupcík, Ján; Májek, Pavel; Armstrong, Daniel W; Sandra, Pat

    2010-09-10

    The orthogonality of three columns coupled in two series was studied for the congener specific comprehensive two-dimensional GC separation of polychlorinated biphenyls (PCBs). A non-polar capillary column coated with poly(5%-phenyl-95%-methyl)siloxane was used as the first ((1)D) column in both series. A polar capillary column coated with 70% cyanopropyl-polysilphenylene-siloxane or a capillary column coated with the ionic liquid 1,12-di(tripropylphosphonium)dodecane bis(trifluoromethane-sulfonyl)imide were used as the second ((2)D) columns. Nine multi-congener standard PCB solutions containing subsets of all native 209 PCBs, a mixture of 209 PCBs as well as Aroclor 1242 and 1260 formulations were used to study the orthogonality of both column series. Retention times of the corresponding PCB congeners on (1)D and (2)D columns were used to construct retention time dependences (apex plots) for assessing orthogonality of both columns coupled in series. For a visual assessment of the peak density of PCBs congeners on a retention plane, 2D images were compared. The degree of orthogonality of both column series was, along the visual assessment of distribution of PCBs on the retention plane, evaluated also by Pearson's correlation coefficient, which was found by correlation of retention times t(R,i,2D) and t(R,i,1D) of corresponding PCB congeners on both column series. It was demonstrated that the apolar+ionic liquid column series is almost orthogonal both for the 2D separation of PCBs present in Aroclor 1242 and 1260 formulations as well as for the separation of all of 209 PCBs. All toxic, dioxin-like PCBs, with the exception of PCB 118 that overlaps with PCB 106, were resolved by the apolar/ionic liquid series while on the apolar/polar column series three toxic PCBs overlapped (105+127, 81+148 and 118+106). Copyright 2010 Elsevier B.V. All rights reserved.

  6. "One-pot" preparation of basic amino acid-silica hybrid monolithic column for capillary electrochromatography.

    PubMed

    Xu, Hongrui; Xu, Zhendong; Yang, Limin; Wang, Qiuquan

    2011-08-01

    A novel "one-pot" strategy was developed for the preparation of amino acid (AA)-silica hybrid monolithic column. The basic AA (L-Arginine, L-Lysine and L-Histidine) was covalently incorporated into the silica hybrid skeleton via the epoxy ring-opening reaction between the amine group and the glycidyl moiety in γ-glycidoxypropyltrimethoxysilane (GPTMS), which was confirmed by elemental analysis and FT-IR studies, while the basic AA was also found to catalyze the polycondensation of tetramethoxysilane and GPTMS. The average mesopore and macropore sizes of the prepared basic AA-silica hybrid monolithic columns were 3.86 nm and 1.71 μm for the L-Lysine-silica hybrid monolith, 5.38 nm and 4.24 μm for the L-Arginine-silica hybrid monolith, and 6.38 nm and 1.24 μm for the L-Histidine-silica hybrid monolith. The hybrid monolith afforded a zwitterionic stationary phase for CEC, the direction and magnitude of EOF can be controlled by the pH of the mobile phase used. Besides an electrophoretic mechanism, the monoliths behave in a typical hydrophilic interaction with the analytes when ACN percentage in the mobile phase is over 40%. Four polar compounds (toluene, DMF, formamide and thiourea) were tested on the three AA-silica hybrid monolithic columns, and the best separation efficiency was observed in the L-Lysine-silica hybrid monolithic column, its theoretical plate height was down to 5.7 μm for thiourea when 20 mM HCOOH-HCOONH4 containing 20% ACN (pH 4.1) was used as a running buffer. The corresponding theoretical plate number for toluene, DMF, formamide and thiourea were 123,385, 103,620, 121,845 and 105,345 plates/m, respectively. Effective separation of phenols and peptides on the L-Lysine-silica hybrid monolithic column was achieved using CEC. We believe that this strategy paves a way for the easy preparation of various functional silica hybrid monolithic columns, aiming at different separation purposes. Copyright © 2011 WILEY-VCH Verlag Gmb

  7. Rapid simultaneous determination of isoflavones in Radix puerariae using high-performance liquid chromatography-triple quadrupole mass spectrometry with novel shell-type column.

    PubMed

    Du, Gang; Zhao, Haiyu; Song, Yuelin; Zhang, Qingwen; Wang, Yitao

    2011-10-01

    A high-performance liquid chromatography (HPLC) coupled with triple quadrupole mass spectrometry (MS/MS) method was developed for rapid determination of 13 isoflavones in Radix puerariae. A novel shell-type column, namely Kinetex core-shell C(18) column (50 mm×2.1 mm id, 2.6 μm), and gradient elution were used during the analysis. The chromatographic peaks of 13 investigated compounds were identified by comparing their retention time and MS data with the related reference compounds. Multiple-reaction monitoring (MRM) was employed for the quantitative analysis with negative ionization mode. All calibration curves showed good linearity (r(2)>0.9990) within test ranges. The LOD and LOQ were lower than 0.017 and 0.873 μg/mL on column, respectively. The intra- and inter-day precisions for 13 analytes were <1.17 and 2.17%, respectively, and the recoveries were 93.1-104.4%. The validated method was applied for quantitative analysis of 13 isoflavones in 7 species of Radix puerariae. The result demonstrated that HPLC-MS/MS system with Kinetex column could be a promising analytical tool for the determination of isoflavones in traditional Chinese medicines, which is helpful for comprehensive evaluation of quality of R. puerariae. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Impact of the column hardware volume on resolution in very high pressure liquid chromatography non-invasive investigations.

    PubMed

    Gritti, Fabrice; McDonald, Thomas; Gilar, Martin

    2015-11-13

    The impact of the column hardware volume (≃ 1.7 μL) on the optimum reduced plate heights of a series of short 2.1 mm × 50 mm columns (hold-up volume ≃ 80-90 μL) packed with 1.8 μm HSS-T3, 1.7 μm BEH-C18, 1.7 μm CSH-C18, 1.6 μm CORTECS-C18+, and 1.7 μm BEH-C4 particles was investigated. A rapid and non-invasive method based on the reduction of the system dispersion (to only 0.15 μL(2)) of an I-class Acquity system and on the corrected plate heights (for system dispersion) of five weakly retained n-alkanophenones in RPLC was proposed. Evidence for sample dispersion through the column hardware volume was also revealed from the experimental plot of the peak capacities for smooth linear gradients versus the corrected efficiency of a weakly retained alkanophenone (isocratic runs). The plot is built for a constant gradient steepness irrespective of the applied flow rates (0.01-0.30 mL/min) and column lengths (2, 3, 5, and 10 cm). The volume variance caused by column endfittings and frits was estimated in between 0.1 and 0.7 μL(2) depending on the applied flow rate. After correction for system and hardware dispersion, the minimum reduced plate heights of short (5 cm) and narrow-bore (2.1mm i.d.) beds packed with sub-2 μm fully and superficially porous particles were found close to 1.5 and 0.7, respectively, instead of the classical h values of 2.0 and 1.4 for the whole column assembly. Copyright © 2015 Elsevier B.V. All rights reserved.

  9. The effect of Si nano-columns in 2-D and 3-D on cellular behaviour: nanotopography-induced CaP deposition from differentiating mesenchymal stem cells.

    PubMed

    Guvendik, S; Trabzon, L; Ramazanoglu, M

    2011-10-01

    Si nano-columns were deposited in 2-D and 3-D in the form of well-defined geometries by physical vapor deposition. The films were grown by e-beam evaporation with an angle between source and substrate. The Si nano-columns were deposited in the shape of spiral with two different incoming atomic flux angle so that the manipulation of nano-columns in 3-D (out-of-plane) was obtained. The Si nano-columns were also grown as vertical stick with square, triangle and linear cross sections in 2D (in-plane). Rat bone marrow mesenchymal stem cells (MSCs) were cultured on these different Si nanosurfaces. MTS assay was carried out to determine the cell proliferation and viability based on different nanotopographies. For the evaluation of cell distribution and morphology, a SEM (Scanning Electron Microscopy) analysis was performed. Any CaP deposition on Si nanosurfaces was observed using energy dispersive X-Ray spectroscopy in SEM (SEM-EDX). After 4 days of culture, there was a higher value of cell proliferation on square columns and spiral Si nano-columns grown with 85 degrees of incoming atomic flux. The cell attachment and spreading was also affected by the geometry of Si nano-columns. While there were still cells showing round/spherical morphology with minimal spreading on conventional Si surfaces, most of the cells cultured on different Si nanotopographies attached on the surface and displayed flattened morphology, especially on the square columns surface. Moreover, CaP deposition was discovered on square columns and spiral films with 85 degrees substrate angle. So, it can be concluded that there is a clear correlation between cell responses and nano-sized geometry on Si surface and it is possible to induce cellular differentiation and CaP formation in certain geometrical constraints.

  10. Mitigation of solvent interference using a short packed column prior to ion mobility spectrometry.

    PubMed

    Jafari, Mohammad T; Saraji, Mohammad; Mossaddegh, Mehdi

    2017-05-15

    This paper introduces a novel approach to overcome the solvent interference in corona discharge-ion mobility spectrometry (CD-IMS) based on the time-resolved signals of the solvent and the analyte. To that end, a short Teflon tube was filled with a low amount of squalene or OV-1, which was prepared and located between the injection port and the entrance of the CD-IMS cell. Through this procedure, a sufficient delay (~5s) was obtained between the introduction of the solvent and the analyte into the reaction region of IMS. This resulted in removing the proton by solvent molecules, as well as increasing the effective collision during the analyte ionization, thereby providing an analysis with more sensitivity, accuracy, and precision. To show the column efficiency, ethion and diazinon (organophosphorus pesticides) were selected as the test compounds and their solutions were analyzed by the proposed method. The amount of sorbent, carrier gas flow rate, and the sorbent temperature affecting the sorbent efficiency were optimized by employing the response surface methodology and the central composite design. The proposed method was exhaustively validated in terms of sensitivity, linearity, and repeatability. In particular, the feasibility of direct injection was successfully verified by the satisfactory results, as compared with those achieved without the prior column. The methodology used in this study is very simple and inexpensive, which can overcome the solvent interference when a solution is directly injected into the CD-IMS. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. Development of an Analytical Method for Explosive Residues in Soil,

    DTIC Science & Technology

    1987-06-01

    confirm peak identities. The eluent for both columns should be 50:50 methanol-water. The elution time for all the analytes of interest on the LC -18 column...nitrate at 1.77 min for LC -8, 1.73 min for LC -DP, and 1.80 for LC -1. 23 Table A2. Instrument calibration results for HMX. Concentration Solution Soil* Peak ...LCT 12 AUG 2 0 W 1M 2j TNT Owl ""r’ L ,,,O MRYX TN L DNS 2 HMX 0 12 LC -CN 110 KMX S 8 TETRYL 6 RDXW 4 DNB and TNB 0 Approved for public release

  12. Estimations of temperature deviations in chromatographic columns using isenthalpic plots. I. Theory for isocratic systems.

    PubMed

    Tarafder, Abhijit; Iraneta, Pamela; Guiochon, Georges; Kaczmarski, Krzysztof; Poe, Donald P

    2014-10-31

    We propose to use constant enthalpy or isenthalpic diagrams as a tool to estimate the extent of the temperature variations caused by the mobile phase pressure drop along a chromatographic column, e.g. of its cooling in supercritical fluid and its heating in ultra-performance liquid chromatography. Temperature strongly affects chromatographic phenomena. Any of its variations inside the column, whether intended or not, can lead to significant changes in separation performance. Although instruments use column ovens in order to keep constant the column temperature, operating conditions leading to a high pressure drop may cause significant variations of the column temperature, both in the axial and the radial directions, from the set value. Different ways of measuring these temperature variations are available but they are too inconvenient to be employed in many practical situations. In contrast, the thermodynamic plot-based method that we describe here can easily be used with only a ruler and a pencil. They should be helpful in developing methods or in analyzing results in analytical laboratories. Although the most effective application area for this approach should be SFC (supercritical fluid chromatography), it can be applied to any chromatographic conditions in which temperature variations take place along the column due to the pressure drop, e.g. in ultra-high pressure liquid chromatography (UHPLC). The method proposed here is applicable to isocractic conditions only. Copyright © 2014 Elsevier B.V. All rights reserved.

  13. Liquid chromatography coupled to on-line post column derivatization for the determination of organic compounds: a review on instrumentation and chemistries.

    PubMed

    Zacharis, Constantinos K; Tzanavaras, Paraskevas D

    2013-10-10

    Analytical derivatization either in pre or post column modes is one of the most widely used sample pretreatment techniques coupled to liquid chromatography. In the present review article we selected to discuss the post column derivatization mode for the analysis of organic compounds. The first part of the review focuses to the instrumentation of post-column setups including not only fundamental components such as pumps and reactors but also less common parts such as static mixers and back-pressure regulators; the second part of the article discusses the most popular "chemistries" that are involved in post column applications, including reagent-less approaches and new sensing platforms such as the popular gold nanoparticles. Some representative recent applications are also presented as tables. Copyright © 2013 Elsevier B.V. All rights reserved.

  14. Approximate analytic solutions to 3D unconfined groundwater flow within regional 2D models

    NASA Astrophysics Data System (ADS)

    Luther, K.; Haitjema, H. M.

    2000-04-01

    We present methods for finding approximate analytic solutions to three-dimensional (3D) unconfined steady state groundwater flow near partially penetrating and horizontal wells, and for combining those solutions with regional two-dimensional (2D) models. The 3D solutions use distributed singularities (analytic elements) to enforce boundary conditions on the phreatic surface and seepage faces at vertical wells, and to maintain fixed-head boundary conditions, obtained from the 2D model, at the perimeter of the 3D model. The approximate 3D solutions are analytic (continuous and differentiable) everywhere, including on the phreatic surface itself. While continuity of flow is satisfied exactly in the infinite 3D flow domain, water balance errors can occur across the phreatic surface.

  15. Analytical and Experimental Evaluation of Digital Control Systems for the Semi-Span Super-Sonic Transport (S4T) Wind Tunnel Model

    NASA Technical Reports Server (NTRS)

    Wieseman, Carol D.; Christhilf, David; Perry, Boyd, III

    2012-01-01

    An important objective of the Semi-Span Super-Sonic Transport (S4T) wind tunnel model program was the demonstration of Flutter Suppression (FS), Gust Load Alleviation (GLA), and Ride Quality Enhancement (RQE). It was critical to evaluate the stability and robustness of these control laws analytically before testing them and experimentally while testing them to ensure safety of the model and the wind tunnel. MATLAB based software was applied to evaluate the performance of closed-loop systems in terms of stability and robustness. Existing software tools were extended to use analytical representations of the S4T and the control laws to analyze and evaluate the control laws prior to testing. Lessons were learned about the complex windtunnel model and experimental testing. The open-loop flutter boundary was determined from the closed-loop systems. A MATLAB/Simulink Simulation developed under the program is available for future work to improve the CPE process. This paper is one of a series of that comprise a special session, which summarizes the S4T wind-tunnel program.

  16. Core/shell Fe3O4/Gd2O3 nanocubes as T1-T2 dual modal MRI contrast agents

    NASA Astrophysics Data System (ADS)

    Li, Fenfen; Zhi, Debo; Luo, Yufeng; Zhang, Jiqian; Nan, Xiang; Zhang, Yunjiao; Zhou, Wei; Qiu, Bensheng; Wen, Longping; Liang, Gaolin

    2016-06-01

    T1-T2 dual modal magnetic resonance imaging (MRI) has attracted considerable interest because it offers complementary diagnostic information, leading to more precise diagnosis. To date, a number of nanostructures have been reported as T1-T2 dual modal MR contrast agents (CAs). However, hybrids of nanocubes with both iron and gadolinium (Gd) elements as T1-T2 dual modal CAs have not been reported. Herein, we report the synthesis of novel core/shell Fe3O4/Gd2O3 nanocubes as T1-T2 dual-modal CAs and their application for enhanced T1-T2 MR imaging of rat livers. A relaxivity study at 1.5 T indicated that our Fe3O4/Gd2O3 nanocubes have an r1 value of 45.24 mM-1 s-1 and an r2 value of 186.51 mM-1 s-1, which were about two folds of those of Gd2O3 nanoparticles and Fe3O4 nanocubes, respectively. In vivo MR imaging of rats showed both T1-positive and T2-negative contrast enhancements in the livers. We envision that our Fe3O4/Gd2O3 nanocubes could be applied as T1-T2 dual modal MR CAs for a wide range of theranostic applications in the near future.T1-T2 dual modal magnetic resonance imaging (MRI) has attracted considerable interest because it offers complementary diagnostic information, leading to more precise diagnosis. To date, a number of nanostructures have been reported as T1-T2 dual modal MR contrast agents (CAs). However, hybrids of nanocubes with both iron and gadolinium (Gd) elements as T1-T2 dual modal CAs have not been reported. Herein, we report the synthesis of novel core/shell Fe3O4/Gd2O3 nanocubes as T1-T2 dual-modal CAs and their application for enhanced T1-T2 MR imaging of rat livers. A relaxivity study at 1.5 T indicated that our Fe3O4/Gd2O3 nanocubes have an r1 value of 45.24 mM-1 s-1 and an r2 value of 186.51 mM-1 s-1, which were about two folds of those of Gd2O3 nanoparticles and Fe3O4 nanocubes, respectively. In vivo MR imaging of rats showed both T1-positive and T2-negative contrast enhancements in the livers. We envision that our Fe3O4/Gd2O3 nanocubes

  17. Successful nonoperative treatment of a three-column thoracic fracture in a patient with ankylosing spondylitis: existence and clinical significance of the fourth column of the spine.

    PubMed

    Shen, Francis H; Samartzis, Dino

    2007-07-01

    A case report. To report the successful nonoperative management of a patient with progressive ankylosing spondylitis who sustained a three-column flexion-distraction injury of the upper thoracic spine with an intact sternal-rib complex, thereby emphasizing the existence and clinical relevance of the fourth-column concept in such patients. Three-column injuries of the cervical and lumbar spine are typically unstable and require surgical stabilization. Patients with ankylosing spondylitis are at an increase risk to sustain three-column injuries of the spine due to their progressive inflammatory disease, a state that renders the spine brittle and alters its biomechanical function. A fourth-column model of the thoracic spine has been proposed and incorporates the sternal-rib complex; however, such a model has rarely been addressed in the literature and its role regarding three-column upper thoracic spine injury with an intact sternal-rib complex in patients with ankylosing spondylitis is unknown. METHODS.: A 68-year-old white man with ankylosing spondylitis and Pickwickian body habitus sustained a three-column flexion-distraction injury at T5 following a ground-level fall. The patient complained of midthoracic back pain; however, he was neurologically intact and ambulated without aids. Because of the patient's numerous active medical issues that substantially increased his perioperative risks combined with symptomatic improvement of his pain, the patient refused surgical stabilization. In addition, because of the patient's body habitus and pulmonary issues, external brace immobilization was not tolerated. At 17 months of follow-up, the patient remained neurologically intact, ambulated well, his midthoracic back pain had subsided, and no progressive kyphosis was noted. This case confirms the existence and clinical relevance of the fourth column of the thoracic spine and its role in providing added spinal stability in the patient with ankylosing spondylitis. As such, it

  18. High-Speed Rotor Analytical Dynamics on Flexible Foundation Subjected to Internal and External Excitation

    NASA Astrophysics Data System (ADS)

    Jivkov, Venelin S.; Zahariev, Evtim V.

    2016-12-01

    The paper presents a geometrical approach to dynamics simulation of a rigid and flexible system, compiled of high speed rotating machine with eccentricity and considerable inertia and mass. The machine is mounted on a vertical flexible pillar with considerable height. The stiffness and damping of the column, as well as, of the rotor bearings and the shaft are taken into account. Non-stationary vibrations and transitional processes are analyzed. The major frequency and modal mode of the flexible column are used for analytical reduction of its mass, stiffness and damping properties. The rotor and the foundation are modelled as rigid bodies, while the flexibility of the bearings is estimated by experiments and the requirements of the manufacturer. The transition effects as a result of limited power are analyzed by asymptotic methods of averaging. Analytical expressions for the amplitudes and unstable vibrations throughout resonance are derived by quasi-static approach increasing and decreasing of the exciting frequency. Analytical functions give the possibility to analyze the influence of the design parameter of many structure applications as wind power generators, gas turbines, turbo-generators, and etc. A numerical procedure is applied to verify the effectiveness and precision of the simulation process. Nonlinear and transitional effects are analyzed and compared to the analytical results. External excitations, as wave propagation and earthquakes, are discussed. Finite elements in relative and absolute coordinates are applied to model the flexible column and the high speed rotating machine. Generalized Newton - Euler dynamics equations are used to derive the precise dynamics equations. Examples of simulation of the system vibrations and nonstationary behaviour are presented.

  19. Chiral separation of G-type chemical warfare nerve agents via analytical supercritical fluid chromatography.

    PubMed

    Kasten, Shane A; Zulli, Steven; Jones, Jonathan L; Dephillipo, Thomas; Cerasoli, Douglas M

    2014-12-01

    Chemical warfare nerve agents (CWNAs) are extremely toxic organophosphorus compounds that contain a chiral phosphorus center. Undirected synthesis of G-type CWNAs produces stereoisomers of tabun, sarin, soman, and cyclosarin (GA, GB, GD, and GF, respectively). Analytical-scale methods were developed using a supercritical fluid chromatography (SFC) system in tandem with a mass spectrometer for the separation, quantitation, and isolation of individual stereoisomers of GA, GB, GD, and GF. Screening various chiral stationary phases (CSPs) for the capacity to provide full baseline separation of the CWNAs revealed that a Regis WhelkO1 (SS) column was capable of separating the enantiomers of GA, GB, and GF, with elution of the P(+) enantiomer preceding elution of the corresponding P(-) enantiomer; two WhelkO1 (SS) columns had to be connected in series to achieve complete baseline resolution. The four diastereomers of GD were also resolved using two tandem WhelkO1 (SS) columns, with complete baseline separation of the two P(+) epimers. A single WhelkO1 (RR) column with inverse stereochemistry resulted in baseline separation of the GD P(-) epimers. The analytical methods described can be scaled to allow isolation of individual stereoisomers to assist in screening and development of countermeasures to organophosphorus nerve agents. © 2014 The Authors. Chirality published by John Wiley Periodicals, Inc.

  20. Chiral Separation of G-type Chemical Warfare Nerve Agents via Analytical Supercritical Fluid Chromatography

    PubMed Central

    Kasten, Shane A; Zulli, Steven; Jones, Jonathan L; Dephillipo, Thomas; Cerasoli, Douglas M

    2014-01-01

    Chemical warfare nerve agents (CWNAs) are extremely toxic organophosphorus compounds that contain a chiral phosphorus center. Undirected synthesis of G-type CWNAs produces stereoisomers of tabun, sarin, soman, and cyclosarin (GA, GB, GD, and GF, respectively). Analytical-scale methods were developed using a supercritical fluid chromatography (SFC) system in tandem with a mass spectrometer for the separation, quantitation, and isolation of individual stereoisomers of GA, GB, GD, and GF. Screening various chiral stationary phases (CSPs) for the capacity to provide full baseline separation of the CWNAs revealed that a Regis WhelkO1 (SS) column was capable of separating the enantiomers of GA, GB, and GF, with elution of the P(+) enantiomer preceding elution of the corresponding P(–) enantiomer; two WhelkO1 (SS) columns had to be connected in series to achieve complete baseline resolution. The four diastereomers of GD were also resolved using two tandem WhelkO1 (SS) columns, with complete baseline separation of the two P(+) epimers. A single WhelkO1 (RR) column with inverse stereochemistry resulted in baseline separation of the GD P(–) epimers. The analytical methods described can be scaled to allow isolation of individual stereoisomers to assist in screening and development of countermeasures to organophosphorus nerve agents. Chirality 26:817–824, 2014. © 2014 The Authors. Chirality published by John Wiley Periodicals, Inc. PMID:25298066

  1. Determination of 3,6-dinitrobenzo[e]pyrene in surface soil and airborne particles by high-performance liquid chromatography with fluorescence detection.

    PubMed

    Hasei, Tomohiro; Watanabe, Tetsushi; Hirayama, Teruhisa

    2006-11-24

    We developed a sensitive analytical method and an efficient clean-up method to quantify 3,6-dinitrobenzo[e]pyrene (3,6-DNBeP) in surface soil and airborne particles. After purification using a silica gel column and two reversed-phase columns, 3,6-DNBeP was reduced to 3,6-diaminobenzo[e]pyrene by a catalyst column and analyzed by high-performance liquid chromatography (HPLC) with a fluorescence detector. 3,6-DNBeP was detected in all of the soil samples and airborne particles examined. The concentration of 3,6-DNBeP in surface soil and airborne particles was determined in the ranges of 347-5007 pg/g of soil and 137-1238 fg/m3, respectively.

  2. Cytokine adsorbing columns.

    PubMed

    Taniguchi, Takumi

    2010-01-01

    Sepsis induces the activation of complement and the release of inflammatory cytokines such as TNF-alpha and IL-1beta. The inflammatory cytokines and nitric oxide induced by sepsis can decrease systemic vascular resistance, resulting in profound hypotension. The combination of hypotension and microvascular occlusion results in tissue ischemia and ultimately leads to multiple organ failure. Recently, several experimental and clinical studies have reported that treatment for adsorption of cytokines is beneficial during endotoxemia and sepsis. Therefore, the present article discusses cytokine adsorbing columns. These columns, such as CytoSorb, CYT-860-DHP, Lixelle, CTR-001 and MPCF-X, the structures of which vary significantly, have excellent adsorption rates for inflammatory cytokines such as TNF-alpha, IL-1beta, IL-6 and IL8. Many studies have demonstrated that treatment with cytokine adsorbing columns has beneficial effects on the survival rate and inflammatory responses in animal septic models. Moreover, several cases have been reported in which treatment with cytokine adsorbing columns is very effective in hemodynamics and organ failures in critically ill patients. Although further investigations and clinical trials are needed, in the future treatment with cytokine adsorbing columns may play a major role in the treatment of hypercytokinemia such as multiple organ failure and acute respiratory distress syndrome. Copyright 2010 S. Karger AG, Basel.

  3. [Influences of the mobile phase constitution, salt concentration and pH value on retention characters of proteins on the metal chelate column].

    PubMed

    Li, R; Di, Z M; Chen, G L

    2001-09-01

    The effects of the nature and concentration of salts, pH value and competitive eluent in the mobile phase on the protein retention have been systematically investigated. A mathematical expression describing the protein retention in metal chelate chromatography has been derived. It is proposed that the eluting power of the salt solution can be expressed by the eluent strength exponent epsilon. According to the retention characters of protein under different chromatographic conditions, the interaction between the various metal chelate ligands and proteins is discussed. The protein retention on the metal chelate column is a cooperative interactions of coordination, electrostatic and hydrophobic interaction. For the strong combined metal column with proteins such as IDA-Cu, the coordination is the most important, and the electrostatic interaction is secondary in chromatographic process. However, for the weak combined metal columns with proteins such as IDA-Ni, IDA-Co and IDA-Zn, the electrostatic interaction between the metal chelate ligands and proteins is the chief one, while the coordination is the next in importance. When the mobile phase contains high concentration of salt which can't form complex with the immobilized metal, the hydrophobic interaction between the protein and stationary phase will be increased. As the interaction between the metal chelate ligand and proteins relates to chromatographic operating conditions closely, different elution processes may be selected for different metal chelate columns. The gradient elution is generally performed by the low concentration of salt or different pH for weakly combined columns with proteins, however the competitive elution procedure is commonly utilized for strongly combined column. The experiment showed that NH3 is an excellent competitive eluent. It isn't only give the efficient separation of proteins, but also has the advantages of cheapness, less bleeding of the immobilized metals and ease of controlling NH3

  4. A spin column-free approach to sodium hydroxide-based glycan permethylation.

    PubMed

    Hu, Yueming; Borges, Chad R

    2017-07-24

    Glycan permethylation was introduced as a tool to facilitate the study of glycans in 1903. Since that time, permethylation procedures have been continually modified to improve permethylation efficiency and qualitative applicability. Typically, however, either laborious preparation steps or cumbersome and uneconomical spin columns have been needed to obtain decent permethylation yields on small glycan samples. Here we describe a spin column-free (SCF) glycan permethylation procedure that is applicable to both O- and N-linked glycans and can be employed upstream to intact glycan analysis by MALDI-MS, ESI-MS, or glycan linkage analysis by GC-MS. The SCF procedure involves neutralization of NaOH beads by acidified phosphate buffer, which eliminates the risk of glycan oxidative degradation and avoids the use of spin columns. Optimization of the new permethylation procedure provided high permethylation efficiency for both hexose (>98%) and HexNAc (>99%) residues-yields which were comparable to (or better than) those of some widely-used spin column-based procedures. A light vs. heavy labelling approach was employed to compare intact glycan yields from a popular spin-column based approach to the SCF approach. Recovery of intact N-glycans was significantly better with the SCF procedure (p < 0.05), but overall yield of O-glycans was similar or slightly diminished (p < 0.05 for tetrasaccharides or smaller). When the SCF procedure was employed upstream to hydrolysis, reduction and acetylation for glycan linkage analysis of pooled glycans from unfractionated blood plasma, analytical reproducibility was on par with that from previous spin column-based "glycan node" analysis results. When applied to blood plasma samples from stage III-IV breast cancer patients (n = 20) and age-matched controls (n = 20), the SCF procedure facilitated identification of three glycan nodes with significantly different distributions between the cases and controls (ROC c-statistics > 0.75; p < 0

  5. A spin column-free approach to sodium hydroxide-based glycan permethylation†

    PubMed Central

    Hu, Yueming; Borges, Chad R.

    2018-01-01

    Glycan permethylation was introduced as a tool to facilitate the study of glycans in 1903. Since that time, permethylation procedures have been continually modified to improve permethylation efficiency and qualitative applicability. Typically, however, either laborious preparation steps or cumbersome and uneconomical spin columns have been needed to obtain decent permethylation yields on small glycan samples. Here we describe a spin column-free (SCF) glycan permethylation procedure that is applicable to both O- and N-linked glycans and can be employed upstream to intact glycan analysis by MALDI-MS, ESI-MS, or glycan linkage analysis by GC-MS. The SCF procedure involves neutralization of NaOH beads by acidified phosphate buffer, which eliminates the risk of glycan oxidative degradation and avoids the use of spin columns. Optimization of the new permethylation procedure provided high permethylation efficiency for both hexose (>98%) and HexNAc (>99%) residues—yields which were comparable to (or better than) those of some widely-used spin column-based procedures. A light vs. heavy labelling approach was employed to compare intact glycan yields from a popular spin-column based approach to the SCF approach. Recovery of intact N-glycans was significantly better with the SCF procedure (p < 0.05), but overall yield of O-glycans was similar or slightly diminished (p < 0.05 for tetrasaccharides or smaller). When the SCF procedure was employed upstream to hydrolysis, reduction and acetylation for glycan linkage analysis of pooled glycans from unfractionated blood plasma, analytical reproducibility was on par with that from previous spin column-based “glycan node” analysis results. When applied to blood plasma samples from stage III–IV breast cancer patients (n = 20) and age-matched controls (n = 20), the SCF procedure facilitated identification of three glycan nodes with significantly different distributions between the cases and controls (ROC c-statistics > 0.75; p

  6. Experimental investigation on temperature distribution of foamed concrete filled steel tube column under standard fire

    NASA Astrophysics Data System (ADS)

    Kado, B.; Mohammad, S.; Lee, Y. H.; Shek, P. N.; Kadir, M. A. A.

    2018-04-01

    Standard fire test was carried out on 3 hollow steel tube and 6 foamed concrete filled steel tube columns. Temperature distribution on the columns was investigated. 1500 kg/m3 and 1800 kg/m3 foamed concrete density at 15%, 20% and 25% load level are the parameters considered. The columns investigated were 2400 mm long, 139.7 mm outer diameter and 6 mm steel tube thickness. The result shows that foamed concrete filled steel tube columns has the highest fire resistance of 43 minutes at 15% load level and low critical temperature of 671 ºC at 25% load level using 1500 kg/m3 foamed concrete density. Fire resistance of foamed concrete filled column increases with lower foamed concrete strength. Foamed concrete can be used to provide more fire resistance to hollow steel column or to replace normal weight concrete in concrete filled columns. Since filling hollow steel with foamed concrete produce column with high fire resistance than unfilled hollow steel column. Therefore normal weight concrete can be substituted with foamed concrete in concrete filled column, it will reduces the self-weight of the structure because of its light weight at the same time providing the desired fire resistance.

  7. Analytical condition inspection and extension of time between overhaul of F3-30 engine

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Nakao, M.; Ikeyama, M.; Abe, S.

    1992-04-01

    F3-30 is the low-bypass-ratio turbofan engine developed to power the T-4 intermediate trainer for the Japan Air Self Defense Force (JASDF). The actual field service was started in Sept., 1988. This paper reports on the program to extend time between overhaul (TBO) of the F3-30 which has been running. Analytical condition inspection (ACI) and accelerated mission testing (AMT) were conducted to confirm sufficient durability to extend TBO. Most deteriorations of parts and performance due to AMT were also found by ACI after field operation with approximately the same deterioration rate. On the other hand, some deteriorations were found by ACImore » only. These results show that ACI after field operation is also necessary to confirm the TBO extension, although AMT simulates the deterioration in field operations very well. The deteriorations that would be caused by the field operation during one extended-TBO were estimated with the results of ACI and AMT, and it was concluded that the F3-30 has sufficient durability for TBO extension to the next step.« less

  8. Self-regenerating column chromatography

    DOEpatents

    Park, Woo K.

    1995-05-30

    The present invention provides a process for treating both cations and anions by using a self-regenerating, multi-ionic exchange resin column system which requires no separate regeneration steps. The process involves alternating ion-exchange chromatography for cations and anions in a multi-ionic exchange column packed with a mixture of cation and anion exchange resins. The multi-ionic mixed-charge resin column works as a multi-function column, capable of independently processing either cationic or anionic exchange, or simultaneously processing both cationic and anionic exchanges. The major advantage offered by the alternating multi-function ion exchange process is the self-regeneration of the resins.

  9. Towards Reconstructing a Doric Column in a Virtual Construction Site

    NASA Astrophysics Data System (ADS)

    Bartzis, D.

    2017-02-01

    This paper deals with the 3D reconstruction of ancient Greek architectural members, especially with the element of the Doric column. The case study for this project is the Choragic monument of Nicias on the South Slope of the Athenian Acropolis, from which a column drum, two capitals and smaller fragments are preserved. The first goal of this paper is to present some benefits of using 3D reconstruction methods not only in documentation but also in understanding of ancient Greek architectural members. The second goal is to take advantage of the produced point clouds. By using the Cloud Compare software, comparisons are made between the actual architectural members and an "ideal" point cloud of the whole column in its original form. Seeking for probable overlaps between the two point clouds could assist in estimating the original position of each member/fragment on the column. This method is expanded with more comparisons between the reference column model and other members/fragments around the Acropolis, which may have not yet been ascribed to the monument of Nicias.

  10. Analysis of essential oils and fragrances with a new generation of highly inert gas chromatographic columns coated with ionic liquids.

    PubMed

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

    2017-04-28

    In the fields of essential oils and fragrances, samples often consist of mixtures of compounds with similar structural and physical characteristics (e.g. mono- and sesquiterpenoids), whose correct identification closely depends on the synergic combination of chromatographic and mass spectral data. This sample complexity means that new GC stationary phases with different selectivities are continually being investigated. Ionic liquids (ILs) are of great interest as GC stationary phases in this field because of their selectivity (significantly different than that of currently phases) and their high temperature stability. A first generation of IL GC columns was found to be competitive when applied to these field, in terms of selectivity and efficiency, compared to conventional columns (polydimethylsiloxane, (e.g. OV-1), methyl-polysiloxane 5%-phenyl (e.g. SE-52), 7%-cyanopropyl, 7%-phenyl polysiloxane (e.g. OV-1701), and polyethylen glycol (e.g. PEG-20M). However, these columns showed significant activity towards polar or active analytes, which primarily affected their quantitative performance. A new generation of highly-inactive columns coated with three of the most widely-used ionic liquid GC stationary phases has recently been introduced; these phases are SLB-IL60i (1,12-di(tripropylphosphonium) dodecane bis(trifluoromethylsulfonyl) imide [NTf 2 ], SLB-IL76i (tri-(tripropylphosphonium-hexanamido)-triethylamine [NTf 2 ]), and SLB-IL111i (1,5-di (2,3-dimethyllimidazolium) pentane [NTf 2 ]). This study carefully tested the new inert IL columns, in view of their routine application in the fragrance and essential oil fields. They were found to have unusually high selectivity, comparable to that of first-generation IL columns, while their inertness and efficiency were competitive with those of currently-used conventional columns. The IL column performance of first and second generations was compared, through the quali-quantitative analysis of components in a group of

  11. Analytical sensitivity and specificity of a loop-mediated isothermal amplification (LAMP) kit prototype for detection of Trypanosoma cruzi DNA in human blood samples

    PubMed Central

    Besuschio, Susana A.; Llano Murcia, Mónica; Benatar, Alejandro F.; Monnerat, Severine; Cruz, Israel; Picado, Albert; Curto, María de los Ángeles; Kubota, Yutaka; Wehrendt, Diana P.; Pavia, Paula; Mori, Yasuyoshi; Puerta, Concepción; Ndung'u, Joseph M.

    2017-01-01

    This study aimed to assess analytical parameters of a prototype LAMP kit that was designed for detection of Trypanosoma cruzi DNA in human blood. The prototype is based on the amplification of the highly repetitive satellite sequence of T.cruzi in microtubes containing dried reagents on the inside of the caps. The reaction is carried out at 65°C during 40 minutes. Calcein allows direct detection of amplified products with the naked eye. Inclusivity and selectivity were tested in purified DNA from Trypanosoma cruzi stocks belonging to the six discrete typing units (DTUs), in DNA from other protozoan parasites and in human DNA. Analytical sensitivity was estimated in serial dilutions of DNA samples from Sylvio X10 (Tc I) and CL Brener (Tc VI) stocks, as well as from EDTA-treated or heparinized blood samples spiked with known amounts of cultured epimastigotes (CL Brener). LAMP sensitivity was compared after DNA extraction using commercial fiberglass columns or after “Boil & Spin” rapid preparation. Moreover, the same DNA and EDTA-blood spiked samples were subjected to standardized qPCR based on the satellite DNA sequence for comparative purposes. A panel of peripheral blood specimens belonging to Chagas disease patients, including acute, congenital, chronic and reactivated cases (N = 23), as well as seronegative controls (N = 10) were evaluated by LAMP in comparison to qPCR. LAMP was able to amplify DNAs from T. cruzi stocks representative of the six DTUs, whereas it did not amplify DNAs from Leishmania sp, T. brucei sp, T. rangeli KPN+ and KPN-, P. falciparum and non-infected human DNA. Analytical sensitivity was 1x10-2 fg/μL of both CL Brener and Sylvio X10 DNAs, whereas qPCR detected up to 1x 10−1 fg/μL of CL Brener DNA and 1 fg/μl of Sylvio X10 DNA. LAMP detected 1x10-2 parasite equivalents/mL in spiked EDTA blood and 1x10-1 par.eq/mL in spiked heparinized blood using fiberglass columns for DNA extraction, whereas qPCR detected 1x10-2 par.eq./mL in EDTA

  12. Column Number Density Expressions Through M = 0 and M = 1 Point Source Plumes Along Any Straight Path

    NASA Technical Reports Server (NTRS)

    Woronowicz, Michael

    2016-01-01

    Analytical expressions for column number density (CND) are developed for optical line of sight paths through a variety of steady free molecule point source models including directionally-constrained effusion (Mach number M = 0) and flow from a sonic orifice (M = 1). Sonic orifice solutions are approximate, developed using a fair simulacrum fitted to the free molecule solution. Expressions are also developed for a spherically-symmetric thermal expansion (M = 0). CND solutions are found for the most general paths relative to these sources and briefly explored. It is determined that the maximum CND from a distant location through directed effusion and sonic orifice cases occurs along the path parallel to the source plane that intersects the plume axis. For the effusive case this value is exactly twice the CND found along the ray originating from that point of intersection and extending to infinity along the plume's axis. For sonic plumes this ratio is reduced to about 4/3. For high Mach number cases the maximum CND will be found along the axial centerline path. Keywords: column number density, plume flows, outgassing, free molecule flow.

  13. Analytical Chemistry: A Literary Approach

    NASA Astrophysics Data System (ADS)

    Lucy, Charles A.

    2000-04-01

    The benefits of incorporating real-world examples of chemistry into lectures and lessons is reflected by the recent inclusion of the Teaching with Problems and Case Studies column in this Journal. However, these examples lie outside the experience of many students, and so much of the impact of "real-world" examples is lost. This paper provides an anthology of references to analytical chemistry techniques from history, popular fiction, and film. Such references are amusing to both instructor and student. Further, the fictional descriptions can serve as a focal point for discussions of a technique's true capabilities and limitations.

  14. Simultaneous multi-mycotoxin determination in nutmeg by ultrasound-assisted solid-liquid extraction and immunoaffinity column clean-up coupled with liquid chromatography and on-line post-column photochemical derivatization-fluorescence detection.

    PubMed

    Kong, Wei-Jun; Liu, Shu-Yu; Qiu, Feng; Xiao, Xiao-He; Yang, Mei-Hua

    2013-05-07

    A simple and sensitive analytical method based on ultrasound-assisted solid-liquid extraction and immunoaffinity column clean-up coupled with high performance liquid chromatography and on-line post-column photochemical derivatization-fluorescence detection (USLE-IAC-HPLC-PCD-FLD) has been developed for simultaneous multi-mycotoxin determination of aflatoxins B1, B2, G1, G2 (AFB1, AFB2, AFG1, AFG2) and ochratoxin A (OTA) in 13 edible and medicinal nutmeg samples marketed in China. AFs and OTA were extracted from nutmeg samples by ultrasonication using a methanol : water (80 : 20, v/v) solution, followed by an IAC clean-up step. Different USL extraction conditions, pre-processing ways for nutmeg sample and clean-up columns for mycotoxins, as well as HPLC-PCD-FLD parameters (mobile phase, column temperature, elution procedure, excitation and emission wavelengths) were optimized. This method, which was appraised for analyzing nutmeg samples, showed satisfactory results with reference to limits of detection (LODs) (from 0.02 to 0.25 μg kg(-1)), limits of quantification (LOQs) (from 0.06 to 0.8 μg kg(-1)), linear ranges (up to 30 ng mL(-1) for AFB1, AFG1 and OTA and 9 ng mL(-1) for AFB2 and AFG2), intra- and inter-day variability (all <2%) and average recoveries (from 79.6 to 90.8% for AFs and from 93.6 to 97.3% for OTA, respectively). The results of the application of developed method in nutmeg samples have elucidated that four samples were detected with contamination of AFs and one with OTA. AFB1 was the most frequently found mycotoxin in 30.8% of nutmeg samples at contamination levels of 0.73-16.31 μg kg(-1). At least two different mycotoxins were co-occurred in three samples, and three AFs were simultaneously detected in one sample.

  15. Spatial and Temporal Variability of Ground and Satellite Column Measurements of NO2 and O3 over the Atlantic Ocean During the Deposition of Atmospheric Nitrogen to Coastal Ecosystems Experiment

    NASA Technical Reports Server (NTRS)

    Martins, Douglas K.; Najjar, Raymond G.; Tzortziou, Maria; Abuhassan, Nader; Thompson, Anne M.; Kollonige, Debra E.

    2016-01-01

    In situ measurements of O3 and nitrogen oxides (NO + NO2=NOx) and remote sensing measurements of total column NO2 and O3 were collected on a ship in the North Atlantic Ocean as part of the Deposition of Atmospheric Nitrogen to Coastal Ecosystems (DANCE) campaign in July August 2014,100 km east of the mid-Atlantic United States. Relatively clean conditions for both surface in situ mixing ratio and total column O3 and NO2 measurements were observed throughout the campaign. Increased surface and column NO2 and O3 amounts were observed when a terrestrial air mass was advected over the study region. Relative to ship-based total column measurements using a Pandora over the entire study, satellite measurements overestimated total column NO2 under these relatively clean atmospheric conditions over offshore waters by an average of 16. Differences are most likely due to proximity, or lack thereof, to surface emissions; spatial averaging due to the field of view of the satellite instrument; and the lack of sensitivity of satellite measurements to the surface concentrations of pollutants. Total column O3 measurements from the shipboard Pandora showed good correlation with the satellite measurements(r 0.96), but satellite measurements were 3 systematically higher than the ship measurements, in agreement with previous studies. Derived values of boundary layer height using the surface in situ and total column measurements of NO2 are much lower than modeled and satellite-retrieved boundary layer heights, which highlight the differences in the vertical distribution between terrestrial and marine environments.

  16. Myelin water and T(2) relaxation measurements in the healthy cervical spinal cord at 3.0T: repeatability and changes with age.

    PubMed

    MacMillan, Erin L; Mädler, Burkhard; Fichtner, Nicole; Dvorak, Marcel F; Li, David K B; Curt, Armin; MacKay, Alex L

    2011-01-15

    Multiecho T(2) relaxation measurements offer specific information about myelin content through the myelin water fraction (MWF), as well as about the water environments through the intra- and extra-cellular (IE), and global, geometric mean T(2) (GMT(2)) times. While these measurements have yielded new insights into brain development and pathologies, they have yet to be thoroughly investigated in the spinal cord. The goals of this study were: (1) to apply a new 3D multiecho T(2) relaxation measurement in the cervical spine with sufficient axial resolution to distinguish grey and white matter; (2) to perform a pilot reliability assessment of the resulting MWF and GMT(2) measures in a target population; and (3) to detect differences in these measures between a younger cohort (20-30 years of age) and an older cohort (50-75 years of age) of healthy adults. The results demonstrated that the MWF in younger healthy adults follows the known pattern of lower myelin content in grey matter (mean (95% confidence interval)) (0.049 (0.030-0.067)) as compared to white matter (0.296 (0.275-0.317), p<0.001). The reliability coefficients were 0.65 and 0.82 for the MWF in the dorsal (DC) and lateral column (LC) white matter, respectively; 0.79 and 0.52 for the IE GMT(2); and 0.74 and 0.73 for the global GMT(2). Significantly lower MWF were found in the older adults than in the younger adults (DC p=0.014; LC p=0.012), as well as lower IE GMT(2) times (DC p=0.008; LC p=0.042), however, the global GMT(2) times did not show any differences. These changes in MWF and IE GMT(2) times, but not in global GMT(2) times, indicate that multiecho T(2) relaxation measures are sensitive to changes in myelin integrity and cell morphology that may not be apparent on conventional T(2) weighted images. Copyright © 2010 Elsevier Inc. All rights reserved.

  17. Capillary ion chromatography with on-column focusing for ultra-trace analysis of methanesulfonate and inorganic anions in limited volume Antarctic ice core samples.

    PubMed

    Rodriguez, Estrella Sanz; Poynter, Sam; Curran, Mark; Haddad, Paul R; Shellie, Robert A; Nesterenko, Pavel N; Paull, Brett

    2015-08-28

    Preservation of ionic species within Antarctic ice yields a unique proxy record of the Earth's climate history. Studies have been focused until now on two proxies: the ionic components of sea salt aerosol and methanesulfonic acid. Measurement of the all of the major ionic species in ice core samples is typically carried out by ion chromatography. Former methods, whilst providing suitable detection limits, have been based upon off-column preconcentration techniques, requiring larger sample volumes, with potential for sample contamination and/or carryover. Here, a new capillary ion chromatography based analytical method has been developed for quantitative analysis of limited volume Antarctic ice core samples. The developed analytical protocol applies capillary ion chromatography (with suppressed conductivity detection) and direct on-column sample injection and focusing, thus eliminating the requirement for off-column sample preconcentration. This limits the total sample volume needed to 300μL per analysis, allowing for triplicate sample analysis with <1mL of sample. This new approach provides a reliable and robust analytical method for the simultaneous determination of organic and inorganic anions, including fluoride, methanesulfonate, chloride, sulfate and nitrate anions. Application to composite ice-core samples is demonstrated, with coupling of the capillary ion chromatograph to high resolution mass spectrometry used to confirm the presence and purity of the observed methanesulfonate peak. Copyright © 2015 Elsevier B.V. All rights reserved.

  18. Quantitative analysis of the immunosuppressant CP-690,550 in whole blood by column-switching high-performance liquid chromatography and mass spectrometry detection.

    PubMed

    Paniagua, Ricardo; Campbell, Andrew; Changelian, Paul S; Reitz, Bruce A; Prakash, Chandra; Borie, Dominic C

    2005-10-01

    A fast and accurate method to quantify the new immunosuppressive JAK3 inhibitor CP-690,550 in whole blood using a dual-pump liquid chromatography-liquid chromatography-mass spectrometry (LC/LC-MS) system was developed and validated in nonhuman primate blood. Before injection, blood samples were prepared by precipitation with a reagent that included methanol and acetonitrile (30:70, vol/vol) along with the internal standard (CP-istd). Column-switching LC/LC-MS analysis used online extraction followed by separation on a C8 analytic column and MS detection of the [M + H] CP-690,550 (m/z = 313.1) and CP internal standard (m/z = 288.1). Linearity was always better than r = 0.99 (n = 7) for CP-690,550 (range 2.5-750 ng/mL), with a lower limit of quantification (LLOQ) of 2.5 ng/mL. The intrarun accuracy and precision ranged from 103.0% to 105.4% and 2.7% to 4.3%, respectively (n = 5), and the interday precision ranged from 8.7% to 11.1%, and the interday accuracy ranged from 98.1% to 103.8% of nominal values (n = 14). The injection repeatability for the method was 1.3% (n = 7). Except for the LLOQ, the intraday accuracy and precision in human blood were also within 15% (n = 5). The combination of simple sample preparation and short analytic run time of this sensitive procedure makes it effective for monitoring the concentration of CP-690,550 in whole blood in organ-transplant recipients.

  19. A T3 and T7 Recombinant Phage Acquires Efficient Adsorption and a Broader Host Range

    PubMed Central

    Lin, Tiao-Yin; Lo, Yi-Haw; Tseng, Pin-Wei; Chang, Shun-Fu; Lin, Yann-Tsyr; Chen, Ton-Seng

    2012-01-01

    It is usually thought that bacteriophage T7 is female specific, while phage T3 can propagate on male and female Escherichia coli. We found that the growth patterns of phages T7M and T3 do not match the above characteristics, instead showing strain dependent male exclusion. Furthermore, a T3/7 hybrid phage exhibits a broader host range relative to that of T3, T7, as well as T7M, and is able to overcome the male exclusion. The T7M sequence closely resembles that of T3. T3/7 is essentially T3 based, but a DNA fragment containing part of the tail fiber gene 17 is replaced by the T7 sequence. T3 displays inferior adsorption to strains tested herein compared to T7. The T3 and T7 recombinant phage carries altered tail fibers and acquires better adsorption efficiency than T3. How phages T3 and T7 recombine was previously unclear. This study is the first to show that recombination can occur accurately within only 8 base-pair homology, where four-way junction structures are identified. Genomic recombination models based on endonuclease I cleavages at equivalent and nonequivalent sites followed by strand annealing are proposed. Retention of pseudo-palindromes can increase recombination frequency for reviving under stress. PMID:22347414

  20. A T3 and T7 recombinant phage acquires efficient adsorption and a broader host range.

    PubMed

    Lin, Tiao-Yin; Lo, Yi-Haw; Tseng, Pin-Wei; Chang, Shun-Fu; Lin, Yann-Tsyr; Chen, Ton-Seng

    2012-01-01

    It is usually thought that bacteriophage T7 is female specific, while phage T3 can propagate on male and female Escherichia coli. We found that the growth patterns of phages T7M and T3 do not match the above characteristics, instead showing strain dependent male exclusion. Furthermore, a T3/7 hybrid phage exhibits a broader host range relative to that of T3, T7, as well as T7M, and is able to overcome the male exclusion. The T7M sequence closely resembles that of T3. T3/7 is essentially T3 based, but a DNA fragment containing part of the tail fiber gene 17 is replaced by the T7 sequence. T3 displays inferior adsorption to strains tested herein compared to T7. The T3 and T7 recombinant phage carries altered tail fibers and acquires better adsorption efficiency than T3. How phages T3 and T7 recombine was previously unclear. This study is the first to show that recombination can occur accurately within only 8 base-pair homology, where four-way junction structures are identified. Genomic recombination models based on endonuclease I cleavages at equivalent and nonequivalent sites followed by strand annealing are proposed. Retention of pseudo-palindromes can increase recombination frequency for reviving under stress.

  1. Anomalous electrical signals associated with microbial activity: Results from Iron and Nitrate-Reducing Columns

    NASA Astrophysics Data System (ADS)

    Aaron, R. B.; Zheng, Q.; Flynn, P.; Singha, K.; Brantley, S.

    2008-12-01

    Three flow-through columns outfitted with Ag/AgCl electrodes were constructed to test the effects of different microbial processes on the geophysical measurements of self potential (SP), bulk electrical conductivity (σ b), and induced polarization (IP). The columns were filled with sieved, Fe-bearing subsurface sediment from the Delmarva Peninsula near Oyster, VA, inoculated (9:1 ratio) with a freshly-collected, shallow subsurface sediment from a wetland floodplain (Dorn Creek) near Madison, WI. Each of the columns was fed anoxic and sterile PIPES buffered artificial groundwater (PBAGW) containing different concentrations of acetate and nitrate. The medium fed to Column 1 (nitrate-reducing) was amended with 100 μM acetate and 2 mM nitrate. Column 2 (iron-reducing) was run with PBAGW containing 1.0 mM acetate and 0 mM nitrate. Column 3 (alternating redox state) was operated under conditions designed to alternately stimulate nitrate-reducing and iron-reducing populations to provide conditions, i.e., the presence of both nitrate and microbially-produced Fe(II), that would allow growth of nitrate-dependent Fe(II)-oxidizing populations. We operated Column 3 with a cycling strategy of 14-18 days of high C medium (1 mM acetate and 100 μ M nitrate) followed by 14-18 days of low C medium (100 μ M acetate and 2 mM nitrate). Effluent chemistry (NO3-, NO2-, NH4+, acetate, and Fe2+) was sampled daily for four months so as to be concurrent with the electrical measurements. We observed chemical evidence of iron reduction (dissolved [Fe(II)] = 0.2mM) in the effluent from the iron reduction and alternating redox columns. Chemical depletion of NO3- ([NO3-] ranged from 1 to 0.02mM), the production of NO2-, and possible production of NH4+ (0.2 mM) was observed in the nitrate reducing column as well as the alternating redox column. All three columns displayed loss of acetate as microbial activity progressed. σ b remained constant in the alternating redox column (~0.15 S

  2. Analytical method development for directed enzyme evolution research: a high throughput high-performance liquid chromatography method for analysis of ribose and ribitol and a capillary electrophoresis method for the separation of ribose enantiomers.

    PubMed

    Sun, Baoguo; Miller, Gregory; Lee, Wan Yee; Ho, Kelvin; Crowe, Michael A; Partridge, Leslie

    2013-01-04

    Analytical methods were developed for a directed enzyme evolution research programme, which pursued high performance enzymes to produce high quality L-ribose using large scale biocatalytic reaction. A high throughput HPLC method with evaporative light-scattering detection was developed to test ribose and ribitol in the enzymatic reaction, a β-cyclobond 2000 analytical column separated ribose and ribitol in 2.3 min, a C(18) guard column was used as an on-line filter to clean up the enzyme sample matrix and a short gradient was applied to wash the column, the enzymatic reaction solution can be directly injected after quenching. Total run time of each sample was approx. 4 min which provided capability of screening 4×96-well plates/day/instrument. Meanwhile, a capillary electrophoresis method was developed for the separation of ribose enantiomers, while 7-aminonaphthalene-1,3-disulfonic acid was used as derivatisation reagent and 25 mM tetraborate with 5 mM β-cyclodextrin was used as electrolyte. 0.35%of D-ribose in L-ribose can be detected which can be translated into 99.3% ee of L-ribose. Derivatisation reagent and sample matrix did not interfere with the measurement. Copyright © 2012 Elsevier B.V. All rights reserved.

  3. An improved 3D MoF method based on analytical partial derivatives

    NASA Astrophysics Data System (ADS)

    Chen, Xiang; Zhang, Xiong

    2016-12-01

    MoF (Moment of Fluid) method is one of the most accurate approaches among various surface reconstruction algorithms. As other second order methods, MoF method needs to solve an implicit optimization problem to obtain the optimal approximate surface. Therefore, the partial derivatives of the objective function have to be involved during the iteration for efficiency and accuracy. However, to the best of our knowledge, the derivatives are currently estimated numerically by finite difference approximation because it is very difficult to obtain the analytical derivatives of the object function for an implicit optimization problem. Employing numerical derivatives in an iteration not only increase the computational cost, but also deteriorate the convergence rate and robustness of the iteration due to their numerical error. In this paper, the analytical first order partial derivatives of the objective function are deduced for 3D problems. The analytical derivatives can be calculated accurately, so they are incorporated into the MoF method to improve its accuracy, efficiency and robustness. Numerical studies show that by using the analytical derivatives the iterations are converged in all mixed cells with the efficiency improvement of 3 to 4 times.

  4. A hybrid fluorous monolithic capillary column with integrated nanoelectrospray ionization emitter for determination of perfluoroalkyl acids by nano-liquid chromatography-nanoelectrospray ionization-mass spectrometry/mass spectrometry.

    PubMed

    Zhang, Haiyang; Ou, Junjie; Wei, Yinmao; Wang, Hongwei; Liu, Zhongshan; Zou, Hanfa

    2016-04-01

    A hybrid fluorous monolithic column was simply prepared via photo-initiated free radical polymerization of an acrylopropyl polyhedral oligomeric silsesquioxane (acryl-POSS) and a perfluorous monomer (2,2,3,3,4,4,5,5,6,6,7,7-dodecafluoroheptyl acrylate) in UV-transparent fused-silica capillaries within 5min. The physical characterization of hybrid fluorous monolith, including scanning electron microscopy (SEM), Fourier transform infrared (FT-IR) spectroscopy, mercury intrusion porosimetry (MIP) and nitrogen adsorption/desorption measurement was performed. Chromatographic performance was also evaluated by capillary liquid chromatography (cLC). Due to the fluorous-fluorous interaction between fluorous monolith and analytes, fluorobenzenes could well be separated, and the column efficiencies reached 86,600-92,500plates/m at the velocity of 0.87mm/s for alkylbenzenes and 51,900-76,000plates/m at the velocity of 1.10mm/s for fluorobenzenes. Meanwhile, an approach to integrate nanoelectrospray ionization (ESI) emitter with hybrid fluorous monolithic column was developed for quantitative determination of perfluoroalkyl acids by nanoHPLC-ESI-MS/MS. The integration design could minimize extracolumn volume, thus excluding undesirable peak broadening and improving separation performance. Copyright © 2016 Elsevier B.V. All rights reserved.

  5. Seismic performance of recycled concrete-filled square steel tube columns

    NASA Astrophysics Data System (ADS)

    Chen, Zongping; Jing, Chenggui; Xu, Jinjun; Zhang, Xianggang

    2017-01-01

    An experimental study on the seismic performance of recycled concrete-filled square steel tube (RCFST) columns is carried out. Six specimens were designed and tested under constant axial compression and cyclic lateral loading. Two parameters, replacement percentage of recycled coarse aggregate (RCA) and axial compression level, were considered in the test. Based on the experimental data, the hysteretic loops, skeleton curves, ductility, energy dissipation capacity and stiffness degradation of RCFST columns were analyzed. The test results indicate that the failure modes of RCFST columns are the local buckling of the steel tube at the bottom of the columns, and the hysteretic loops are full and their shapes are similar to normal CFST columns. Furthermore, the ductility coefficient of all specimens are close to 3.0, and the equivalent viscous damping coefficient corresponding to the ultimate lateral load ranges from 0.323 to 0.360, which demonstrates that RCFST columns exhibit remarkable seismic performance.

  6. Phenolic composition of pomegranate peel extracts using an liquid chromatography-mass spectrometry approach with silica hydride columns.

    PubMed

    Young, Joshua E; Pan, Zhongli; Teh, Hui Ean; Menon, Veena; Modereger, Brent; Pesek, Joseph J; Matyska, Maria T; Dao, Lan; Takeoka, Gary

    2017-04-01

    The peels of different pomegranate cultivars (Molla Nepes, Parfianka, Purple Heart, Wonderful and Vkunsyi) were compared in terms of phenolic composition and total phenolics. Analyses were performed on two silica hydride based stationary phases: phenyl and undecanoic acid columns. Quantitation was accomplished by developing a liquid chromatography with mass spectrometry approach for separating different phenolic analytes, initially in the form of reference standards and then with pomegranate extracts. The high-performance liquid chromatography columns used in the separations had the ability to retain a wide polarity range of phenolic analytes, as well as offering beneficial secondary selectivity mechanisms for resolving the isobaric compounds, catechin and epicatechin. The Vkunsyi peel extract had the highest concentration of phenolics (as determined by liquid chromatography with mass spectrometry) and was the only cultivar to contain the important compound punicalagin. The liquid chromatography with mass spectrometry data were compared to the standard total phenolics content as determined by using the Folin-Ciocalteu assay. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Microfabricated packed gas chromatographic column

    DOEpatents

    Kottenstette, Richard; Matzke, Carolyn M.; Frye-Mason, Gregory C.

    2003-12-16

    A new class of miniaturized gas chromatographic columns has been invented. These chromatographic columns are formed using conventional micromachining techniques, and allow packed columns having lengths on the order of a meter to be fabricated with a footprint on the order of a square centimeter.

  8. Analytical method for the accurate determination of tricothecenes in grains using LC-MS/MS: a comparison between MRM transition and MS3 quantitation.

    PubMed

    Lim, Chee Wei; Tai, Siew Hoon; Lee, Lin Min; Chan, Sheot Harn

    2012-07-01

    The current food crisis demands unambiguous determination of mycotoxin contamination in staple foods to achieve safer food for consumption. This paper describes the first accurate LC-MS/MS method developed to analyze tricothecenes in grains by applying multiple reaction monitoring (MRM) transition and MS(3) quantitation strategies in tandem. The tricothecenes are nivalenol, deoxynivalenol, deoxynivalenol-3-glucoside, fusarenon X, 3-acetyl-deoxynivalenol, 15-acetyldeoxynivalenol, diacetoxyscirpenol, and HT-2 and T-2 toxins. Acetic acid and ammonium acetate were used to convert the analytes into their respective acetate adducts and ammonium adducts under negative and positive MS polarity conditions, respectively. The mycotoxins were separated by reversed-phase LC in a 13.5-min run, ionized using electrospray ionization, and detected by tandem mass spectrometry. Analyte-specific mass-to-charge (m/z) ratios were used to perform quantitation under MRM transition and MS(3) (linear ion trap) modes. Three experiments were made for each quantitation mode and matrix in batches over 6 days for recovery studies. The matrix effect was investigated at concentration levels of 20, 40, 80, 120, 160, and 200 μg kg(-1) (n = 3) in 5 g corn flour and rice flour. Extraction with acetonitrile provided a good overall recovery range of 90-108% (n = 3) at three levels of spiking concentration of 40, 80, and 120 μg kg(-1). A quantitation limit of 2-6 μg kg(-1) was achieved by applying an MRM transition quantitation strategy. Under MS(3) mode, a quantitation limit of 4-10 μg kg(-1) was achieved. Relative standard deviations of 2-10% and 2-11% were reported for MRM transition and MS(3) quantitation, respectively. The successful utilization of MS(3) enabled accurate analyte fragmentation pattern matching and its quantitation, leading to the development of analytical methods in fields that demand both analyte specificity and fragmentation fingerprint-matching capabilities that are

  9. Βiocolloid and colloid transport through water-saturated columns packed with glass beads: Effect of gravity

    NASA Astrophysics Data System (ADS)

    Chrysikopoulos, C. V.; Syngouna, V. I.

    2013-12-01

    The role of gravitational force on biocolloid and colloid transport in water-saturated columns packed with glass beads was investigated. Transport experiments were performed with biocolloids (bacteriophages: ΦΧ174, MS2) and colloids (clays: kaolinite KGa-1b, montmorillonite STx-1b). The packed columns were placed in various orientations (horizontal, vertical, and diagonal) and a steady flow rate of Q=1.5 mL/min was applied in both up-flow and down-flow modes. All experiments were conducted under electrostatically unfavorable conditions. The experimental data were fitted with a newly developed, analytical, one dimensional, colloid transport model, accounting for gravity effects. The results revealed that flow direction has a significant influence on particle deposition. The rate of particle deposition was shown to be greater for up-flow than for down-flow direction, suggesting that gravity was a significant driving force for biocolloid and colloid deposition. Schematic illustration of a packed column with up-flow velocity having orientation (-i) with respect to gravity. The gravity vector components are: g(i)= g(-z) sinβ i, and g(-j)= -g(-z) cosβ j. Experimental setup showing the various column arrangements: (a) horizontal, (b) diagonal, and (c) vertical.

  10. [Three-dimensional Finite Element Analysis to T-shaped Fracture of Pelvis in Sitting Position].

    PubMed

    Fan, Yanping; Lei, Jianyin; Liu, Haibo; Li, Zhiqiang; Cai, Xianhua; Chen, Weiyi

    2015-10-01

    We developed a three-dimensional finite element model of the pelvis. According to Letournel methods, we established a pelvis model of T-shaped fracture with its three different fixation systems, i. e. double column reconstruction plates, anterior column plate combined with posterior column screws and anterior column plate combined with quadrilateral area screws. It was found that the pelvic model was effective and could be used to simulate the mechanical behavior of the pelvis. Three fixation systems had great therapeutic effect on the T-shaped fracture. All fixation systems could increase the stiffness of the model, decrease the stress concentration level and decrease the displacement difference along the fracture line. The quadrilateral area screws, which were drilled into cortical bone, could generate beneficial effect on the T-type fracture. Therefore, the third fixation system mentioned above (i. e. the anterior column plate combined with quadrilateral area screws) has the best biomechanical stability to the T-type fracture.

  11. T.Rex

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    2016-06-08

    T.Rex is used to explore tabular data sets containing up to ten million records to help rapidly understand a previously unknown data set. Analysis can quickly identify patterns of interest and the records and fields that capture those patterns. T.Rex contains a growing set of deep analytical tools and supports robust export capabilities that selected data can be incorporated into to other specialized tools for further analysis. T.Rex is flexible in ingesting different types and formats of data, allowing the user to interactively experiment and perform trial and error guesses on the structure of the data; and also has amore » variety of linked visual analytic tools that enable exploration of the data to find relevant content, relationships among content, trends within the content, and capture knowledge about the content. Finally, T.Rex has a rich export capability, to extract relevant subsets of a larger data source, to further analyze their data in other analytic tools.« less

  12. Inflatable Column Structure

    NASA Technical Reports Server (NTRS)

    Hedgepeth, J. M.

    1985-01-01

    Lightweight structural member easy to store. Billowing between circumferential loops of fiber inflated column becomes series of cells. Each fiber subjected to same tension along entire length (though tension is different in different fibers). Member is called "isotensoid" column. Serves as jack for automobiles or structures during repairs. Also used as support for temporary bleachers or swimming pools.

  13. Characterization of hyaluronate binding proteins isolated from 3T3 and murine sarcoma virus transformed 3T3 cells

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Turley, E.A.; Moore, D.; Hayden, L.J.

    1987-06-02

    A hyaluronic acid binding fraction was purified from the supernatant media of both 3T3 and murine sarcoma virus (MSV) transformed 3T3 cultures by hyaluronate and immunoaffinity chromatography. Sodium dodecyl sulfate-polyacrylamide gel electrophoresis resolved the hyaluronate affinity-purified fraction into three major protein bands of estimated molecular weight (M/sub r,e/) 70K, 66K, and 56K which contained hyaluronate binding activity and which were termed hyaluronate binding proteins (HABP). Hyaluronate affinity chromatography combined with immunoaffinity chromatography, using antibody directed against the larger HABP, allowed a 20-fold purification of HABP. Fractions isolated from 3T3 supernatant medium also contained additional binding molecules in the molecular weightmore » range of 20K. This material was present in vanishingly small amounts and was not detected with a silver stain or with (/sup 35/S)methionine label. The three protein species isolated by hyaluronate affinity chromatography (M/sub r,e/ 70K, 66K, and 56K) were related to one another since they shared antigenic determinants and exhibited similar pI values. In isocratic conditions, HABP occurred as aggregates of up to 580 kilodaltons. Their glycoprotein nature was indicated by their incorporation of /sup 3/H-sugars. Enzyme-linked immunoadsorbent assay showed they were antigenically distinct from other hyaluronate binding proteins such as fibronectin, cartilage link protein, and the hyaluronate binding region of chondroitin sulfate proteoglycan. The results are discussed with regard both to the functional significance of hyaluronate-cell surface interactions in transformed as well as normal cells and to the relationship of HABP to other reported hyaluronate binding proteins.« less

  14. A core-shell column approach to a comprehensive high-performance liquid chromatography phenolic analysis of Vitis vinifera L. and interspecific hybrid grape juices, wines, and other matrices following either solid phase extraction or direct injection.

    PubMed

    Manns, David C; Mansfield, Anna Katharine

    2012-08-17

    Four high-throughput reverse-phase chromatographic protocols utilizing two different core-shell column chemistries have been developed to analyze the phenolic profiles of complex matrices, specifically targeting juices and wines produced from interspecific hybrid grape cultivars. Following pre-fractionation via solid-phase extraction or direct injection, individual protocols were designed to resolve, identify and quantify specific chemical classes of compounds including non-anthocyanin monomeric phenolics, condensed tannins following acid hydrolysis, and anthocyanins. Detection levels ranging from 1.2 ppb to 27.5 ppb, analyte %RSDs ranging from 0.04 to 0.38, and linear ranges of quantitation approaching five orders of magnitude were achieved using conventional HPLC instrumentation. Using C(18) column chemistry, the non-anthocyanin monomeric protocol effectively separated a set of 16 relevant phenolic compounds comprised flavan-3-ols, hydroxycinnamic acids, and flavonols in under 14 min. The same column was used to develop a 15-min protocol for hydrolyzed condensed tannin analysis. Two anthocyanin protocols are presented, one utilizing the same C(18) column, best suited for anthocyanidin and monoglucoside analysis, the other utilizing a pentafluorophenyl chemistry optimized to effectively separate complex mixtures of coexisting mono- and diglucoside anthocyanins. These protocols and column chemistries have been used initially to explore a wide variety of complex phenolic matrices, including red and white juices and wines produced from Vitis vinifera and interspecific hybrid grape cultivars, juices, teas, and plant extracts. Each protocol displayed robust matrix responses as written, yet are flexible enough to be easily modified to suit specifically tailored analytical requirements. Copyright © 2012 Elsevier B.V. All rights reserved.

  15. Stress Analysis of Columns and Beam Columns by the Photoelastic Method

    NASA Technical Reports Server (NTRS)

    Ruffner, B F

    1946-01-01

    Principles of similarity and other factors in the design of models for photoelastic testing are discussed. Some approximate theoretical equations, useful in the analysis of results obtained from photoelastic tests are derived. Examples of the use of photoelastic techniques and the analysis of results as applied to uniform and tapered beam columns, circular rings, and statically indeterminate frames, are given. It is concluded that this method is an effective tool for the analysis of structures in which column action is present, particularly in tapered beam columns, and in statically indeterminate structures in which the distribution of loads in the structures is influenced by bending moments due to axial loads in one or more members.

  16. Supramolecular separation mechanism of pentafluorophenyl column using ibuprofen and omeprazole as markers: LC-MS and simulation study.

    PubMed

    Hussain, Afzal; AlAjmi, Mohamed F; Ali, Imran

    2018-06-01

    The pentafluorophenyl (PFP) column is emerging as a new advancement in separation science to analyze a wide range of analytes and, thus, its separation mechanism at supramolecular level is significant. We developed a mechanism for the separation of ibuprofen and omeprazole using different combinations (ranging from 50:50 to 60:40) of water-acetonitrile containing 0.1% formic acid as the mobile phase. The column used was Waters Acquity UPLC HSS PFP (75 × 2.1 mm, 1.8 μm). The reverse order of elution was observed in different combinations of the mobile phases. The docking study indicated hydrogen bonding between ibuprofen and PFP stationary phase (binding energy was -11.30 kJ/mol). Separation at PFP stationary phase is controlled by hydrogen bonding along with π-π interactions. This stationary phase may be used to analyze both aromatic and aliphatic analytes. The developed mechanism will be useful to separate various analytes by considering the possible interactions, leading to saving of energy, time and money. In addition, this work will be highly useful in preparative chromatography where separation is the major problem at a large scale. Moreover, the developed LC-MS-QTOF method may be used to analyze ibuprofen and omeprazole in an unknown sample owing to the low value of detection limits. Copyright © 2018 John Wiley & Sons, Ltd.

  17. 3-D Vector Flow Estimation With Row-Column-Addressed Arrays.

    PubMed

    Holbek, Simon; Christiansen, Thomas Lehrmann; Stuart, Matthias Bo; Beers, Christopher; Thomsen, Erik Vilain; Jensen, Jorgen Arendt

    2016-11-01

    Simulation and experimental results from 3-D vector flow estimations for a 62 + 62 2-D row-column (RC) array with integrated apodization are presented. A method for implementing a 3-D transverse oscillation (TO) velocity estimator on a 3-MHz RC array is developed and validated. First, a parametric simulation study is conducted, where flow direction, ensemble length, number of pulse cycles, steering angles, transmit/receive apodization, and TO apodization profiles and spacing are varied, to find the optimal parameter configuration. The performance of the estimator is evaluated with respect to relative mean bias ~B and mean standard deviation ~σ . Second, the optimal parameter configuration is implemented on the prototype RC probe connected to the experimental ultrasound scanner SARUS. Results from measurements conducted in a flow-rig system containing a constant laminar flow and a straight-vessel phantom with a pulsating flow are presented. Both an M-mode and a steered transmit sequence are applied. The 3-D vector flow is estimated in the flow rig for four representative flow directions. In the setup with 90° beam-to-flow angle, the relative mean bias across the entire velocity profile is (-4.7, -0.9, 0.4)% with a relative standard deviation of (8.7, 5.1, 0.8)% for ( v x , v y , v z ). The estimated peak velocity is 48.5 ± 3 cm/s giving a -3% bias. The out-of-plane velocity component perpendicular to the cross section is used to estimate volumetric flow rates in the flow rig at a 90° beam-to-flow angle. The estimated mean flow rate in this setup is 91.2 ± 3.1 L/h corresponding to a bias of -11.1%. In a pulsating flow setup, flow rate measured during five cycles is 2.3 ± 0.1 mL/stroke giving a negative 9.7% bias. It is concluded that accurate 3-D vector flow estimation can be obtained using a 2-D RC-addressed array.

  18. On-column reduction of catecholamine quinones in stainless steel columns during liquid chromatography.

    PubMed

    Xu, R; Huang, X; Kramer, K J; Hawley, M D

    1995-10-10

    The chromatographic behavior of quinones derived from the oxidation of dopamine and N-acetyldopamine has been studied using liquid chromatography (LC) with both a diode array detector and an electrochemical detector that has parallel dual working electrodes. When stainless steel columns are used, an anodic peak for the oxidation of the catecholamine is observed at the same retention time as a cathodic peak for the reduction of the catecholamine quinone. In addition, the anodic peak exhibits a tail that extends to a second anodic peak for the catecholamine. The latter peak occurs at the normal retention time of the catecholamine. The origin of this phenomenon has been studied and metallic iron in the stainless steel components of the LC system has been found to reduce the quinones to their corresponding catecholamines. The simultaneous appearance of a cathodic peak for the reduction of catecholamine quinone and an anodic peak for the oxidation of the corresponding catecholamine occurs when metallic iron in the exit frit reduces some of the quinones as the latter exits the column. This phenomenon is designated as the "concurrent anodic-cathodic response." It is also observed for quinones of of 3,4-dihydroxybenzoic acid and probably occurs with o- or p-quinones of other dihydroxyphenyl compounds. The use of nonferrous components in LC systems is recommended to eliminate possible on-column reduction of quinones.

  19. Controlled Pd(0)/t Bu3P Catalyzed Suzuki Cross-Coupling Polymerization of AB-Type Monomers with ArPd(t Bu3P)X or Pd2(dba)3/t Bu3P/ArX as the Initiator

    DOE PAGES

    Zhang, Honghai; Xing, Chun-Hui; Hu, Qiao-Sheng; ...

    2015-02-05

    The synthesis of well-defined and functionalized conjugated polymers, which are essential in the development of efficient organic electronics, through Suzuki cross-coupling polymerizations has been a challenging task. We developed controlled Pd(0)/t-Bu3P-catalyzed Suzuki cross-coupling polymerizations of AB-type monomers via the chain-growth mechanism with a series of in situ generated ArPd(t-Bu3P)X (X = I, Br, Cl) complexes as initiators. Among them, the combinations of Pd2(dba)3/t-Bu3P/p-BrC6H4I, Pd2(dba)3/t-Bu3P/p-BrC6H4CH2OH and Pd2(dba)3/t-Bu3P/p-PhCOC6H4Br were identified as highly robust initiator systems, resulting in polymers with predictable molecular weight and narrow polydispersity (PDI~1.13-1.20). In addition, Pd2(dba)3/t-Bu3P/p-BrC6H4CH2OH and Pd2(dba)3/t-Bu3P/p-PhCOC6H4Br initiator systems afforded functional polymers with >95% fidelity. Our results pavedmore » the road to access well-defined conjugated polymers, including conjugated polymers with complex polymer architectures such as block copolymers and branch copolymers.« less

  20. Orbital-optimized MP2.5 and its analytic gradients: Approaching CCSD(T) quality for noncovalent interactions

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Bozkaya, Uğur, E-mail: ugur.bozkaya@atauni.edu.tr; Center for Computational Molecular Science and Technology, School of Chemistry and Biochemistry, and School of Computational Science and Engineering, Georgia Institute of Technology, Atlanta, Georgia 30332; Sherrill, C. David

    2014-11-28

    Orbital-optimized MP2.5 [or simply “optimized MP2.5,” OMP2.5, for short] and its analytic energy gradients are presented. The cost of the presented method is as much as that of coupled-cluster singles and doubles (CCSD) [O(N{sup 6}) scaling] for energy computations. However, for analytic gradient computations the OMP2.5 method is only half as expensive as CCSD because there is no need to solve λ{sub 2}-amplitude equations for OMP2.5. The performance of the OMP2.5 method is compared with that of the standard second-order Møller–Plesset perturbation theory (MP2), MP2.5, CCSD, and coupled-cluster singles and doubles with perturbative triples (CCSD(T)) methods for equilibrium geometries, hydrogenmore » transfer reactions between radicals, and noncovalent interactions. For bond lengths of both closed and open-shell molecules, the OMP2.5 method improves upon MP2.5 and CCSD by 38%–43% and 31%–28%, respectively, with Dunning's cc-pCVQZ basis set. For complete basis set (CBS) predictions of hydrogen transfer reaction energies, the OMP2.5 method exhibits a substantially better performance than MP2.5, providing a mean absolute error of 1.1 kcal mol{sup −1}, which is more than 10 times lower than that of MP2.5 (11.8 kcal mol{sup −1}), and comparing to MP2 (14.6 kcal mol{sup −1}) there is a more than 12-fold reduction in errors. For noncovalent interaction energies (at CBS limits), the OMP2.5 method maintains the very good performance of MP2.5 for closed-shell systems, and for open-shell systems it significantly outperforms MP2.5 and CCSD, and approaches CCSD(T) quality. The MP2.5 errors decrease by a factor of 5 when the optimized orbitals are used for open-shell noncovalent interactions, and comparing to CCSD there is a more than 3-fold reduction in errors. Overall, the present application results indicate that the OMP2.5 method is very promising for open-shell noncovalent interactions and other chemical systems with difficult electronic structures.« less

  1. Evaluation of Ginger (Zingiber officinale Roscoe) Bioactive Compounds in Increasing the Ratio of T-cell Surface Molecules of CD3+CD4+:CD3+CD8+ In-Vitro.

    PubMed

    Tejasari, Dr

    2007-09-01

    The potential ability of ginger bioactive compounds in increasing the ratio of T-cell surface molecules of CD3+CD4+:CD3+CD8+ was investigated using dual tagging FITC and PE of monoclonal antibody anti-human with its fluorescence measured by flow cytometer. Oleoresin was extracted using sinkhole distillation technique. Its components namely, gingerol in fraction-1, shogaol in fraction 2 and zingeron in fraction-3 were separated by column vacuum chromatography method. The doses of oleoresin, gingerol, shogaol, and zingeron tested were 50, 100,150, 200, and 250 μg/ml. Lymphocytes (2x106 cell/ml) from human peripheral blood were isolated using ficoll density gradient technique, and cultured in the presence of the compounds in RPMI-1640 medium and phytohemaglutinin (PHA) mitogen for 96 h under normal conditions. Percentages of T-cell surface molecules (CD4+ and CD8+) were determined using dual-tagging FITC and PE fluorescents labeled on monoclonal antibody anti human. The fluorescence-labeled bands on the T-cell surface molecules were counted using flow cytometer. The experiment revealed that oleoresin and its three fractions increased the percentage of CD3+CD4+. The compound in fraction 3 of oleoresin at 200 μg/ml increased by the highest percentage of CD3+CD4+ of 9%, but slightly decreased the percentage of CD3+CD8+. These ginger bioactive compounds increased the ratio of CD3+CD4:CD3+CD8+ T-cells with the highest increment of 30% from effects of 200 μg/ml fraction 3 of oleoresin. This in vitro finding revealed that ginger bioactive compounds potentially increased cellular and humoral immune response. Further clinical studies are needed to confirm the benefits of these ginger bioactive compounds as a potential functional food for testing on HIV infected patients.

  2. Green analytical method development for statin analysis.

    PubMed

    Assassi, Amira Louiza; Roy, Claude-Eric; Perovitch, Philippe; Auzerie, Jack; Hamon, Tiphaine; Gaudin, Karen

    2015-02-06

    Green analytical chemistry method was developed for pravastatin, fluvastatin and atorvastatin analysis. HPLC/DAD method using ethanol-based mobile phase with octadecyl-grafted silica with various grafting and related-column parameters such as particle sizes, core-shell and monolith was studied. Retention, efficiency and detector linearity were optimized. Even for column with particle size under 2 μm, the benefit of keeping efficiency within a large range of flow rate was not obtained with ethanol based mobile phase compared to acetonitrile one. Therefore the strategy to shorten analysis by increasing the flow rate induced decrease of efficiency with ethanol based mobile phase. An ODS-AQ YMC column, 50 mm × 4.6 mm, 3 μm was selected which showed the best compromise between analysis time, statin separation, and efficiency. HPLC conditions were at 1 mL/min, ethanol/formic acid (pH 2.5, 25 mM) (50:50, v/v) and thermostated at 40°C. To reduce solvent consumption for sample preparation, 0.5mg/mL concentration of each statin was found the highest which respected detector linearity. These conditions were validated for each statin for content determination in high concentrated hydro-alcoholic solutions. Solubility higher than 100mg/mL was found for pravastatin and fluvastatin, whereas for atorvastatin calcium salt the maximum concentration was 2mg/mL for hydro-alcoholic binary mixtures between 35% and 55% of ethanol in water. Using atorvastatin instead of its calcium salt, solubility was improved. Highly concentrated solution of statins offered potential fluid for per Buccal Per-Mucous(®) administration with the advantages of rapid and easy passage of drugs. Copyright © 2014 Elsevier B.V. All rights reserved.

  3. T-kininogen can either induce or inhibit proliferation in Balb/c 3T3 fibroblasts, depending on the route of administration.

    PubMed

    Aravena, M; Pérez, C; Pérez, V; Acuña-Castillo, C; Gómez, C; Leiva-Salcedo, E; Nishimura, S; Sabaj, V; Walter, R; Sierra, F

    2005-03-01

    T-kininogen (T-KG) is a precursor of T-kinin, the most abundant kinin in rat serum, and also acts as a strong and specific cysteine proteinase inhibitor. Its expression is strongly induced during aging in rats, and expression of T-KG in Balb/c 3T3 fibroblasts results in inhibition of cell proliferation. However, T-KG is a serum protein produced primarily in the liver, and thus, most cells are only exposed to the protein from the outside. To test the effect of T-KG on fibroblasts exposed to exogenous T-KG, we purified the protein from the serum of K-kininogen-deficient Katholiek rats. In contrast to the results obtained by transfection, exposure of Balb/c 3T3 fibroblasts to exogenously added T-KG leads to a dose-dependent increase in [3H]-thymidine incorporation. This response does not require kinin receptors, but it is clearly mediated by activation of the ERK pathway. As a control, we repeated the transfection experiments, using a different promoter. The results are consistent with our published data showing that, under these circumstances, T-KG inhibits cell proliferation. We conclude that T-KG exerts opposite effects on fibroblast proliferation, depending exclusively on the way that it is administered to the cells (transfection versus exogenous addition).

  4. Synthesis and characterization of two layered aluminophosphates, ( T) 2HAl 2P 3O 12 ( T=2-BuNH 3+) and ( T)H 2Al 2P 3O 12 ( T=pyH +)

    NASA Astrophysics Data System (ADS)

    Chippindale, Ann M.; Powell, Anthony V.; Bull, Lucy M.; Jones, Richard H.; Cheetham, Anthony K.; Thomas, John M.; Xu, Ruren

    1992-01-01

    Two new aluminophosphates, ( T) 2HAl 2P 3O 12 ( T=2-BuNH 3+) ( I) and ( T)H 2Al 2P 3O 12 ( T=pyH +) ( II) with the same framework stoichiometry but different layer structures have been prepared under nonaqueous conditions and the structures determined by single-crystal X-ray diffraction. Compound ( I) crystallizes in the monoclinic space group P2 1/ c ( Z=4), with lattice parameters a=9.261(1) b=8.365(6), c=27.119(4) Å, β=91.50(1)δ, and V=2100.1 Å 3 ( R=0.072 and R w=0.090). The structure consists of Al-and P-centered tetrahedra linked to form layers. Protonated 2-butylamine molecules are located in the interlayer spaces and hydrogen bonded to the layers through NH 3+ groups. Weak hydrophobic van der Waals' interactions between alkyl groups of the 2-BuNH 3+ cations hold the layers together. Compound ( II) crystallizes in the triclinic space group P-1 ( Z=2), with a=8.574(2), b=8.631(3), c=10.371(2) Å, α=81.84(3), β=87.53(2), γ=69.07(2)δ, and V=709.49Å 3 ( R=0.039 and R w=0.052). The structure contains tetrahedrally coordinated P atoms and both tetrahedral and trigonal pyramidal Al atoms linked to form layers which are held together through hydrogen bonding, creating cavities in which pyH + cations reside.

  5. Potential of capillary-column-switching liquid chromatography-tandem mass spectrometry for the quantitative trace analysis of small molecules. Application to the on-line screening of drugs in water.

    PubMed

    Pitarch, Elena; Hernandez, Felix; ten Hove, Jan; Meiring, Hugo; Niesing, Willem; Dijkman, Ellen; Stolker, Linda; Hogendoorn, Elbert

    2004-03-26

    We have investigated the potential of capillary-column-switching liquid chromatography coupled to tandem mass spectrometry (cLC-MS-MS) for the quantitative on-line trace analysis of target compounds in aqueous solutions. The technical design of the nano-scale cLC system developed at our Institute for peptide and protein identification has been tested and evaluated for the direct trace analysis of drugs in water samples. Sulphametoxazole, bezafibrate, metoprolol, carbamazepine and bisoprolol occurring frequently in Dutch waters, were selected as test compounds. Adequate conditions for trapping, elution and MS-MS detection were investigated by employing laboratory made 200 microm i.d. capillary columns packed with 5 microm aqua C18 material. In the final cLC-MS-MS conditions, a 1 cm length trapping column and a 4 cm length analytical column were selected. Under these conditions, the target compounds could be directly determined in water down to a level of around 50 ng/l employing only 25 microl of water sample. Validation was done by recovery experiments in ground-, surface- and drinking-water matrices as well as by the analysis of water samples with incurred residues and previously analyzed with a conventional procedure involving off-line solid-phase extraction and narrow-bore LC with MS-MS detection. The new methodology provided recoveries (50-500 ng/l level) between 50 and 114% with RSDs (n = 3, each level) below 20% for most of the compounds. Despite the somewhat less analytical performance in comparison to the conventional procedure, the on-line approach of the new methodology is very suitable for screening of drugs in aqueous samples.

  6. Preparation of a poly(3'-azido-3'-deoxythymidine-co-propargyl methacrylate-co-pentaerythritol triacrylate) monolithic column by in situ polymerization and a click reaction for capillary liquid chromatography of small molecules and proteins.

    PubMed

    Lin, Zian; Yu, Ruifang; Hu, Wenli; Zheng, Jiangnan; Tong, Ping; Zhao, Hongzhi; Cai, Zongwei

    2015-07-07

    Combining free radical polymerization with click chemistry via a copper-mediated azide/alkyne cycloaddition (CuAAC) reaction in a "one-pot" process, a facile approach was developed for the preparation of a poly(3'-azido-3'-deoxythymidine-co-propargyl methacrylate-co-pentaerythritol triacrylate) (AZT-co-PMA-co-PETA) monolithic column. The resulting poly(AZT-co-PMA-co-PETA) monolith showed a relatively homogeneous monolithic structure, good permeability and mechanical stability. Different ratios of monomers and porogens were used for optimizing the properties of a monolithic column. A series of alkylbenzenes, amides, anilines, and benzoic acids were used to evaluate the chromatographic properties of the polymer monolith in terms of hydrophobic, hydrophilic and cation-exchange interactions, and the results showed that the poly(AZT-co-PMA-co-PETA) monolith exhibited more flexible adjustment in chromatographic selectivity than that of the parent poly(PMA-co-PETA) and AZT-modified poly(PMA-co-PETA) monoliths. Column efficiencies for toluene, DMF, and formamide with 35,000-48,000 theoretical plates per m could be obtained at a linear velocity of 0.17 mm s(-1). The run-to-run, column-to-column, and batch-to-batch repeatabilities of the retention factors were less than 4.2%. In addition, the proposed monolith was also applied to efficient separation of sulfonamides, nucleobases and nucleosides, anesthetics and proteins for demonstrating its potential.

  7. Optimization and validation of the reversed-phase high-performance liquid chromatography with fluorescence detection method for the separation of tocopherol and tocotrienol isomers in cereals, employing a novel sorbent material.

    PubMed

    Irakli, Maria N; Samanidou, Victoria F; Papadoyannis, Ioannis N

    2012-03-07

    The separation and determination of tocopherols (Ts) and tocotrienols (T3s) by reversed-phase high-performance liquid chromatography with fluorescence detection has been developed and validated after optimization of various chromatographic conditions and other experimental parameters. Analytes were separated on a PerfectSil Target ODS-3 (250 × 4.6 mm, 3 μm) column filled with a novel sorbent material of ultrapure silica gel. The separation of Ts and T3s was optimized in terms of mobile-phase composition and column temperature on the basis of the best compromise among efficiency, resolution, and analysis time. Using a gradient elution of mobile phase composed of isopropanol/water and 7 °C column temperature, a satisfactory resolution was achieved within 62 min. For the quantitative determination, α-T acetate (50 μg/mL) was used as the internal standard. Detection limits ranged from 0.27 μg/mL (γ-T) to 0.76 μg/mL (γ-T3). The validation of the method was examined performing intraday (n = 5) and interday (n = 3) assays and was found to be satisfactory, with high accuracy and precision results. Solid-phase extraction provided high relative extraction recoveries from cereal samples: 87.0% for γ-T3 and 115.5% for δ-T. The method was successfully applied to cereals, such as durum wheat, bread wheat, rice, barley, oat, rye, and corn.

  8. Analytical and experimental studies on detection of longitudinal, L and inverted T cracks in isotropic and bi-material beams based on changes in natural frequencies

    NASA Astrophysics Data System (ADS)

    Ravi, J. T.; Nidhan, S.; Muthu, N.; Maiti, S. K.

    2018-02-01

    An analytical method for determination of dimensions of longitudinal crack in monolithic beams, based on frequency measurements, has been extended to model L and inverted T cracks. Such cracks including longitudinal crack arise in beams made of layered isotropic or composite materials. A new formulation for modelling cracks in bi-material beams is presented. Longitudinal crack segment sizes, for L and inverted T cracks, varying from 2.7% to 13.6% of length of Euler-Bernoulli beams are considered. Both forward and inverse problems have been examined. In the forward problems, the analytical results are compared with finite element (FE) solutions. In the inverse problems, the accuracy of prediction of crack dimensions is verified using FE results as input for virtual testing. The analytical results show good agreement with the actual crack dimensions. Further, experimental studies have been done to verify the accuracy of the analytical method for prediction of dimensions of three types of crack in isotropic and bi-material beams. The results show that the proposed formulation is reliable and can be employed for crack detection in slender beam like structures in practice.

  9. Preliminary results from a microvolume, dynamically heated analytical column for preconcentration and separation of simple gases prior to stable isotopic analysis

    NASA Astrophysics Data System (ADS)

    Panetta, Robert James; Seed, Mike

    2016-04-01

    Stable isotope applications that call for preconcentration (i.e., greenhouse gas measurements, small carbonate samples, etc.) universally call for cryogenic fluids such as liquid nitrogen, dry ice slurries, or expensive external recirculation chillers. This adds significant complexity, first and foremost in the requirements to store and handle such dangerous materials. A second layer of complexity is the instrument itself - with mechanisms to physically move either coolant around the trap, or move a trap in or out of the coolant. Not to mention design requirements for hardware that can safely isolate the fluid from other sensitive areas. In an effort to simplify the isotopic analysis of gases requiring preconcentration, we have developed a new separation technology, UltiTrapTM (patent pending), which leverage's the proprietary Advanced Purge & Trap (APT) Technology employed in elemental analysers from Elementar Analysensysteme GmbH products. UltiTrapTM has been specially developed as a micro volume, dynamically heated GC separation column. The introduction of solid-state cooling technology enables sub-zero temperatures without cryogenics or refrigerants, eliminates all moving parts, and increases analytical longevity due to no boiling losses of coolant . This new technology makes it possible for the system to be deployed as both a focussing device and as a gas separation device. Initial data on synthetic gas mixtures (CO2/CH4/N2O in air), and real-world applications including long-term room air and a comparison between carbonated waters of different origins show excellent agreement with previous technologies.

  10. Apoptosis observed in BALB/3T3 cells having ingested Staphylococcus aureus.

    PubMed

    Murai, M; Sakurada, J; Seki, K; Shinji, H; Hirota, Y; Masuda, S

    1999-01-01

    Staphylococcus aureus was previously shown to be internalized by murine fibroblast. We examined the intracellular events of S. aureus ingested by BALB/3T3 cells. After uptake of strains A191 and A151, isolates from atopic lesion, and a laboratory strain, Cowan I, for 1 hr, BALB/3T3 cells were incubated with 1.25 microg/ml lysostaphin. Laddering of the DNA in multiples of approximately 180 bp occurred within 4 hr following bacterial addition in BALB/3T3 cells infected with A191 and within 18 hr in BALB/3T3 cells infected with A151: histochemical staining by the terminal deoxynucleotidyl transferase-mediated dUTP-biotin nick end labeling method revealed that the rate of the fragmentation of nucleic DNA in Cowan I-infected BALB/3T3 cells at 21 hr following bacterial addition was 0.52 +/- 0.25%, significantly higher than that in the control cells. Transmission electron micrographs of BALB/3T3 cells at 4 hr following A191 addition showed that the apoptotic features, including electron-dense nucleus and plasma membrane blebbing, occurred in some cells in which many staphylococci escaped the endosome and went on to cell division. At the same time, A151 organisms enclosed with endosome membrane were static in the intact BALB/3T3 cells. The significant increase of A191 was confirmed by counting intracellular live bacteria during 2- to 6-hr incubation. These results suggest that internalized S. aureus escapes the endosome, multiplies and induces apoptosis in the fibroblast cell.

  11. Measurement of bromate in bread by liquid chromatography with post-column flow reactor detection.

    PubMed

    Himata, K; Noda, M; Ando, S; Yamada, Y

    2000-01-01

    This method is suitable for the determination of bromate residues in a variety of baked goods. The peer-verified method trial was performed on white bread, multigrain bread, and coffee cake spiked with known levels of potassium bromate. The analytical portion is extracted with deionized water to remove bromate from the bulk of the baked product. The aqueous extract is carried through a series of steps to remove co-extractives that would interfere with the liquid chromatography (LC) in the determinative step or hasten the deterioration of the LC column. The extract is filtered before passing it through a reversed-phase solid-phase extraction (SPE) column and a cation-exchange column in the silver form to remove lipids and chloride, respectively. Ultrafiltration is then used to remove proteins with molecular weights of >30,000 daltons. Finally, a cation-exchange column in the sodium form is used to remove silver ions from the extract. The determinative step uses LC with a reversed-phase column and an ion-pairing agent in the mobile phase. Detection is based on the post-column reaction of bromate with o-dianisidine to form an oxidation product that is quantitated spectrophotometrically at 450 nm. Overall agreement between the submitting and peer laboratories was quite good. For bromate levels of 10-52 ppb, overall mean recoveries were 76.9 and 78.8% for the submitting and peer laboratories, respectively. The standard deviations were higher for the results of the peer laboratory, probably because of the generally higher level of baseline noise present in the chromatograms. The results demonstrate that the method provides adequate accuracy with low-fat as well as high-fat foods. Bromate at levels as low as 5 ppb (ng/g) can be detected with the method.

  12. Stage-frit: A straightforward sub-2 μm nano-liquid chromatography column fabrication for proteomic analysis.

    PubMed

    Hsieh, Ming-Yueh; Hsiao, He-Hsuan

    2015-07-30

    In this work we demonstrated a facile method for the fabrication of C18 coordination polymer gel in a capillary, called stage-frit, which was efficiently applied to pack sub-2 μm C18 beads into the capillary by a high pressure bomb for the online separation of proteolytic peptides. The back pressure of the column with 10 cm × 75 μm i.d. is regularly lower than 170 bar at a flow rate of 300 nl/min, which could be operated on a common nanoLC system instead of nanoUPLC system due to the good permeability, low back pressure and high mechanical stress of the frit that will totally reduce the cost for the purchase of instrument. The stage-frit allows long-term continuous flow of the solvent and no significant beads loss or pressure instability was observed during the period. The repeatability of retention time for fifteen BSA tryptic peaks was found to be less than 1.08% (RSD) in six time nanoLC-ESI-MS/MS experiments. The average full width at half maximum (FWHM) of peptide peaks is 5.87 s. The sub-2 μm stage-frit nanoLC column showed better sensitivity than the commercial available for large scale proteomic analysis of total tissue proteins from human spleen. The number of identified peptides is approximately 0.4-fold and 0.2-fold higher than that obtained by utilizing commercial columns packed with 3 μm and 1.8 μm C18 materials, respectively. In the field of analytical chemistry, particularly the use of nanoLC systems, stage-frit nanoLC column offers a great potential for the separation of complex mixtures. Copyright © 2015 Elsevier B.V. All rights reserved.

  13. Cellular organization of cortical barrel columns is whisker-specific

    PubMed Central

    Meyer, Hanno S.; Egger, Robert; Guest, Jason M.; Foerster, Rita; Reissl, Stefan; Oberlaender, Marcel

    2013-01-01

    The cellular organization of the cortex is of fundamental importance for elucidating the structural principles that underlie its functions. It has been suggested that reconstructing the structure and synaptic wiring of the elementary functional building block of mammalian cortices, the cortical column, might suffice to reverse engineer and simulate the functions of entire cortices. In the vibrissal area of rodent somatosensory cortex, whisker-related “barrel” columns have been referred to as potential cytoarchitectonic equivalents of functional cortical columns. Here, we investigated the structural stereotypy of cortical barrel columns by measuring the 3D neuronal composition of the entire vibrissal area in rat somatosensory cortex and thalamus. We found that the number of neurons per cortical barrel column and thalamic “barreloid” varied substantially within individual animals, increasing by ∼2.5-fold from dorsal to ventral whiskers. As a result, the ratio between whisker-specific thalamic and cortical neurons was remarkably constant. Thus, we hypothesize that the cellular architecture of sensory cortices reflects the degree of similarity in sensory input and not columnar and/or cortical uniformity principles. PMID:24101458

  14. Investigation of rectangular concrete columns reinforced or prestressed with fiber reinforced polymer (FRP) bars or tendons

    NASA Astrophysics Data System (ADS)

    Choo, Ching Chiaw

    Fiber reinforced polymer (FRP) composites have been increasingly used in concrete construction. This research focused on the behavior of concrete columns reinforced with FRP bars, or prestressed with FRP tendons. The methodology was based the ultimate strength approach where stress and strain compatibility conditions and material constitutive laws were applied. Axial strength-moment (P-M) interaction relations of reinforced or prestressed concrete columns with FRP, a linearly-elastic material, were examined. The analytical results identified the possibility of premature compression and/or brittle-tension failure occurring in FRP reinforced and prestressed concrete columns where sudden and explosive type failures were expected. These failures were related to the rupture of FRP rebars or tendons in compression and/or in tension prior to concrete reaching its ultimate strain and strength. The study also concluded that brittle-tension failure was more likely to occur due to the low ultimate tensile strain of FRP bars or tendons as compared to steel. In addition, the failures were more prevalent when long term effects such as creep and shrinkage of concrete, and creep rupture of FRP were considered. Barring FRP failure, concrete columns reinforced with FRP, in some instances, gained significant moment resistance. As expected the strength interaction of slender steel or FRP reinforced concrete columns were dependent more on column length rather than material differences between steel and FRP. Current ACI minimum reinforcement ratio for steel (rhomin) reinforced concrete columns may not be adequate for use in FRP reinforced concrete columns. Design aids were developed in this study to determine the minimum reinforcement ratio (rhof,min) required for rectangular reinforced concrete columns by averting brittle-tension failure to a failure controlled by concrete crushing which in nature was a less catastrophic and more gradual type failure. The proposed method using rhof

  15. Three column intermittent simulated moving bed chromatography: 3. Cascade operation for center-cut separations.

    PubMed

    Jermann, Simon; Meijssen, Mattheus; Mazzotti, Marco

    2015-01-23

    A general design methodology for chromatographic three fraction separation by application of the three column intermittent simulated moving bed (3C-ISMB) cascade is proposed and experimentally validated by studying the purification of an intermediately retained stereoisomer of nadolol, from an equimolar mixture of its four stereoisomers. The theoretical part shows that the 3C-ISMB cascade can be easily designed by applying Triangle Theory. Moreover, a re-scaling approach for the second stage is proposed so as to account for the fact that the feed flow rates to stage 2 are generally higher as compared to stage 1 due to dilution in the latter. Scaling the columns of the second stage accordingly enables to run both stages under optimal conditions with respect to switching time and step ratio, which is an important advantage as compared to integrated ternary processes. The experimental part starts with studying the linear adsorption behavior of nadolol in heptane/ethanol/DEA on Chiralpak AD for varying ratios of heptane and ethanol. Based on that, a solvent composition of Hept/EtOH/DEA 30/70/0.3 (v/v/v) is selected and the competitive multi-component Langmuir isotherm of the quaternary mixture is determined by frontal analysis. The resulting isotherm parameters are used to design several first stage experiments aiming at removal of the most retained component. The resulting ternary intermediate product is reprocessed in several second stage experiments studying various configurations. Finally, the dilution of the intermediate product with Hept/DEA yielding a solvent composition of Hept/EtOH/DEA 60/40/0.3 (v/v/v) is examined showing that the resulting increase in retention is beneficial for final product purities. Moreover, the reduction in viscosity compensates for the dilution as it enables higher flow rates. Dilution of the intermediate product is hence the best option, yielding highest overall cascade productivity (2.10gl(-1)h(-1)) and highest product purity (97

  16. IDEAL 3D spoiled gradient echo of the articular cartilage of the knee on 3.0 T MRI: a comparison with conventional 3.0 T fast spin-echo T2 fat saturation image.

    PubMed

    Han, Chul Hee; Park, Hee Jin; Lee, So Yeon; Chung, Eun Chul; Choi, Seon Hyeong; Yun, Ji Sup; Rho, Myung Ho

    2015-12-01

    Many two-dimensional (2D) morphologic cartilage imaging sequences have disadvantages such as long acquisition time, inadequate spatial resolution, suboptimal tissue contrast, and image degradation secondary to artifacts. IDEAL imaging can overcome these disadvantages. To compare sound-to-noise ratio (SNR), contrast-to-noise ratio (CNR), and quality of two different methods of imaging that include IDEAL 3D SPGR and 3.0-T FSE T2 fat saturation (FS) imaging and to evaluate the utility of IDEAL 3D SPGR for knee joint imaging. SNR and CNR of the patellar and femoral cartilages were measured and calculated. Two radiologists performed subjective scoring of all images for three measures: general image quality, FS, and cartilage evaluation. SNR and CNR values were compared by paired Student's t-tests. Mean SNRs of patellar and femoral cartilages were 90% and 66% higher, respectively, for IDEAL 3D SPGR. CNRs of patellar cartilages and joint fluids were 2.4 times higher for FSE T2 FS, and CNR between the femoral cartilage and joint fluid was 2.2 times higher for FSE T2 FS. General image quality and FS were superior using FSE T2 FS compared to those of IDEAL 3D SPGR imaging according to both readers, while cartilage evaluation was superior using IDEAL 3D SPGR. Additionally, cartilage injuries were more prominent in IDEAL 3D SPGR than in FSE T2FS according to both readers. IDEAL 3D SPGR images show excellent visualization of patellar and femoral cartilages in 3.0 T and can compensate for the weaknesses of FSE T2 FS in the evaluation of cartilage injuries. © The Foundation Acta Radiologica 2014.

  17. Mediator subunit MED1 is a T3-dependent and T3-independent coactivator on the thyrotropin β gene promoter

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Matsui, Keiji; Oda, Kasumi; Mizuta, Shumpei

    2013-10-11

    Highlights: •MED1 is a bona fide T3-dependent coactivator on TSHB promoter. •Mice with LxxLL-mutant MED1 have attenuated TSHβ mRNA and thyroid hormone levels. •MED1 activates TSHB promoter T3-dependently in cultured cells. •T3-dependent MED1 action is enhanced when SRC1/SRC2 or HDAC2 is downregulated. •MED1 is also a T3-independent GATA2/Pit1 coactivator on TSHB promoter. -- Abstract: The MED1 subunit of the Mediator transcriptional coregulator complex is a nuclear receptor-specific coactivator. A negative feedback mechanism of thyroid-stimulating hormone (TSH, or thyrotropin) expression in the thyrotroph in the presence of triiodothyronine (T3) is employed by liganded thyroid hormone receptor β (TRβ) on the TSHβmore » gene promoter, where conventional histone-modifying coactivators act as corepressors. We now provide evidence that MED1 is a ligand-dependent positive cofactor on this promoter. TSHβ gene transcription was attenuated in MED1 mutant mice in which the nuclear receptor-binding ability of MED1 was specifically disrupted. MED1 stimulated GATA2- and Pit1-mediated TSHβ gene promoter activity in a ligand-independent manner in cultured cells. MED1 also stimulated transcription from the TSHβ gene promoter in a T3-dependent manner. The transcription was further enhanced when the T3-dependent corepressors SRC1, SRC2, and HDAC2 were downregulated. Hence, MED1 is a T3-dependent and -independent coactivator on the TSHβ gene promoter.« less

  18. Definition of a safe zone for antegrade lag screw fixation of fracture of posterior column of the acetabulum by 3D technology.

    PubMed

    Feng, Xiaoreng; Zhang, Sheng; Luo, Qiang; Fang, Jintao; Lin, Chaowen; Leung, Frankie; Chen, Bin

    2016-03-01

    The objective of this study was to define a safe zone for antegrade lag screw fixation of fracture of posterior column of the acetabulum using a novel 3D technology. Pelvic CT data of 59 human subjects were obtained to reconstruct three-dimensional (3D) models. The transparency of 3D models was then downgraded along the axial perspective (the view perpendicular to the cross section of the posterior column axis) to find the largest translucent area. The outline of the largest translucent area was drawn on the iliac fossa. The line segments of OA, AB, OC, CD, the angles of OAB and OCD that delineate the safe zone (ABDC) were precisely measured. The resultant line segments OA, AB, OC, CD, and angles OAB and OCD were 28.46mm(13.15-44.97mm), 45.89mm (34.21-62.85mm), 36.34mm (18.68-55.56mm), 53.08mm (38.72-75.79mm), 37.44° (24.32-54.96°) and 55.78° (43.97-79.35°) respectively. This study demonstrates that computer-assisted 3D modelling techniques can aid in the precise definition of the safe zone for antegrade insertion of posterior column lag screws. A full-length lag screw can be inserted into the zone (ABDC), permitting a larger operational error. Copyright © 2016 Elsevier Ltd. All rights reserved.

  19. Determination of ammonium in wastewaters by capillary electrophoresis on a column-coupling chip with conductivity detection.

    PubMed

    Luc, Milan; Kruk, Pavol; Masár, Marián

    2011-07-01

    Analytical potentialities of a chip-based CE in determination of ammonium in wastewaters were investigated. CZE with the electric field and/or ITP sample stacking was performed on a column-coupling (CC) chip with integrated conductivity detectors. Acetate background electrolytes (pH ∼3) including 18-crown-6-ether (18-crown-6) and tartaric acid were developed to reach rapid (in 7-8 min) CZE and ITP-CZE resolutions of ammonium from other cations (sodium, potassium, calcium and magnesium) present in wastewater samples. Under preferred working conditions (suppressed hydrodynamic flow (HDF) and EOF on the column-coupling chip), both the employed methods did provide very good repeatabilities of the migration (RSD of 0.2-0.8% for the migration time) and quantitative (RSD of 0.3-4.9% for the peak area) parameters in the model and wastewater samples. Using a 900-nL sample injection volume, LOD for ammonium were obtained at 20 and 40 μg/L concentrations in CZE and ITP-CZE separations, respectively. Very good agreements of the CZE and ITP-CZE determinations of ammonium in six untreated wastewater samples (only filtration and dilution) with the results obtained by a reference spectrometric method indicate a very good accuracy of both the CE methods presented. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Pre-Column Derivatization HPLC Procedure for the Quantitation of Aluminium Chlorohydrate in Antiperspirant Creams Using Quercetin as Chromogenic Reagent.

    PubMed

    Kalogria, Eleni; Varvaresou, Athanasia; Papageorgiou, Spyridon; Protopapa, Evaggelia; Tsaknis, Ioannis; Matikas, Alexios; Panderi, Irene

    2014-01-01

    This article describes the development and validation of a selective high-performance liquid chromatography method that allows, after liquid-liquid extraction and pre-column derivatization reaction with quercetin, the quantification of aluminium chlorohydrate in antiperspirant creams. Chromatographic separation was achieved on an XTerra MS C18 analytical column (150 × 3.0 mm i.d., particle size 5 μm) using a mobile phase of acetonitrile:water (15:85, v/v) containing 0.08 % trifluoroacetic acid at a flow rate of 0.30 mL min -1 . Ultraviolet spectrophotometric detection at 415 nm was used. The assay was linear over a concentration range of 3.7-30.6 μg mL -1 for aluminium with a limit of quantitation of 3.74 μg mL -1 . Quality control samples (4.4, 17.1 and 30.6 μg mL -1 ) in five replicates from five different runs of analysis demonstrated intra-assay precision (% coefficient of variation <3.8 %), inter-assay precision (% coefficient of variation <5.4 %) and an overall accuracy (% recovery) between 96 and 101 %. The method was used to quantify aluminium in antiperspirant creams containing 11.0, 13.0 and 16.0 % (w/w) aluminium chlorohydrate, respectively.

  1. Tonic ubiquitylation controls T-cell receptor:CD3 complex expression during T-cell development.

    PubMed

    Wang, Haopeng; Holst, Jeff; Woo, Seng-Ryong; Guy, Cliff; Bettini, Matt; Wang, Yao; Shafer, Aaron; Naramura, Mayumi; Mingueneau, Michaël; Dragone, Leonard L; Hayes, Sandra M; Malissen, Bernard; Band, Hamid; Vignali, Dario A A

    2010-04-07

    Expression of the T-cell receptor (TCR):CD3 complex is tightly regulated during T-cell development. The mechanism and physiological role of this regulation are unclear. Here, we show that the TCR:CD3 complex is constitutively ubiquitylated in immature double positive (DP) thymocytes, but not mature single positive (SP) thymocytes or splenic T cells. This steady state, tonic CD3 monoubiquitylation is mediated by the CD3varepsilon proline-rich sequence, Lck, c-Cbl, and SLAP, which collectively trigger the dynamin-dependent downmodulation, lysosomal sequestration and degradation of surface TCR:CD3 complexes. Blocking this tonic ubiquitylation by mutating all the lysines in the CD3 cytoplasmic tails significantly upregulates TCR levels on DP thymocytes. Mimicking monoubiquitylation by expression of a CD3zeta-monoubiquitin (monoUb) fusion molecule significantly reduces TCR levels on immature thymocytes. Moreover, modulating CD3 ubiquitylation alters immunological synapse (IS) formation and Erk phosphorylation, thereby shifting the signalling threshold for positive and negative selection, and regulatory T-cell development. Thus, tonic TCR:CD3 ubiquitylation results in precise regulation of TCR expression on immature T cells, which is required to maintain the fidelity of T-cell development.

  2. Tonic ubiquitylation controls T-cell receptor:CD3 complex expression during T-cell development

    PubMed Central

    Wang, Haopeng; Holst, Jeff; Woo, Seng-Ryong; Guy, Cliff; Bettini, Matt; Wang, Yao; Shafer, Aaron; Naramura, Mayumi; Mingueneau, Michaël; Dragone, Leonard L; Hayes, Sandra M; Malissen, Bernard; Band, Hamid; Vignali, Dario A A

    2010-01-01

    Expression of the T-cell receptor (TCR):CD3 complex is tightly regulated during T-cell development. The mechanism and physiological role of this regulation are unclear. Here, we show that the TCR:CD3 complex is constitutively ubiquitylated in immature double positive (DP) thymocytes, but not mature single positive (SP) thymocytes or splenic T cells. This steady state, tonic CD3 monoubiquitylation is mediated by the CD3ɛ proline-rich sequence, Lck, c-Cbl, and SLAP, which collectively trigger the dynamin-dependent downmodulation, lysosomal sequestration and degradation of surface TCR:CD3 complexes. Blocking this tonic ubiquitylation by mutating all the lysines in the CD3 cytoplasmic tails significantly upregulates TCR levels on DP thymocytes. Mimicking monoubiquitylation by expression of a CD3ζ-monoubiquitin (monoUb) fusion molecule significantly reduces TCR levels on immature thymocytes. Moreover, modulating CD3 ubiquitylation alters immunological synapse (IS) formation and Erk phosphorylation, thereby shifting the signalling threshold for positive and negative selection, and regulatory T-cell development. Thus, tonic TCR:CD3 ubiquitylation results in precise regulation of TCR expression on immature T cells, which is required to maintain the fidelity of T-cell development. PMID:20150895

  3. Comparison of FSE T2 W PROPELLER and 3D-FIESTA of 3 T MR for the internal auditory canal.

    PubMed

    Wu, Hai-Bo; Yuan, Hui-Shu; Ma, Furong; Zhao, Qiang

    The study compared the use of periodically rotated overlapping parallel lines with enhanced reconstruction (PROPELLER) technique fast spin echo (FSE) T2 W and the sequence of three-dimensional fast imaging employing steady-state acquisition (3D-FIESTA) technique in the MRI of the internal auditory canal for overall image quality improvement. One hundred thirty-two patients undergoing FSE T2 W PROPELLER and 3D-FIESTA examinations of the internal auditory canal were included. All examinations were performed at 3.0 T with comparison of a sagittal oblique FSE T2 W sequence with the PROPELLER technique to 3D-FIESTA in the same reconstructed orientation with PROPELLER. Image quality was evaluated by two radiologists using a 4-point scale. The Wilcoxon signed rank test was used to compare the data of the two techniques. The image quality of FSE T2 W PROPELLER was significantly improved compared to the reconstructed images of 3D-FIESTA. Observer 1: median FSE T2 W with PROPELLER, 4 [mean, 3.455] versus median reconstructed 3D-FIESTA, 3 [mean, 3.15], (P<.001); Observer 2: median FSE T2 W with PROPELLER, 4 [mean, 3.47] versus median reconstructed 3D-FIESTA, 3 [mean, 3.25], (P<.001). Interobserver agreement was good (k value, 0.73) for the rating of the overall image quality. The FSE T2 W PROPELLER technique for MRI of internal auditory canal reduced uncertainty caused by motion artifact and improved the quality of the image compared to the reconstructed 3D-FIESTA. It was affected by different parameters including the blade width, echo train length (ETL). This is explained by data oversampling at the center region of k-space, which requires additional imaging time over conventional MRI techniques. Increasing blade was expected to improve motion correction effects but also the signal-to-noise ratio. ETL increases the image sharpness and the overall image quality. Copyright © 2016. Published by Elsevier Inc.

  4. Simple determination of betaine, l-carnitine and choline in human urine using self-packed column and column-switching ion chromatography with nonsuppressed conductivity detection.

    PubMed

    Wei, Dan; Zhu, Yan; Guo, Ming

    2018-02-01

    A sequential online extraction, clean-up and separation system for the determination of betaine, l-carnitine and choline in human urine using column-switching ion chromatography with nonsuppressed conductivity detection was developed in this work. A self-packed pretreatment column (50 × 4.6 mm, i.d.) was used for the extraction and clean-up of betaine, l-carnitine and choline. The separation was achieved using self-packed cationic exchange column (150 × 4.6 mm, i.d.), followed by nonsuppressed conductivity detection. Under optimized experimental conditions, the developed method presented good analytical performance, with excellent linearity in the range of 0.60-100 μg mL -1 for betaine, 0.75-100 μg mL -1 for l-carnitine and 0.50-100 μg mL -1 for choline, with all correlation coefficients (R 2 ) >0.99 in urine. The limits of detection were 0.15 μg mL -1 for betaine, 0.20 μg mL -1 for l-carnitine and 0.09 μg mL -1 for choline. The intra- and inter-day accuracy and precision for all quality controls were within ±10.32 and ±9.05%, respectively. Satisfactory recovery was observed between 92.8 and 102.0%. The validated method was successfully applied to the detection of urinary samples from 10 healthy people. The values detected in human urine using the proposed method showed good agreement with the measurement reported previously. Copyright © 2017 John Wiley & Sons, Ltd.

  5. Sustained Benefit Lasting One Year from T4 Instead of T3-T4 Sympathectomy for Isolated Axillary Hyperhidrosis

    PubMed Central

    Munia, Marco Antonio S.; Wolosker, Nelson; Kaufmann, Paulo; de Campos, José Ribas Milanes; Puech-Leão, Pedro

    2008-01-01

    INTRODUCTION Level T4 video-assisted thoracoscopic sympathectomy proved superior to T3-T4 treatment for controlling axillary hyperhidrosis at the initial and six-month follow-ups of these patients. OBJECTIVE To compare the results of two levels of sympathectomy (T3-T4 vs. T4) for treating axillary sudoresis over one year of follow-up. METHODS Sixty-four patients with axillary hyperhidrosis were randomized to denervation of T3-T4 or T4 alone and followed prospectively. All patients were examined preoperatively and were followed postoperatively for one year. Axillary hyperhidrosis treatment was evaluated, along with the presence, location, and severity of compensatory hyperhidrosis and self-reported quality of life. RESULTS According to patient reports after one year, all cases of axillary hyperhidrosis were successfully treated by surgery. There were no instances of treatment failure. After six months, compensatory hyperhidrosis was present in 27 patients of the T3-T4 group (87.1%) and in 16 patients of the T4 group (48.5%). After one year, all T3-T4 patients experienced some degree of compensatory hyperhidrosis, compared to only 14 patients in the T4 group (42.4%). In addition, compensatory hyperhidrosis was less severe in the T4 patients (p < 0.01). Quality of life was poor before surgery, and it improved in both groups at six months and one year of follow-up (p = 0.002). There were no cases of mortality, no significant postoperative complications, and no need for conversion to thoracotomy in either group. CONCLUSION Both techniques were effective for treating axillary hyperhidrosis, but the T4 group showed milder compensatory hyperhidrosis and greater patient satisfaction at the one-year follow-up. PMID:19060999

  6. Simultaneous analysis method for GHB, ketamine, norketamine, phenobarbital, thiopental, zolpidem, zopiclone and phenytoin in urine, using C18 poroshell column.

    PubMed

    Anilanmert, Beril; Çavuş, Fatma; Narin, Ibrahim; Cengiz, Salih; Sertler, Şefika; Özdemir, Ali Acar; Açikkol, Münevver

    2016-06-01

    Date-rape drugs have the potential to be used in drug-facilitated sexual assault, organ theft and property theft. Since they are colorless, tasteless and odorless, victims can drink without noticing, when added to the beverages. These drugs must be detected in time, before they are cleared up from the biofluids. A simultaneous extraction and determination method in urine for GHB, ketamine, norketamine, phenobarbital, thiopental, zolpidem, zopiclone and phenytoin (an anticonvulsant and antiepileptic drug) with LC-MS/MS was developed for the first time with analytically acceptable recoveries and validated. A 4 steps liquid-liquid extraction was applied, using only 1.000mL urine. A new age commercial C18 poroshell column with high column efficiency was used for LC-MS/MS analysis with a fast isocratic elution as 5.5min. A new MS transition were introduced for barbital. 222.7>179.8 with the effect of acetonitrile. Recoveries (%) were between 80.98-99.27 for all analytes, except for GHB which was 71.46. LOD and LOQ values were found in the ranges of 0.59-49.50 and 9.20-80.80ngmL(-1) for all the analytes (except for GHB:3.44 and 6.00μgmL(-1)). HorRat values calculated (between 0.25-1.21), revealed that the inter-day and interanalist precisions (RSD%≤14.54%) acceptable. The simultaneous extraction and determination of these 8 analytes in urine is challenging because of the difficulty arising from the different chemical properties of some. Since the procedure can extract drugs from a wide range of polarity and pKa, it increases the window of detection. Group representatives from barbiturates, z-drugs, ketamine, phenytoin and polar acidic drugs (GHB) have been successfully analyzed in this study with low detection limits. The method is important from the point of determining the combined or single use of these drugs in crimes and finding out the reasons of deaths related to these drugs. Copyright © 2016 Elsevier B.V. All rights reserved.

  7. Confirmatory analysis of 17beta-boldenone, 17alpha-boldenone and androsta-1,4-diene-3,17-dione in bovine urine by liquid chromatography-tandem mass spectrometry.

    PubMed

    Draisci, Rosa; Palleschi, Luca; Ferretti, Emanuele; Lucentini, Luca; delli Quadri, Fernanda

    2003-06-15

    A sensitive and selective liquid chromatography-tandem mass spectrometry (LC-MS-MS) method for confirmatory analysis of 17beta-boldenone (17beta-BOL), 17alpha-boldenone (17alpha-BOL) and androsta-1,4-diene-3,17-dione (ADD) in bovine urine was developed. [2H(2)]17beta-Testosterone (17beta-T-d(2)) was used as the internal standard. Sample preparation involved enzymatic hydrolysis and purification on a C(18) solid-phase extraction column. Chromatographic separation of the analytes was obtained using an RP-C(18) HPLC column. LC-MS-MS detection was carried out with an atmospheric pressure chemical ionisation (APCI) source equipped with a heated nebulizer (HN) interface operating in the positive ion mode. For unambiguous hormone confirmation, three analyte precursor-product ion combinations were monitored during multiple-reaction monitoring (MRM) LC-MS-MS analysis. Overall recovery (%), repeatability (relative standard deviations, RSD, %) and within-laboratory reproducibility (RSD, %) ranged from 92.2 to 97.7%, from 6.50 to 2.94% and from 13.50 to 5.04%, respectively, for all analytes. The limit of quantification in bovine urine was 0.20 ng ml(-1) for 17beta-BOL and ADD and 0.50 ng ml(-1) for 17alpha-BOL. The validated method was successfully applied for determination of 17beta-BOL, 17alpha-BOL and ADD in a large number of bovine urine samples collected within the national Official Residue Control Program.

  8. SoilJ - An ImageJ plugin for semi-automatized image-processing of 3-D X-ray images of soil columns

    NASA Astrophysics Data System (ADS)

    Koestel, John

    2016-04-01

    3-D X-ray imaging is a formidable tool for quantifying soil structural properties which are known to be extremely diverse. This diversity necessitates the collection of large sample sizes for adequately representing the spatial variability of soil structure at a specific sampling site. One important bottleneck of using X-ray imaging is however the large amount of time required by a trained specialist to process the image data which makes it difficult to process larger amounts of samples. The software SoilJ aims at removing this bottleneck by automatizing most of the required image processing steps needed to analyze image data of cylindrical soil columns. SoilJ is a plugin of the free Java-based image-processing software ImageJ. The plugin is designed to automatically process all images located with a designated folder. In a first step, SoilJ recognizes the outlines of the soil column upon which the column is rotated to an upright position and placed in the center of the canvas. Excess canvas is removed from the images. Then, SoilJ samples the grey values of the column material as well as the surrounding air in Z-direction. Assuming that the column material (mostly PVC of aluminium) exhibits a spatially constant density, these grey values serve as a proxy for the image illumination at a specific Z-coordinate. Together with the grey values of the air they are used to correct image illumination fluctuations which often occur along the axis of rotation during image acquisition. SoilJ includes also an algorithm for beam-hardening artefact removal and extended image segmentation options. Finally, SoilJ integrates the morphology analyses plugins of BoneJ (Doube et al., 2006, BoneJ Free and extensible bone image analysis in ImageJ. Bone 47: 1076-1079) and provides an ASCII file summarizing these measures for each investigated soil column, respectively. In the future it is planned to integrate SoilJ into FIJI, the maintained and updated edition of ImageJ with selected

  9. Fast gradient screening of pharmaceuticals with 5 cm long, narrow bore reversed-phase columns packed with sub-3 μm core-shell and sub-2 μm totally porous particles.

    PubMed

    Fekete, Szabolcs; Fekete, Jeno

    2011-04-15

    The performance of 5 cm long narrow-bore columns packed with 2.6-2.7 μm core-shell particles and a column packed with 1.7 μm totally porous particles was compared in very fast gradient separations of polar neutral active pharmaceutical compounds. Peak capacities as a function of flow-rate and gradient time were measured. Peak capacities around 160-170 could be achieved within 25 min with these 5 cm long columns. The highest peak capacity was obtained with the Kinetex column however it was found that as the flow-rate increases, the peak capacity of the new Poroshell-120 column is getting closer to that obtained with the Kinetex column. Considering the column permeability, peak capacity per unit time and per unit pressure was also calculated. In this comparison the advantage of sub-3 μm core-shell particles is more significant compared to sub-2 μm totally porous particles. Moreover it was found that the very similar sized (d(p)=2.7 μm) and structured (ρ=0.63) new Poroshell-120 and the earlier introduced Ascentis Express particles showed different efficiency. Results obtained showed that the 5 cm long narrow bore columns packed with sub-3 μm core-shell particles offer the chance of very fast and efficient gradient separations, thus these columns can be applied for fast screening measurements of routine pharmaceutical analysis such as cleaning validation. Copyright © 2011 Elsevier B.V. All rights reserved.

  10. Pretreatment method for immunoassay of polychlorinated biphenyls in transformer oil using multilayer capillary column and microfluidic liquid-liquid partitioning.

    PubMed

    Aota, Arata; Date, Yasumoto; Terakado, Shingo; Ohmura, Naoya

    2013-01-01

    Polychlorinated biphenyls (PCBs) are persistent organic pollutants that are present in the insulating oil inside a large number of transformers. To aid in eliminating PCB-contaminated transformers, PCBs in oil need to be measured using a rapid and cost-effective analytical method. We previously reported a pretreatment method for the immunoassay of PCBs in oil using a large-scale multilayer column and a microchip with multiple microrecesses, which permitted concentrated solvent extraction. In this paper, we report on a more rapid and facile pretreatment method, without an evaporation process, by improving the column and the microchip. In a miniaturized column, the decomposition and separation of oil were completed in 2 min. PCBs can be eluted from the capillary column at concentrations seven-times higher than those from the previous column. The total volume of the microrecesses was increased by improving the microrecess structure, the enabling extraction of four-times the amount of PCBs achieved with the previous system. By interfacing the capillary column with the improved microchip, PCBs in the eluate from the column were extracted into dimethyl sulfoxide in microrecesses with high enrichment and without the need for evaporation. Pretreatment was completed within 20 min. The pretreated oil was analyzed using a flow-based kinetic exclusion immunoassay. The limit of detection of PCBs in oil was 0.15 mg kg(-1), which satisfies the criterion set in Japan of 0.5 mg kg(-1).

  11. Expression and Purification of Functional Ligand-binding Domains of T1R3 Taste Receptors

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Nie,Y.; Hobbs, J.; Vigues, S.

    2006-01-01

    Chemosensory receptors, including odor, taste, and vomeronasal receptors, comprise the largest group of G protein-coupled receptors (GPCRs) in the mammalian genome. However, little is known about the molecular determinants that are critical for the detection and discrimination of ligands by most of these receptors. This dearth of understanding is due in part to difficulties in preparing functional receptors suitable for biochemical and biophysical analyses. Here we describe in detail two strategies for the expression and purification of the ligand-binding domain of T1R taste receptors, which are constituents of the sweet and umami taste receptors. These class C GPCRs contain amore » large extracellular N-terminal domain (NTD) that is the site of interaction with most ligands and that is amenable to expression as a separate polypeptide in heterologous cells. The NTD of mouse T1R3 was expressed as two distinct fusion proteins in Escherichia coli and purified by column chromatography. Spectroscopic analysis of the purified NTD proteins shows them to be properly folded and capable of binding ligands. This methodology should not only facilitate the characterization of T1R ligand interactions but may also be useful for dissecting the function of other class C GPCRs such as the large family of orphan V2R vomeronasal receptors.« less

  12. Internet delivered question and answer column for patients with schizophrenia.

    PubMed

    Maijala, Riikka; Anttila, Minna; Koivunen, Marita; Pitkänen, Anneli; Kuosmanen, Lauri; Välimäki, Maritta

    2015-01-01

    The purpose of this study was to describe the use of an Internet delivered question and answer column among patients with schizophrenia. The column was developed for research purposes. The study sample consisted of patients (N = 100) admitted to acute inpatient psychiatric care in two hospital districts. Descriptive data were collected from the column to which a nurse replied within 3 days and analysed using qualitative content analysis. The column had four to five questions weekly. The most common age of users was 18-24 years, and the gender distribution was almost equal. Column use was heaviest among students (44%) and least among unemployed people (19%). Out of 85 questions or comments sent to the column, 25 (29%) were related to program training and the remaining 60 (71%) were related to medication (31%), illness and tests (25%), other questions or comments (9%), daily life and coping with it (4%), and places to receive treatment (2%). An Internet delivered question and answer column can be included in the care of patients with schizophrenia. However, it requires a new type of basic and additional education in the field of mental health care in order for nurses to be able to provide nursing via the Internet forum.

  13. Osteoblast-like MC3T3-E1 Cells Prefer Glycolysis for ATP Production but Adipocyte-like 3T3-L1 Cells Prefer Oxidative Phosphorylation.

    PubMed

    Guntur, Anyonya R; Gerencser, Akos A; Le, Phuong T; DeMambro, Victoria E; Bornstein, Sheila A; Mookerjee, Shona A; Maridas, David E; Clemmons, David E; Brand, Martin D; Rosen, Clifford J

    2018-06-01

    Mesenchymal stromal cells (MSCs) are early progenitors that can differentiate into osteoblasts, chondrocytes, and adipocytes. We hypothesized that osteoblasts and adipocytes utilize distinct bioenergetic pathways during MSC differentiation. To test this hypothesis, we compared the bioenergetic profiles of preosteoblast MC3T3-E1 cells and calvarial osteoblasts with preadipocyte 3T3L1 cells, before and after differentiation. Differentiated MC3T3-E1 osteoblasts met adenosine triphosphate (ATP) demand mainly by glycolysis with minimal reserve glycolytic capacity, whereas nondifferentiated cells generated ATP through oxidative phosphorylation. A marked Crabtree effect (acute suppression of respiration by addition of glucose, observed in both MC3T3-E1 and calvarial osteoblasts) and smaller mitochondrial membrane potential in the differentiated osteoblasts, particularly those incubated at high glucose concentrations, indicated a suppression of oxidative phosphorylation compared with nondifferentiated osteoblasts. In contrast, both nondifferentiated and differentiated 3T3-L1 adipocytes met ATP demand primarily by oxidative phosphorylation despite a large unused reserve glycolytic capacity. In sum, we show that nondifferentiated precursor cells prefer to use oxidative phosphorylation to generate ATP; when they differentiate to osteoblasts, they gain a strong preference for glycolytic ATP generation, but when they differentiate to adipocytes, they retain the strong preference for oxidative phosphorylation. Unique metabolic programming in mesenchymal progenitor cells may influence cell fate and ultimately determine the degree of bone formation and/or the development of marrow adiposity. © 2018 American Society for Bone and Mineral Research. © 2018 American Society for Bone and Mineral Research.

  14. What we-authors, reviewers and editors of scientific work-can learn from the analytical history of biological 3-nitrotyrosine.

    PubMed

    Tsikas, Dimitrios

    2017-07-15

    Tyrosine and tyrosine residues in proteins are attacked by the reactive oxygen and nitrogen species peroxynitrite (O=N-OO - ) to generate 3-nitrotyrosine (3-NT) and 3-nitrotyrosine-proteins (3-NTProt), respectively. 3-NT and 3-NTProt are widely accepted as biomarkers of nitr(os)ative stress. Over the years many different analytical methods have been reported for 3-NT and 3-NTProt. Reported concentrations often differ by more than three orders of magnitude, indicative of serious analytical problems. Strategies to overcome pre-analytical and analytical shortcomings and pitfalls have been proposed. The present review investigated whether recently published work on the quantitative measurement of biological 3-nitrotyrosine did adequately consider the analytical past of this biomolecule. 3-Nitrotyrosine was taken as a representative of biomolecules that occur in biological samples in the pM-to-nM concentration range. This examination revealed that in many cases the main protagonists involved in the publication of scientific work, i.e., authors, reviewers and editors, failed to do so. Learning from the analytical history of 3-nitrotyrosine means advancing analytical and biological science and implies the following key issues. (1) Choosing the most reliable analytical approach in terms of sensitivity and accuracy; presently this is best feasible by stable-isotope dilution tandem mass spectrometry coupled with gas chromatography (GC-MS/MS) or liquid chromatography (LC-MS/MS). (2) Minimizing artificial formation of 3-nitrotyrosine during sample work up, a major pitfall in 3-nitrotyrosine analysis. (3) Validating adequately the final method in the intendent biological matrix and the established concentration range. (4) Inviting experts in the field for critical evaluation of the novelty and reliability of the proposed analytical method, placing special emphasis on the compliance of the analytical outcome with 3-nitrotyrosine concentrations obtained by validated GC-MS/MS and

  15. Compact electron beam focusing column

    NASA Astrophysics Data System (ADS)

    Persaud, Arun; Leung, Ka-Ngo; Reijonen, Jani

    2001-12-01

    A novel design for an electron beam focusing column has been developed at LBNL. The design is based on a low-energy spread multicusp plasma source which is used as a cathode for electron beam production. The focusing column is 10 mm in length. The electron beam is focused by means of electrostatic fields. The column is designed for a maximum voltage of 50 kV. Simulations of the electron trajectories have been performed by using the 2D simulation code IGUN and EGUN. The electron temperature has also been incorporated into the simulations. The electron beam simulations, column design and fabrication will be discussed in this presentation.

  16. CD4+CD62L+ Central Memory T Cells Can Be Converted to Foxp3+ T Cells

    PubMed Central

    Zhang, Xiaolong; Chang Li, Xian; Xiao, Xiang; Sun, Rui; Tian, Zhigang; Wei, Haiming

    2013-01-01

    The peripheral Foxp3+ Treg pool consists of naturally arising Treg (nTreg) and adaptive Treg cells (iTreg). It is well known that naive CD4+ T cells can be readily converted to Foxp3+ iTreg in vitro, and memory CD4+ T cells are resistant to conversion. In this study, we investigated the induction of Foxp3+ T cells from various CD4+ T-cell subsets in human peripheral blood. Though naive CD4+ T cells were readily converted to Foxp3+ T cells with TGF-β and IL-2 treatment in vitro, such Foxp3+ T cells did not express the memory marker CD45RO as do Foxp3+ T cells induced in the peripheral blood of Hepatitis B Virus (HBV) patients. Interestingly, a subset of human memory CD4+ T cells, defined as CD62L+ central memory T cells, could be induced by TGF-β to differentiate into Foxp3+ T cells. It is well known that Foxp3+ T cells derived from human CD4+CD25- T cells in vitro are lack suppressive functions. Our data about the suppressive functions of CD4+CD62L+ central memory T cell-derived Foxp3+ T cells support this conception, and an epigenetic analysis of these cells showed a similar methylation pattern in the FOXP3 Treg-specific demethylated region as the naive CD4+ T cell-derived Foxp3+ T cells. But further research showed that mouse CD4+ central memory T cells also could be induced to differentiate into Foxp3+ T cells, such Foxp3+ T cells could suppress the proliferation of effector T cells. Thus, our study identified CD4+CD62L+ central memory T cells as a novel potential source of iTreg. PMID:24155942

  17. Reconstruction of Thoracic Spine Using a Personalized 3D-Printed Vertebral Body in Adolescent with T9 Primary Bone Tumor.

    PubMed

    Choy, Wen Jie; Mobbs, Ralph J; Wilcox, Ben; Phan, Steven; Phan, Kevin; Sutterlin, Chester E

    2017-09-01

    Neurosurgery and spine surgery have the potential to benefit from the use of 3-dimensional printing (3DP) technology due to complex anatomic considerations and the delicate nature of surrounding structures. We report a procedure that uses a 3D-printed titanium T9 vertebral body implant post T9 vertebrectomy for a primary bone tumor. A 14-year-old female presented with progressive kyphoscoliosis and a pathologic fracture of the T9 vertebra with sagittal and coronal deformity due to a destructive primary bone tumor. Surgical resection and reconstruction was performed in combination with a 3D-printed, patient-specific implant. Custom design features included porous titanium end plates, corrective angulation of the implant to restore sagittal balance, and pedicle screw holes in the 3D implant to assist with insertion of the device. In addition, attachment of the anterior column construct to the posterior pedicle screw construct was possible due to the customized features of the patient-specific implant. An advantage of 3DP is the ability to manufacture patient-specific implants, as in the current case example. Additionally, the use of 3DP has been able to reduce operative time significantly. Surgical procedures can be preplanned using 3DP patient-specific models. Surgeons can train before performing complex procedures, which enhances their presurgical planning in order to maximize patient outcomes. When considering implants and prostheses, the use of 3DP allows a superior anatomic fit for the patient, with the potential to improve restoration of anatomy. Copyright © 2017 Elsevier Inc. All rights reserved.

  18. Magnetic resonance spectroscopy of the canine brain at 3.0 T and 7.0 T.

    PubMed

    Martin-Vaquero, Paula; da Costa, Ronaldo C; Echandi, Rita L; Sammet, Christina L; Knopp, Michael V; Sammet, Steffen

    2012-08-01

    The purpose of this study was to evaluate the feasibility of proton magnetic resonance spectroscopy (1H MRS) to study the concentration of metabolites in the brain of dogs at 3.0 and 7.0 T. Four healthy male beagles were scanned using 3.0 T and 7.0 T human magnetic resonance imaging (MRI) units. The results obtained showed that all dogs had excellent quality spectra for a small (1 cm3) and large (8 cm3) voxel at 3.0 T, whereas only 2 dogs had high quality spectra at 7.0 T due to insufficient water suppression. 1H MRS at 3.0 T appears to be a reliable method to study metabolite concentrations in the canine brain. The development of more advanced water suppression techniques is necessary to improve the results at 7.0 T. Copyright © 2011 Elsevier Ltd. All rights reserved.

  19. A method for determining the column curve from tests of columns with equal restraints against rotation on the ends

    NASA Technical Reports Server (NTRS)

    Lundquist, Eugene E; Rossman, Carl A; Houbolt, John C

    1943-01-01

    The results are presented of a theoretical study for the determination of the column curve from tests of column specimens having ends equally restrained against rotation. The theory of this problem is studied and a curve is shown relating the fixity coefficient c to the critical load, the length of the column, and the magnitude of the elastic restraint. A method of using this curve for the determination of the column curve for columns with pin ends from tests of columns with elastically restrained ends is presented. The results of the method as applied to a series of tests on thin-strip columns of stainless steel are also given.

  20. Lysophosphatidic acid receptor-5 negatively regulates cellular responses in mouse fibroblast 3T3 cells

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Dong, Yan; Hirane, Miku; Araki, Mutsumi

    2014-04-04

    Highlights: • LPA{sub 5} inhibits the cell growth and motile activities of 3T3 cells. • LPA{sub 5} suppresses the cell motile activities stimulated by hydrogen peroxide in 3T3 cells. • Enhancement of LPA{sub 5} on the cell motile activities inhibited by LPA{sub 1} in 3T3 cells. • The expression and activation of Mmp-9 were inhibited by LPA{sub 5} in 3T3 cells. • LPA signaling via LPA{sub 5} acts as a negative regulator of cellular responses in 3T3 cells. - Abstract: Lysophosphatidic acid (LPA) signaling via G protein-coupled LPA receptors (LPA{sub 1}–LPA{sub 6}) mediates a variety of biological functions, including cellmore » migration. Recently, we have reported that LPA{sub 1} inhibited the cell motile activities of mouse fibroblast 3T3 cells. In the present study, to evaluate a role of LPA{sub 5} in cellular responses, Lpar5 knockdown (3T3-L5) cells were generated from 3T3 cells. In cell proliferation assays, LPA markedly stimulated the cell proliferation activities of 3T3-L5 cells, compared with control cells. In cell motility assays with Cell Culture Inserts, the cell motile activities of 3T3-L5 cells were significantly higher than those of control cells. The activity levels of matrix metalloproteinases (MMPs) were measured by gelatin zymography. 3T3-L5 cells stimulated the activation of Mmp-2, correlating with the expression levels of Mmp-2 gene. Moreover, to assess the co-effects of LPA{sub 1} and LPA{sub 5} on cell motile activities, Lpar5 knockdown (3T3a1-L5) cells were also established from Lpar1 over-expressing (3T3a1) cells. 3T3a1-L5 cells increased the cell motile activities of 3T3a1 cells, while the cell motile activities of 3T3a1 cells were significantly lower than those of control cells. These results suggest that LPA{sub 5} may act as a negative regulator of cellular responses in mouse fibroblast 3T3 cells, similar to the case for LPA{sub 1}.« less

  1. Capillary Flow in an Interior Corner

    NASA Technical Reports Server (NTRS)

    Weislogel, Mark Milton

    1996-01-01

    The design of fluids management processes in the low-gravity environment of space requires an accurate model and description of capillarity-controlled flow in containers of irregular geometry. Here we consider the capillary rise of a fluid along an interior corner of a container following a rapid reduction in gravity. The analytical portion of the work presents an asymptotic formulation in the limit of a slender fluid column, slight surface curvature along the corner, small inertia, and low gravity. New similarity solutions are found and a list of closed form expressions is provided for flow rate and column length. In particular, it is found that the flow is proportional to t(exp 1/2) for a constant height boundary condition, t(exp 2/5) for a spreading drop, and t(exp 3/5) for constant flow. In the experimental portion of the work, measurements from a 2.2s drop tower are reported. An extensive data set, collected over a previously unexplored range of flow parameters, includes estimates of repeatability and accuracy, the role of inertia and column slenderness, and the effects of corner angle, container geometry, and fluid properties. Comprehensive comparisons are made which illustrate the applicability of the analytic results to low-g fluid systems design.

  2. "In situ" extraction of essential oils by use of Dean-Stark glassware and a Vigreux column inside a microwave oven: a procedure for teaching green analytical chemistry.

    PubMed

    Chemat, Farid; Perino-Issartier, Sandrine; Petitcolas, Emmanuel; Fernandez, Xavier

    2012-08-01

    One of the principal objectives of sustainable and green processing development remains the dissemination and teaching of green chemistry in colleges, high schools, and academic laboratories. This paper describes simple glassware that illustrates the phenomenon of extraction in a conventional microwave oven as energy source and a process for green analytical chemistry. Simple glassware comprising a Dean-Stark apparatus (for extraction of aromatic plant material and recovery of essential oils and distilled water) and a Vigreux column (as an air-cooled condenser inside the microwave oven) was designed as an in-situ extraction vessel inside a microwave oven. The efficiency of this experiment was validated for extraction of essential oils from 30 g fresh orange peel, a by-product in the production of orange juice. Every laboratory throughout the world can use this equipment. The microwave power is 100 W and the irradiation time 15 min. The method is performed at atmospheric pressure without added solvent or water and furnishes essential oils similar to those obtained by conventional hydro or steam distillation. By use of GC-MS, 22 compounds in orange peel were separated and identified; the main compounds were limonene (72.1%), β-pinene (8.4%), and γ-terpinene (6.9%). This procedure is appropriate for the teaching laboratory, does not require any special microwave equipment, and enables the students to learn the skills of extraction, and chromatographic and spectroscopic analysis. They are also exposed to a dramatic visual example of rapid, sustainable, and green extraction of an essential oil, and are introduced to successful sustainable and green analytical chemistry.

  3. Characterisation of RPLC columns packed with porous sub-2 microm particles.

    PubMed

    Petersson, Patrik; Euerby, Melvin R

    2007-08-01

    Eight commercially available sub-2 microm octadecyl silane columns (C18 columns) have been characterised by the Tanaka protocol. The columns can be grouped into two groups that display large differences in selectivity and peak shape due to differences in hydrophobicity, degree of surface coverage and silanol activity. Measurements of particle size distributions were made using automated microscopy and electrical sensing zone measurements. Only a weak correlation could be found between efficiency and particle size. Large differences in column backpressure were observed. These differences are not related to particle size distribution. A more likely explanation is differences in packing density. In order to take full advantage of 100-150 mm columns packed with sub-2 microm particles, it is often necessary to employ not only an elevated pressure but also an elevated temperature. A comparison between columns packed with sub-2, 3 and 5 microm versions of the same packing indicates potential method transferability problems for several of the columns due to selectivity differences. Currently, the best alternative for fast high-resolution LC is the use of sub-2 microm particles in combination with elevated pressure and temperature. However, as shown in this study additional efforts are needed to improve transferability as well as column performance.

  4. Time-lapse 3D imaging of calcite precipitation in a microporous column

    NASA Astrophysics Data System (ADS)

    Godinho, Jose R. A.; Withers, Philip J.

    2018-02-01

    Time-lapse X-ray computed tomography is used to image the evolution of calcite precipitation during flow through microporous quartz over the course of 400 h. The growth rate decreases by more than seven times, which is linked to the clogging of flow paths that restricts flow to some regions of the column. Fewer precipitates are observed as a function of column depth, which is found to be related to a differential nucleation density along the sample. A higher nucleation density closer to the inlet implies more crystal volume increase per unit of time without affecting the rate if normalized to the surface area of crystals. Our overall growth rates measured in porous media are orders of magnitude slower than growth rates derived from traditional precipitation experiments on free surfaces. Based on our time-lapse results we hypothesize a scenario where the evolving distribution of precipitates within a pore structure during precipitation progressively modifies the local transport through the pores. Within less permeable regions the saturation index may be lower than along the main flow paths. Therefore, the reactive crystal surfaces within those regions grow at a slower rate than that expected from the bulk fluid composition. Since the amount of reactive surface area within these less permeable regions increases over time, the overall growth rate decreases without a necessary significant change of the bulk fluid composition along more permeable flow paths. In conclusion, the overall growth rates in an evolving porous media expected from bulk fluid compositions alone can be overestimated due to the development of stagnant sub-regions where the reactive surface area is bath by a solution with lower saturation index. In this context we highlight the value of time-lapse 3D studies for understanding the dynamics of mineral precipitation in porous media.

  5. High-capacity cation-exchange column for enhanced resolution of adjacent peaks of cations in ion chromatography.

    PubMed

    Rey, M A

    2001-06-22

    One of the advantages of ion chromatography [Anal Chem. 47 (1975) 1801] as compared to other analytical techniques is that several ions may be analyzed simultaneously. One of the most important contributions of cation-exchange chromatography is its sensitivity to ammonium ion, which is difficult to analyze by other techniques [J. Weiss, in: E.L. Johnson (Ed.), Handbook of Ion Chromatography, Dionex, Sunnyvale, CA, USA]. The determination of low concentrations of ammonium ion in the presence of high concentrations of sodium poses a challenge in cation-exchange chromatography [J. Weiss, Ion Chromatography, VCH, 2nd Edition, Weinheim, 1995], as both cations have similar selectivities for the common stationary phases containing either sulfonate or carboxylate functional groups. The task was to develop a new cation-exchange stationary phase (for diverse concentration ratios of adjacent peaks) to overcome limitations experienced in previous trails. Various cation-exchange capacities and column body formats were investigated to optimize this application and others. The advantages and disadvantages of two carboxylic acid columns of different cation-exchange capacities and different column formats will be discussed.

  6. New York State Department of Environmental Conservation PAMS monitoring system using a 3-column, double identification GC

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Sierzenga, P.M.; Boynton, G.A.; Aho, B.J.

    1996-12-31

    New York State conducted its 1995 PAMS measurements for New York City in the Bronx borough (New York Botanical Gardens) using a Perkin-Elmer ATD-400 Thermal Desorbtion Unit with an 8000 Series Gas Chromatograph. Data was collected in New York City, transferred to Albany, and processed in the central office. The system was checked on a daily basis from Albany to verify operation. Quality assurance for the system was provided by collecting a one hour collocated canister sample every day with analysis performed in Albany using a GC-MS system. The normal configuration for the Perkin-Elmer system uses only two columns, amore » PLOT column to separate low weight hydrocarbons (C{sub 2}-C{sub 5}) and a BP-1 column to separate higher weight hydrocarbons (C{sub 6}-C{sub 10}). New York`s custom designed system uses a third RTX-5 column to provide a second identification and quantitation of most target hydrocarbons. Analysis of the 1995 data provides insight into the usefulness of the third column in correcting both misidentified peaks and over-quantification of compound concentrations found using the standard configuration alone. The 1995 data set also allows an examination of the increased complexity versus the benefits of the system modification. 6 figs., 1 tab.« less

  7. Evaluating the precision of passive sampling methods using PRCs in the water column.

    EPA Science Inventory

    To assess these models, four different thicknesses of low-density polyethylene (LDPE) passive samplers were co-deployed for 28 days in the water column at three sites in New Bedford Harbor, MA, USA. Each sampler was pre-loaded with six PCB performance reference compounds (PRCs) t...

  8. Determination of phenylenediamine isomers in hair dyes by coal cinders micro-column extraction and MEKC.

    PubMed

    Wu, Yiwei; Jiang, Feng; Chen, Lin; Zheng, Jing; Deng, Zhenli; Tao, Qing; Zhang, Jing; Han, Lijuan; Wei, Xiaoshu; Yu, Aimin; Zhang, Haili

    2011-06-01

    A new micellar electrokinetic chromatography (MEKC) method using beta-cyclodextrins (β-CDs) and 1-butyl-3-methylimidazolium hexafluorophosphates (ionic liquids) as additives was successfully developed for determination of para-, meta-, and ortho-phenylenediamines isomers (p-P, m-P, and o-P) in hair dyes. To improve the sensitivity of the MEKC-UV, a simple and cheap flow injection (FI) technique using a micro-column packed with coal cinders (the by-products from combustion in a boiler) as solid-phase extractant was also investigated. In the presence of 20 mmol L(-1) phosphates at pH 5.5, addition of 12 mmol L(-1) ionic liquids and 8 mmol L(-1) β-CDs greatly improved the separation efficiency. The three analytes could be quantitatively adsorbed by coal cinders, and desorbed readily with 0.15 mL of 0.01 mol L(-1) NaOH. Under the optimum conditions, an enrichment factor (EF) of 33.3 was obtained, and determination limits of p-P, m-P, and o-P were 1.97 × 10(-7), 0.99 × 10(-7), and 0.61 × 10(-7) mol L(-1), respectively. The adsorption capacities of the coal cinders micro-column for p-P, m-P, and o-P were all 1.20 mg g(-1). The presented procedure was successfully applied to the determination of p-P, m-P, and o-P in hair dyes with satisfactory results.

  9. Low-Level Analytical Methodology Updates to Support Decontaminant Performance Evaluations

    DTIC Science & Technology

    2011-06-01

    from EPDM and tire rubber coupon materials that were spiked with a known amount of the chemical agent VX, treated with bleach decontaminant, and...to evaluate the performance of bleach decontaminant on EPDM and tire rubber coupons. Dose-confirmation or Tool samples were collected by delivering...components • An aging or damaged analytical column • Dirty detector • Other factors related to general instrument and/or sample analysis performance

  10. Reaction of the thermo-labile triazenide Na[tBu3SiNNNSiMe3] with CO2: formation of the imido carbonate (tBu3SiO)(Me3SiO)C[double bond, length as m-dash]N-SitBu3 and carbamine acid (tBu3SiO)CONH2.

    PubMed

    Lerner, H-W; Bolte, M; Wagner, M

    2017-07-11

    The thermo-labile triazenide Na[tBu 3 SiNNNSiMe 3 ] was prepared by the reaction of Me 3 SiN 3 with Na(thf) 2 [SitBu 3 ] in pentane at -78 °C. Treatment of Na[tBu 3 SiNNNSiMe 3 ] with an excess of carbon dioxide in pentane at -78 °C yielded the imido carbonate (tBu 3 SiO)(Me 3 SiO)C[double bond, length as m-dash]N-SitBu 3 and the carbamine acid (tBu 3 SiO)CONH 2 along with other products. From the reaction solution we could isolate the imido carbonate (tBu 3 SiO)(Me 3 SiO)C[double bond, length as m-dash]N-SitBu 3 and carbamine acid (tBu 3 SiO)CONH 2 . At first single crystals of the carbamine acid (tBu 3 SiO)CONH 2 (triclinic, space group P1[combining macron]) were grown from this solution at room temperature. A second crop of crystals were obtained by concentrating the solution. The second charge consisted of the imido carbonate (tBu 3 SiO)(Me 3 SiO)C[double bond, length as m-dash]N-SitBu 3 (monoclinic, space group P2 1 /n).

  11. Adjustable bias column end joint assembly

    NASA Technical Reports Server (NTRS)

    Wallsom, Richard E. (Inventor); Bush, Harold G. (Inventor)

    1994-01-01

    An adjustable mechanical end joint system for connecting structural column elements and eliminating the possibility of free movement between joint halves during loading or vibration has a node joint body having a cylindrical engaging end and a column end body having a cylindrical engaging end. The column end joint body has a compressible preload mechanism and plunger means housed therein. The compressible preload mechanism may be adjusted from the exterior of the column end joint body through a port.

  12. Forced degradation and impurity profiling: recent trends in analytical perspectives.

    PubMed

    Jain, Deepti; Basniwal, Pawan Kumar

    2013-12-01

    This review describes an epigrammatic impression of the recent trends in analytical perspectives of degradation and impurities profiling of pharmaceuticals including active pharmaceutical ingredient (API) as well as drug products during 2008-2012. These recent trends in forced degradation and impurity profiling were discussed on the head of year of publication; columns, matrix (API and dosage forms) and type of elution in chromatography (isocratic and gradient); therapeutic categories of the drug which were used for analysis. It focuses distinctly on comprehensive update of various analytical methods including hyphenated techniques for the identification and quantification of thresholds of impurities and degradants in different pharmaceutical matrices. © 2013 Elsevier B.V. All rights reserved.

  13. Clinical radiobiology of stage T2-T3 bladder cancer.

    PubMed

    Majewski, Wojciech; Maciejewski, Boguslaw; Majewski, Stanislaw; Suwinski, Rafal; Miszczyk, Leszek; Tarnawski, Rafal

    2004-09-01

    To evaluate the relationship between total radiation dose and overall treatment time (OTT) with the treatment outcome, with adjustment for selected clinical factors, in patients with Stage T2-T3 bladder cancer treated with curative radiotherapy (RT). The analysis was based on 480 patients with Stage T2-T3 bladder cancer who were treated at the Center of Oncology in Gliwice between 1975 and 1995. The mean total radiation dose was 65.5 Gy, and the mean OTT was 51 days. In 261 patients (54%), planned and unplanned gaps occurred during RT. Four fractionation schedules were used: (1) conventional fractionation (once daily, 1.8-2.5 Gy/fraction); (2) protracted fractionation (pelvic RT, once daily, 1.6-1.7 Gy/fraction, boost RT, once daily, 2.0 Gy/fraction); (3) accelerated hyperfractionated boost (pelvic RT, once daily, 2.0 Gy/fraction; boost RT, twice daily, 1.3-1.4 Gy/fraction); and (4) accelerated hyperfractionation (pelvic and boost RT, twice daily, 1.2-1.5 Gy/fraction). In all fractionation schedules, the total radiation dose was similar (average 65.5 Gy), but the OTT was different (mean 53 days for conventional fractionation, 62 days for protracted fractionation, 45 days for accelerated hyperfractionated boost, and 41 days for accelerated hyperfractionation). A Cox proportional hazard model and maximum likelihood logistic model were used to evaluate the relationship between the treatment-related parameters (total radiation dose, dose per fraction, and OTT) and clinical factors (clinical T stage, hemoglobin level and bladder capacity before RT) and treatment outcome. With a median follow-up of 76 months, the actuarial 5-year local control rate was 47%, and the overall survival rate was 40%. The logistic analysis, which included the total dose, OTT, and T stage, revealed that all of these factors were significantly related to tumor control probability (p = 0.021 for total radiation dose, p = 0.038 for OTT, and p = 0.00068 for T stage). A multivariate Cox model, which

  14. Solid-phase extraction and on-disc derivatization of the major benzodiazepines in urine using enzyme hydrolysis and Toxi-Lab VC MP3 column.

    PubMed

    King, J W; King, L J

    1996-01-01

    Because of the increase in use of the newer benzodiazepines, we explored the opportunity to develop a gas chromatographic-mass spectrometric (GC-MS) method that encompasses most of the widely prescribed benzodiazepines in use today. The benzodiazepines included in our study are nordiazepam, oxazepam, temazepam, lorazepam, alpha-hydroxyalprazolam, alpha-hydroxytriazolam, desalkylflurazepam, and 2-hydroxyethylflurazepam. Using 1.0 mL of urine as the matrix, we added the enzyme Glusulase and incubated the specimens for 2 h to obtain the free drugs. The hydrolyzed samples were then loaded onto a Toxi-Lab Spec VC MP3 column containing a 15-mg disc. On-disc derivatization was accomplished by adding N-methyl-N-(t-butyldimethylsilyl) trifluroacetamide (MTBSTFA) with 1% TBDMSCI to the disc. The derivatives were then placed in a GC vial and analyzed by GC-MS in the selected ion monitoring mode. These results were then compared to confirmed positives by the traditional acid hydrolysis GC-MS method.

  15. Foxp3+ regulatory T cells impede the priming of protective CD8+ T cells

    PubMed Central

    Ertelt, James M.; Rowe, Jared H.; Mysz, Margaret A.; Singh, Charanjeet; Roychowdhury, Monika; Aguilera, Marijo N.; Way, Sing Sing

    2011-01-01

    T cell activation is controlled by incompletely defined opposing stimulation and suppression signals that together sustain the balance between optimal host defense against infection and peripheral tolerance. Herein, we explored the impacts of Foxp3+ regulatory T cell (Treg) suppression in priming antigen-specific T cell activation under non-infection and infection conditions. We find the transient ablation of Foxp3+ Tregs unleashes the robust expansion and activation of peptide stimulated CD8+ T cells that provide protection against Listeria monocytogenes (Lm) infection in an antigen-specific fashion. By contrast, Treg-ablation had non-significant impacts on the CD8+ T cell response primed by infection with recombinant Lm. Similarly, non-recombinant Lm administered with peptide stimulated the expansion and activation of CD8+ T cells that paralleled the response primed by Treg-ablation. Interestingly, these adjuvant properties of Lm did not require CD8+ T cell stimulation by IL-12 produced in response to infection, but instead were associated with sharp reductions in Foxp3+ Treg suppressive potency. Therefore, Foxp3+ Tregs impose critical barriers that when overcome naturally during infection or artificially with ablation allows the priming of protective antigen-specific CD8+ T cells. PMID:21810602

  16. PULSE COLUMN

    DOEpatents

    Grimmett, E.S.

    1964-01-01

    This patent covers a continuous countercurrent liquidsolids contactor column having a number of contactor states each comprising a perforated plate, a layer of balls, and a downcomer tube; a liquid-pulsing piston; and a solids discharger formed of a conical section at the bottom of the column, and a tubular extension on the lowest downcomer terminating in the conical section. Between the conical section and the downcomer extension is formed a small annular opening, through which solids fall coming through the perforated plate of the lowest contactor stage. This annular opening is small enough that the pressure drop thereacross is greater than the pressure drop upward through the lowest contactor stage. (AEC)

  17. Measurement of the eddy diffusion term in chromatographic columns. I. Application to the first generation of 4.6mm I.D. monolithic columns.

    PubMed

    Gritti, Fabrice; Guiochon, Georges

    2011-08-05

    The corrected heights equivalent to a theoretical plate (HETP) of three 4.6mm I.D. monolithic Onyx-C(18) columns (Onyx, Phenomenex, Torrance, CA) of different lengths (2.5, 5, and 10 cm) are reported for retained (toluene, naphthalene) and non-retained (uracil, caffeine) small molecules. The moments of the peak profiles were measured according to the accurate numerical integration method. Correction for the extra-column contributions was systematically applied. The peak parking method was used in order to measure the bulk diffusion coefficients of the sample molecules, their longitudinal diffusion terms, and the eddy diffusion term of the three monolithic columns. The experimental results demonstrate that the maximum efficiency was 60,000 plates/m for retained compounds. The column length has a large impact on the plate height of non-retained species. These observations were unambiguously explained by a large trans-column eddy diffusion term in the van Deemter HETP equation. This large trans-rod eddy diffusion term is due to the combination of a large trans-rod velocity bias (≃3%), a small radial dispersion coefficient in silica monolithic columns, and a poorly designed distribution and collection of the sample streamlets at the inlet and outlet of the monolithic rod. Improving the performance of large I.D. monolithic columns will require (1) a detailed knowledge of the actual flow distribution across and along these monolithic rod and (2) the design of appropriate inlet and outlet distributors designed to minimize the nefarious impact of the radial flow heterogeneity on band broadening. Copyright © 2011 Elsevier B.V. All rights reserved.

  18. Behaviour of Reinforced Concrete Columns of Various Cross-Sections Subjected to Fire

    NASA Astrophysics Data System (ADS)

    Balaji, Aneesha; Muhamed Luquman, K.; Nagarajan, Praveen; Madhavan Pillai, T. M.

    2016-09-01

    Fire resistance is one of the crucial design regulations which are now mandatory in most of the design codes. Therefore, a thorough knowledge of behaviour of structures exposed to fire is required in this aspect. Columns are the most vulnerable structural member to fire as it can be exposed to fire from all sides. However, the data available for fire resistant design for columns are limited. Hence the present work is focused on the effect of cross-sectional shape of column in fire resistance design. The various cross-sections considered are Square, Ell (L), Tee (T), and Plus (`+') shape. Also the effect of size and shape and distribution of steel reinforcement on fire resistance of columns is studied. As the procedure for determining fire resistance is not mentioned in Indian Standard code IS 456 (2000), the simplified method (500 °C isotherm method) recommended in EN 1992-1-2:2004 (E) (Eurocode 2) is adopted. The temperature profiles for various cross-sections are developed using finite element method and these profiles are used to predict fire resistance capability of compression members. The fire resistance based on both numerical and code based methods are evaluated and compared for various types of cross-section.

  19. Status of the KM3NeT project

    NASA Astrophysics Data System (ADS)

    Margiotta, A.

    2014-04-01

    KM3NeT is a deep-sea research infrastructure being constructed in the Mediterranean Sea. It will be installed at three sites: KM3NeT-Fr, offshore Toulon, France, KM3NeT-It, offshore Portopalo di Capo Passero, Sicily (Italy) and KM3NeT-Gr, offshore Pylos, Peloponnese, Greece. It will host the next generation Cherenkov neutrino telescope and nodes for a deep sea multidisciplinary observatory, providing oceanographers, marine biologists, and geophysicists with real time measurements. The neutrino telescope will search for Galactic and extra-Galactic sources of neutrinos, complementing IceCube in its field of view. The detector will have a modular structure and consists of six building blocks, each including about one hundred Detection Units (DUs). Each DU will be equipped with 18 multi-PMT digital optical modules. The first phase of construction has started and shore and deep-sea infrastructures hosting the future KM3NeT detector are being prepared in France near Toulon and in Italy, near Capo Passero in Sicily. The technological solutions for KM3NeT and the expected performance of the detector are presented and discussed.

  20. Determination of pesticides in composite dietary samples by gas chromatography/mass spectrometry in the selected ion monitoring mode by using a temperature-programmable large volume injector with preseparation column.

    PubMed

    Rosenblum, L; Hieber, T; Morgan, J

    2001-01-01

    Use of a temperature-programmable preseparation column in the gas chromatographic (GC) injection port permits determination of a wide range of semi-volatile pesticides including organochlorines, organophosphates, triazines, and anilines in fatty composite dietary samples while reducing sample preparation time and solvent consumption. Dietary samples are mixed with diatomaceous earth and are Soxhlet-extracted with an azeotropic solution of hexane and acetone. Sample preparation uses liquid-liquid partitioning over diatomaceous earth followed by normal phase chromatography over partially deactivated alumina. The final cleanup step occurs in a preseparation column in the GC injector, which is able to perform splitless transfer of the analytes to the analytical column and purge 99% of the high molecular weight residue. Detection is performed by GC/mass spectrometry (MS) in the selected ion monitoring mode. Method detection limits were at or below 2 ng/g for 24 of 35 pesticides studied, with recovery between 70 and 125% for 27 pesticides in samples fortified at 10 ng/g. Recovery was not dependent on fat content when measured in laboratory fortified samples containing 1, 5, and 10% fat by weight. Precision over multiple injections was acceptable, with a relative standard deviation of 2.6-15% for 25 analytes.

  1. Determination of carotenoids in Taraxacum formosanum by HPLC-DAD-APCI-MS and preparation by column chromatography.

    PubMed

    Kao, T H; Loh, C H; Inbaraj, B Stephen; Chen, B H

    2012-07-01

    The objectives of this study were to determine the variety and content of carotenoids in Taraxacum formosanum, a traditional Chinese herb possessing vital biological activities, by developing an HPLC-DAD-APCI-MS method and a preparative column chromatographic method for carotenoid isolation. A total of 25 carotenoids were resolved within 66 min by employing a YMC C30 column and a gradient mobile phase of methanol-acetonitrile-water (79:14:7, v/v/v) and methylene chloride (100%) with flow rate at 1.0 mL/min and detection at 450 nm. All-trans-canthaxanthin was shown to be an appropriate internal standard for quantitation, with all-trans-β-carotene and its cis isomers present in largest amount (413.6 μg/g), followed by all-trans-violoxanthin and its cis isomers (209.5 μg/g), all-trans-lutein and its cis isomers (212.4 μg/g), all-trans-neoxanthin and its cis isomers (134.6 μg/g), antheraxanthin (16.5 μg/g), all-trans-β-cryptoxanthin and its cis isomers (5.8 μg/g), all-trans-zeaxanthin (3.6 μg/g) and neochrome (0.1 μg/g). For preparative chromatography, with a glass column containing 52 g of magnesium oxide-diatomaceous earth (1:3, w/w) as adsorbent, the carotenoid fraction was eluted with 300 mL of ethyl acetate with flow rate at 10 mL/min. Some more epoxides and cis isomers of carotenoids were generated during preparative column chromatography. Nevertheless, the carotenoids isolated from T. formosanum may be used as raw material for possible production of health food in the future. Copyright © 2012 Elsevier B.V. All rights reserved.

  2. Reversed-phase HPLC analysis of levetiracetam in tablets using monolithic and conventional C18 silica columns.

    PubMed

    Can, Nafiz O; Arli, Goksel

    2010-01-01

    Development and validation of an RP-HPLC method for determination of levetiracetam in pharmaceutical tablets is described. The separation and quantification of levetiracetam and caffeine (internal standard) were performed using a single analytical procedure with two different types of stationary phases, conventional Phenomenex Gemini C18 (100 x 4.6 mm, 5 microm) and Merck Chromolith Performance RP18e (100 x 4.6 mm, macropore size 2 mm, micropore size 13 nm) monolithic silica. Five-microliter aliquots of samples were injected into the system and eluted using water-acetonitrile (90 + 10, v/v) mobile phase pumped at the rate of 1 mL/min. The analyte peaks were detected at 200 nm using a diode array detector with adequate resolution. Validation studies were performed using the method recommended by the International Conference on Harmonization, the U.S. Pharmacopeia, and AOAC INTERNATIONAL, which includes accuracy, precision, range, limits, robustness, and system suitability parameters. Levetiracetam and caffeine were detected in about 7 min using the conventional column, whereas less than 5 min was required when the monolithic column was used. Calibration plots had r values close to unity in the range of 0.8-8.0 microg/mL. Assay of levetiracetam in a tablet formulation was demonstrated as an application to real samples.

  3. Preparation and application of poly 3, 4-ethylenedioxythiophene (PEDOT) nanofibers in the pretreatment of samples before the determination of elements in children fingernails

    NASA Astrophysics Data System (ADS)

    Qiu, J. L.; Kang, X. J.; Ma, L.; Huang, W. Y.; Ge, Q. Y.

    2015-07-01

    Solid phase extraction (SPE) has been used widely for sample preparation in the analytical process. Many efforts have focused on developing novel adsorbents to enrich and purify the analytes effectively. In this study, poly-3, 4-ethylenedioxythiophene (PEDOT) nanofiber was prepared and used as the SPE adsorbent. The fiber performed good in extraction of metal ions, Cd, Sn, Hg, Pb, Al, and As, with the extraction recoveries ranged from 53.9% to 99.6% in the wet digested samples of fingernails. A PEDOT namofibers SPE column coupled with ICP-MS was established for assay of elements in fingernails. The levels of elements (Cd, Sn, Hg, Pb, Al, and As) in the fingernails of 77 healthy Chinese children (6-7 and 10-11 years) were determined. Independent t test shows that no significance has been found between boys and girls. On the contrary, there was obvious difference on the levels of most elements between the two grade groups.

  4. In Vivo Photo-Cross-Linking to Study T3S Interactions Demonstrated Using the Yersinia pestis T3S System.

    PubMed

    Henderson, Thomas A; Nilles, Matthew L

    2017-01-01

    Cross-linking of proteins is effective in determining protein-protein interactions. The use of photo-cross-linkers was developed to study protein interactions in several manners. One method involved the incorporation of photo-activatable cross-linking groups into chemically synthesized peptides. A second approach relies on incorporation of photo-activatable cross-linking groups into proteins using tRNAs with chemically bound photo-activatable amino acids with suppressor tRNAs translational systems to incorporate the tags into specific sites. A third system was made possible by the development of photoreactive amino acids that use the normal cellular tRNAs and aminoacyl tRNA synthetases. In this method, the third system is used to demonstrate its utility for the study of T3S system interactions. This method describes how two photo-activatable amino acids, photo-methionine and photo-leucine, that use the normal cellular machinery are incorporated into Yersinia pestis and used to study interactions in the T3S system. To demonstrate the system, the method was used to cross-link the T3S regulatory proteins LcrG and LcrV.

  5. An Analytical Study of Icing Similitude for Aircraft Engine Testing. Revision

    DTIC Science & Technology

    1987-02-01

    MODELING GEOMETRIES Component Cowl Spinner Fan Blade Fan Stator Exit Vane Probe Approximating Geometry NACA 0012 Airfoil Sphere NACA 0012...DOT/FAA/CT·86/35 AEDC·TR·86·26 An Analytical Study of Icing Similitude for Aircraft Engine Testing c. Scott Bartlett Sverdrup Technology, Inc...8217~,feCa.ORI A n AnalYtical Study )f Icin~ Similitude for Aircraft Engine Tes t tu~ 12. PERSONAL AUTHOR/S) B a r t l e t t , C. Scot t , Sverdrup

  6. Antidiabetic screening of commercial botanical products in 3T3-L1 adipocytes and db/db mice.

    PubMed

    Babish, John G; Pacioretty, Linda M; Bland, Jeffrey S; Minich, Deanna M; Hu, Jeffrey; Tripp, Matthew L

    2010-06-01

    Numerous botanicals are purported to improve glucose metabolism and diabetic risk factors with varying degrees of supportive evidence. We investigated 203 commercially available botanical products representing 90 unique botanical species for effects on lipogenic activity in differentiating 3T3-L1 adipocytes. Anti-inflammatory activity of 21 of these products was further assessed in tumor necrosis factor alpha (TNFalpha)-stimulated, mature 3T3-L1 adipocytes. From these results, rho-isoalpha acids, Acacia nilotica bark, fennel, and wasabi were tested in the db/db mouse model. Fifty-nine percent of the 90 unique botanicals increased adipogenesis as did the standard troglitazone relative to the solvent controls. Botanical species with the greatest percentage of positive products were Centella asiatica, Panax quinquefolius, and Phyllanthus amarus at 100%, Vitis vinifera at 80%, Humulus lupulus at 71%, Aloe barbadensis at 66%, and Momordica charantia, Phaseolus vulgaris, and Punica granatum at 60%. All 21 subset samples inhibited TNFalpha-stimulated free fatty acid release and attenuated TNFalpha inhibition of adiponectin secretion. Both rho-isoalpha acids and A. nilotica reduced nonfasting glucose in the db/db mouse model, whereas A. nilotica also decreased nonfasting insulin levels. A post hoc analysis of the screening results indicated that the positive predictive value of the lipogenesis assay alone was 72%, while adding the criterion of a positive response in the anti-inflammatory assays increased this figure to 82%. Moreover, this large-scale evaluation demonstrates that antidiabetic, in vitro efficacy of botanicals is more a function of manufacturing or quality control differences than the presence of marker compounds and further underscores the need to develop functional as well as analytical bases for standardization of dietary supplements.

  7. High-resolution 3D-constructive interference in steady-state MR imaging and 3D time-of-flight MR angiography in neurovascular compression: a comparison between 3T and 1.5T.

    PubMed

    Garcia, M; Naraghi, R; Zumbrunn, T; Rösch, J; Hastreiter, P; Dörfler, A

    2012-08-01

    High-resolution MR imaging is useful for diagnosis and preoperative planning in patients with NVC. Because high-field MR imaging promises higher SNR and resolution, the aim of this study was to determine the value of high-resolution 3D-CISS and 3D-TOF MRA at 3T compared with 1.5T in patients with NVC. Forty-seven patients with NVC, trigeminal neuralgia, hemifacial spasm, and glossopharyngeal neuralgia were examined at 1.5T and 3T, including high-resolution 3D-CISS and 3D-TOF MRA sequences. Delineation of anatomic structures, overall image quality, severity of artifacts, visibility of NVC, and assessment of the SNR and CNR were compared between field strengths. SNR and CNR were significantly higher at 3T (P < .001). Significantly better anatomic conspicuity, including delineation of CNs, nerve branches, and assessment of small vessels, was obtained at 3T (P < .02). Severity of artifacts was significantly lower at 3T (P < .001). Consequently, overall image quality was significantly higher at 3T. NVC was significantly better delineated at 3T (P < .001). Six patients in whom NVC was not with certainty identifiable at 1.5T were correctly diagnosed at 3T. Patients with NVC may benefit from the higher resolution and greater sensitivity of 3T for preoperative assessment of NVC, and 3T may be of particular value when 1.5T is equivocal.

  8. 26 CFR 1.7519-3T - Effective date (temporary).

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... 26 Internal Revenue 13 2010-04-01 2010-04-01 false Effective date (temporary). 1.7519-3T Section 1.7519-3T Internal Revenue INTERNAL REVENUE SERVICE, DEPARTMENT OF THE TREASURY (CONTINUED) INCOME TAX (CONTINUED) INCOME TAXES The Tax Court § 1.7519-3T Effective date (temporary). The provisions of §§ 1.7519-1T...

  9. 40 CFR 799.6756 - TSCA partition coefficient (n-octanol/water), generator column method.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... method, or any other reliable quantitative procedure must be used for those compounds that do not absorb... any other reliable quantitative method, aqueous solutions from the generator column enter a collecting... Research of the National Bureau of Standards, 86:361-366 (1981). (7) Fujita, T. et al. “A New Substituent...

  10. 40 CFR 799.6756 - TSCA partition coefficient (n-octanol/water), generator column method.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... method, or any other reliable quantitative procedure must be used for those compounds that do not absorb... any other reliable quantitative method, aqueous solutions from the generator column enter a collecting... Research of the National Bureau of Standards, 86:361-366 (1981). (7) Fujita, T. et al. “A New Substituent...

  11. 40 CFR 799.6756 - TSCA partition coefficient (n-octanol/water), generator column method.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... method, or any other reliable quantitative procedure must be used for those compounds that do not absorb... any other reliable quantitative method, aqueous solutions from the generator column enter a collecting... Research of the National Bureau of Standards, 86:361-366 (1981). (7) Fujita, T. et al. “A New Substituent...

  12. Determination of cocaine and metabolites in hair by column-switching LC-MS-MS analysis.

    PubMed

    Alves, Marcela Nogueira Rabelo; Zanchetti, Gabriele; Piccinotti, Alberto; Tameni, Silvia; De Martinis, Bruno Spinosa; Polettini, Aldo

    2013-07-01

    A method for rapid, selective, and robust determination of cocaine (CO) and metabolites in 5-mg hair samples was developed and fully validated using a column-switching liquid chromatography-tandem mass spectrometry system (LC-MS-MS). Hair samples were decontaminated, segmented, incubated overnight in diluted HCl, and centrifuged, and the diluted (1:10 with distilled water) extracts were analyzed in positive ionization mode monitoring two reactions per analyte. Quantifier transitions were: m/z 304.2→182.2 for CO, m/z 290.1→168.1 for benzoylecgonine (BE), and m/z 318.2→196.2 for cocaethylene (CE). The lower limit of quantification (LLOQ) was set at 0.05 ng/mg for CO and CE, and 0.012 ng/mg for BE. Imprecision and inaccuracy at LLOQ were lower than 20 % for all analytes. Linearity ranged between 0.05 and 50.0 ng/mg for CO and CE and 0.012 and 12.50 ng/mg for BE. Selectivity, matrix effect, process efficiency, recovery, carryover, cross talk, and autosampler stability were also evaluated during validation. Eighteen real hair samples and five samples from a commercial proficiency testing program were comparatively examined with the proposed multidimensional chromatography coupled with tandem mass spectrometry procedure and our reference gas chromatography coupled to mass spectrometry (GC-MS) method. Compared with our reference GC-MS method, column-switching technique and the high sensitivity of the tandem mass spectrometry detection system allowed to significantly reduce sample amount (×10) with increased sensitivity (×2) and sample throughput (×4), to simplify sample preparation, and to avoid that interfering compounds and ions impaired the ionization and detection of the analytes and deteriorate the performance of the ion source.

  13. Complete temperature profiles in ultra-high-pressure liquid chromatography columns.

    PubMed

    Gritti, Fabrice; Guiochon, Georges

    2008-07-01

    The temperature profiles were calculated along and across seven packed columns (lengths 30, 50, 100, and 150 mm, i.d., 1 and 2.1 mm, all packed with Acquity UPLC, BEH-C 18 particles, average d(p) approximately 1.7 microm) and their stainless steel tubes (o.d. 4.53 and 6.35 mm). These columns were kept horizontal and sheltered from forced air convection (i.e., under still air conditions), at room temperature. They were all percolated with pure acetonitrile, either under the maximum pressure drop (1034 bar) or at the maximum flow rate (2 mL/min) permitted by the chromatograph. The heat balance equation of chromatographic columns was discretized and solved numerically with minimum approximation. Both the compressibility and the thermal expansion of the eluent were taken into account. The boundary conditions were determined from the experimental measurements of the column inlet pressure and of the temperature profile along the column wall, which were made with a precision better than +/-0.1 K. These calculation results provide the 3-D temperature profiles along and across the columns. The axial and radial temperature gradients are discussed in relationship with the experimental conditions used. The temperature map obtained permits a prediction of the chromatographic data obtained under a very high pressure gradient.

  14. Determination of trigonelline, nicotinic acid, and caffeine in Yunnan Arabica coffee by microwave-assisted extraction and HPLC with two columns in series.

    PubMed

    Liu, Hongcheng; Shao, Jinliang; Li, Qiwan; Li, Yangang; Yan, Hong Mei; He, Lizhong

    2012-01-01

    A simple, rapid method was developed for simultaneous extraction of trigonelline, nicotinic acid, and caffeine from coffee, and separation by two chromatographic columns in series. The trigonelline, nicotinic acid, and caffeine were extracted with microwave-assisted extraction (MAE). The optimal conditions selected were 3 min, 200 psi, and 120 degrees C. The chromatographic separation was performed with two columns in series, polyaromatic hydrocarbon C18 (250 x 4.6 mm id, 5 microm particle size) and Bondapak NH2 (300 x 3.9 mm id, 5 microm particle size). Isocratic elution was with 0.02 M phosphoric acid-methanol (70 + 30, v/v) mobile phase at a flow rate of 0.8 mL/min. Good recoveries and RSD values were found for all analytes in the matrix. The LOD of the three compounds was 0.02 mg/L, and the LOQ was 0.005% in the matrix. The concentrations of trigonelline, nicotinic acid, and caffeine in instant coffee, roasted coffee, and raw coffee (Yunnan Arabica coffee) were assessed by MAE and hot water extraction; the correlation coefficients between concentrations of the three compounds obtained were close to 1.

  15. Numerical Uncertainty Analysis for Computational Fluid Dynamics using Student T Distribution -- Application of CFD Uncertainty Analysis Compared to Exact Analytical Solution

    NASA Technical Reports Server (NTRS)

    Groves, Curtis E.; Ilie, marcel; Shallhorn, Paul A.

    2014-01-01

    Computational Fluid Dynamics (CFD) is the standard numerical tool used by Fluid Dynamists to estimate solutions to many problems in academia, government, and industry. CFD is known to have errors and uncertainties and there is no universally adopted method to estimate such quantities. This paper describes an approach to estimate CFD uncertainties strictly numerically using inputs and the Student-T distribution. The approach is compared to an exact analytical solution of fully developed, laminar flow between infinite, stationary plates. It is shown that treating all CFD input parameters as oscillatory uncertainty terms coupled with the Student-T distribution can encompass the exact solution.

  16. Fate and Transport of CL-20 and RDX in Unsaturated Laboratory Columns

    NASA Astrophysics Data System (ADS)

    Lemond, L. A.; Gamerdinger, A. P.; Szecsody, J. E.

    2005-05-01

    This research examines the fate and transport of two explosive compounds, Hexanitrohexaazaisowurtzitane (CL-20) and Hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX) in unsaturated laboratory columns. The transport and fate of these compounds were studied under saturated and unsaturated conditions in three natural soils: coarse sand, sandy loam, and a silt loam. Unsaturated column experiments were conducted using an ultra-centrifugation method. Sorption and degradation parameters were determined by moment analysis and hydrodynamic parameters were assessed with a two-region flow model. Differences in these parameters were evaluated as a function of water content. The fate and transport of CL-20 is highly dependent on 1) the soil type and 2) the compound's residence time in the soil and 3) water content of the media. Sorption of CL-20 was rate-limited. CL-20 degradation in saturated columns produced a half-life of as much as 22hr, but in unsaturated columns the degradation rate increased considerably, producing a half life of as little as 2hr. The fate and transport of RDX are also affected by the soil type, but sorption appeared to be instantaneous. Degradation of RDX was negligible. Our results suggest that at very low water content immobile water regions may become (at least in effect) isolated water regions and significantly alter the retardation of the tracer. In the sandy loam, there was as much as a 20-fold over-prediction of the retardation factor in the unsaturated saturated columns when predicted by Kd values derived from saturated columns. In the coarse sand, Kd values derived from saturated columns over-predicted retardation in the unsaturated columns by as much as 30%. In the silt loam, retardation factors were over-predicted by as much as 80%. At very low water contents, predictions of tracer behavior become very difficult because of changes in the flow regime that cannot be directly accounted for.

  17. Self-assembly of dendronized perylene bisimides into complex helical columns.

    PubMed

    Percec, Virgil; Peterca, Mihai; Tadjiev, Timur; Zeng, Xiangbing; Ungar, Goran; Leowanawat, Pawaret; Aqad, Emad; Imam, Mohammad R; Rosen, Brad M; Akbey, Umit; Graf, Robert; Sekharan, Sivakumar; Sebastiani, Daniel; Spiess, Hans W; Heiney, Paul A; Hudson, Steven D

    2011-08-10

    The synthesis of perylene 3,4:9,10-tetracarboxylic acid bisimides (PBIs) dendronized with first-generation dendrons containing 0 to 4 methylenic units (m) between the imide group and the dendron, (3,4,5)12G1-m-PBI, is reported. Structural analysis of their self-organized arrays by DSC, X-ray diffraction, molecular modeling, and solid-state (1)H NMR was carried out on oriented samples with heating and cooling rates of 20 to 0.2 °C/min. At high temperature, (3,4,5)12G1-m-PBI self-assemble into 2D-hexagonal columnar phases with intracolumnar order. At low temperature, they form orthorhombic (m = 0, 2, 3, 4) and monoclinic (m = 1) columnar arrays with 3D periodicity. The orthorhombic phase has symmetry close to hexagonal. For m = 0, 2, 3, 4 ,they consist of tetramers as basic units. The tetramers contain a pair of two molecules arranged side by side and another pair in the next stratum of the column, turned upside-down and rotated around the column axis at different angles for different m. In contrast, for m = 1, there is only one molecule in each stratum, with a four-strata 2(1) helical repeat. All molecules face up in one column, and down in the second column, of the monoclinic cell. This allows close and extended π-stacking, unlike in the disruptive up-down alteration from the case of m = 0, 2, 3, 4. Most of the 3D structures were observed only by cooling at rates of 1 °C/min or less. This complex helical self-assembly is representative for other classes of dendronized PBIs investigated for organic electronics and solar cells. © 2011 American Chemical Society

  18. Conventional and narrow bore short capillary columns with cyclodextrin derivatives as chiral selectors to speed-up enantioselective gas chromatography and enantioselective gas chromatography-mass spectrometry analyses.

    PubMed

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

    2008-11-28

    The analysis of complex real-world samples of vegetable origin requires rapid and accurate routine methods, enabling laboratories to increase sample throughput and productivity while reducing analysis costs. This study examines shortening enantioselective-GC (ES-GC) analysis time following the approaches used in fast GC. ES-GC separations are due to a weak enantiomer-CD host-guest interaction and the separation is thermodynamically driven and strongly influenced by temperature. As a consequence, fast temperature rates can interfere with enantiomeric discrimination; thus the use of short and/or narrow bore columns is a possible approach to speeding-up ES-GC analyses. The performance of ES-GC with a conventional inner diameter (I.D.) column (25 m length x 0.25 mm I.D., 0.15 microm and 0.25 microm d(f)) coated with 30% of 2,3-di-O-ethyl-6-O-tert-butyldimethylsilyl-beta-cyclodextrin in PS-086 is compared to those of conventional I.D. short column (5m length x 0.25 mm I.D., 0.15 microm d(f)) and of different length narrow bore columns (1, 2, 5 and 10 m long x 0.10 mm I.D., 0.10 microm d(f)) in analysing racemate standards of pesticides and in the flavour and fragrance field and real-world-samples. Short conventional I.D. columns gave shorter analysis time and comparable or lower resolutions with the racemate standards, depending mainly on analyte volatility. Narrow-bore columns were tested under different analysis conditions; they provided shorter analysis time and resolutions comparable to those of conventional I.D. ES columns. The narrow-bore columns offering the most effective compromise between separation efficiency and analysis time are the 5 and 2m columns; in combination with mass spectrometry as detector, applied to lavender and bergamot essential oil analyses, these reduced analysis time by a factor of at least three while separation of chiral markers remained unaltered.

  19. How to select equivalent and complimentary reversed phase liquid chromatography columns from column characterization databases.

    PubMed

    Borges, Endler M

    2014-01-07

    Three RP-LC column characterization protocols [Tanaka et al. (1989), Snyder et al. (PQRI, 2002), and NIST SRM 870 (2000)] were evaluated using both Euclidian distance and Principal Components Analysis to evaluate effectiveness at identifying equivalent columns. These databases utilize specific chromatographic properties such as hydrophobicity, hydrogen bonding, shape/steric selectivity, and ion exchange capacity of stationary phases. The chromatographic parameters of each test were shown to be uncorrelated. Despite this, the three protocols were equally successful in identifying similar and/or dissimilar stationary phases. The veracity of the results has been supported by some real life pharmaceutical separations. The use of Principal Component Analysis to identify similar/dissimilar phases appears to have some limitations in terms of loss of information. In contrast, the use of Euclidian distances is a much more convenient and reliable approach. The use of auto scaled data is favoured over the use of weighted factors as the former data transformation is less affected by the addition or removal of columns from the database. The use of these free databases and their corresponding software tools shown to be valid for identifying similar columns with equivalent chromatographic selectivity and retention as a "backup column". In addition, dissimilar columns with complimentary chromatographic selectivity can be identified for method development screening strategies. Copyright © 2013 Elsevier B.V. All rights reserved.

  20. Design procedures for fiber composite structural components: Rods, columns and beam columns

    NASA Technical Reports Server (NTRS)

    Chamis, C. C.

    1983-01-01

    Step by step procedures are described which are used to design structural components (rods, columns, and beam columns) subjected to steady state mechanical loads and hydrothermal environments. Illustrative examples are presented for structural components designed for static tensile and compressive loads, and fatigue as well as for moisture and temperature effects. Each example is set up as a sample design illustrating the detailed steps that are used to design similar components.

  1. Modafinil in Forensic and Clinical Toxicology-Case Reports, Analytics and Literature.

    PubMed

    Radünz, Lars; Reuter, Hannah; Andresen-Streichert, Hilke

    2018-06-01

    Modafinil is used because of its wakefulness-promoting properties for treatment of diseases associated with extreme sleepiness (i.e., narcolepsy). Additionally, it is misused as a "cognitive enhancer" to increase alertness and to improve concentration. We present modafinil concentrations in serum samples in five cases of our routine work measured by high-performance liquid chromatography coupled with a photo diode array detector after solid-phase extraction. One sample was analyzed for clinical toxicology purposes. The other four were investigated for the police: three cases of driving under the influence of drugs and one case of bodily harm. Sample preparation consisted of solid-phase extraction using Bond Elut® C18 columns. Papaverine was used as internal standard. Chromatographic separation was carried out using a Polaris C18-A column in an isocratic run. Wavelengths used for UV-detection were 220 nm for modafinil and 239 nm for the internal standard, respectively. The method was validated with a reduced validation design for rare analytes. A six-point-calibration from 0.5 to 5.0 mg/L, covering the therapeutic range (0.9-3.3 mg/L), was used for quantification. Concentrations in serum were in the range of 1.3 to ~34 mg/L (median: 3.6 mg/L; mean: 9.0 mg/L). To our knowledge, there are only few publications concerning the serum concentrations of modafinil in cases of (suspected) misuse, forensic cases or intoxications. In our discussion, the serum concentrations we determined are compared with the levels described in the literature so far.

  2. Extracellular ATP is a mitogen for 3T3, 3T6, and A431 cells and acts synergistically with other growth factors.

    PubMed Central

    Huang, N; Wang, D J; Heppel, L A

    1989-01-01

    Extracellular ATP in concentrations of 5-50 microM displayed very little mitogenic activity by itself but it caused synergistic stimulation of [3H]thymidine incorporation in the presence of phorbol 12-tetradecanoate 13-acetate, epidermal growth factor, platelet-derived growth factor, insulin, adenosine, or 5'-(N-ethyl)carboxamidoadenosine. Cultures of Swiss 3T3, Swiss 3T6, A431, DDT1-MF2, and HFF cells were used. The percent of cell nuclei labeled with [3H]thymidine and cell number were also increased. ADP was equally mitogenic, while UTP and ITP were much less active. The effect of ATP was not due to hydrolysis by ectoenzymes to form adenosine, a known growth factor. Thus, the nonhydrolyzable analogue adenosine 5'-[beta, gamma-imido]triphosphate was mitogenic. In addition, it was found that ATP showed synergism in 3T6 and 3T3 cells when present for only the first hour of an incorporation assay, during which time no significant hydrolysis occurred. Furthermore, prolonged preincubation of cells with ATP reduced the mitogenic response to ATP but not to adenosine; preincubation with adenosine or N6-(R-phenylisopropyl)adenosine had the reverse effect. Finally, the effect of adenosine, but not of ATP, was inhibited by aminophylline. We conclude that extracellular ATP is a mitogen that interacts with P2 purinoceptors on the plasma membrane. PMID:2813367

  3. Highly efficient monolithic silica capillary columns modified with poly(acrylic acid) for hydrophilic interaction chromatography.

    PubMed

    Horie, Kanta; Ikegami, Tohru; Hosoya, Ken; Saad, Nabil; Fiehn, Oliver; Tanaka, Nobuo

    2007-09-14

    Monolithic silica capillary columns for hydrophilic interaction liquid chromatography (HILIC) were prepared by on-column polymerization of acrylic acid on monolithic silica in a fused silica capillary modified with anchor groups. The products maintained the high permeability (K=5 x 10(-14)m(2)) and provided a plate height (H) of less than 10 microm at optimum linear velocity (u) and H below 20 microm at u=6mm/s for polar solutes including nucleosides and carbohydrates. The HILIC mode monolithic silica capillary column was able to produce 10000 theoretical plates (N) with column dead time (t(0)) of 20s at a pressure drop of 20 MPa or lower. The total performance was much higher than conventional particle-packed HILIC columns currently available. The gradient separations of peptides by a capillary LC-electrospray mass spectrometry system resulted in very different retention selectivity between reversed-phase mode separations and the HILIC mode separations with a peak capacity of ca. 100 in a 10 min gradient time in either mode. The high performance observed with the monolithic silica capillary column modified with poly(acrylic acid) suggests that the HILIC mode can be an alternative to the reversed-phase mode for a wide range of compounds, especially for those of high polarity in isocratic as well as gradient elution.

  4. Neuronal 3',3,5-triiodothyronine (T3) uptake and behavioral phenotype of mice deficient in Mct8, the neuronal T3 transporter mutated in Allan-Herndon-Dudley syndrome.

    PubMed

    Wirth, Eva K; Roth, Stephan; Blechschmidt, Cristiane; Hölter, Sabine M; Becker, Lore; Racz, Ildiko; Zimmer, Andreas; Klopstock, Thomas; Gailus-Durner, Valerie; Fuchs, Helmut; Wurst, Wolfgang; Naumann, Thomas; Bräuer, Anja; de Angelis, Martin Hrabé; Köhrle, Josef; Grüters, Annette; Schweizer, Ulrich

    2009-07-29

    Thyroid hormone transport into cells requires plasma membrane transport proteins. Mutations in one of these, monocarboxylate transporter 8 (MCT8), have been identified as underlying cause for the Allan-Herndon-Dudley syndrome, an X-linked mental retardation in which the patients also present with abnormally high 3',3,5-triiodothyronine (T(3)) plasma levels. Mice deficient in Mct8 replicate the thyroid hormone abnormalities observed in the human condition. However, no neurological deficits have been described in mice lacking Mct8. Therefore, we subjected Mct8-deficient mice to a comprehensive immunohistochemical, neurological, and behavioral screen. Several behavioral abnormalities were found in the mutants. Interestingly, some of these behavioral changes are compatible with hypothyroidism, whereas others rather indicate hyperthyroidism. We thus hypothesized that neurons exclusively dependent on Mct8 are in a hypothyroid state, whereas neurons expressing other T(3) transporters become hyperthyroid, if they are exposed directly to the high plasma T(3). The majority of T(3) uptake in primary cortical neurons is mediated by Mct8, but pharmacological inhibition suggested functional expression of additional T(3) transporter classes. mRNAs encoding six T(3) transporters, including L-type amino acid transporters (LATs), were coexpressed with Mct8 in isolated neurons. We then demonstrated Lat2 expression in cultured neurons and throughout murine brain development. In contrast, LAT2 is expressed in microglia in the developing human brain during gestation, but not in neurons. We suggest that lack of functional complementation by alternative thyroid hormone transporters in developing human neurons precipitates the devastating neurodevelopmental phenotype in MCT8-deficient patients, whereas Mct8-deficient mouse neurons are functionally complemented by other transporters, for possibly Lat2.

  5. The handedness of historiated spiral columns.

    PubMed

    Couzin, Robert

    2017-09-01

    Trajan's Column in Rome (AD 113) was the model for a modest number of other spiral columns decorated with figural, narrative imagery from antiquity to the present day. Most of these wind upwards to the right, often with a congruent spiral staircase within. A brief introductory consideration of antique screw direction in mechanical devices and fluted columns suggests that the former may have been affected by the handedness of designers and the latter by a preference for symmetry. However, for the historiated columns that are the main focus of this article, the determining factor was likely script direction. The manner in which this operated is considered, as well as competing mechanisms that might explain exceptions. A related phenomenon is the reversal of the spiral in a non-trivial number of reproductions of the antique columns, from Roman coinage to Renaissance and baroque drawings and engravings. Finally, the consistent inattention in academic literature to the spiral direction of historiated columns and the repeated publication of erroneous earlier reproductions warrants further consideration.

  6. Acoustic emission of retrofitted fiber-wrapped columns

    NASA Astrophysics Data System (ADS)

    El Echary, Hazem; Mirmiran, Amir

    1998-03-01

    In recent years, fiber-wrapping technique has become increasingly popular for retrofitting of existing bridge pier columns in seismic zones. By the way of confinement, the external jacket enhances strength, ductility and shear performance of the column. However, since state of the concrete core is not visible from outside of the jacket, it is of great necessity to develop proper non-destructive methods to evaluate structural integrity of the column. Extensive research on FRP-confined concrete at the University of Central Florida has shown that failure of such hybrid columns is often accompanied by considerable audible and sub-audible noise, making acoustic emission (AE) a viable NDE technique for retrofitted columns. Acoustic emission from fiber-wrapped concrete specimens were monitored. A total of 24 concrete specimens with two types of construction (bonded and unbonded) and four different number of layers (1, 3, 5 and 7) were tested under uniaxial compression. All specimens were made of S-glass fabric and polyester resin with a core diameter of 6' and a length of 12'. Some of the specimens were subjected to cycles of loading and unloading to examine the presence of the Kaiser and the Felicity effects. A 4-channel AEDSP-32/16 (Mistras-2001) machine from Physical Acoustics Corp. was used for the experiments. Results indicate that AE energy and the number of AE counts can both be good representatives for the response of confined concrete. Further, plots of AE energy versus load follows the same bilinear trend that has been observed in the stress-strain response of such specimens. Finally, Felicity effect was observed in all composite specimens.

  7. 3D-MICE: integration of cross-sectional and longitudinal imputation for multi-analyte longitudinal clinical data.

    PubMed

    Luo, Yuan; Szolovits, Peter; Dighe, Anand S; Baron, Jason M

    2018-06-01

    A key challenge in clinical data mining is that most clinical datasets contain missing data. Since many commonly used machine learning algorithms require complete datasets (no missing data), clinical analytic approaches often entail an imputation procedure to "fill in" missing data. However, although most clinical datasets contain a temporal component, most commonly used imputation methods do not adequately accommodate longitudinal time-based data. We sought to develop a new imputation algorithm, 3-dimensional multiple imputation with chained equations (3D-MICE), that can perform accurate imputation of missing clinical time series data. We extracted clinical laboratory test results for 13 commonly measured analytes (clinical laboratory tests). We imputed missing test results for the 13 analytes using 3 imputation methods: multiple imputation with chained equations (MICE), Gaussian process (GP), and 3D-MICE. 3D-MICE utilizes both MICE and GP imputation to integrate cross-sectional and longitudinal information. To evaluate imputation method performance, we randomly masked selected test results and imputed these masked results alongside results missing from our original data. We compared predicted results to measured results for masked data points. 3D-MICE performed significantly better than MICE and GP-based imputation in a composite of all 13 analytes, predicting missing results with a normalized root-mean-square error of 0.342, compared to 0.373 for MICE alone and 0.358 for GP alone. 3D-MICE offers a novel and practical approach to imputing clinical laboratory time series data. 3D-MICE may provide an additional tool for use as a foundation in clinical predictive analytics and intelligent clinical decision support.

  8. Influence of detergent formulation on nutrient movement through sand columns simulating mound and conventional septic system drainfields

    NASA Astrophysics Data System (ADS)

    Alhajjar, Bashar J.; Linn Gould, C.; Chesters, Gordon; Harkin, John M.

    1990-12-01

    The effects of phosphate (P) and zeolite (Z) -built detergents on leaching of N and P through sand columns simulating septic system drainfields were examined in laboratory columns. To simulate mound septic system drainfields, paired sets of columns were dosed intermittently with septic tank effluent from households using P- or Z-built detergent. Two other paired sets of columns were flooded with P- or Z-effluent to simulate new conventional septic system drainfields; after clogging mats or "crusts" developed at infiltration surface, the subsurfaces of the columns were aerated to simulate mature (crusted) conventional septic system drainfields. NO 3 loading in leachate was 1.1 times higher and ortho-P loading was 4.3 times lower when columns were dosed with Z- than with P-effluent. Dosed columns removed P poorly; total phosphorus (TP) loading in leachate was 81 and 19 g m -2 yr -1 with P- and Z-effluent, respectively. In flooded columns 1.3, 2.0 and 1.8 times more NH 4, organic nitrogen (ON) and total nitrogen (TN) respectively, were leached with Z- than with P-effluent; NO 3 leaching was similar. Flooded columns removed P efficiently; TP leached through flooded systems was 2.5 and 1.4 g m -2 yr -1 with P- and Z effluent, respectively. Crusted columns fed Z-effluent leached 1.2, 2.6, 1.4 and 2.1 times more NH 4, NO 3, ON and TN, respectively, than those with P-effluent but 1.8 times less TP. Crusted columns removed P satisfactorily: 8.2 and 4.6 g m -2 yr -1 TP with P- and Z-effluent, respectively. The P-built detergent substantially improves the efficiency of N removal with satisfactory P removal in columns simulating conventional septic system drainfield. Simultaneous removal of N and P under flooded conditions might be explained by precipitation of struvite-type minerals. Dosed system drainfields were less efficient in removing N and P compared to flooded and crusted system drainfelds.

  9. Modifications of the Relation Between Cosmic Ray Ionization Rate ζ and H_{3}^{+} Column Density in the Central Molecular Zone of the Galactic Center

    NASA Astrophysics Data System (ADS)

    Oka, Takeshi

    2017-06-01

    In deriving the simple formula, ζL=2k_eN(H_{3}^{+})(n_C/n_H)_SVR/f(H_{2}), used to estimate cosmic ray H_{2} ionization rate ζ from observed H_3^+ column density N(H_3^+) in the Central Molecular Zone (CMZ) of the Galactic center (GC), the following two effects were neglected: (1) the charge exchange reaction H_2^+ + H → H_2 + H^+ which significantly reduces H_3^+ production rate if the fraction of molecular hydrogen f(H_2) is much lower than 1, and (2) the production of electrons from ionization of H_2 and H which greatly increases the H_3^+ destruction rate if ζ is much higher than 10^{-15} s^{-1}. (Only electrons from VUV first ionization of C atoms had been considered). Recent more extensive analysis using the Meudon PDR code by Le Petit et al. has indicated that these effects are not negligible in the CMZ. While an extensive chemical model calculation is beyond the scope of our analysis, we have attempted to use our simple model considering only hydrogenic species and electrons to take these two effects into account. When (1) is introduced, the rate of H_3^+ production is approximated to be ζn_H[f(H_2)]^2, which is ˜ 3 times lower than the previous value for f(H_2) = 0.6 reported by Le Petit et al.^{c} When (2) is taken into account, the electron number density is approximated to be n_e = n_CR + ζn_H/[2k_en(H_3^+)] where the first and second term represents electrons from the C atoms and those from H_2 and H, respectively. The first term (in which R represents the increase of metallicity from the solar vicinity to the GC, R ≥ 3) has the electron fraction x_e = 5 × 10^{-4} and the second term becomes significant at ζ ˜ 10^{-15} s^{-1}. This introduces a non-linearity between ζ and N(H_3^+) and the latter reaches a maximum at ζ ˜ 10^{-14} s^{-1} and decreases as ζ increases further. Application of the results to the observed N(H_3^+) will be discussed. Oka, T., Geballe, T. R., Goto, M., Usuda, T., McCall, B. J. 2005, ApJ, 632, 882 Indriolo, N

  10. Clinical 3T MR imaging: mastering the challenges.

    PubMed

    Tanenbaum, Lawrence N

    2006-02-01

    3T MRI is ready to meet the needs of clinical practice. SAR limitations are minimized by technical advances and surface coils are available for all core applications. With appropriate adjustments to scanning protocols, one can master the challenges of scanning at 3T; studies of the brain, spine, chest, abdomen, pelvis, vasculature, and extremities can be consistently higher in quality than are those obtained at 1.5T. The superior studies that are obtainable at 3T have great appeal to clinicians who are sophisticated about MR technology in areas, such as neurology, orthopedics, vascular surgery, and oncology,and encourage a shift in referrals toward practices that invest in higher field technology. The greater sensitivity to magnetic susceptibility offers unique benefits in functional neuroimaging, and available software/hardware packages enhance clinical setting feasibility, which adds a source of new referrals. The greater overall signal of 3T can be manipulated to make scanning more comfortable and with less motion artifact because scan times could be half as long. Spectacular anatomic delineation that is provided by high-definition scanning at true 1024 resolution can improve preoperative assessment and may improve sensitivity to smaller lesions. 3T provides practices with an advantage that is sought increasingly by high field strength purchasers in a competitive market. Only cost considerations stand in the way of the eventual domination of 3T systems in the high field strength market.

  11. Method for determination of aflatoxin M₁ in cheese and butter by HPLC using an immunoaffinity column.

    PubMed

    Sakuma, Hisako; Kamata, Yoichi; Sugita-Konishi, Yoshiko; Kawakami, Hiroshi

    2011-01-01

    A rapid, sensitive convenient method for determination of aflatoxin M₁ (AFM₁) in cheese and butter by HPLC was developed and validated. The method employs a safe extraction solution (mixture of acetonitrile, methanol and water) and an immunoaffinity column (IAC) for clean-up. Compared with the widely used method employing chloroform and a Florisil column, the IAC method has a short analytical time and there are no interference peaks. The limits of quantification (LOQ) of the IAC method were 0.12 and 0.14 µg/kg, while those of the Florisil column method were 0.47 and 0.23 µg/kg in cheese and buffer, respectively. The recovery and relative standard deviation (RSD) for cheese (spiked at 0.5 µg/kg) in the IAC method were 92% and 7%, respectively, while for the Florisil column method the corresponding values were 76% and 10%. The recovery and RSD for butter (spiked at 0.5 µg/kg) in the IAC method were 97% and 9%, and those in the Florisil method were 74% and 9%, respectively. In the IAC method, the values of in-house precision (n=2, day=5) of cheese and butter (spiked at 0.5 µg/kg) were 9% and 13%, respectively. The IAC method is superior to the Florisil column method in terms of safety, ease of handling, sensitivity and reliability. A survey of AFM₁ contamination in imported cheese and butter in Japan was conducted by the IAC method. AFM₁ was not detected in 60 samples of cheese and 30 samples of butter.

  12. Statistical power comparisons at 3T and 7T with a GO / NOGO task.

    PubMed

    Torrisi, Salvatore; Chen, Gang; Glen, Daniel; Bandettini, Peter A; Baker, Chris I; Reynolds, Richard; Yen-Ting Liu, Jeffrey; Leshin, Joseph; Balderston, Nicholas; Grillon, Christian; Ernst, Monique

    2018-07-15

    The field of cognitive neuroscience is weighing evidence about whether to move from standard field strength to ultra-high field (UHF). The present study contributes to the evidence by comparing a cognitive neuroscience paradigm at 3 Tesla (3T) and 7 Tesla (7T). The goal was to test and demonstrate the practical effects of field strength on a standard GO/NOGO task using accessible preprocessing and analysis tools. Two independent matched healthy samples (N = 31 each) were analyzed at 3T and 7T. Results show gains at 7T in statistical strength, the detection of smaller effects and group-level power. With an increased availability of UHF scanners, these gains may be exploited by cognitive neuroscientists and other neuroimaging researchers to develop more efficient or comprehensive experimental designs and, given the same sample size, achieve greater statistical power at 7T. Published by Elsevier Inc.

  13. Ion chromatography for determination of nitrite and nitrate in seawater using monolithic ODS columns.

    PubMed

    Ito, Kazuaki; Takayama, Yohichi; Makabe, Nobuyuki; Mitsui, Ryo; Hirokawa, Takeshi

    2005-08-12

    A fast and highly sensitive ion chromatographic method using monolithic ODS columns was developed for the determination of nitrite (NO2-) and nitrate (NO3-) in seawater. Two monolithic ODS columns (50 mm x 4.6 mm i.d. + 100 mm x 4.6 mm i.d.) connected in series were coated and equilibrated with 5 mM cetyltrimethylammonium chloride (CTAC) aqueous solution. The column efficiency with 0.5 M NaCl as the mobile phase did not decrease in spite of the increase in flow rate of the mobile phase. Thus, good chromatograms were obtained within 3 minutes for NO2- and NO3 in artificial seawater without interferences by coexisting ions. The detection limit (S/N = 3) with UV detection at 225 nm was 0.8 and 1.6 microg/L for NO2- and NO3-, respectively. The characteristics of the monolithic CTA(+)-coated ODS columns were discussed. The present method was successfully applied to the fast and sensitive determination of NO2- and NO3- in real seawater samples.

  14. Transport of Escherichia coli in 25 m quartz sand columns

    NASA Astrophysics Data System (ADS)

    Lutterodt, G.; Foppen, J. W. A.; Maksoud, A.; Uhlenbrook, S.

    2011-01-01

    To help improve the prediction of bacteria travel distances in aquifers laboratory experiments were conducted to measure the distant dependent sticking efficiencies of two low attaching Escherichia coli strains (UCFL-94 and UCFL-131). The experimental set up consisted of a 25 m long helical column with a diameter of 3.2 cm packed with 99.1% pure-quartz sand saturated with a solution of magnesium sulfate and calcium chloride. Bacteria mass breakthrough at sampling distances ranging from 6 to 25.65 m were observed to quantify bacteria attachment over total transport distances ( αL) and sticking efficiencies at large intra-column segments ( αi) (> 5 m). Fractions of cells retained ( Fi) in a column segment as a function of αi were fitted with a power-law distribution from which the minimum sticking efficiency defined as the sticking efficiency of 0.001% bacteria fraction of the total input mass retained that results in a 5 log removal were extrapolated. Low values of αL in the order 10 - 4 and 10 - 3 were obtained for UCFL-94 and UCFL-131 respectively, while αi-values ranged between 10 - 6 to 10 - 3 for UCFL-94 and 10 - 5 to 10 - 4 for UCFL-131. In addition, both αL and αi reduced with increasing transport distance, and high coefficients of determination (0.99) were obtained for power-law distributions of αi for the two strains. Minimum sticking efficiencies extrapolated were 10 - 7 and 10 - 8 for UCFL-94 and UCFL-131, respectively. Fractions of cells exiting the column were 0.19 and 0.87 for UCFL-94 and UCL-131, respectively. We concluded that environmentally realistic sticking efficiency values in the order of 10 - 4 and 10 - 3 and much lower sticking efficiencies in the order 10 - 5 are measurable in the laboratory, Also power-law distributions in sticking efficiencies commonly observed for limited intra-column distances (< 2 m) are applicable at large transport distances(> 6 m) in columns packed with quartz grains. High fractions of bacteria populations

  15. Infiltration of γ⁢δ T cells, IL-17+ T cells and FoxP3+ T cells in human breast cancer

    PubMed Central

    Allaoui, Roni; Hagerling, Catharina; Desmond, Eva; Warfvinge, Carl-Fredrik; Jirström, Karin; Leandersson, Karin

    2017-01-01

    BACKGROUND: Tumor-infiltrating lymphocytes (TILs) have a strong prognostic value in various forms of cancers. These data often refer to use of the pan-T cell marker CD3, or the cytotoxic T lymphocyte marker CD8α. However, T cells are a heterogeneous group of cells with a wide array of effector mechanisms ranging from immunosuppression to cytotoxicity. OBJECTIVE: In this study we have investigated the prognostic effects of some unconventional T cell subtypes in breast cancer; γ⁢δ T cells, IL-17+ T cells and FoxP3+ T cells (Tregs) in relation to the conventional CD3 and CD8α T cell markers. METHODS: This was done using immunohistochemistry on a human breast cancer tissue microarray consisting of 498 consecutive cases of primary breast cancer. RESULTS: Infiltration of γ⁢δ T cells and T cell infiltration in general (CD3), correlated with a good prognosis, while Treg infiltration with a worse. Infiltration of γ⁢δ T cells was associated with a significantly improved clinical outcome in all breast cancer subtypes except triple negative tumors. Only infiltration of either CD3+ or CD8α+ cells was independently associated with better prognosis for all breast cancer patients. CONCLUSIONS: This study sheds further light on the prognostic impact of various T cell subtypes in breast cancer. PMID:29060923

  16. Biogeochemical impacts of aquifer thermal energy storage at 5, 12, 25 and 60°C investigated with anoxic column experiments

    NASA Astrophysics Data System (ADS)

    Bonte, M.; van Breukelen, B. M.; Van Der Wielen, P. W. J. J.; Stuyfzand, P. J.

    2012-04-01

    Aquifer thermal energy storage (ATES) uses groundwater to store energy for heating or cooling purposes in the built environment. ATES systems are often located in the same aquifers used for public drinking water supply, leading to urgent questions on its environmental impacts. This contribution presents the results of research on the biogeochemical impacts of ATES in anoxic column experiments at 5, 12, 25, and 60° C. In- and effluents are analyzed for major ions, trace elements, heavy metals, dissolved organic carbon (DOC) and UV extinction. Terminal restriction fragment length polymorphism (T-RFLP) of 16S rRNA genes and analysis of adenosine triphosphate (ATP) were used to detect changes in the microbiological population and activity. Results from the column experiments at 5, 25, and 60° C compared to the reference column at 12° C showed a number of changes in biogeochemical conditions: At 5° C, only changes were observed in alkalinity and calcium concentrations, resulting from calcite dissolution. The 25° C and 60° C column effluents from a sediment containing Fe-(hydr)oxides showed an increase in arsenic concentrations, well above the drinking water limit. This is due to either (reductive) dissolution of, or desorption from, iron(hydro)xides containing arsenic. In addition, at these two temperatures sulfate reduction occurred while this was undetectable at 5 and 12° C within the given timeframe (25 days) and analytical accuracy. The carbon source for sulfate reduction is inferred to be sedimentary organic carbon. Increasing DOC with residence time in the 60° C effluent suggests that at 60° C the terminal sulfate reduction step is rate limiting, while at 25° C the enzymatic hydrolization step in sulfate reducing bacteria is overall rate limiting. Specific ultraviolet absorption (SUVA, the ratio of UV extinction and DOC) however shows a clear decrease in reactivity of the humic acid fraction in DOC. This means that the DOC accumulation at 60° C could

  17. Improved online δ18O measurements of nitrogen- and sulfur-bearing organic materials and a proposed analytical protocol

    USGS Publications Warehouse

    Qi, H.; Coplen, T.B.; Wassenaar, L.I.

    2011-01-01

    It is well known that N2 in the ion source of a mass spectrometer interferes with the CO background during the δ18O measurement of carbon monoxide. A similar problem arises with the high-temperature conversion (HTC) analysis of nitrogenous O-bearing samples (e.g. nitrates and keratins) to CO for δ18O measurement, where the sample introduces a significant N2 peak before the CO peak, making determination of accurate oxygen isotope ratios difficult. Although using a gas chromatography (GC) column longer than that commonly provided by manufacturers (0.6 m) can improve the efficiency of separation of CO and N2 and using a valve to divert nitrogen and prevent it from entering the ion source of a mass spectrometer improved measurement results, biased δ18O values could still be obtained. A careful evaluation of the performance of the GC separation column was carried out. With optimal GC columns, the δ18O reproducibility of human hair keratins and other keratin materials was better than ±0.15 ‰ (n = 5; for the internal analytical reproducibility), and better than ±0.10 ‰ (n = 4; for the external analytical reproducibility).

  18. Reversed Phase Column HPLC-ICP-MS Conditions for Arsenic Speciation Analysis of Rice Flour.

    PubMed

    Narukawa, Tomohiro; Matsumoto, Eri; Nishimura, Tsutomu; Hioki, Akiharu

    2015-01-01

    New measurement conditions for arsenic speciation analysis of rice flour were developed using HPLC-ICP-MS equipped with a reversed phase ODS column. Eight arsenic species, namely, arsenite [As(III)], arsenate [As(V)], monomethylarsonic acid (MMAA), dimethylarsinic acid (DMAA), trimethylarsine oxide (TMAO), tetramethylarsonium (TeMA), arsenobetaine (AsB) and arsenocholine (AsC), were separated and determined under the proposed conditions. In particular, As(III) and MMAA and DMAA and AsB were completely separated using a newly proposed eluent containing ammonium dihydrogen phosphate. Importantly, the sensitivity changes, in particular those of As(V) and As(III) caused by coexisting elements and by complex matrix composition, which had been problematical in previously reported methods, were eliminated. The new eluent can be applied to C8, C18 and C30 ODS columns with the same effectiveness and with excellent repeatability. The proposed analytical method was successfully applied to extracts of rice flour certified reference materials.

  19. Flexural stiffness of the composite steel and fibre-reinforced concrete circular hollow section column

    NASA Astrophysics Data System (ADS)

    Tretyakov, A.; Tkalenko, I.; Wald, F.; Novak, J.; Stefan, R.; Kohoutková, A.

    2017-09-01

    The recent development in technology of production and transportation of steel fibre-reinforced concrete enables its utilization in composite steel-concrete structures. This work is a part of a project which focuses on development of mechanical behaviour of circular hollow section (CHS) composite steel and fibre-concrete (SFRC) columns at elevate temperature. Research includes two levels of accuracy/complexity, allowing simplified or advanced approach for design that follows upcoming changes in European standard for composite member design in fire EN1994-1-2 [1]. One part is dedicated to determination and description of flexural stiffness of the SFRC CHS columns. To determinate flexural stiffness were prepared series of pure bending tests at elevated and ambient temperature. Presented paper focuses on the results of the tests and determination of flexural stiffness at ambient temperature. Obtained outputs were compared to data of existing studies about concrete-filled tube members with plain concrete and values analytically calculated according to the existing European standard EN1994-1-1 [2].

  20. HPLC-MS-MS Determination of ZCZ-011, A Novel Pharmacological Tool for Investigation of the Cannabinoid Receptor in Mouse Brain Using Clean Screen FASt™ Column Extraction.

    PubMed

    Poklis, Justin L; Clay, Deborah J; Ignatowska-Jankowska, Bogna M; Zanato, Chiara; Ross, Ruth A; Greig, Iain R; Abdullah, Rehab A; Mustafa, Mohammed A; Lichtman, Aron H; Poklis, Alphonse

    2015-06-01

    A high-performance liquid chromatography tandem mass spectrometry method was developed for the detection and quantification of 6-methyl-3-(2-nitro-1-(thiophen-2-yl)propyl)-2-phenyl-1H-indole (ZCZ-011) using 2-phenylindole as the internal standard (ISTD). ZCZ-011 was synthesized as a possible positive allosteric modulator with the CB1 cannabinoid receptor. The analytical method employs a rapid extraction technique using Clean Screen FASt™ columns with a Positive Pressure Manifold. FASt™ columns were originally developed for urine drug analysis but we have successfully adapted them to the extraction of brain tissue. Chromatographic separation was performed on a Restek Allure Biphenyl 5 µ, 100 × 3.2 mm column (Bellefonte, PA). The mobile phase consisted of 1:9 deionized water with 10 mmol ammonium acetate and 0.1% formic acid-methanol. The following transition ions (m/z) were monitored for ZCZ-011: 363 > 207 and 363 > 110 and for the ISTD: 194 > 165 and 194 > 89. The FASt™ columns lowered and stabilized the ion suppression over the linear range of the assay (40-4,000 ng/g). The method was evaluated for recovery, ion suppression, accuracy/bias, intraday and interday precision, bench-top stability, freeze-thaw and post-preparative stability. The method was successfully applied to brain tissue from C57BL/6J mice that received intraperitoneal (i.p.) injections with 40 mg/kg of ZCZ-011 or vehicle. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  1. Temperature induced modulation of lipid oxidation and lipid accumulation in palmitate-mediated 3T3-L1 adipocytes and 3T3-L1 adipocytes.

    PubMed

    Lin, Xiaofen; Li, Yi; Leung, Polly Hangmei; Li, Jiashen; Hu, Junyan; Liu, Xuan; Li, Zhi

    2016-05-01

    Human skin temperature can vary widely depending on anatomical location and ambient temperature. It is also known that local changes in skin and subcutaneous temperature can affect fat metabolism. This study aimed to explore the potential effects of surrounding thermal environment on fat by investigating cell viability, lipid oxidation, and lipid accumulation in 3T3-L1 adipocytes and palmitate-treated adipocytes after 4h incubation. No significant differences of viability in 3T3-L1 adipocytes were detected under different temperature conditions. Despite no significant increase being observed under warm temperature (39°C) conditions, a similarly significant suppression of intracellular reactive oxygen species (ROS) and lipid peroxidation were found in 3T3-L1 adipocytes and palmitate-treated adipocytes under 4h exposure to cooler temperatures of 31-33°C (P<0.01). ROS, chemically reactive molecules containing oxygen, are currently understood to be a major contributor to oxidantive stress in obesity. Additionally, cooler temperatures (31-33°C) could improve the size of lipid droplets in 3T3-L1 adipocytes (P<0.01), but no significant effect was generated by temperature change on lipid droplets in palmitate-treated adipocytes. In the palmitate-induced adiposity model, although excessive ROS and lipid peroxidation has been attenuated by temperature decrease (P<0.01), it still does not positively modulate lipid droplet size (P>0.05) and remedy the palmitate damage induced cell death (P<0.01). These findings provide preliminary support for potential interventions based on temperature manipulation for cell metabolism of adipocytes. Copyright © 2016 Elsevier Ltd. All rights reserved.

  2. tDCS polarity effects in motor and cognitive domains: a meta-analytical review.

    PubMed

    Jacobson, Liron; Koslowsky, Meni; Lavidor, Michal

    2012-01-01

    In vivo effects of transcranial direct current stimulation (tDCS) have attracted much attention nowadays as this area of research spreads to both the motor and cognitive domains. The common assumption is that the anode electrode causes an enhancement of cortical excitability during stimulation, which then lasts for a few minutes thereafter, while the cathode electrode generates the opposite effect, i.e., anodal-excitation and cathodal-inhibition effects (AeCi). Yet, this dual-polarity effect has not been observed in all tDCS studies. Here, we conducted a meta-analytical review aimed to investigate the homogeneity/heterogeneity of the effect sizes of the AeCi dichotomy in both motor and cognitive functions. The AeCi effect was found to occur quite commonly with motor investigations and rarely in cognitive studies. When the anode electrode is applied over a non-motor area, in most cases, it will cause an excitation as measured by a relevant cognitive or perceptual task; however, the cathode electrode rarely causes an inhibition. We found homogeneity in motor studies and heterogeneity in cognitive studies with the electrode's polarity serving as a moderator that can explain the source of heterogeneity in cognitive studies. The lack of inhibitory cathodal effects might reflect compensation processes as cognitive functions are typically supported by rich brain networks. Further insights as to the polarity and domain interaction are offered, including subdivision to different classes of cognitive functions according to their likelihood of being affected by stimulation.

  3. GPR Diagnostics of columns in archaeological contexts

    NASA Astrophysics Data System (ADS)

    Soldovieri, Francesco; Masini, Nicola; Persico, Raffaele; Catapano, Ilaria

    2017-04-01

    columns during a previous work carried out about thirty years ago and whose memory documentation was lost. Both the GPR surveys were carried out by using the K2-RIS IDS system equipped with a high frequency antenna, working at the central frequency of 2GHz. Moreover, the imaging results have been obtained by processing the raw data by means of the end-user friendly software interface designed at the Institute for Electromagnetic Sensing of the Environment - National Research Council of Italy. This interface was some years ago to make possible a simple management of 2D and 3D microwave tomographic approaches based on the Born approximation [4-6].The GPR surveys have confirmed the presence of metallic elements inside few of the investigated columns. [1] Masini N., Nuzzo L., Rizzo E. 2007, GPR investigations for the study and the restoration of the Rose Window of Troia Cathedral (Southern Italy), Near Surface Geophysics, 5 (5), pp. 287-300, doi: 10.3997/1873-0604.2007010 [2] Leucci G., Masini N., Persico R., Soldovieri F. 2011. GPR and sonic tomography for structural restoration: the case of the cathedral of Tricarico, Journal of Geophysics and Engineering, 8 (3), 76-92, doi: 10.1088/1742-2132/8/3/S08 [3] Masini N., Persico R., Rizzo E., Calia A., Giannotta M.T., Quarta G., Pagliuca A. 2010, Integrated Techniques for Analysis and Monitoring of Historical Monuments: the case of S.Giovanni al Sepolcro in Brindisi (Southern Italy), Near Surface Geophysics, 8(5), 423-432, doi:10.3997/1873-0604.2010012 [4] F. Soldovieri, J. Hugenschmidt, R. Persico, G. Leone, A linear inverse scattering algorithm for realistic GPR applications. Near Surf. Geophys. 5(1), 29-42 (2007) [5] I. Catapano, A. Affinito, G. Gennarelli, F.di Maio, A. Loperte, F. Soldovieri, "Full three-dimensional imaging via ground penetrating radar: assessment in controlled conditions and on field for archaeological prospecting", Appl. Phys. A, 2013 [6] I. Catapano, A. Affinito, F. Soldovieri, A user friendly interface

  4. A simple subcritical chromatographic test for an extended ODS high performance liquid chromatography column classification.

    PubMed

    Lesellier, Eric; Tchapla, Alain

    2005-12-23

    This paper describes a new test designed in subcritical fluid chromatography (SFC) to compare the commercial C18 stationary phase properties. This test provides, from a single analysis of carotenoid pigments, the absolute hydrophobicity, the silanol activity and the steric separation factor of the ODS stationary phases. Both the choice of the analytical conditions and the validation of the information obtained from the chromatographic measurements are detailed. Correlations of the carotenoid test results with results obtained from other tests (Tanaka, Engelhard, Sander and Wise) performed both in SFC and HPLC are discussed. Two separation factors, calculated from the retention of carotenoid pigments used as probe, allowed to draw a first classification diagram. Columns, which present identical chromatographic behaviors are located in the same area on this diagram. This location can be related to the stationary phase properties: endcapping treatments, bonding density, linkage functionality, specific area or silica pore diameter. From the first classification, eight groups of columns are distinguished. One group of polymer coated silica, three groups of polymeric octadecyl phases, depending on the pore size and the endcapping treatment, and four groups of monomeric stationary phases. An additional classification of the four monomeric groups allows the comparison of these stationary phases inside each group by using the total hydrophobicity. One hundred and twenty-nine columns were analysed by this simple and rapid test, which allows a comparison of columns with the aim of helping along their choice in HPLC.

  5. States of phage T3/T7 capsids: buoyant density centrifugation and cryo-EM.

    PubMed

    Serwer, Philip; Wright, Elena T; Demeler, Borries; Jiang, Wen

    2018-04-01

    Mature double-stranded DNA bacteriophages have capsids with symmetrical shells that typically resist disruption, as they must to survive in the wild. However, flexibility and associated dynamism assist function. We describe biochemistry-oriented procedures used to find previously obscure flexibility for capsids of the related phages, T3 and T7. The primary procedures are hydration-based buoyant density ultracentrifugation and purified particle-based cryo-electron microscopy (cryo-EM). We review the buoyant density centrifugation in detail. The mature, stable T3/T7 capsid is a shell flexibility-derived conversion product of an initially assembled procapsid (capsid I). During DNA packaging, capsid I expands and loses a scaffolding protein to form capsid II. The following are observations made with capsid II. (1) The in vivo DNA packaging of wild type T3 generates capsid II that has a slight (1.4%), cryo-EM-detected hyper-expansion relative to the mature phage capsid. (2) DNA packaging in some altered conditions generates more extensive hyper-expansion of capsid II, initially detected by hydration-based preparative buoyant density centrifugation in Nycodenz density gradients. (3) Capsid contraction sometimes occurs, e.g., during quantized leakage of DNA from mature T3 capsids without a tail.

  6. Monolithic silica spin column extraction and simultaneous derivatization of amphetamines and 3,4-methylenedioxyamphetamines in human urine for gas chromatographic-mass spectrometric detection.

    PubMed

    Nakamoto, Akihiro; Nishida, Manami; Saito, Takeshi; Kishiyama, Izumi; Miyazaki, Shota; Murakami, Katsunori; Nagao, Masataka; Namura, Akira

    2010-02-19

    A simple, sensitive, and specific method with gas chromatography-mass spectrometry was developed for simultaneous extraction and derivatization of amphetamines (APs) and 3,4-methylenedioxyamphetamines (MDAs) in human urine by using a monolithic silica spin column. All the procedures, such as sample loading, washing, and elution were performed by centrifugation. APs and MDAs in urine were adsorbed on the monolithic silica and derivatized with propyl chloroformate in the column. Methamphetamine-d(5) was used as an internal standard. The linear ranges were 0.01-5.0 microg mL(-1) for methamphetamine (MA) and 3,4-methylenedioxymethamphetamine (MDMA) and 0.02-5.0 microg mL(-1) for amphetamine (AP) and 3,4-methylenedioxyamphetamine (MDA) (coefficient of correlation > or = 0.995). The recovery of APs and MDAs in urine was 84-94%, and the relative standard deviation of the intra- and interday reproducibility for urine samples containing 0.1, 1.0, and 4.0 microg mL(-1) of APs and MDAs ranged from 1.4% to 13.6%. The lowest detection limit (signal-to-noise ratio > or = 3) in urine was 5 ng mL(-1) for MA and MDMA and 10 ng mL(-1) for AP and MDA. The proposed method can be used to perform simultaneous extraction and derivatization on spin columns that have been loaded with a small quantity of solvent by using centrifugation. Copyright 2009 Elsevier B.V. All rights reserved.

  7. Optimum Parameters of a Tuned Liquid Column Damper in a Wind Turbine Subject to Stochastic Load

    NASA Astrophysics Data System (ADS)

    Alkmim, M. H.; de Morais, M. V. G.; Fabro, A. T.

    2017-12-01

    Parameter optimization for tuned liquid column dampers (TLCD), a class of passive structural control, have been previously proposed in the literature for reducing vibration in wind turbines, and several other applications. However, most of the available work consider the wind excitation as either a deterministic harmonic load or random load with white noise spectra. In this paper, a global direct search optimization algorithm to reduce vibration of a tuned liquid column damper (TLCD), a class of passive structural control device, is presented. The objective is to find optimized parameters for the TLCD under stochastic load from different wind power spectral density. A verification is made considering the analytical solution of undamped primary system under white noise excitation by comparing with result from the literature. Finally, it is shown that different wind profiles can significantly affect the optimum TLCD parameters.

  8. Repetitive Regeneration of Media #1 in a Dynamic Column Extraction using Brine #1

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Gary Garland

    This data is from a regeneration study from a dynamic column extraction experiment where we ran a solution of REE's through a column of media #1 then stripped the REE's off the media using 2M HNO3 solution. We then re-equilibrated the media and repeated the process of running a REE solution through the column and stripping the REE's off the media and comparing the two runs.

  9. RDX degradation in bioaugmented model aquifer columns under aerobic and low oxygen conditions.

    PubMed

    Fuller, Mark E; Hatzinger, Paul B; Condee, Charles W; Andaya, Christina; Rezes, Rachel; Michalsen, Mandy M; Crocker, Fiona H; Indest, Karl J; Jung, Carina M; Alon Blakeney, G; Istok, Jonathan D; Hammett, Steven A

    2017-07-01

    Degradation of hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX) in laboratory columns following biostimulation and bioaugmentation was investigated using sediment and groundwater from a contaminated aquifer at a US Navy facility. No RDX degradation was observed following aerobic biostimulation with either fructose or lactate (both 0.1 mM) prior to bioaugmentation. Replicate columns were then bioaugmented with either Gordonia sp. KTR9, Pseudomonas fluorescens I-C (Ps I-C), or both strains. Under aerobic conditions (influent dissolved oxygen (DO) >6 mg/L), RDX was degraded following the addition of fructose, and to a lesser extent with lactate, in columns bioaugmented with KTR9. No degradation was observed in columns bioaugmented with only Ps I-C under aerobic conditions, consistent with the known anaerobic RDX degradation pathway for this strain. When influent DO was reduced to <2 mg/L, good RDX degradation was observed in the KTR9-bioaugmented column, and some degradation was also observed in the Ps I-C-bioaugmented column. After DO levels were kept below 1 mg/L for more than a month, columns bioaugmented with KTR9 became unresponsive to fructose addition, while RDX degradation was still observed in the Ps I-C-bioaugmented columns. These results indicate that bioaugmentation with the aerobic RDX degrader KTR9 could be effective at sites where site geology or geochemistry allow higher DO levels to be maintained. Further, inclusion of strains capable of anoxic RDX degradation such as Ps I-C may facilitate bimodal RDX removal when DO levels decrease.

  10. High‐precision determination of lithium and magnesium isotopes utilising single column separation and multi‐collector inductively coupled plasma mass spectrometry

    PubMed Central

    Misra, Sambuddha; Lloyd, Nicholas; Elderfield, Henry; Bickle, Mike J.

    2017-01-01

    Rationale Li and Mg isotopes are increasingly used as a combined tool within the geosciences. However, established methods require separate sample purification protocols utilising several column separation procedures. This study presents a single‐step cation‐exchange method for quantitative separation of trace levels of Li and Mg from multiple sample matrices. Methods The column method utilises the macro‐porous AGMP‐50 resin and a high‐aspect ratio column, allowing quantitative separation of Li and Mg from natural waters, sediments, rocks and carbonate matrices following the same elution protocol. High‐precision isotope determination was conducted by multi‐collector inductively coupled plasma mass spectrometry (MC‐ICPMS) on the Thermo Scientific™ NEPTUNE Plus™ fitted with 1013 Ω amplifiers which allow accurate and precise measurements at ion beams ≤0.51 V. Results Sub‐nanogram Li samples (0.3–0.5 ng) were regularly separated (yielding Mg masses of 1–70 μg) using the presented column method. The total sample consumption during isotopic analysis is <0.5 ng Li and <115 ng Mg with long‐term external 2σ precisions of ±0.39‰ for δ7Li and ±0.07‰ for δ26Mg. The results for geological reference standards and seawater analysed by our method are in excellent agreement with published values despite the order of magnitude lower sample consumption. Conclusions The possibility of eluting small sample masses and the low analytical sample consumption make this method ideal for samples of limited mass or low Li concentration, such as foraminifera, mineral separates or dilute river waters. PMID:29078008

  11. New analytical spiral tube assembly for separation of proteins by counter-current chromatography.

    PubMed

    Ma, Xiaofeng; Ito, Yoichiro

    2015-07-31

    A new spiral column assembly for analytical separation by counter-current chromatography is described. The column is made from a plastic spiral tube support which has 12 interwoven spiral grooves. The PTFE tubing of 1.6mm ID was first flattened by extruding through a narrow slit and inserted into the grooves to make 5 spiral layers with about 60ml capacity. The performance of the spiral column assembly was tested with separation of three stable protein samples including cytochrome C, myoglobin and lysozyme in a polymer phase system composed of polyethylene glycol 1000 and dibasic potassium phosphate each at 12.5% (w/w) in water. At 2ml/min, three protein samples were well resolved in 1h. The separation time may be further shortened by application of higher revolution speed and flow rate by improving the strength of the spiral tube support in the future. Published by Elsevier B.V.

  12. Avoid problems during distillation column startups

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Sloley, A.W.

    1996-07-01

    The startup of a distillation column is the end product of the design process. Indeed, startup is the culmination of the theory and practice of designing the column to meet the process objectives. The author will direct most of this discussion towards column revamps due to their inherent complexity; however, the points apply equally to new columns, as well. The most important question that must be answered prior to a startup is how will the distillation system changes affect initial startup, process control of the system, and normal day-to-day operations? How will the operators run the system? Steady-state distillation-column simulationsmore » alone cannot provide an authoritative answer and, indeed, engineers` over-reliance on software too often has led them to ignore many practical aspects. Computer modeling, while an important engineering tool, is not reality. Distillation columns are real functioning pieces of equipment that require practical skills to successfully modify. They are not steady-state solutions that result from converged computer simulations. Early planning, coupled with thorough inspections and comprehensive reviews of instrumentation and procedures, can play a key role in assuring smooth startups.« less

  13. The program FANS-3D (finite analytic numerical simulation 3-dimensional) and its applications

    NASA Technical Reports Server (NTRS)

    Bravo, Ramiro H.; Chen, Ching-Jen

    1992-01-01

    In this study, the program named FANS-3D (Finite Analytic Numerical Simulation-3 Dimensional) is presented. FANS-3D was designed to solve problems of incompressible fluid flow and combined modes of heat transfer. It solves problems with conduction and convection modes of heat transfer in laminar flow, with provisions for radiation and turbulent flows. It can solve singular or conjugate modes of heat transfer. It also solves problems in natural convection, using the Boussinesq approximation. FANS-3D was designed to solve heat transfer problems inside one, two and three dimensional geometries that can be represented by orthogonal planes in a Cartesian coordinate system. It can solve internal and external flows using appropriate boundary conditions such as symmetric, periodic and user specified.

  14. Development, validation and evaluation of an analytical method for the determination of monomeric and oligomeric procyanidins in apple extracts.

    PubMed

    Hollands, Wendy J; Voorspoels, Stefan; Jacobs, Griet; Aaby, Kjersti; Meisland, Ane; Garcia-Villalba, Rocio; Tomas-Barberan, Francisco; Piskula, Mariusz K; Mawson, Deborah; Vovk, Irena; Needs, Paul W; Kroon, Paul A

    2017-04-28

    There is a lack of data for individual oligomeric procyanidins in apples and apple extracts. Our aim was to develop, validate and evaluate an analytical method for the separation, identification and quantification of monomeric and oligomeric flavanols in apple extracts. To achieve this, we prepared two types of flavanol extracts from freeze-dried apples; one was an epicatechin-rich extract containing ∼30% (w/w) monomeric (-)-epicatechin which also contained oligomeric procyanidins (Extract A), the second was an oligomeric procyanidin-rich extract depleted of epicatechin (Extract B). The parameters considered for method optimisation were HPLC columns and conditions, sample heating, mass of extract and dilution volumes. The performance characteristics considered for method validation included standard linearity, method sensitivity, precision and trueness. Eight laboratories participated in the method evaluation. Chromatographic separation of the analytes was best achieved utilizing a Hilic column with a binary mobile phase consisting of acidic acetonitrile and acidic aqueous methanol. The final method showed linearity for epicatechin in the range 5-100μg/mL with a correlation co-efficient >0.999. Intra-day and inter-day precision of the analytes ranged from 2 to 6% and 2 to 13% respectively. Up to dp3, trueness of the method was >95% but decreased with increasing dp. Within laboratory precision showed RSD values <5 and 10% for monomers and oligomers, respectively. Between laboratory precision was 4 and 15% (Extract A) and 7 and 30% (Extract B) for monomers and oligomers, respectively. An analytical method for the separation, identification and quantification of procyanidins in an apple extract was developed, validated and assessed. The results of the inter-laboratory evaluation indicate that the method is reliable and reproducible. Copyright © 2017. Published by Elsevier B.V.

  15. Separation and purification of epigallocatechin-3-gallate (EGCG) from green tea using combined macroporous resin and polyamide column chromatography.

    PubMed

    Jin, Xin; Liu, Mingyan; Chen, Zaixing; Mao, Ruikun; Xiao, Qinghuan; Gao, Hua; Wei, Minjie

    2015-10-01

    Epigallocatechin-3-gallate (EGCG) is a major bioactive ingredient of green tea that produces beneficial neuroprotective effects. In this paper, to optimize the EGCG enrichment, thirteen macroporous resins with different chemical and physical properties were systemically evaluated. Among the thirteen tested resins, the H-bond resin HPD826 exhibited best adsorption/desorption capabilities and desorption ratio, as well as weakest affinity for caffeine. The absorption of EGCG on the HPD826 resin followed the pseudo-second-order kinetics and Langmuir isotherm model. The separation parameters of EGCG were optimized by dynamic adsorption/desorption experiments with the HPD826 resin column. Under the optimal condition, the content of EGCG in the 30% ethanol eluent increased by 5.8-fold from 7.7% to 44.6%, with the recovery yield of 72.1%. After further purification on a polyamide column, EGCG with 74.8% purity was obtained in the 40-50% ethanol fraction with a recovery rate of 88.4%. In addition, EGCG with 95.1% purity could be easily obtained after one-step crystallization in distilled water. Our study suggests that the combined macroporous resin and polyamide column chromatography is a simple method for large-scale separation and purification of EGCG from natural plants for food and pharmaceutical applications. Copyright © 2015 Elsevier B.V. All rights reserved.

  16. [Preparation and applications of a supported liquid-liquid extraction column with a composite diatomite material].

    PubMed

    Bao, Jianmin; Ma, Zhishuang; Sun, Ying; Wang, Yongzun; Li, Youxin

    2012-08-01

    A rapid and special supported liquid-liquid extraction (SLE) column was developed with a composite diatomite material. The SLE column was evaluated by high performance liquid chromatography (HPLC) with acidic, neutral and alkaline compounds dissolved in water. Furthermore, some real complex samples were also analyzed by HPLC with the SLE method. The recoveries of benzoic acid (acidic), p-nitroaniline (alkaline) and 4-hydroxy-benzoic methyl ester (neutral) treated by the SLE column were 90.6%, 98.1% and 97.7%. However, the recoveries of the three compounds treated by traditional liquid-liquid extraction (LLE) method were 71.9%, 81.9% and 83.9%. The results showed that the SLE technique had higher recoveries than the traditional LLE method. The spiked recoveries of the complex samples, such as benzoic acid in Sprite and dexamethasone acetate, chlorphenamine maleate, indomethacin in bovine serum, were between 80% and 110% and the relative standard deviations (RSDs) were less than 15%. For biological specimen, the results could be accepted. Meantime, many disadvantages associated with traditional LLE method, such as emulsion formation, didn't occur using SLE column. The SLE column technique is a good sample preparation method with many advantages, such as rapid, simple, robust, easily automated, high recovery and high-throughput, which would be widely used in the future.

  17. Spa47 is an oligomerization-activated type three secretion system (T3SS) ATPase from Shigella flexneri.

    PubMed

    Burgess, Jamie L; Jones, Heather B; Kumar, Prashant; Toth, Ronald T; Middaugh, C Russell; Antony, Edwin; Dickenson, Nicholas E

    2016-05-01

    Gram-negative pathogens often use conserved type three secretion systems (T3SS) for virulence. The Shigella type three secretion apparatus (T3SA) penetrates the host cell membrane and provides a unidirectional conduit for injection of effectors into host cells. The protein Spa47 localizes to the base of the apparatus and is speculated to be an ATPase that provides the energy for T3SA formation and secretion. Here, we developed an expression and purification protocol, producing active Spa47 and providing the first direct evidence that Spa47 is a bona fide ATPase. Additionally, size exclusion chromatography and analytical ultracentrifugation identified multiple oligomeric species of Spa47 with the largest greater than 8 fold more active for ATP hydrolysis than the monomer. An ATPase inactive Spa47 point mutant was then engineered by targeting a conserved Lysine within the predicted Walker A motif of Spa47. Interestingly, the mutant maintained a similar oligomerization pattern as active Spa47, but was unable to restore invasion phenotype when used to complement a spa47 null S. flexneri strain. Together, these results identify Spa47 as a Shigella T3SS ATPase and suggest that its activity is linked to oligomerization, perhaps as a regulatory mechanism as seen in some related pathogens. Additionally, Spa47 catalyzed ATP hydrolysis appears to be essential for host cell invasion, providing a strong platform for additional studies dissecting its role in virulence and providing an attractive target for anti-infective agents. © 2016 The Protein Society.

  18. Incidental pT2-T3 gallbladder cancer after a cholecystectomy: outcome of staging at 3 months prior to a radical resection

    PubMed Central

    Ausania, Fabio; Tsirlis, Theodoris; White, Steven A; French, Jeremy J; Jaques, Bryon C; Charnley, Richard M; Manas, Derek M

    2013-01-01

    Introduction Patients with incidental pT2-T3 gallbladder cancer (IGC) after a cholecystectomy may benefit from a radical re-resection although their optimal treatment strategy is not well defined. In this Unit, such patients undergo delayed staging at 3 months after a cholecystectomy to assess the evidence of a residual tumour, extra hepatic spread and the biological behaviour of the tumour. The aim of this study was to evaluate the outcome of patients who had delayed staging at 3 months after a cholecystectomy. Methods From July 2003 to July 2011, 56 patients with T2-T3 gallbladder cancer were referred to this Unit of which 49 were diagnosed incidentally on histology after a cholecystectomy. All 49 patients underwent delayed pre-operative staging using multi-detector computed tomography (MDCT) followed selectively by laparoscopy at 3 months after a cholecystectomy. Data were collected from a prospectively held database. The peri-operative and long-term outcomes of patients were analysed. SPSS software was used for statistical analysis. Results There were 38 pT2 and 11 pT3 tumours. After delayed staging, 24/49 (49%) patients underwent a radical resection, 24/49 (49%) were found to be inoperable on pre-operative assessment and 1/49 (2%) patient underwent an exploratory laparotomy and were found to be unresectable. The overall median survival from referral was 20.7 months (54.8 months for the group who had a radical re-resection versus 9.7 months for the group who had unresectable disease, P < 0.001). These results compare favourably with the reported outcome of fast-track management for incidental pT2-T3 gallbladder cancer from other major series in the literature. Conclusion Delayed staging in patients with incidental T2-T3 gallbladder cancer after a cholecystectomy is a useful strategy to select patients who will benefit from a resection and avoid unnecessary major surgery. PMID:23458168

  19. Evaluation of columns packed with shell particles with compounds of pharmaceutical interest.

    PubMed

    Ruta, Joséphine; Zurlino, Daria; Grivel, Candice; Heinisch, Sabine; Veuthey, Jean-Luc; Guillarme, Davy

    2012-03-09

    The commercial C18 columns packed with sub-3 μm shell particles were tested and compared to a reference UHPLC column, in terms of kinetic performance as well as selectivity, retention capability, peak shape and loading capacity. For this purpose, a set of pharmaceutically relevant molecules was selected, including acidic, neutral and basic drugs. Regarding kinetic performance, h(opt) values for the shell particles were found between 1.7 and 2, while the UHPLC column provided a value of approximately 2.5. However, this impressive performance should be considered with caution, particularly for the construction of kinetic plots since h(opt) values were sometimes related to the column dimensions, depending on the provider (h(opt) comprised between 1.8 and 2.6 for longer columns of 150 mm packed with shell particles). Despite the non-porous inner core of the shell particles representing between 25 and 36% of the particle, we demonstrated that the decrease in retention was on the maximum equal to 15% for Ascentis column while Acquity and Poroshell were strictly equivalent in terms of retention. Concerning loading capacity, it remains comparable to that of fully porous sub-2 μm particles and always more pronounced with 0.1% formic acid vs. phosphate buffer. The loading capacity of the different columns was found to be better correlated to the pore volume or surface coverage than the shell thickness. Experimentally, the most pronounced overloading was observed with the Poroshell. Finally, the selectivity and peak shape were evaluated using a mixture of basic and acidic drugs. It appears that results were very similar between sub-3 μm shell particles and fully porous sub-2-μm particles for our mixture of compounds, showing the ability to transfer existing methods to shell particles, with only limited adjustments. This study confirms the potential of columns packed with shell particles and demonstrates the interest of such column technology with pharmaceutical compounds

  20. Linkage of T3 and Cpa pilins in the Streptococcus pyogenes M3 pilus.

    PubMed

    Quigley, Bernard R; Zähner, Dorothea; Hatkoff, Matthew; Thanassi, David G; Scott, June R

    2009-06-01

    The important human pathogen Streptococcus pyogenes (group A streptococcus, GAS) initiates infection by pilus-mediated attachment to host tissue. Thus, the pilus is an excellent target for design of anti-infective strategies. The T3 pilus of GAS is composed of multiple covalently linked subunits of the T3 protein to which the two minor pilins, Cpa and OrfB, are covalently attached. Because the proteins of GAS pili do not contain either of the motifs required for pilus polymerization in other Gram-positive bacteria, we investigated the residues involved in their linkage. We show that linkage of Cpa to T3 by the sortase family transpeptidase SrtC2 requires the VPPTG motif in the cell wall-sorting signal of Cpa. We also demonstrate that K173 of T3 is required both for T3 polymerization and for attachment of Cpa to T3. Therefore, attachment of Cpa to K173 of a T3 subunit would block further addition of T3 subunits to this end of the growing pilus. This implies that Cpa is located exclusively at the pilus tip, a location supported by immunogold electron microscopy, and suggests that, as for well-studied pili on Gram-negative bacteria, the role of the pilus is to present the adhesin external to the bacterial capsule.

  1. Optimisation and validation of the analytical procedure for the determination of acrylamide in coffee by LC-MS/MS with SPE clean up.

    PubMed

    Gielecińska, Iwona; Mojska, Hanna

    2013-01-01

    Numerous studies have demonstrated acrylamide to be both neurotoxic and carcinogenic. At present it is widely recognised that acrylamide is mainly formed through the Maillard reaction from free asparagine and reducing sugars. The major sources of dietary acrylamide are potato products, processed cereals and coffee. To optimise and validate an analytical method for determining acrylamide in coffee by liquid chromatography and tandem mass spectrometry analysis (LC/MS/MS) using SPE clean-up. Analytical separation of acrylamide from roasted coffee was performed by liquid chromatography using a Hypercarb column followed by LC/MS/MS analysis, with 2,3,3-d3 acrylamide as an internal standard. The method was based on two purification steps: the first with hexane and Carrez solutions in order to remove of fat and to precipitate proteins, respectively; and the second with a solid-phase extraction (SPE) column which proved to be efficient in the elimination of the main chromatographic interferences. Limit of quantification (LOQ) for measuring acrylamide in coffee was 50 microg/kg. The described method demonstrates satisfactory precision (RSD = 2.5%), repeatability (RSD = 9.2%) and accuracy (mean recovery - 97.4%). Our results confirm that LC-MS/MS with SPE clean-up is selective and suitable for determination of acrylamide in coffee. Indeed, this method meets the criteria of EU Commission Recommendations (No. 2007/331/EC and No. 2010/307/EU), on the monitoring of acrylamide levels in food.

  2. Application of a simple column-switching ion chromatography technique for removal of matrix interferences and sensitive fluorescence determination of acidic compounds (pharmaceutical drugs) in complex samples.

    PubMed

    Muhammad, Nadeem; Subhani, Qamar; Wang, Fenglian; Guo, Dandan; Zhao, Qiming; Wu, Shuchao; Zhu, Yan

    2017-09-15

    This work illustrates the introduction of a simple, rugged and flexible column-switching ion chromatography (IC) technique for an automated on-line QuEChERS extracted samples extracts washing followed by sensitive fluorescence (FLD) determination of five acidic pharmaceutical drugs namely; clofibric acid (CLO), ibuprofen (IBU), aspirin (ASP), naproxen (NAP) and flurobrofen (FLU) in three complex samples (spinach, apple and hospital sewage sludge). An old anion exchange column IonPac ® AS11-HC was utilized as a pre-treatment column for on-line washing of inorganic and organic interferences followed by isocratic separation of five acidic drugs with another anion exchange IonPac ® AS12A analytical column by exploiting the column-switching technique. This novel method exhibited good linearity with correlation coefficients (r 2 ) for all drugs were in the range 0.976-0.996. The limit of detection and quantification of all five acidic drugs were in the range 0.024μg/kg to 8.70μg/kg and 0.082μg/kg to 0.029mg/kg, respectively, and better recoveries in the range 81.17-112.5% with percentage relative standard deviations (RSDs) less than 17.8% were obtained. This on-line sample pre-treatment method showed minimum matrix effect in the range of 0.87-1.25 except for aspirin. This simple rugged and flexible column-switching system required only 28min for maximum elimination of matrices and interferences in three complex samples extracts, isocratic separation of five acidic drugs and for the continuous regeneration of pre-treatment column prior to every subsequent analysis. Finally, this simple automated IC system was appeared so rugged and flexible, which can eliminate and wash out most of interference, impurities and matrices in complex samples, simply by adjusting the NaOH and acetonitrile concentration in washing mobile phase with maximum recoveries of acidic analytes of interest. Copyright © 2017. Published by Elsevier B.V.

  3. A novel approach to signal normalisation in atmospheric pressure ionisation mass spectrometry.

    PubMed

    Vogeser, Michael; Kirchhoff, Fabian; Geyer, Roland

    2012-07-01

    The aim of our study was to test an alternative principle of signal normalisation in LC-MS/MS. During analyses, post column infusion of the target analyte is done via a T-piece, generating an "area under the analyte peak" (AUP). The ratio of peak area to AUP is assessed as assay response. Acceptable analytical performance of this principle was found for an exemplary analyte. Post-column infusion may allow normalisation of ion suppression not requiring any additional standard compound. This approach can be useful in situations where no appropriate compound is available for classical internal standardisation. Copyright © 2012 Elsevier B.V. All rights reserved.

  4. Organelle relationships in cultured 3T3-L1 preadipocytes

    PubMed Central

    1980-01-01

    In differentiating 3T3-L1 cells, lipid spheres, the endoplasmic reticulum (ER), microperoxisomes, and mitochondria form "constellations" that may reflect the interplay of lipid metabolizing enzymes in these organelles. ER cisternae are also situated very close to "rosettes,"plasmalemmal specializations found in mature adipocytes in vivo. As in hepatocytes and absorptive cells of the intestine, this spatial relationship of ER and plasmalemma suggests a role for rosettes in the uptake of exogenous lipid precursors. The morphological differentiation of 3T3-L1 preadipocytes includes the loss of "stress fibers" and the appearance of microfilament like structures that encase, in a complex manner, the cytosolic lipid spheres that appear during differentiation. Other features described for the first time in 3T3-L1 preadipocytes include: (a) the presence of an extensive acid phosphatase (AcPase) positive GERL from which coated vesicles apparently arise (these coated vesicles display AcPase activity and are much smaller and far more numerous than the coated vesicles that seem to arise from the plasmalemmal coated pits); (b) the abundance of AcPase-positive autophagic vacuoles; and (c) a high level of alpha- naphthyl-acetate-esterase activity which, by light microscopy cytochemistry, appears to be localized in the cytosol. PMID:7191426

  5. Rapid determination of caffeoylquinic acid derivatives in Cynara scolymus L. by ultra-fast liquid chromatography/tandem mass spectrometry based on a fused core C18 column.

    PubMed

    Shen, Qing; Dai, Zhiyuan; Lu, Yanbin

    2010-10-01

    An ultra-fast high-performance LC-ESI-MS/MS method was developed for the analysis and quantification of caffeoylquinic acid derivatives, including chlorogenic acid, 1,3-di-O-caffeoylquinic acid (cynarin) and 1,5-di-O-caffeoylquinic acid, in artichoke (Cynara scolymus L.) heads and leaves. The rapid separation (less than 4  min) was achieved based on a Halo fused core C18-silica column (50  mm × 2.1  mm id, 2.7  μm). The target compounds were detected and quantified by a triple-quadrupole mass spectrometer in multiple-reaction monitoring mode. The calibration function is linear from 0.06 to 2800  ng/mL for chlorogenic acid, 0.3-3000  ng/mL for cynarin and 0.24-4800  ng/mL for 1,5-di-O-caffeoylquinic acid, respectively. The average recoveries ranged from 92.1 to 113.2% with RSDs ≤6.5%. Moreover, four batches of artichoke head and leaf extracts were analyzed using the established method. The results indicated that the Halo fused core column provided much faster separations and higher sample throughput without sacrificing column ruggedness and reliability, and triple-quadrupole MS provided extraordinarily lower LOQs for most of the target analytes. Comparing to conventional quantitative approaches, the established method was fast, sensitive and reliable for the determination of caffeoylquinic acid derivatives in artichoke.

  6. Ability of γδ T cells to modulate the Foxp3 T cell response is dependent on adenosine.

    PubMed

    Liang, Dongchun; Woo, Jeong-Im; Shao, Hui; Born, Willi K; O'Brien, Rebecca L; Kaplan, Henry J; Sun, Deming

    2018-01-01

    Whether γδ T cells inhibit or enhance the Foxp3 T cell response depends upon their activation status. The critical enhancing effector in the supernatant is adenosine. Activated γδ T cells express adenosine receptors at high levels, which enables them to deprive Foxp3+ T cells of adenosine, and to inhibit their expansion. Meanwhile, cell-free supernatants of γδ T cell cultures enhance Foxp3 T cell expansion. Thus, inhibition and enhancement by γδ T cells of Foxp3 T cell response are a reflection of the balance between adenosine production and absorption by γδ T cells. Non-activated γδ T cells produce adenosine but bind little, and thus enhance the Foxp3 T cell response. Activated γδ T cells express high density of adenosine receptors and have a greatly increased ability to bind adenosine. Extracellular adenosine metabolism and expression of adenosine receptor A2ARs by γδ T cells played a major role in the outcome of γδ and Foxp3 T cell interactions. A better understanding of the functional conversion of γδ T cells could lead to γδ T cell-targeted immunotherapies for related diseases.

  7. Cytotoxicity of Titanate-Calcium Complexes to MC3T3 Osteoblast-Like Cells

    DOE PAGES

    Chen, Yen-Wei; Drury, Jeanie L.; Moussi, Joelle; ...

    2016-11-30

    Monosodium titanates (MST) are a relatively novel form of particulate titanium dioxide that have been proposed for biological use as metal sorbents or delivery agents, most recently calcium (II). In these roles, the toxicity of the titanate or its metal complex is crucial to its biological utility. The aim of this study was to determine the cytotoxicity of MST and MST-calcium complexes with MC3T3 osteoblast-like cells; MST-Ca(II) complexes could be useful to promote bone formation in various hard tissue applications. MC3T3 cells were exposed to native MST or MST-Ca(II) complexes for 24–72 h. A CellTiter-Blue ® assay was employed tomore » assess the metabolic activity of the cells. The results showed that MST and MST-Ca(II) suppressed MC3T3 metabolic activity significantly in a dose-, time-, and cell-density-dependent fashion. MST-Ca(II) suppressed MC3T3 metabolism in a statistically identical manner as native MST at all concentrations. We concluded that MST and MST-Ca(II) are significantly cytotoxic to MC3T3 cells through a mechanism yet unknown; this is a potential problem to the biological utility of these complexes.« less

  8. Cytotoxicity of Titanate-Calcium Complexes to MC3T3 Osteoblast-Like Cells

    PubMed Central

    Drury, Jeanie L.; Moussi, Joelle; Taylor-Pashow, Kathryn M. L.

    2016-01-01

    Monosodium titanates (MST) are a relatively novel form of particulate titanium dioxide that have been proposed for biological use as metal sorbents or delivery agents, most recently calcium (II). In these roles, the toxicity of the titanate or its metal complex is crucial to its biological utility. The aim of this study was to determine the cytotoxicity of MST and MST-calcium complexes with MC3T3 osteoblast-like cells; MST-Ca(II) complexes could be useful to promote bone formation in various hard tissue applications. MC3T3 cells were exposed to native MST or MST-Ca(II) complexes for 24–72 h. A CellTiter-Blue® assay was employed to assess the metabolic activity of the cells. The results showed that MST and MST-Ca(II) suppressed MC3T3 metabolic activity significantly in a dose-, time-, and cell-density-dependent fashion. MST-Ca(II) suppressed MC3T3 metabolism in a statistically identical manner as native MST at all concentrations. We concluded that MST and MST-Ca(II) are significantly cytotoxic to MC3T3 cells through a mechanism yet unknown; this is a potential problem to the biological utility of these complexes. PMID:28044136

  9. 6-gingerol inhibits rosiglitazone-induced adipogenesis in 3T3-L1 adipocytes.

    PubMed

    Tzeng, Thing-Fong; Chang, Chia Ju; Liu, I-Min

    2014-02-01

    We investigated the effects of 6-gingerol ((S)-5-hydroxy-1-(4-hydroxy-3-methoxyphenyl)-3-decanone) on the inhibition of rosiglitazone (RGZ)-induced adipogenesis in 3T3-L1 cells. The morphological changes were photographed based on staining lipid accumulation by Oil-Red O in RGZ (1 µmol/l)-treated 3T3-L1 cells without or with various concentrations of 6-gingerol on differentiation day 8. Quantitation of triglycerides content was performed in cells on day 8 after differentiation induction. Differentiated cells were lysed to detect mRNA and protein levels of adipocyte-specific transcription factors by real-time reverse transcription-polymerase chain reaction and Western blot analysis, respectively. 6-gingerol (50 µmol/l) effectively suppressed oil droplet accumulation and reduced the sizes of the droplets in RGZ-induced adipocyte differentiation in 3T3-L1 cells. The triglyceride accumulation induced by RGZ in differentiated 3T3-L1 cells was also reduced by 6-gingerol (50 µmol/l). Treatment of differentiated 3T3-L1 cells with 6-gingerol (50 µmol/l) antagonized RGZ-induced gene expression of peroxisome proliferator-activated receptor (PPAR)γ and CCAAT/enhancer-binding protein α. Additionally, the increased levels of mRNA and protein in adipocyte-specific fatty acid binding protein 4 and fatty acid synthase induced by RGZ in 3T3-L1 cells were decreased upon treatment with 6-gingerol. Our data suggests that 6-gingerol may be beneficial in obesity, by reducing adipogenesis partly through the down-regulating PPARγ activity. Copyright © 2013 John Wiley & Sons, Ltd.

  10. Schinus terebinthifolius countercurrent chromatography (Part III): Method transfer from small countercurrent chromatography column to preparative centrifugal partition chromatography ones as a part of method development.

    PubMed

    das Neves Costa, Fernanda; Hubert, Jane; Borie, Nicolas; Kotland, Alexis; Hewitson, Peter; Ignatova, Svetlana; Renault, Jean-Hugues

    2017-03-03

    Countercurrent chromatography (CCC) and centrifugal partition chromatography (CPC) are support free liquid-liquid chromatography techniques sharing the same basic principles and features. Method transfer has previously been demonstrated for both techniques but never from one to another. This study aimed to show such a feasibility using fractionation of Schinus terebinthifolius berries dichloromethane extract as a case study. Heptane - ethyl acetate - methanol -water (6:1:6:1, v/v/v/v) was used as solvent system with masticadienonic and 3β-masticadienolic acids as target compounds. The optimized separation methodology previously described in Part I and II, was scaled up from an analytical hydrodynamic CCC column (17.4mL) to preparative hydrostatic CPC instruments (250mL and 303mL) as a part of method development. Flow-rate and sample loading were further optimized on CPC. Mobile phase linear velocity is suggested as a transfer invariant parameter if the CPC column contains sufficient number of partition cells. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. Phosphoinositide 3–kinase γ participates in T cell receptor–induced T cell activation

    PubMed Central

    Alcázar, Isabela; Marqués, Miriam; Kumar, Amit; Hirsch, Emilio; Wymann, Matthias; Carrera, Ana C.; Barber, Domingo F.

    2007-01-01

    Class I phosphoinositide 3–kinases (PI3Ks) constitute a family of enzymes that generates 3-phosphorylated polyphosphoinositides at the cell membrane after stimulation of protein tyrosine (Tyr) kinase–associated receptors or G protein–coupled receptors (GPCRs). The class I PI3Ks are divided into two types: class IA p85/p110 heterodimers, which are activated by Tyr kinases, and the class IB p110γ isoform, which is activated by GPCR. Although the T cell receptor (TCR) is a protein Tyr kinase–associated receptor, p110γ deletion affects TCR-induced T cell stimulation. We examined whether the TCR activates p110γ, as well as the consequences of interfering with p110γ expression or function for T cell activation. We found that after TCR ligation, p110γ interacts with Gαq/11, lymphocyte-specific Tyr kinase, and ζ-associated protein. TCR stimulation activates p110γ, which affects 3-phosphorylated polyphosphoinositide levels at the immunological synapse. We show that TCR-stimulated p110γ controls RAS-related C3 botulinum substrate 1 activity, F-actin polarization, and the interaction between T cells and antigen-presenting cells, illustrating a crucial role for p110γ in TCR-induced T cell activation. PMID:17998387

  12. Comparison of 3T and 7T susceptibility-weighted angiography of the substantia nigra in diagnosing Parkinson disease.

    PubMed

    Cosottini, M; Frosini, D; Pesaresi, I; Donatelli, G; Cecchi, P; Costagli, M; Biagi, L; Ceravolo, R; Bonuccelli, U; Tosetti, M

    2015-03-01

    Standard neuroimaging fails in defining the anatomy of the substantia nigra and has a marginal role in the diagnosis of Parkinson disease. Recently 7T MR target imaging of the substantia nigra has been useful in diagnosing Parkinson disease. We performed a comparative study to evaluate whether susceptibility-weighted angiography can diagnose Parkinson disease with a 3T scanner. Fourteen patients with Parkinson disease and 13 healthy subjects underwent MR imaging examination at 3T and 7T by using susceptibility-weighted angiography. Two expert blinded observers and 1 neuroradiology fellow evaluated the 3T and 7T images of the sample to identify substantia nigra abnormalities indicative of Parkinson disease. Diagnostic accuracy and intra- and interobserver agreement were calculated separately for 3T and 7T acquisitions. Susceptibility-weighted angiography 7T MR imaging can diagnose Parkinson disease with a mean sensitivity of 93%, specificity of 100%, and diagnostic accuracy of 96%. 3T MR imaging diagnosed Parkinson disease with a mean sensitivity of 79%, specificity of 94%, and diagnostic accuracy of 86%. Intraobserver and interobserver agreement was excellent at 7T. At 3T, intraobserver agreement was excellent for experts, and interobserver agreement ranged between good and excellent. The less expert reader obtained a diagnostic accuracy of 89% at 3T. Susceptibility-weighted angiography images obtained at 3T and 7T differentiate controls from patients with Parkinson disease with a higher diagnostic accuracy at 7T. The capability of 3T in diagnosing Parkinson disease might encourage its use in clinical practice. The use of the more accurate 7T should be supported by a dedicated cost-effectiveness study. © 2015 by American Journal of Neuroradiology.

  13. Leaching behaviour of azoxystrobin and metabolites in soil columns.

    PubMed

    Ghosh, Rakesh Kumar; Singh, Neera

    2009-09-01

    Azoxystrobin [methyl (E)-2-{2-[6-(2-cyanophenoxy)pyrimidin-4-yloxy]phenyl}-3-methoxyacrylate], a strobilurin fungicide, is a broad-spectrum, systemic and soil-applied fungicide. Azoxystrobin has been registered for rice cultivation in India, but no information is available on its leaching behaviour in Indian soils. Therefore, leaching behaviour of azoxystrobin was studied in packed and intact soil columns under different irrigation regimes. Azoxystrobin did not leach out of the 300 mm long columns after 126 and 362 mm rainfall. After percolating water equivalent to 362 mm rainfall, azoxystrobin leached down to 10-15 cm (packed columns) and 15-20 cm (intact columns) depth. Azoxystrobin was not detected in the leachate from the packed column leached with 94.5 mL water every week (140 mm rainfall per month) during the 28 weeks of the study period. However, azoxystrobin acid, formed by azoxystrobin degradation, was detected in the leachate after 18 weeks. At the end of the study, azoxystrobin had leached down to 5-10 cm depth, and only 60% of initially applied azoxystrobin was recovered from the soil. The results indicate that azoxystrobin is fairly immobile in sandy loam soil, but azoxystrobin acid, a major metabolite of azoxystrobin, is quite mobile and may pose a threat of soil and groundwater contamination. Copyright 2009 Society of Chemical Industry.

  14. Understanding Business Analytics

    DTIC Science & Technology

    2015-01-05

    analytics have been used in organizations for a variety of reasons for quite some time; ranging from the simple (generating and understanding business analytics...process. understanding business analytics 3 How well these two components are orchestrated will determine the level of success an organization has in

  15. Significance of fixation of the vertebral column for spinal cord injury experiments.

    PubMed

    Liu, Fei; Luo, Zhuo-Jin; You, Si-Wei; Jiao, Xi-Ying; Meng, Xiao-Mei; Shi, Ming; Wang, Chun-Ting; Ju, Gong

    2003-08-01

    consistently far better than the unfixed group. The quantitative analyses were as follows (fixed/unfixed): 1)volume of secondary degeneration: 1.07 +/- 0.20/1.81 +/- 0.43 mm3 (P < 0.01); 2) volume of meningeal scar: 2.38 +/- 0.55/4.34 +/- 1.40 mm3 (P < 0.05); 3) distance between cord stumps: 1.38 +/- 0.34/2.35 +/- 0.79 mm (P < 0.05); 4) the mean thinnest dimension of the meningeal scar: 0.90 +/- 0.43/1.98 +/- 0.85 mm (P < 0.05). Vertebral column fixation is a crucial procedure for spinal cord animal experiments.

  16. Results of the eruptive column model inter-comparison study

    USGS Publications Warehouse

    Costa, Antonio; Suzuki, Yujiro; Cerminara, M.; Devenish, Ben J.; Esposti Ongaro, T.; Herzog, Michael; Van Eaton, Alexa; Denby, L.C.; Bursik, Marcus; de' Michieli Vitturi, Mattia; Engwell, S.; Neri, Augusto; Barsotti, Sara; Folch, Arnau; Macedonio, Giovanni; Girault, F.; Carazzo, G.; Tait, S.; Kaminski, E.; Mastin, Larry G.; Woodhouse, Mark J.; Phillips, Jeremy C.; Hogg, Andrew J.; Degruyter, Wim; Bonadonna, Costanza

    2016-01-01

    This study compares and evaluates one-dimensional (1D) and three-dimensional (3D) numerical models of volcanic eruption columns in a set of different inter-comparison exercises. The exercises were designed as a blind test in which a set of common input parameters was given for two reference eruptions, representing a strong and a weak eruption column under different meteorological conditions. Comparing the results of the different models allows us to evaluate their capabilities and target areas for future improvement. Despite their different formulations, the 1D and 3D models provide reasonably consistent predictions of some of the key global descriptors of the volcanic plumes. Variability in plume height, estimated from the standard deviation of model predictions, is within ~ 20% for the weak plume and ~ 10% for the strong plume. Predictions of neutral buoyancy level are also in reasonably good agreement among the different models, with a standard deviation ranging from 9 to 19% (the latter for the weak plume in a windy atmosphere). Overall, these discrepancies are in the range of observational uncertainty of column height. However, there are important differences amongst models in terms of local properties along the plume axis, particularly for the strong plume. Our analysis suggests that the simplified treatment of entrainment in 1D models is adequate to resolve the general behaviour of the weak plume. However, it is inadequate to capture complex features of the strong plume, such as large vortices, partial column collapse, or gravitational fountaining that strongly enhance entrainment in the lower atmosphere. We conclude that there is a need to more accurately quantify entrainment rates, improve the representation of plume radius, and incorporate the effects of column instability in future versions of 1D volcanic plume models.

  17. TEFLON BELLOWS PULSE GENERATORS FOR SOLVENT EXTRACTION PULSE COLUMNS

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    McCarthy, P.B.

    1954-01-01

    A Teflon bellows-type pulse generator is described which consists of two 3-in. nominal diameter Teflon bellows mounted on either end of a flanged spool piece and rigidly connected internally by a push rod so that the two of bellows move in tandem. The ends of the two bellows are closed by means of blind flanges. Tne spool piece is designed for insertion in a 6-in. diameter nozzle on a solvent extraction pulse column. The double bellows arrangement constitutes a safety feature to prevent loss of the column contents in the event of failure of the inner bellows in contact withmore » column solution. Failure of the inner bellows may be detected by a conductivity probe mounted in the air space inside of the double bellows assembly. Reciprocating motion is imcrank arm rigidly connected through a cross head and push rod to the face of the external bellows flange. The push rod is guided by means of linear ball bushings. Frequency variation over a range of 30 to 100 cycles/ min.was obtained by use of a Thymotrol-controlled electric motor to drive the crank arm. Variable stroke adjustment (0 to 1-in. range) was possible by adjustment of linkages on the crank arm. A load compensating spring was founnd desirable to counteract the thrust on the push rod resulting tom the static pressure at the bottom of the solvent extraction column. Without the spring, accelerated wear of the bearing on the crank arm occured. The pulse generator operated uneventfully for 1776 hours (6.61x lO/sup 6/ cycles) at a frequency of 62 cycles/min. and a bellows travel of l-in. (equivalent to a displacement of 1.6 in. in a 3-in. diam. column). (auth)« less

  18. Chromatographic properties PLOT multicapillary columns.

    PubMed

    Nikolaeva, O A; Patrushev, Y V; Sidelnikov, V N

    2017-03-10

    Multicapillary columns (MCCs) for gas chromatography make it possible to perform high-speed analysis of the mixtures of gaseous and volatile substances at a relatively large amount of the loaded sample. The study was performed using PLOT MCCs for gas-solid chromatography (GSC) with different stationary phases (SP) based on alumina, silica and poly-(1-trimethylsilyl-1-propyne) (PTMSP) polymer as well as porous polymers divinylbenzene-styrene (DVB-St), divinylbenzene-vinylimidazole (DVB-VIm) and divinylbenzene-ethylene glycol dimethacrylate (DVB-EGD). These MCCs have the efficiency of 4000-10000 theoretical plates per meter (TP/m) and at a column length of 25-30cm can separate within 10-20s multicomponent mixtures of substances belonging to different classes of chemical compounds. The sample amount not overloading the column is 0.03-1μg and depends on the features of a porous layer. Examples of separations on some of the studied columns are considered. Copyright © 2017 Elsevier B.V. All rights reserved.

  19. Observed and simulated time evolution of HCl, ClONO2, and HF total columns

    NASA Astrophysics Data System (ADS)

    Ruhnke, Roland; Geomon, Ndacc Infrared, Modelling Working Group

    2010-05-01

    GEOmon, NDACC Infrared, and Modelling Working Group: M.P. Chipperfield (2), M. De Mazière (3), J. Notholt (4), S. Barthlott (1), R.L. Batchelor (5,17), R.D. Blatherwick (16), Th. Blumenstock (1), M.T. Coffey (17), P. Duchatelet (6), H. Fast (7), W. Feng (2), A. Goldman (16), D.W.T. Griffith (8), K. Hamann (1), J.W. Hannigan (17), F. Hase (1), N.B. Jones (8), A. Kagawa (9,10), Y. Kasai (9), O. Kirner (19), R. Kohlhepp (1), W. Kouker (1), I. Kramer (1), R. Lindenmaier (5), E. Mahieu (6), R.L. Mittermeier (7), B. Monge-Sanz (2), I. Murata (12), H. Nakajima (13), I. Morino (11), M. Palm (4), C. Paton-Walsh (8), Th. Reddmann (1), M. Rettinger (15), C.P. Rinsland (18), M. Schneider (1), C. Senten (3), B.-M. Sinnhuber (4), D. Smale (14), K. Strong (5), R. Sussmann (15), J.R. Taylor (5), G. Vanhaelewyn (3), T. Warneke (4), C. Whaley (5), M. Wiehle (1), and S.W. Wood (14) (1) Karlsruhe Institute of Technology (KIT), IMK-ASF, Karlsruhe, Germany, (2) University of Leeds, Leeds, United Kingdom, (3) Belgian Institute for Space Aeronomy (BIRA-IASB), Brussels, Belgium, (4) University of Bremen, Institute of Environmental Physics, Bremen, Germany, (5) Department of Physics, University of Toronto, Toronto, Ontario, Canada, (6) University of Liège, Institute of Astrophysics and Geophysics, Liège, Belgium, (7) Environment Canada, Toronto, Ontario, Canada, (8) Centre for Atmospheric Chemistry, University of Wollongong, Wollongong, Australia, (9) National Institute of Information and Communications Technology, Tokyo, Japan, (10) Fujitsu FIP Corporation, Tokyo, Japan, (11) Center for Global Environmental Research, National Institute for Environmental Studies (NIES), Japan, (12) Department of Environmental Studies, Graduate School of Environmental Studies, Tohoku University, Japan, (13) Atmospheric Environment Division, National Institute for Environmental Studies, Japan, (14) National Institute of Water and Atmospheric Research Ltd (NIWA), Lauder, New Zealand, (15) Karlsruhe

  20. Effect of Preexisting Corrosion on Fatigue Cracking of Aluminum Alloys 2024-T3 and 7075-T6

    DTIC Science & Technology

    1995-08-01

    alloys 2024 -T3 and 7075-T6. It was determined that preexisting corrosion has a detrimental effect on the fatigue life of aluminum alloys 2024 -T3 and...following conclusions were drawn: 1. Preexisting corrosion has a detrimental effect on the fatigue life of aluminum alloys 2024 -T3 and 7075-T6. The...corrosion has a detrimental effect on the fatigue life of aluminum alloys

  1. Determination of Total Biotin by Liquid Chromatography Coupled with Immunoaffinity Column Cleanup Extraction: Multilaboratory Testing, Final Action 2016.02.

    PubMed

    Joseph, George; Devi, Ranjani; Marley, Elaine C; Leeman, David

    2018-05-01

    Single- and multilaboratory testing data have provided systematic scientific evidence that a simple, selective, accurate, and precise method can be used as a potential candidate reference method for dispute resolution in determining total biotin in all forms of infant, adult, and/or pediatric formula. Using LC coupled with immunoaffinity column cleanup extraction, the method fully meets the intended purpose and applicability statement in AOAC Standard Method Performance Requirement 2014.005. The method was applied to a cross-section of infant formula and adult nutritional matrixes, and acceptable precision and accuracy were established. The analytical platform is inexpensive, and the method can be used in almost any laboratory worldwide with basic facilities. The immunoaffinity column cleanup extraction is the key step to successful analysis.

  2. Seismic retrofit of cruciform-shaped columns in the Aurora Avenue Bridge using FRP wrapping.

    DOT National Transportation Integrated Search

    2010-08-01

    Experimental tests were conducted on seven 1/3-scale column specimens to evaluate the vulnerabilities of existing cruciform-shaped columns and to develop appropriate retrofit measures that address the identified vulnerabilities. The specimens represe...

  3. Validation of a multi-analyte HPLC-DAD method for determination of uric acid, creatinine, homovanillic acid, niacinamide, hippuric acid, indole-3-acetic acid and 2-methylhippuric acid in human urine.

    PubMed

    Remane, Daniela; Grunwald, Soeren; Hoeke, Henrike; Mueller, Andrea; Roeder, Stefan; von Bergen, Martin; Wissenbach, Dirk K

    2015-08-15

    During the last decades exposure sciences and epidemiological studies attracts more attention to unravel the mechanisms for the development of chronic diseases. According to this an existing HPLC-DAD method for determination of creatinine in urine samples was expended for seven analytes and validated. Creatinine, uric acid, homovanillic acid, niacinamide, hippuric acid, indole-3-acetic acid, and 2-methylhippuric acid were separated by gradient elution (formate buffer/methanol) using an Eclipse Plus C18 Rapid Resolution column (4.6mm×100mm). No interfering signals were detected in mobile phase. After injection of blank urine samples signals for the endogenous compounds but no interferences were detected. All analytes were linear in the selected calibration range and a non weighted calibration model was chosen. Bias, intra-day and inter-day precision for all analytes were below 20% for quality control (QC) low and below 10% for QC medium and high. The limits of quantification in mobile phase were in line with reported reference values but had to be adjusted in urine for homovanillic acid (45mg/L), niacinamide 58.5(mg/L), and indole-3-acetic acid (63mg/L). Comparison of creatinine data obtained by the existing method with those of the developed method showing differences from -120mg/L to +110mg/L with a mean of differences of 29.0mg/L for 50 authentic urine samples. Analyzing 50 authentic urine samples, uric acid, creatinine, hippuric acid, and 2-methylhippuric acid were detected in (nearly) all samples. However, homovanillic acid was detected in 40%, niacinamide in 4% and indole-3-acetic acid was never detected within the selected samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  4. 3D volumetry comparison using 3T magnetic resonance imaging between normal and adenoma-containing pituitary glands.

    PubMed

    Roldan-Valadez, Ernesto; Garcia-Ulloa, Ana Cristina; Gonzalez-Gutierrez, Omar; Martinez-Lopez, Manuel

    2011-01-01

    Computed-assisted three-dimensional data (3D) allows for an accurate evaluation of volumes compared with traditional measurements. An in vitro method comparison between geometric volume and 3D volumetry to obtain reference data for pituitary volumes in normal pituitary glands (PGs) and PGs containing adenomas. Prospective, transverse, analytical study. Forty-eight subjects underwent brain magnetic resonance imaging (MRI) with 3D sequencing for computer-aided volumetry. PG phantom volumes by both methods were compared. Using the best volumetric method, volumes of normal PGs and PGs with adenoma were compared. Statistical analysis used the Bland-Altman method, t-statistics, effect size and linear regression analysis. Method comparison between 3D volumetry and geometric volume revealed a lower bias and precision for 3D volumetry. A total of 27 patients exhibited normal PGs (mean age, 42.07 ± 16.17 years), although length, height, width, geometric volume and 3D volumetry were greater in women than in men. A total of 21 patients exhibited adenomas (mean age 39.62 ± 10.79 years), and length, height, width, geometric volume and 3D volumetry were greater in men than in women, with significant volumetric differences. Age did not influence pituitary volumes on linear regression analysis. Results from the present study showed that 3D volumetry was more accurate than the geometric method. In addition, the upper normal limits of PGs overlapped with lower volume limits during early stage microadenomas.

  5. Silica-based monolithic column with evaporative light scattering detector for HPLC analysis of bacosides and apigenin in Bacopa monnieri.

    PubMed

    Bhandari, Pamita; Kumar, Neeraj; Singh, Bikram; Singh, Virendra; Kaur, Inderjeet

    2009-08-01

    A high performance liquid chromatographic method using a silica-based monolithic column coupled with evaporative light scattering detector (HPLC-ELSD) was developed and validated for simultaneous quantification of bacosides (bacoside A, bacopaside I, bacoside A(3), bacopaside II, bacopaside X, bacopasaponin C) and apigenin in Bacopa monnieri. The chromatographic resolution was achieved on a Chromolith RP-18 (100x4.6 mm) column with acetonitrile/water (30:70) as mobile phase in isocratic elution at a flow rate of 0.7 mL/min. The drift tube temperature of the ELSD was set to 95 degrees C, and the nitrogen flow rate was 2.0 SLM (standard liter per minute). The calibration curves revealed a good linear relationship (r(2) > 0.9988) within the test ranges. The detection limits (S/N = 3) and the quantification limits (S/N = 10) for the compounds were in the range of 0.54-6.06 and 1.61-18.78 microg/mL, respectively. Satisfactory average recovery was observed in the range of 95.8-99.0%. The method showed good reproducibility for the quantification of these compounds in B. monnieri with intra- and inter-day precision of less than 0.69 and 0.67%, respectively. The validated method was successfully applied to quantify analytes in nine accessions of B. monnieri and thus provides a new basis for overall quality assessment of B. monnieri.

  6. Determination of ochratoxin A in wine by means of immunoaffinity and aminopropyl solid-phase column cleanup and fluorometric detection.

    PubMed

    Longobardi, Francesco; Iacovelli, Vito; Catucci, Lucia; Panzarini, Giuseppe; Pascale, Michelangelo; Visconti, Angelo; Agostiano, Angela

    2013-02-27

    A new analytical method for the determination of ochratoxin A (OTA) in red wine has been developed by using a double-extract cleanup and a fluorometric measurement after spectral deconvolution. Wine samples were diluted with a solution containing 1% polyethylene glycol and 5% sodium hydrogencarbonate, filtered, and purified by immunoaffinity and aminopropyl solid-phase column. OTA contents in the purified extract were determined by a spectrofluorometer (excitation wavelength, 330 nm; emission wavelength, 470 nm) after deconvolution of fluorescence spectra. Average recoveries from wine samples spiked with OTA at levels ranging from 0.5 to 3.0 ng/mL were 94.5-105.4% with relative standard deviations (RSD) of <15% (n = 4). The limit of detection (LOD) was 0.2 ng/mL, and the total time of analysis was 30 min. The developed method was tested on 18 red wine samples (naturally contaminated and spiked with OTA at levels ranging from 0.4 to 3.0 ng/mL) and compared with AOAC Official Method 2001.01, based on immunoaffinity column cleanup and HPLC with fluorescence detector. A good correlation (r(2) = 0.9765) was observed between OTA levels obtained with the two methods, highlighting the reliability of the proposed method, the main advantage of which is the simple OTA determination by a benchtop fluorometer with evident reductions of cost and time of analysis.

  7. Feasibility of imaging superficial palmar arch using micro-ultrasound, 7T and 3T magnetic resonance imaging.

    PubMed

    Pruzan, Alison N; Kaufman, Audrey E; Calcagno, Claudia; Zhou, Yu; Fayad, Zahi A; Mani, Venkatesh

    2017-02-28

    To demonstrate feasibility of vessel wall imaging of the superficial palmar arch using high frequency micro-ultrasound, 7T and 3T magnetic resonance imaging (MRI). Four subjects (ages 22-50 years) were scanned on a micro-ultrasound system with a 45-MHz transducer (Vevo 2100, VisualSonics). Subjects' hands were then imaged on a 3T clinical MR scanner (Siemens Biograph MMR) using an 8-channel special purpose phased array carotid coil. Lastly, subjects' hands were imaged on a 7T clinical MR scanner (Siemens Magnetom 7T Whole Body Scanner) using a custom built 8-channel transmit receive carotid coil. All three imaging modalities were subjectively analyzed for image quality and visualization of the vessel wall. Results of this very preliminary study indicated that vessel wall imaging of the superficial palmar arch was feasible with a whole body 7T and 3T MRI in comparison with micro-ultrasound. Subjective analysis of image quality (1-5 scale, 1: poorest, 5: best) from B mode, ultrasound, 3T SPACE MRI and 7T SPACE MRI indicated that the image quality obtained at 7T was superior to both 3T MRI and micro-ultrasound. The 3D SPACE sequence at both 7T and 3T MRI with isotropic voxels allowed for multi-planar reformatting of images and allowed for less operator dependent results as compared to high frequency micro-ultrasound imaging. Although quantitative analysis revealed that there was no significant difference between the three methods, the 7T Tesla trended to have better visibility of the vessel and its wall. Imaging of smaller arteries at the 7T is feasible for evaluating atherosclerosis burden and may be of clinical relevance in multiple diseases.

  8. Functional and genomic analyses of FOXP3-transduced Jurkat-T cells as regulatory T (Treg)-like cells

    DOE Office of Scientific and Technical Information (OSTI.GOV)

    Kim, Joon-Young; Kim, Han-Jong; Hurt, Elaine M.

    2007-10-12

    FOXP3, a forkhead transcription factor is essential for the development and function of CD4{sup +}CD25{sup +} regulatory T cells (Tregs). In contrast to conversion of murine naive T cells to Tregs by transduction of Foxp3, it is controversial whether ectopic expression of FOXP3 in human CD4{sup +} T cells is sufficient for acquisition of suppressive activity. Here, we show that retroviral transduction of FOXP3 induces a Treg phenotype in human leukemic CD4{sup +} Jurkat-T cells, evidenced by increased expression of Treg-associated cell surface markers as well as inhibition of cytokine production. Furthermore, FOXP3-transduced Jurkat-T cells suppress the proliferation of humanmore » CD4{sup +}CD25{sup -} T cells. Additionally, DNA microarray analysis identifies Treg-related genes regulated by FOXP3. Our study demonstrates that enforced expression of FOXP3 confers Treg-like properties on Jurkat-T cells, which can be a convenient and efficient Treg-like cell model for further study to identify Treg cell surface markers and target genes regulated by FOXP3.« less

  9. Distinct human and mouse membrane trafficking systems for sweet taste receptors T1r2 and T1r3.

    PubMed

    Shimizu, Madoka; Goto, Masao; Kawai, Takayuki; Yamashita, Atsuko; Kusakabe, Yuko

    2014-01-01

    The sweet taste receptors T1r2 and T1r3 are included in the T1r taste receptor family that belongs to class C of the G protein-coupled receptors. Heterodimerization of T1r2 and T1r3 is required for the perception of sweet substances, but little is known about the mechanisms underlying this heterodimerization, including membrane trafficking. We developed tagged mouse T1r2 and T1r3, and human T1R2 and T1R3 and evaluated membrane trafficking in human embryonic kidney 293 (HEK293) cells. We found that human T1R3 surface expression was only observed when human T1R3 was coexpressed with human T1R2, whereas mouse T1r3 was expressed without mouse T1r2 expression. A domain-swapped chimera and truncated human T1R3 mutant showed that the Venus flytrap module and cysteine-rich domain (CRD) of human T1R3 contain a region related to the inhibition of human T1R3 membrane trafficking and coordinated regulation of human T1R3 membrane trafficking. We also found that the Venus flytrap module of both human T1R2 and T1R3 are needed for membrane trafficking, suggesting that the coexpression of human T1R2 and T1R3 is required for this event. These results suggest that the Venus flytrap module and CRD receive taste substances and play roles in membrane trafficking of human T1R2 and T1R3. These features are different from those of mouse receptors, indicating that human T1R2 and T1R3 are likely to have a novel membrane trafficking system.

  10. Genes that characterize T3-predominant Graves' thyroid tissues.

    PubMed

    Matsumoto, Chisa; Ito, Mitsuru; Yamada, Hiroya; Yamakawa, Noriko; Yoshida, Hiroshi; Date, Arisa; Watanabe, Mikio; Hidaka, Yoh; Iwatani, Yoshinori; Miyauchi, Akira; Takano, Toru

    2013-02-01

    3,5,3'-Triiodothyronine (T(3))-predominant Graves' disease is characterized by the increasing volume of thyroid goiter resulting in poor prognosis. Although type 1 and type 2 iodothyronine deiodinases (DIO1 and DIO2 respectively) are known to be overexpressed in the thyroid tissues of T(3)-predominant Graves' disease, the pathogenesis of this disease is still unclear. The aim of our study is to identify genes that characterize T(3)-predominant Graves' disease tissue in order to clarify the molecular mechanism of this disease. mRNAs from two thyroid tissues of both typical T(3)-predominant and common-type Graves' disease were analyzed with DNA microarrays with probes for 28 869 genes. Genes identified to be differentially expressed between the two groups were further analyzed in the second and third screenings using 70 Graves' thyroid tissues by real-time quantitative RT-PCR. Twenty-three candidate genes were selected as being differentially expressed in the first screening with microarrays. Among these, seven genes, leucine-rich repeat neuronal 1 (LRRN1), bone morphogenetic protein 8a (BMP8A), N-cadherin (CDH2), phosphodiesterase 1A (PDE1A), creatine kinase mitochondrial 2 (CKMT2), integrin beta-3 (ITGB3), and protein tyrosine phosphatase non-receptor type 4 (PTPN4), were confirmed to be differentially expressed in DIO1 or DIO2 over- and underexpressing Graves' tissues. These genes are related to the characteristics of T(3)-predominant Graves' disease, such as high titer level of serum anti-TSH receptor antibody, high free T(3) to free thyroxine ratio, and a large goiter size. They might play a role in the pathogenesis of T(3)-predominant Graves' disease.

  11. Variational Assimilation of GOME Total-Column Ozone Satellite Data in a 2D Latitude-Longitude Tracer-Transport Model.

    NASA Astrophysics Data System (ADS)

    Eskes, H. J.; Piters, A. J. M.; Levelt, P. F.; Allaart, M. A. F.; Kelder, H. M.

    1999-10-01

    A four-dimensional data-assimilation method is described to derive synoptic ozone fields from total-column ozone satellite measurements. The ozone columns are advected by a 2D tracer-transport model, using ECMWF wind fields at a single pressure level. Special attention is paid to the modeling of the forecast error covariance and quality control. The temporal and spatial dependence of the forecast error is taken into account, resulting in a global error field at any instant in time that provides a local estimate of the accuracy of the assimilated field. The authors discuss the advantages of the 4D-variational (4D-Var) approach over sequential assimilation schemes. One of the attractive features of the 4D-Var technique is its ability to incorporate measurements at later times t > t0 in the analysis at time t0, in a way consistent with the time evolution as described by the model. This significantly improves the offline analyzed ozone fields.

  12. Analytic energy gradients for the orbital-optimized third-order Møller-Plesset perturbation theory

    NASA Astrophysics Data System (ADS)

    Bozkaya, Uǧur

    2013-09-01

    Analytic energy gradients for the orbital-optimized third-order Møller-Plesset perturbation theory (OMP3) [U. Bozkaya, J. Chem. Phys. 135, 224103 (2011)], 10.1063/1.3665134 are presented. The OMP3 method is applied to problematic chemical systems with challenging electronic structures. The performance of the OMP3 method is compared with those of canonical second-order Møller-Plesset perturbation theory (MP2), third-order Møller-Plesset perturbation theory (MP3), coupled-cluster singles and doubles (CCSD), and coupled-cluster singles and doubles with perturbative triples [CCSD(T)] for investigating equilibrium geometries, vibrational frequencies, and open-shell reaction energies. For bond lengths, the performance of OMP3 is in between those of MP3 and CCSD. For harmonic vibrational frequencies, the OMP3 method significantly eliminates the singularities arising from the abnormal response contributions observed for MP3 in case of symmetry-breaking problems, and provides noticeably improved vibrational frequencies for open-shell molecules. For open-shell reaction energies, OMP3 exhibits a better performance than MP3 and CCSD as in case of barrier heights and radical stabilization energies. As discussed in previous studies, the OMP3 method is several times faster than CCSD in energy computations. Further, in analytic gradient computations for the CCSD method one needs to solve λ-amplitude equations, however for OMP3 one does not since λ _{ab}^{ij(1)} = t_{ij}^{ab(1)} and λ _{ab}^{ij(2)} = t_{ij}^{ab(2)}. Additionally, one needs to solve orbital Z-vector equations for CCSD, but for OMP3 orbital response contributions are zero owing to the stationary property of OMP3. Overall, for analytic gradient computations the OMP3 method is several times less expensive than CCSD (roughly ˜4-6 times). Considering the balance of computational cost and accuracy we conclude that the OMP3 method emerges as a very useful tool for the study of electronically challenging chemical

  13. Analytic energy gradients for the orbital-optimized third-order Møller-Plesset perturbation theory.

    PubMed

    Bozkaya, Uğur

    2013-09-14

    Analytic energy gradients for the orbital-optimized third-order Møller-Plesset perturbation theory (OMP3) [U. Bozkaya, J. Chem. Phys. 135, 224103 (2011)] are presented. The OMP3 method is applied to problematic chemical systems with challenging electronic structures. The performance of the OMP3 method is compared with those of canonical second-order Møller-Plesset perturbation theory (MP2), third-order Møller-Plesset perturbation theory (MP3), coupled-cluster singles and doubles (CCSD), and coupled-cluster singles and doubles with perturbative triples [CCSD(T)] for investigating equilibrium geometries, vibrational frequencies, and open-shell reaction energies. For bond lengths, the performance of OMP3 is in between those of MP3 and CCSD. For harmonic vibrational frequencies, the OMP3 method significantly eliminates the singularities arising from the abnormal response contributions observed for MP3 in case of symmetry-breaking problems, and provides noticeably improved vibrational frequencies for open-shell molecules. For open-shell reaction energies, OMP3 exhibits a better performance than MP3 and CCSD as in case of barrier heights and radical stabilization energies. As discussed in previous studies, the OMP3 method is several times faster than CCSD in energy computations. Further, in analytic gradient computations for the CCSD method one needs to solve λ-amplitude equations, however for OMP3 one does not since λ(ab)(ij(1))=t(ij)(ab(1)) and λ(ab)(ij(2))=t(ij)(ab(2)). Additionally, one needs to solve orbital Z-vector equations for CCSD, but for OMP3 orbital response contributions are zero owing to the stationary property of OMP3. Overall, for analytic gradient computations the OMP3 method is several times less expensive than CCSD (roughly ~4-6 times). Considering the balance of computational cost and accuracy we conclude that the OMP3 method emerges as a very useful tool for the study of electronically challenging chemical systems.

  14. INFLUENCE OF MATERIAL MODELS ON PREDICTING THE FIRE BEHAVIOR OF STEEL COLUMNS.

    PubMed

    Choe, Lisa; Zhang, Chao; Luecke, William E; Gross, John L; Varma, Amit H

    2017-01-01

    Finite-element (FE) analysis was used to compare the high-temperature responses of steel columns with two different stress-strain models: the Eurocode 3 model and the model proposed by National Institute of Standards and Technology (NIST). The comparisons were made in three different phases. The first phase compared the critical buckling temperatures predicted using forty seven column data from five different laboratories. The slenderness ratios varied from 34 to 137, and the applied axial load was 20-60 % of the room-temperature capacity. The results showed that the NIST model predicted the buckling temperature as or more accurately than the Eurocode 3 model for four of the five data sets. In the second phase, thirty unique FE models were developed to analyze the W8×35 and W14×53 column specimens with the slenderness ratio about 70. The column specimens were tested under steady-heating conditions with a target temperature in the range of 300-600 °C. The models were developed by combining the material model, temperature distributions in the specimens, and numerical scheme for non-linear analyses. Overall, the models with the NIST material properties and the measured temperature variations showed the results comparable to the test data. The deviations in the results from two different numerical approaches (modified Newton Raphson vs. arc-length) were negligible. The Eurocode 3 model made conservative predictions on the behavior of the column specimens since its retained elastic moduli are smaller than those of the NIST model at elevated temperatures. In the third phase, the column curves calibrated using the NIST model was compared with those prescribed in the ANSI/AISC-360 Appendix 4. The calibrated curve significantly deviated from the current design equation with increasing temperature, especially for the slenderness ratio from 50 to 100.

  15. [A comparison between 3.0 T MRI and histopathology for preoperative T staging of potentially resectable esophageal cancer].

    PubMed

    Wang, Z Q; Zhang, F G; Guo, J; Zhang, H K; Qin, J J; Zhao, Y; Ding, Z D; Zhang, Z X; Zhang, J B; Yuan, J H; Li, H L; Qu, J R

    2017-03-21

    Objective: To explore the value of 3.0 T MRI using multiple sequences (star VIBE+ BLADE) in evaluating the preoperative T staging for potentially resectable esophageal cancer (EC). Methods: Between April 2015 and March 2016, a total of 66 consecutive patients with endoscopically proven resectable EC underwent 3.0T MRI in the Affiliated Cancer Hospital of Zhengzhou University.Two independent readers were assigned a T staging on MRI according to the 7th edition of UICC-AJCC TNM Classification, the results of preoperative T staging were compared and analyzed with post-operative pathologic confirmation. Results: The MRI T staging of two readers were highly consistent with histopathological findings, and the sensitivity, specificity and accuracy of preoperative T staging MR imaging were also very high. Conclusion: 3.0 T MRI using multiple sequences is with high accuracy for patients of potentially resectable EC in T staging. The staging accuracy of T1, T2 and T3 is better than that of T4a. 3.0T MRI using multiple sequences could be used as a noninvasive imaging method for pre-operative T staging of EC.

  16. Characterization of peak capacity of microbore liquid chromatography columns using gradient kinetic plots.

    PubMed

    Hetzel, Terence; Blaesing, Christina; Jaeger, Martin; Teutenberg, Thorsten; Schmidt, Torsten C

    2017-02-17

    The performance of micro-liquid chromatography columns with an inner diameter of 0.3mm was investigated on a dedicated micro-LC system for gradient elution. Core-shell as well as fully porous particle packed columns were compared on the basis of peak capacity and gradient kinetic plot limits. The results for peak capacity showed the superior performance of columns packed with sub-2μm fully porous particles compared to 3.0μm fully porous and 2.7μm core-shell particles within a range of different gradient time to column void time ratios. For ultra-fast chromatography a maximum peak capacity of 16 can be obtained using a 30s gradient for the sub-2μm fully porous particle packed column. A maximum peak capacity of 121 can be achieved using a 5min gradient. In addition, the influence of an alternative detector cell on the basis of optical waveguide technology and contributing less to system variance was investigated showing an increased peak capacity for all applied gradient time/column void time ratios. Finally, the influence of pressure was evaluated indicating increased peak capacity for maximum performance whereas a limited benefit for ultra-fast chromatography with gradient times below 30s was observed. Copyright © 2017 Elsevier B.V. All rights reserved.

  17. T3 receptors in human pituitary tumors.

    PubMed

    Machiavelli, Gloria A; Pauni, Micaela; Heredia Sereno, Gastón M; Szijan, Irene; Basso, Armando; Burdman, José A

    2009-11-01

    The purpose of this work was to investigate the synthesis of T3 receptors in human tumors of the anterior pituitary gland, its relationship with the hormone synthesized and/or secreted by the tumor and the post-surgical evolution of the patient. Patients were evaluated clinically and by magnetic nuclear resonance to classify the adenoma according to their size. Hormonal concentrations in sera were determined by radioimmunoassay. Immunohistochemistry of the pituitary hormones was performed in the tumors. Tumors were obtained at surgery and immediately frozen in ice, transported to the laboratory and stored at -70 degrees C. Reverse transcription was performed with purified RNA from the tumors. Out of 33 pituitary tumors, 29 had RNA for T3 receptors synthesis (88%). They were present in different histological specimens, the tumors were grades 1-4 according to their size, and there was no relationship between the size of the tumor and the presence of T3 receptor RNAs. The post-surgical evolution of the patient was mostly dependent on the size and not on the presence of T3 receptors. The presence of thyroid hormone receptors in pituitary tumors is in line with two important characteristics of these tumors: they are histologically benign and well differentiated.

  18. REDISTRIBUTOR FOR LIQUID-LIQUID EXTRACTION COLUMNS

    DOEpatents

    Bradley, J.G.

    1957-10-29

    An improved baffle plate construction to intimately mix immiscible liquid solvents for solvent extraction processes in a liquid-liquid pulse column is described. To prevent the light and heavy liquids from forming separate continuous homogeneous vertical channels through sections of the column, a baffle having radially placed rectangular louvers with deflection plates opening upon alternate sides of the baffle is placed in the column, normal to the axis. This improvement substantially completely reduces strippiig losses due to poor mixing.

  19. CT and 3-T MRI accurately identify T3c disease in colon cancer, which strongly predicts disease-free survival.

    PubMed

    Hunter, C; Siddiqui, M; Georgiou Delisle, T; Blake, H; Jeyadevan, N; Abulafi, M; Swift, I; Toomey, P; Brown, G

    2017-04-01

    To compare the preoperative staging accuracy of computed tomography (CT) and 3-T magnetic resonance imaging (MRI) in colon cancer, and to investigate the prognostic significance of identified risk factors. Fifty-eight patients undergoing primary resection of their colon cancer were prospectively recruited, with 53 patients included for final analysis. Accuracy of CT and MRI were compared for two readers, using postoperative histology as the reference standard. Patients were followed-up for a median of 39 months. Risk factors were compared by modality and reader in terms of metachronous metastases and disease-free survival (DFS), stratified for adjuvant chemotherapy. Accuracy for the identification of T3c+ disease was non-significantly greater on MRI (75% and 79%) than CT (70% and 77%). Differences in the accuracy of MRI and CT for identification of T3+ disease (MRI 75% and 57%, CT 72% and 66%) and N+ disease (MRI 62% and 63%, CT 62% and 56%) were also non-significant. Identification of extramural venous invasion (EMVI+) disease was significantly greater on MRI (75% and 75%) than CT (79% and 54%) for one reader (p=0.029). T3c+ disease at histopathology was the only risk factor that demonstrated a significant difference in rate of metachronous metastases (odds ratio [OR] 8.6, p=0.0044) and DFS stratified for adjuvant therapy (OR=4, p=0.048). T3c or greater disease is the strongest risk factor for predicting DFS in colon cancer, and is accurately identified on imaging. T3c+ disease may therefore be the best imaging entry criteria for trials of neoadjuvant treatment. Copyright © 2017 The Royal College of Radiologists. Published by Elsevier Ltd. All rights reserved.

  20. Determination of free formaldehyde in cosmetics containing formaldehyde-releasing preservatives by reversed-phase dispersive liquid-liquid microextraction and liquid chromatography with post-column derivatization.

    PubMed

    Miralles, Pablo; Chisvert, Alberto; Alonso, M José; Hernandorena, Sandra; Salvador, Amparo

    2018-03-30

    An analytical method for the determination of traces of formaldehyde in cosmetic products containing formaldehyde-releasing preservatives has been developed. The method is based on reversed-phase dispersive liquid-liquid microextraction (RP-DLLME), that allows the extraction of highly polar compounds, followed by liquid chromatography-ultraviolet/visible (LC-UV/vis) determination with post-column derivatization. The variables involved in the RP-DLLME process were studied to provide the best enrichment factors. Under the selected conditions, a mixture of 500 μL of acetonitrile (disperser solvent) and 50 μL of water (extraction solvent) was rapidly injected into 5 mL of toluene sample solution. The extracts were injected into the LC-UV/vis system using phosphate buffer 6 mmol L -1 at pH 2 as mobile phase. After chromatographic separation, the eluate merged with a flow stream of pentane-2,4-dione in ammonium acetate solution as derivatizing reagent and passed throughout a post-column reactor at 85 °C in order to derivatize formaldehyde into 3,5-diacetyl-1,4-dihydrolutidine, according to Hantzsch reaction, which was finally measured spectrophotometrically at 407 nm. The method was successfully validated showing good linearity, an enrichment factor of 86 ± 2, limits of detection and quantification of 0.7 and 2.3 ng mL -1 , respectively, and good repeatability (RSD < 9.2%). Finally, the proposed analytical method was applied to the determination of formaldehyde in different commercial cosmetic samples containing formaldehyde-releasing preservatives, such as bronopol, diazolidinyl urea, imidazolidinyl urea, and DMDM hydantoin, with good relative recovery values (91-113%) thus showing that matrix effects were negligible. The good analytical features of the proposed method besides of its simplicity and affordability, make it useful to carry out the quality control of cosmetic products containing formaldehyde-releasing preservatives. Copyright

  1. High Strength Concrete Columns under Axial Compression Load: Hybrid Confinement Efficiency of High Strength Transverse Reinforcement and Steel Fibers

    PubMed Central

    Perceka, Wisena; Liao, Wen-Cheng; Wang, Yo-de

    2016-01-01

    Addition of steel fibers to high strength concrete (HSC) improves its post-peak behavior and energy absorbing capability, which can be described well in term of toughness. This paper attempts to obtain both analytically and experimentally the efficiency of steel fibers in HSC columns with hybrid confinement of transverse reinforcement and steel fibers. Toughness ratio (TR) to quantify the confinement efficiency of HSC columns with hybrid confinement is proposed through a regression analysis by involving sixty-nine TRs of HSC without steel fibers and twenty-seven TRs of HSC with hybrid of transverse reinforcement and steel fibers. The proposed TR equation was further verified by compression tests of seventeen HSC columns conducted in this study, where twelve specimens were reinforced by high strength rebars in longitudinal and transverse directions. The results show that the efficiency of steel fibers in concrete depends on transverse reinforcement spacing, where the steel fibers are more effective if the spacing transverse reinforcement becomes larger in the range of 0.25–1 effective depth of the section column. Furthermore, the axial load–strain curves were developed by employing finite element software (OpenSees) for simulating the response of the structural system. Comparisons between numerical and experimental axial load–strain curves were carried out. PMID:28773391

  2. T11TS immunotherapy repairs PI3K-AKT signaling in T-cells: Clues toward enhanced T-cell survival in rat glioma model.

    PubMed

    Chaudhuri, Suhnrita; Singh, Manoj K; Bhattacharya, Debanjan; Datta, Ankur; Hazra, Iman; Mondal, Somnath; Faruk Sk Md, Omar; Ronsard, Larance; Ghosh, Tushar K; Chaudhuri, Swapna

    2018-02-01

    Malignant glioma is the most fatal of astrocytic lineage tumors despite therapeutic advances. Onset and progression of gliomas is accompanied by severe debilitation of T-cell defense and T-cell survival. One of the chief contributors to T-cell survival downstream of activation is the PI3K-AKT pathway. Our prior studies showed that the novel immunotherapeutic molecule T11-target structure (T11TS) blocks T-cell apoptosis in glioma. We also showed activation of immunological synapse components and calcineurin-NFAT pathway following T11TS immunotherapy of glioma-bearing rats. This lead to investigations whether such T-cell activation upon T11TS therapy translates into activation of downstream PI3K/AKT signals which may be related to observed blockade of T-cell apoptosis. For the purpose, we assessed by flowcytometry and immunoblotting, expressions of PI3K, PDK1, AKT, p-AKT, and PTEN in splenic T-cells of normal, experimentally-induced glioma-bearing rats and glioma-bearing rats receiving first, second and third doses of T11TS. We also determined comparative nuclear translocation of NF-κB across groups. We found significant increases in T-cell expressions of PDK1, PI3K, and p-AKT in T11TS-treated animal groups compared to sharp downregulations in glioma. AKT levels remained unchanged across groups. PTEN levels declined sharply after T11TS immunotherapy. T11TS also caused enhanced NF-κB translocation to the T-cell nucleus compared to glioma group. Results showed heightened activation of the PI3K-AKT pathway in glioma-bearing rats following T11TS immunotherapy. These results illustrate the novel role of T11TS immunotherapy in ameliorating the PI3K pathway in T-cells in glioma-bearing animals to enhance T-cell survival, according greater defense against glioma. The study thus has far-reaching clinical outcomes. © 2017 Wiley Periodicals, Inc.

  3. Analytical study on the thermal performance of a partially wet constructal T-shaped fin

    NASA Astrophysics Data System (ADS)

    Hazarika, Saheera Azmi; Zeeshan, Mohd; Bhanja, Dipankar; Nath, Sujit

    2017-07-01

    The present paper addresses the thermal analysis of a T-shaped fin under partially wet condition by adopting a cubic variation of the humidity ratio of saturated air with the corresponding fin surface temperature. The point separating the dry and wet parts may lie either in the flange or stem part of the fin and so, two different cases having different governing equations and boundary conditions are analyzed in this paper. Since the governing equations are highly non-linear, they are solved by using an analytical technique called the Differential Transform Method and subsequently, the dry fin length, temperature distribution and fin performances are evaluated and analyzed for a wide range of the various psychometric, geometric and thermo-physical parameters. Finally, it can be highlighted that relative humidity has a pronounced effect on the performance parameters when the fin surface is partially wet whereas this effect is marginally small for fully wet surface.

  4. Simultaneous determination of quinolones in fish by liquid chromatography coupled with fluorescence detection: comparison of sub-2 microm particles and conventional C18 columns.

    PubMed

    Zhang, Hong; Chen, Si; Lu, Yanbin; Dai, Zhiyuan

    2010-07-01

    A simple and effective multi-residue analysis method is presented for the extraction and determination of eleven quinolones (pipemidic acid, enoxacin, norfloxacin, ciprofloxacin, lomefloxacin, enrofloxacin, gatifloxacin, difloxacin, oxolinic acid, nalidixic acid and flumequine) in fish tissues. In this study, multi-residue separations on four columns packed with 5 microm or sub-2 microm particles were simultaneously developed for the purpose of comparison. Various gradients were optimized and best resolutions were achieved on each column. A short and sub-2 microm particle-sized HPLC column was chosen for its advantages in analysis time and column performance. Additionally, considering the matrix effect of the complex crude fish tissue, an effective extraction protocol was also established for sample pre-treatment procedure. Good recoveries (71-98%) were obtained from samples fortified with a mix of eleven quinolones at three levels, with satisfactory relative standard deviations and limits of detection. As a result, the sub-2 microm HPLC column and proposed analytical procedures have been evaluated and applied to the analysis of different fish tissues. Detectable residues were observed in 8 of 30 samples, at concentrations ranging from 4.74 to 23.27 microg/kg.

  5. Pre-analytical and analytical factors influencing Alzheimer's disease cerebrospinal fluid biomarker variability.

    PubMed

    Fourier, Anthony; Portelius, Erik; Zetterberg, Henrik; Blennow, Kaj; Quadrio, Isabelle; Perret-Liaudet, Armand

    2015-09-20

    A panel of cerebrospinal fluid (CSF) biomarkers including total Tau (t-Tau), phosphorylated Tau protein at residue 181 (p-Tau) and β-amyloid peptides (Aβ42 and Aβ40), is frequently used as an aid in Alzheimer's disease (AD) diagnosis for young patients with cognitive impairment, for predicting prodromal AD in mild cognitive impairment (MCI) subjects, for AD discrimination in atypical clinical phenotypes and for inclusion/exclusion and stratification of patients in clinical trials. Due to variability in absolute levels between laboratories, there is no consensus on medical cut-off value for the CSF AD signature. Thus, for full implementation of this core AD biomarker panel in clinical routine, this issue has to be solved. Variability can be explained both by pre-analytical and analytical factors. For example, the plastic tubes used for CSF collection and storage, the lack of reference material and the variability of the analytical protocols were identified as important sources of variability. The aim of this review is to highlight these pre-analytical and analytical factors and describe efforts done to counteract them in order to establish cut-off values for core CSF AD biomarkers. This review will give the current state of recommendations. Copyright © 2015. Published by Elsevier B.V.

  6. Microengineered open tubular columns for GC analysis

    NASA Astrophysics Data System (ADS)

    Wiranto, Goib; Haskard, Malcolm R.; Mulcahy, Dennis E.; Davey, David E.; Dawes, Ernest F.

    1999-09-01

    Microengineered open tubular (MOT) columns with semi rectangular cross-sections have been designed and fabricated using microengineering techniques. The creation of 100-micrometers wide, 20-micrometers deep, and 125-cm long columns employed isotropic etching on (100) silicon and anodic bonding with a Pyrex 7740 glass cover plate. Column geometry has been optimized to achieve maximum efficiency and allow extreme operating conditions. The walls of the microcolumns were coated with a non-polar liquid stationary phase. Performances of the MOT columns have been demonstrated by their ability to completely separate a series of hydrocarbon mixture in less than 1.25 min under isothermal condition of 150 degrees C. The achievable column efficiencies as measured in terms of theoretical plate height ranged from 0.57 to 1.45 mm, which agreed well with theoretical predictions.

  7. Nonlinear wave interaction in a plasma column

    NASA Technical Reports Server (NTRS)

    Larsen, J.

    1972-01-01

    Two particular cases of nonlinear wave interaction in a plasma column were investigated. The frequencies of the waves were on the order of magnitude of the electron plasma frequency, and ion motion was neglected. The nonlinear coupling of slow waves on a plasma column was studied by means of cold plasma theory, and the case of a plasma column surrounded by an infinite dielectric in the absence of a magnetic field was also examined. Nonlinear scattering from a plasma column in an electromagnetic field having it's magnetic field parallel to the axis of the column was investigated. Some experimental results on mode conversion in the presence of loss are presented along with some observations of nonlinear scattering, The effect of the earth's magnetic field and of discharge symmetry on the radiation pattern are discussed.

  8. Parallel array of independent thermostats for column separations

    DOEpatents

    Foret, Frantisek; Karger, Barry L.

    2005-08-16

    A thermostat array including an array of two or more capillary columns (10) or two or more channels in a microfabricated device is disclosed. A heat conductive material (12) surrounded each individual column or channel in array, each individual column or channel being thermally insulated from every other individual column or channel. One or more independently controlled heating or cooling elements (14) is positioned adjacent to individual columns or channels within the heat conductive material, each heating or cooling element being connected to a source of heating or cooling, and one or more independently controlled temperature sensing elements (16) is positioned adjacent to the individual columns or channels within the heat conductive material. Each temperature sensing element is connected to a temperature controller.

  9. The total carbon column observing network.

    PubMed

    Wunch, Debra; Toon, Geoffrey C; Blavier, Jean-François L; Washenfelder, Rebecca A; Notholt, Justus; Connor, Brian J; Griffith, David W T; Sherlock, Vanessa; Wennberg, Paul O

    2011-05-28

    A global network of ground-based Fourier transform spectrometers has been founded to remotely measure column abundances of CO(2), CO, CH(4), N(2)O and other molecules that absorb in the near-infrared. These measurements are directly comparable with the near-infrared total column measurements from space-based instruments. With stringent requirements on the instrumentation, acquisition procedures, data processing and calibration, the Total Carbon Column Observing Network (TCCON) achieves an accuracy and precision in total column measurements that is unprecedented for remote-sensing observations (better than 0.25% for CO(2)). This has enabled carbon-cycle science investigations using the TCCON dataset, and allows the TCCON to provide a link between satellite measurements and the extensive ground-based in situ network. © 2011 The Royal Society

  10. Determination of strontium-90 in deer bones by liquid scintillation spectrometry after separation on Sr-specific ion exchange columns.

    PubMed

    Landstetter, Claudia; Wallner, Gabriele

    2006-01-01

    The activity concentration of (90)Sr was determined in several deer bones from Austria. Strontium specific ion exchange columns with 4',4''(5'')-di-t-butylcyclohexane-18-crown-6 from Eichrom Industries, Inc. were used for separation. The yield of the chemical procedure was quantified with AAS. Directly after column separation, the solution containing (90)Sr was mixed with the scintillation cocktail HiSafe III and measured by liquid scintillation counting. Prevention of (210)Pb contamination and reusability of the separation columns was investigated as well as the activity distribution within the bones. Results were compared with pre-Chernobyl measurements in Austria; a correlation between activity concentration of (90)Sr and site altitude was found.

  11. Comparison of T1 and T2 metabolite relaxation times in glioma and normal brain at 3 T

    PubMed Central

    Li, Yan; Srinivasan, Radhika; Ratiney, Helene; Lu, Ying; Chang, Susan M.; Nelson, Sarah J.

    2011-01-01

    Purpose To measure T1 and T2 relaxation times of metabolites in glioma patients at 3T and to investigate how these values influence the observed metabolite levels. Materials and Methods Twenty-three patients with gliomas and ten volunteers were studied with single voxel 2D J-resolved PRESS using a 3T MR scanner. Voxels were chosen in normal appearing white matter and in regions of tumor. The T1 and T2 of choline containing compounds (Cho), creatine (Cr) and N-acetyl aspartate (NAA) were estimated. Results Metabolite T1 relaxation values in gliomas were not significantly different from values in normal white matter. The T2 of Cho and Cr were statistically significantly longer for Grade 4 gliomas than for normal white matter but the T2 of NAA was similar. These differences were large enough to impact the corrections of metabolite levels for relaxation times with tumor grade in terms of metabolite ratios (P<0.001). Conclusion The differential increase in T2 for Cho and Cr relative to NAA means that the ratios of Cho/NAA and Cr/NAA are higher in tumor at longer echo times relative to values in normal appearing brain. Having this information may be useful in defining the acquisition parameters for optimizing contrast between tumor and normal tissue in MRSI data, where limited time is available and only one echo time can be used. PMID:18666155

  12. Synthesis, characterization and analytical application of hybrid; acrylamide zirconium (IV) arsenate a cation exchanger, effect of dielectric constant on distribution coefficient of metal ions.

    PubMed

    Nabi, Syed A; Shalla, Aabid H

    2009-04-30

    A new hybrid inorganic-organic cation exchanger acrylamide zirconium (IV) arsenate has been synthesized, characterized and its analytical application explored. The effect of experimental parameters such as mixing ratio of reagents, temperature, and pH on the properties of material has been studied. FTIR, TGA, X-ray, UV-vis spectrophotometry, SEM and elemental analysis were used to determine the physiochemical properties of this hybrid ion exchanger. The material behaves as a monofunctional acid with ion-exchange capacity of 1.65 meq/g for Na(+) ions. The chemical stability data reveals that the exchanger is quite stable in mineral acids, bases and fairly stable in organic solvents, while as thermal analysis shows that the material retain 84% of its ion-exchange capacity up to 600 degrees C. Adsorption behavior of metal ions in solvents with increasing dielectric constant has also been explored. The sorption studies reveal that the material is selective for Pb(2+) ions. The analytical utility of the material has been explored by achieving some binary separations of metal ions on its column. Pb(2+) has been selectively removed from synthetic mixtures containing Mg(2+), Ca(2+), Sr(2+), Zn(2+) and Cu(2+), Al(3+), Ni(2+), Fe(3+). In order to demonstrate practical utility of the material quantitative separation of the Cu(2+) and Zn(2+) in brass sample has been achieved on its columns.

  13. Quantitative Mapping of Human Cartilage at 3.0T

    PubMed Central

    Wang, Ligong; Regatte, Ravinder R.

    2014-01-01

    Rationale and Objectives The objectives of this study were to measure the parallel changes of transverse relaxation times (T2), spin-lattice relaxation time in the rotating frame (T1ρ), and the delayed gadolinium-enhanced magnetic resonance imaging of cartilage (dGEMRIC)-T1 mapping of human knee cartilage in detecting cartilage degeneration at 3.0T. Materials and Methods Healthy volunteers (n = 10, mean age 35.6 years) and patients (n = 10, mean age 65 years) with early knee osteoarthritis (OA) were scanned at 3.0T MR using an 8-channel phased array knee coil (transmit–receive). Quantitative assessment of T2, T1ρ, and dGEMRIC-T1 values (global and regional) were correlated between asymptomatic subjects and patients with OA. Results The average T2 (39 ± 2 milliseconds [mean ± standard deviation] vs. 47 ± 6 milliseconds, P < .0007) and T1ρ (48 ± 3 vs. 62 ± 8 milliseconds, P < .0002) values were all markedly increased in all patients with OA when compared to healthy volunteers. The average dGEMRIC-T1 (1244 ± 134 vs. 643 ± 227 milliseconds, P < .000002) value was sharply decreased after intravenous administration of gadolinium contrast agent in all patients with OA. Conclusions The research results showed that all the T2, T1ρ, and dGEMRIC-T1 relaxation times varied with the cartilage degeneration. The dGEMRIC-T1 and T1ρ relaxation times seem to be more sensitive than T2 in detecting early cartilage degeneration. The preliminary study demonstrated that the early biochemical changes in knee osteoarthritic patients could be detected noninvasively in in vivo using T1ρ and dGEMRIC-T1 mapping. PMID:24594416

  14. T2 Mapping of the Sacroiliac Joints With 3-T MRI: A Preliminary Study.

    PubMed

    Lefebvre, Guillaume; Bergère, Antonin; Rafei, Mazen El; Duhamel, Alain; Teixeira, Pedro; Cotten, Anne

    2017-08-01

    The objective of this study was to assess the feasibility of T2 relaxation time measurements of the sacroiliac joints. The sacroiliac joints of 40 patients were imaged by 3-T MRI using an oblique axial multislice multiecho spin-echo T2-weighted sequence. Manual plotting and automatic subdivision of ROIs allowed us to obtain T2 values for up to 48 different areas per patient (posterior and anterior parts, sacral, intermediate, and iliac parts). Intraand interobserver reproducibility of T2 values were calculated after independent assessment by two musculoskeletal radiologists. A total of 1656 measurement sites could be analyzed. Mean (± SD) T2 values were 40.6 ± 6.7 ms and 41.2 ± 6.3 ms for observer 1 and 39.9 ± 6.6 ms for observer 2. The intraobserver intraclass correlation coefficient was 0.72 (95% CI, 0.70-0.74), and the interobserver intraclass correlation coefficient was 0.71 (95% CI, 0.68-0.72). Our study shows the feasibility of T2 relaxation time measurements at the sacroiliac joints.

  15. tDCS Stimulation of the dlPFC Selectively Moderates the Detrimental Impact of Emotion on Analytical Reasoning.

    PubMed

    Trémolière, Bastien; Maheux-Caron, Véronique; Lepage, Jean-François; Blanchette, Isabelle

    2018-01-01

    There is evidence of a detrimental effect of emotion on reasoning. Recent studies suggest that this relationship is mediated by working memory, a function closely associated with the dorsolateral prefrontal cortex (dlPFC). Relying on transcranial direct current stimulation (tDCS), the present research explores the possibility that anodal stimulation of the dlPFC has the potential to prevent the effect of emotion on analytical reasoning. Thirty-four participants took part in a lab experiment and were tested twice: one session using offline anodal stimulation (with a 2 mA current stimulation applied to the left dlPFC for 20 min), one session using a control (sham) stimulation. In each session, participants solved syllogistic reasoning problems featuring neutral and emotionally negative contents. Results showed that anodal stimulation diminished the deleterious effect of emotion on syllogistic reasoning, but only for a subclass of problems: problems where the conclusion was logically valid. We discuss our results in the light of the reasoning literature as well as the apparent variability of tDCS effects.

  16. Quantitative water content mapping at clinically relevant field strengths: a comparative study at 1.5 T and 3 T.

    PubMed

    Abbas, Zaheer; Gras, Vincent; Möllenhoff, Klaus; Oros-Peusquens, Ana-Maria; Shah, Nadim Joni

    2015-02-01

    Quantitative water content mapping in vivo using MRI is a very valuable technique to detect, monitor and understand diseases of the brain. At 1.5 T, this technology has already been successfully used, but it has only recently been applied at 3T because of significantly increased RF field inhomogeneity at the higher field strength. To validate the technology at 3T, we estimate and compare in vivo quantitative water content maps at 1.5 T and 3T obtained with a protocol proposed recently for 3T MRI. The proposed MRI protocol was applied on twenty healthy subjects at 1.5 T and 3T; the same post-processing algorithms were used to estimate the water content maps. The 1.5 T and 3T maps were subsequently aligned and compared on a voxel-by-voxel basis. Statistical analysis was performed to detect possible differences between the estimated 1.5 T and 3T water maps. Our analysis indicates that the water content values obtained at 1.5 T and 3T did not show significant systematic differences. On average the difference did not exceed the standard deviation of the water content at 1.5 T. Furthermore, the contrast-to-noise ratio (CNR) of the estimated water content map was increased at 3T by a factor of at least 1.5. Vulnerability to RF inhomogeneity increases dramatically with the increasing static magnetic field strength. However, using advanced corrections for the sensitivity profile of the MR coils, it is possible to preserve quantitative accuracy while benefiting from the increased CNR at the higher field strength. Indeed, there was no significant difference in the water content values obtained in the brain at 1.5 T and 3T. Copyright © 2014 Elsevier Inc. All rights reserved.

  17. Musculoskeletal MRI at 3.0 T and 7.0 T: a comparison of relaxation times and image contrast.

    PubMed

    Jordan, Caroline D; Saranathan, Manojkumar; Bangerter, Neal K; Hargreaves, Brian A; Gold, Garry E

    2013-05-01

    The purpose of this study was to measure and compare the relaxation times of musculoskeletal tissues at 3.0 T and 7.0 T, and to use these measurements to select appropriate parameters for musculoskeletal protocols at 7.0 T. We measured the T₁ and T₂ relaxation times of cartilage, muscle, synovial fluid, bone marrow and subcutaneous fat at both 3.0 T and 7.0 T in the knees of five healthy volunteers. The T₁ relaxation times were measured using a spin-echo inversion recovery sequence with six inversion times. The T₂ relaxation times were measured using a spin-echo sequence with seven echo times. The accuracy of both the T₁ and T₂ measurement techniques was verified in phantoms at both magnetic field strengths. We used the measured relaxation times to help design 7.0 T musculoskeletal protocols that preserve the favorable contrast characteristics of our 3.0 T protocols, while achieving significantly higher resolution at higher SNR efficiency. The T₁ relaxation times in all tissues at 7.0 T were consistently higher than those measured at 3.0 T, while the T₂ relaxation times at 7.0 T were consistently lower than those measured at 3.0 T. The measured relaxation times were used to help develop high resolution 7.0 T protocols that had similar fluid-to-cartilage contrast to that of the standard clinical 3.0 T protocols for the following sequences: proton-density-weighted fast spin-echo (FSE), T₂-weighted FSE, and 3D-FSE-Cube. The T₁ and T₂ changes were within the expected ranges. Parameters for musculoskeletal protocols at 7.0 T can be optimized based on these values, yielding improved resolution in musculoskeletal imaging with similar contrast to that of standard 3.0 T clinical protocols. Copyright © 2011 Elsevier Ireland Ltd. All rights reserved.

  18. Postoperative dysesthesia in lumbar three-column resection osteotomies.

    PubMed

    Zhang, Zhengfeng; Wang, Honggang; Zheng, Wenjie

    2016-08-01

    Three-column lumbar spinal resection osteotomies including pedicle subtraction osteotomy (PSO), vertebral column resection (VCR), and total en bloc spondylectomy (TES) can potentially lead to dorsal root ganglion (DRG) injury which may cause postoperative dysesthesia (POD). The purpose of retrospective study was to describe the uncommon complication of POD in lumbar spinal resection osteotomies. Between January 2009 and December 2013, 64 patients were treated with lumbar three-column spinal resection osteotomies (PSO, n = 31; VCR, n = 29; TES, n = 4) in investigator group. POD was defined as dysesthetic pain or burning dysesthesia at a proper DRG innervated region, whether spontaneous or evoked. Non-steroidal antiinflammatory drugs, central none-opioid analgesic agent, neuropathic pain drugs and/or intervertebral foramen block were selectively used to treat POD. There were 5 cases of POD (5/64, 7.8 %), which consisted of 1 patient in PSO (1/31, 3.2 %), 3 patients in PVCR (3/29, 10.3 %), and 1 patient in TES (1/4, 25 %). After the treatment by drugs administration plus DRG block, all patients presented pain relief with duration from 8 to 38 days. A gradual pain moving to distal end of a proper DRG innervated region was found as the beginning of end. Although POD is a unique and rare complication and maybe misdiagnosed as nerve root injury in lumbar spinal resection osteotomies, combination drug therapy and DRG block have an effective result of pain relief. The appearance of a gradual pain moving to distal end of a proper DRG innervated region during recovering may be used as a sign for the good prognosis.

  19. Cyanidin-3-rutinoside increases glucose uptake by activating the PI3K/Akt pathway in 3T3-L1 adipocytes.

    PubMed

    Choi, Kyung Ha; Lee, Hyun Ah; Park, Mi Hwa; Han, Ji-Sook

    2017-09-01

    In this study, the effect of cyanidin-3-rutinoside (C3R) on glucose uptake by 3T3-L1 adipocytes was studied. C3R significantly increased glucose uptake, which was associated with enhanced plasma membrane glucose transporter type 4 (PM-GLUT4) expression in 3T3-L1 adipocytes. The potentiating effect of C3R on glucose uptake and PM-GLUT4 expression was related to enhanced phosphorylation of insulin receptor substrate 1 (IRS-1) and Akt, as well as augmented activation of phosphatidylinositol-3-kinase (PI3K) in the insulin signaling pathway. C3R induced glucose uptake was inhibited only by the PI3K inhibitor, but not by an AMPK inhibitor in 3T3-L1 adipocytes. Therefore, C3R likely up-regulates glucose uptake and PM-GLUT4 expression in 3T3-L1 adipocytes by activating the PI3K/Akt pathways. Copyright © 2017 Elsevier B.V. All rights reserved.

  20. Induction and prevention of low-T3 syndrome in exercising women.

    PubMed

    Loucks, A B; Callister, R

    1993-05-01

    To investigate the influence of exercise on thyroid metabolism, 46 healthy young regularly menstruating sedentary women were randomly assigned to a 3 x 2 experimental design of aerobic exercise and energy availability treatments. Energy availability was defined as dietary energy intake minus energy expenditure during exercise. After 4 days of treatments, low energy availability (8 vs. 30 kcal.kg body wt-1.day-1) had reduced 3,5,3'-triiodothyronine (T3) by 15% and free T3 (fT3) by 18% and had increased thyroxine (T4) by 7% and reverse T3 (rT3) by 24% (all P < 0.01), whereas free T4 (fT4) was unchanged (P = 0.08). Exercise quantity (0 vs. 1,300 kcal/day) and intensity (40 vs. 70% of aerobic capacity) did not affect any thyroid hormone (all P > 0.10). That is, low-T3 syndrome was induced by the energy cost of exercise and was prevented in exercising women by increasing dietary energy intake. Selective observation of low-T3 syndrome in amenorrheic and not in regularly menstruating athletes suggests that exercise may compromise the availability of energy for reproductive function in humans. If so, athletic amenorrhea might be prevented or reversed through dietary reform without reducing exercise quantity or intensity.