Multi-Column Experimental Test Bed for Xe/Kr Separation

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

Greenhalgh, Mitchell Randy; Garn, Troy Gerry; Welty, Amy Keil

Previous research studies have shown that INL-developed engineered form sorbents are capable of capturing both Kr and Xe from various composite gas streams. The previous experimental test bed provided single column testing for capacity evaluations over a broad temperature range. To advance research capabilities, the employment of an additional column to study selective capture of target species to provide a defined final gas composition for waste storage was warranted. The second column addition also allows for compositional analyses of the final gas product to provide for final storage determinations. The INL krypton capture system was modified by adding an additionalmore » adsorption column in order to create a multi-column test bed. The purpose of this modification was to investigate the separation of xenon from krypton supplied as a mixed gas feed. The extra column was placed in a Stirling Ultra-low Temperature Cooler, capable of controlling temperatures between 190 and 253K. Additional piping and valves were incorporated into the system to allow for a variety of flow path configurations. The new column was filled with the AgZ-PAN sorbent which was utilized as the capture medium for xenon while allowing the krypton to pass through. The xenon-free gas stream was then routed to the cryostat filled with the HZ-PAN sorbent to capture the krypton at 191K. Selectivities of xenon over krypton were determined using the new column to verify the system performance and to establish the operating conditions required for multi-column testing. Results of these evaluations verified that the system was operating as designed and also demonstrated that AgZ-PAN exhibits excellent selectivity for xenon over krypton in air at or near room temperature. Two separation tests were performed utilizing a feed gas consisting of 1000 ppmv xenon and 150 ppmv krypton with the balance being made up of air. The AgZ-PAN temperature was held at 295 or 253K while the HZ-PAN was held at 191K for both tests. The effluent from the AgZ-PAN column was monitored via GC-TCD during the tests with no xenon being observed exiting the column during either test. Samples from each column were taken via evacuated sample bombs and were analyzed by GC-MS analysis. The results demonstrated the ability to separate xenon from krypton from a mixed gas feed utilizing the new multi-column system.« less

Classification of LC columns based on the QSRR method and selectivity toward moclobemide and its metabolites.

PubMed

Plenis, Alina; Olędzka, Ilona; Bączek, Tomasz

2013-05-05

This paper focuses on a comparative study of the column classification system based on the quantitative structure-retention relationships (QSRR method) and column performance in real biomedical analysis. The assay was carried out for the LC separation of moclobemide and its metabolites in human plasma, using a set of 24 stationary phases. The QSRR models established for the studied stationary phases were compared with the column test performance results under two chemometric techniques - the principal component analysis (PCA) and the hierarchical clustering analysis (HCA). The study confirmed that the stationary phase classes found closely related by the QSRR approach yielded comparable separation for moclobemide and its metabolites. Therefore, the QSRR method could be considered supportive in the selection of a suitable column for the biomedical analysis offering the selection of similar or dissimilar columns with a relatively higher certainty. Copyright © 2013 Elsevier B.V. All rights reserved.

Determining the Influence of Groundwater Composition on the Performance of Arsenic Adsorption Columns Using Rapid Small-Scale Column Tests

NASA Astrophysics Data System (ADS)

Aragon, A. R.; Siegel, M.

2004-12-01

The USEPA has established a more stringent drinking water standard for arsenic, reducing the maximum contaminant level (MCL) from 50 μ g/L to 10 μ g/L. This will affect many small communities in the US that lack the appropriate treatment infrastructure and funding to reduce arsenic to such levels. For such communities, adsorption systems are the preferred technology based on ease of operation and relatively lower costs. The performance of adsorption media for the removal of arsenic from drinking water is dependent on site-specific water quality. At certain concentrations, co-occurring solutes will compete effectively with arsenic for sorption sites, potentially reducing the sorption capacity of the media. Due to the site-specific nature of water quality and variations in media properties, pilot scale studies are typically carried out to ensure that a proposed treatment technique is cost effective before installation of a full-scale system. Sandia National Laboratories is currently developing an approach to utilize rapid small-scale columns in lieu of pilot columns to test innovative technologies that could significantly reduce the cost of treatment in small communities. Rapid small-scale column tests (RSSCTs) were developed to predict full-scale treatment of organic contaminants by adsorption onto granular activated carbon (GAC). This process greatly reduced the time and costs required to verify performance of GAC adsorption columns. In this study, the RSSCT methodology is used to predict the removal of inorganic arsenic using mixed metal oxyhydroxide adsorption media. The media are engineered and synthesized from materials that control arsenic behavior in natural and disturbed systems. We describe the underlying theory and application of RSSCTs for the performance evaluation of novel media in several groundwater compositions. Results of small-scale laboratory columns are being used to predict the performance of pilot-scale systems and ultimately to design full-scale systems. RSSCTs will be performed on a suite of water compositions representing the variety of water supplies in the United States that are affected by the new drinking water standard. Ultimately, this approach will be used to carry out inexpensive short-term pilot studies at a large number of sites where large-scale pilots are not economically feasible. Sandia National Laboratories is a multi-program laboratory operated by Sandia Corporation, a Lockheed Martin company, for the United States Department of Energy's National Nuclear Security Administration under Contract DE-AC04-94AL85000.

Biomechanical investigation of two plating systems for medial column fusion in foot

PubMed Central

Simons, Paul; Sommerer, Theresia; Zderic, Ivan; Wahl, Dieter; Lenz, Mark; Skulev, Hristo; Knobe, Matthias; Gueorguiev, Boyko; Richards, R. Geoff; Klos, Kajetan

2017-01-01

Background Arthrodesis of the medial column (navicular, cuneiform I and metatarsal I) is performed for reasons such as Charcot arthropathy, arthritis, posttraumatic reconstruction or severe pes planus. However, the complication rate is still high and mainly resulting from inadequate fixation. Special plates, designed for medial column arthrodesis, seem to offer potential to reduce the complication rate. The aim of this study was to investigate biomechanically plantar and dorsomedial fusion of the medial column using two new plating systems. Methods Eight matched pairs of human cadaveric lower legs were randomized in two groups and medial column fusion was performed using either plantar or dorsomedial variable-angle locking compression plates. The specimens were biomechanically tested under cyclic progressively increasing axial loading with physiological profile of each cycle. In addition to the machine data, mediolateral x-rays were taken every 250 cycles and motion tracking was performed to determine movements at the arthrodesis site. Statistical analysis of the parameters of interest was performed at a level of significance p = 0.05. Results Displacement of the talo-navicular joint after 1000, 2000 and 4000 cycles was significantly lower for plantar plating (p≤0.039) while there was significantly less movement in the naviculo-cuneiform I joint for dorsal plating post these cycle numbers (p<0.001). Displacements in all three joints of the medial column, as well as angular and torsional deformations between the navicular and metatarsal I increased significantly for each plating technique between 1000, 2000 and 4000 cycles (p≤0.021). The two plating systems did not differ significantly with regard to stiffness and cycles to failure (p≥0.171). Conclusion From biomechanical point of view, although dorsomedial plating showed less movement than plantar plating in the current setup under dynamic loading, there was no significant difference between the two plating systems with regard to stiffness and cycles to failure. Both tested techniques for dorsomedial and plantar plating appear to be applicable for arthrodesis of the medial column of the foot and other considerations, such as access morbidity, associated deformities or surgeon's preference, may also guide the choice of plating pattern. Further clinical studies are necessary before definitive recommendations can be given. PMID:28222170

Biomechanical investigation of two plating systems for medial column fusion in foot.

PubMed

Simons, Paul; Sommerer, Theresia; Zderic, Ivan; Wahl, Dieter; Lenz, Mark; Skulev, Hristo; Knobe, Matthias; Gueorguiev, Boyko; Richards, R Geoff; Klos, Kajetan

2017-01-01

Arthrodesis of the medial column (navicular, cuneiform I and metatarsal I) is performed for reasons such as Charcot arthropathy, arthritis, posttraumatic reconstruction or severe pes planus. However, the complication rate is still high and mainly resulting from inadequate fixation. Special plates, designed for medial column arthrodesis, seem to offer potential to reduce the complication rate. The aim of this study was to investigate biomechanically plantar and dorsomedial fusion of the medial column using two new plating systems. Eight matched pairs of human cadaveric lower legs were randomized in two groups and medial column fusion was performed using either plantar or dorsomedial variable-angle locking compression plates. The specimens were biomechanically tested under cyclic progressively increasing axial loading with physiological profile of each cycle. In addition to the machine data, mediolateral x-rays were taken every 250 cycles and motion tracking was performed to determine movements at the arthrodesis site. Statistical analysis of the parameters of interest was performed at a level of significance p = 0.05. Displacement of the talo-navicular joint after 1000, 2000 and 4000 cycles was significantly lower for plantar plating (p≤0.039) while there was significantly less movement in the naviculo-cuneiform I joint for dorsal plating post these cycle numbers (p<0.001). Displacements in all three joints of the medial column, as well as angular and torsional deformations between the navicular and metatarsal I increased significantly for each plating technique between 1000, 2000 and 4000 cycles (p≤0.021). The two plating systems did not differ significantly with regard to stiffness and cycles to failure (p≥0.171). From biomechanical point of view, although dorsomedial plating showed less movement than plantar plating in the current setup under dynamic loading, there was no significant difference between the two plating systems with regard to stiffness and cycles to failure. Both tested techniques for dorsomedial and plantar plating appear to be applicable for arthrodesis of the medial column of the foot and other considerations, such as access morbidity, associated deformities or surgeon's preference, may also guide the choice of plating pattern. Further clinical studies are necessary before definitive recommendations can be given.

Comparison of various types of stationary phases in non-aqueous reversed-phase high-performance liquid chromatography-mass spectrometry of glycerolipids in blackcurrant oil and its enzymatic hydrolysis mixture.

PubMed

Lísa, Miroslav; Holcapek, Michal; Sovová, Helena

2009-11-20

The selection of column packing during the development of high-performance liquid chromatography method is a crucial step to achieve sufficient chromatographic resolution of analyzed species in complex mixtures. Various stationary phases are tested in this paper for the analysis of complex mixture of triacylglycerols (TGs) in blackcurrant oil using non-aqueous reversed-phase (NARP) system with acetonitrile-2-propanol mobile phase. Conventional C(18) column in the total length of 45 cm is used for the separation of TGs according to their equivalent carbon number, the number and positions of double bonds and acyl chain lengths. The separation of TGs and their more polar hydrolysis products after the partial enzymatic hydrolysis of blackcurrant oil in one chromatographic run is achieved using conventional C(18) column. Retention times of TGs are reduced almost 10 times without the loss of the chromatographic resolution using ultra high-performance liquid chromatography with 1.7 microm C(18) particles. The separation in NARP system on C(30) column shows an unusual phenomenon, because the retention order of TGs changes depending on the column temperature, which is reported for the first time. The commercial monolithic column modified with C(18) is used for the fast analysis of TGs to increase the sample throughput but at cost of low resolution.

Two-dimensional preparative liquid chromatography system for preparative separation of minor amount components from complicated natural products.

PubMed

Qiu, Ying-Kun; Chen, Fang-Fang; Zhang, Ling-Ling; Yan, Xia; Chen, Lin; Fang, Mei-Juan; Wu, Zhen

2014-04-11

An on-line comprehensive two-dimensional preparative liquid chromatography system was developed for preparative separation of minor amount components from complicated natural products. Medium-pressure liquid chromatograph (MPLC) was applied as the first dimension and preparative HPLC as the second one, in conjunction with trapping column and makeup pump. The performance of the trapping column was evaluated, in terms of column size, dilution ratio and diameter-height ratio, as well as system pressure from the view of medium pressure liquid chromatograph. Satisfactory trapping efficiency can be achieved using a commercially available 15 mm × 30 mm i.d. ODS pre-column. The instrument operation and the performance of this MPLC×preparative HPLC system were illustrated by gram-scale isolation of crude macro-porous resin enriched water extract of Rheum hotaoense. Automated multi-step preparative separation of 25 compounds, whose structures were identified by MS, (1)H NMR and even by less-sensitive (13)C NMR, could be achieved in a short period of time using this system, exhibiting great advantages in analytical efficiency and sample treatment capacity compared with conventional methods. Copyright © 2014 Elsevier B.V. All rights reserved.

Numerical simulation of CFRP-repaired reinforced concrete columns.

DOT National Transportation Integrated Search

2014-07-01

The overarching goal of this study was to investigate the influence of repair to individual reinforced concrete bridge columns on the : post-repair seismic performance of the bridge system. A method was developed to rapidly repair an earthquake-damag...

Ultra high-performance liquid chromatography of porphyrins in clinical materials: column and mobile phase selection and optimisation.

PubMed

Benton, Christopher M; Lim, Chang Kee; Moniz, Caje; Jones, Donald J L

2012-06-01

Ultra high-performance liquid chromatographic (UHPLC) systems on columns packed with materials ranging from 1.9 to 2.7 µm average particle size were assessed for the fast and sensitive analysis of porphyrins in clinical materials. The fastest separation was achieved on an Agilent Poroshell C(18) column (2.7 µm particle size, 50 × 4.6 mm i.d.), followed by a Thermo Hypersil Gold C(18) column (1.9 µm particle size, 50 × 2.1 mm i.d.) and the Thermo Hypersil BDS C(18) column (2.4 µm particle size, 100 × 2.1 mm i.d.). All columns required a mobile phase containing 1 m ammonium acetate buffer, pH 5.16, with a mixture of acetonitrile and methanol as the organic modifiers for optimum resolution of the type I and III isomers, particularly for uroporphyrin I and III isomers. All UHPLC columns were suitable and superior to conventional HPLC columns packed with 5 µm average particle size materials for clinical sample analysis. Copyright © 2011 John Wiley & Sons, Ltd.

Relative importance of column and adsorption parameters on the productivity in preparative liquid chromatography II: Investigation of separation systems with competitive Langmuir adsorption isotherms.

PubMed

Forssén, Patrik; Samuelsson, Jörgen; Fornstedt, Torgny

2014-06-20

In this study we investigated how the maximum productivity for commonly used, realistic separation system with a competitive Langmuir adsorption isotherm is affected by changes in column length, packing particle size, mobile phase viscosity, maximum allowed column pressure, column efficiency, sample concentration/solubility, selectivity, monolayer saturation capacity and retention factor of the first eluting compound. The study was performed by generating 1000 random separation systems whose optimal injection volume was determined, i.e., the injection volume that gives the largest achievable productivity. The relative changes in largest achievable productivity when one of the parameters above changes was then studied for each system and the productivity changes for all systems were presented as distributions. We found that it is almost always beneficial to use shorter columns with high pressure drops over the column and that the selectivity should be greater than 2. However, the sample concentration and column efficiency have very limited effect on the maximum productivity. The effect of packing particle size depends on the flow rate limiting factor. If the pumps maximum flow rate is the limiting factor use smaller packing, but if the pressure of the system is the limiting factor use larger packing up to about 40μm. Copyright © 2014 Elsevier B.V. All rights reserved.

Ten-year monitoring of high-rise building columns using long-gauge fiber optic sensors

NASA Astrophysics Data System (ADS)

Glisic, B.; Inaudi, D.; Lau, J. M.; Fong, C. C.

2013-05-01

A large-scale lifetime building monitoring program was implemented in Singapore in 2001. The monitoring aims of this unique program were to increase safety, verify performance, control quality, increase knowledge, optimize maintenance costs, and evaluate the condition of the structures after a hazardous event. The first instrumented building, which has now been monitored for more than ten years, is presented in this paper. The long-gauge fiber optic strain sensors were embedded in fresh concrete of ground-level columns, thus the monitoring started at the birth of both the construction material and the structure. Measurement sessions were performed during construction, upon completion of each new story and the roof, and after the construction, i.e., in-service. Based on results it was possible to follow and evaluate long-term behavior of the building through every stage of its life. The results of monitoring were analyzed at a local (column) and global (building) level. Over-dimensioning of one column was identified. Differential settlement of foundations was detected, localized, and its magnitude estimated. Post-tremor analysis was performed. Real long-term behavior of concrete columns was assessed. Finally, the long-term performance of the monitoring system was evaluated. The researched monitoring method, monitoring system, rich results gathered over approximately ten years, data analysis algorithms, and the conclusions on the structural behavior and health condition of the building based on monitoring are presented in this paper.

Effects of Cabin Upsets on Adsorption Columns for Air Revitalization

NASA Technical Reports Server (NTRS)

LeVan, Douglas

1999-01-01

The National Aeronautics and Space Administration (NASA) utilizes adsorption technology as part of contaminant removal systems designed for long term missions. A variety of trace contaminants can be effectively removed from gas streams by adsorption onto activated carbon. An activated carbon adsorption column meets NASA's requirements of a lightweight and efficient means of controlling trace contaminant levels aboard spacecraft and space stations. The activated carbon bed is part of the Trace Contaminant Control System (TCCS) which is utilized to purify the cabin atmosphere. TCCS designs oversize the adsorption columns to account for irregular fluctuations in cabin atmospheric conditions. Variations in the cabin atmosphere include changes in contaminant concentrations, temperature, and relative humidity. Excessively large deviations from typical conditions can result from unusual crew activity, equipment malfunctions, or even fires. The research carried out under this award focussed in detail on the effects of cabin upsets on the performance of activated carbon adsorption columns. Both experiments and modeling were performed with an emphasis on the roll of a change in relative humidity on adsorption of trace contaminants. A flow through fixed-bed apparatus was constructed at the NASA Ames Research Center, and experiments were performed there. Modeling work was performed at the University of Virginia.

Axial thermal gradients in microchip gas chromatography.

PubMed

Wang, Anzi; Hynynen, Sampo; Hawkins, Aaron R; Tolley, Samuel E; Tolley, H Dennis; Lee, Milton L

2014-12-29

Fabrication technologies for microelectromechanical systems (MEMS) allow miniaturization of conventional benchtop gas chromatography (GC) to portable, palm-sized microfabricated GC (μGC) devices, which are suitable for on-site chemical analysis and remote sensing. The separation performance of μGC systems, however, has not been on par with conventional GC. Column efficiency, peak symmetry and resolution are often compromised by column defects and non-ideal injections. The relatively low performance of μGC devices has impeded their further commercialization and broader application. In this work, the separation performance of μGC columns was improved by incorporating thermal gradient gas chromatography (TGGC). The analysis time was ∼20% shorter for TGGC separations compared to conventional temperature-programmed GC (TPGC) when a wide sample band was introduced into the column. Up to 50% reduction in peak tailing was observed for polar analytes, which improved their resolution. The signal-to-noise ratios (S/N) of late-eluting peaks were increased by 3-4 fold. The unique focusing effect of TGGC overcomes many of the previous shortcomings inherent in μGC analyses. Copyright © 2014 Elsevier B.V. All rights reserved.

Fully automated multifunctional ultrahigh pressure liquid chromatography system for advanced proteome analyses

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

Lee, Jung Hwa; Hyung, Seok-Won; Mun, Dong-Gi

2012-08-03

A multi-functional liquid chromatography system that performs 1-dimensional, 2-dimensional (strong cation exchange/reverse phase liquid chromatography, or SCX/RPLC) separations, and online phosphopeptides enrichment using a single binary nano-flow pump has been developed. With a simple operation of a function selection valve, which is equipped with a SCX column and a TiO2 (titanium dioxide) column, a fully automated selection of three different experiment modes was achieved. Because the current system uses essentially the same solvent flow paths, the same trap column, and the same separation column for reverse-phase separation of 1D, 2D, and online phosphopeptides enrichment experiments, the elution time information obtainedmore » from these experiments is in excellent agreement, which facilitates correlating peptide information from different experiments.« less

Microfluidic integration of parallel solid-phase liquid chromatography.

PubMed

Huft, Jens; Haynes, Charles A; Hansen, Carl L

2013-03-05

We report the development of a fully integrated microfluidic chromatography system based on a recently developed column geometry that allows for robust packing of high-performance separation columns in poly(dimethylsiloxane) microfluidic devices having integrated valves made by multilayer soft lithography (MSL). The combination of parallel high-performance separation columns and on-chip plumbing was used to achieve a fully integrated system for on-chip chromatography, including all steps of automated sample loading, programmable gradient generation, separation, fluorescent detection, and sample recovery. We demonstrate this system in the separation of fluorescently labeled DNA and parallel purification of reverse transcription polymerase chain reaction (RT-PCR) amplified variable regions of mouse immunoglobulin genes using a strong anion exchange (AEX) resin. Parallel sample recovery in an immiscible oil stream offers the advantage of low sample dilution and high recovery rates. The ability to perform nucleic acid size selection and recovery on subnanogram samples of DNA holds promise for on-chip genomics applications including sequencing library preparation, cloning, and sample fractionation for diagnostics.

Characterization of the efficiency of microbore liquid chromatography columns by van Deemter and kinetic plot analysis.

PubMed

Hetzel, Terence; Loeker, Denise; Teutenberg, Thorsten; Schmidt, Torsten C

2016-10-01

The efficiency of miniaturized liquid chromatography columns with inner diameters between 200 and 300 μm has been investigated using a dedicated micro-liquid chromatography system. Fully porous, core-shell and monolithic commercially available stationary phases were compared applying van Deemter and kinetic plot analysis. The sub-2 μm fully porous as well as the 2.7 μm core-shell particle packed columns showed superior efficiency and similar values for the minimum reduced plate heights (2.56-2.69) before correction for extra-column contribution compared to normal-bore columns. Moreover, the influence of extra-column contribution was investigated to demonstrate the difference between apparent and intrinsic efficiency by replacing the column by a zero dead volume union to determine the band spreading caused by the system. It was demonstrated that 72% of the intrinsic efficiency could be reached. The results of the kinetic plot analysis indicate the superior performance of the sub-2 μm fully porous particle packed column for ultra-fast liquid chromatography. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Development and application of a specially designed heating system for temperature-programmed high-performance liquid chromatography using subcritical water as the mobile phase.

PubMed

Teutenberg, T; Goetze, H-J; Tuerk, J; Ploeger, J; Kiffmeyer, T K; Schmidt, K G; Kohorst, W gr; Rohe, T; Jansen, H-D; Weber, H

2006-05-05

A specially designed heating system for temperature-programmed HPLC was developed based on experimental measurements of eluent temperature inside a stainless steel capillary using a very thin thermocouple. The heating system can be operated at temperatures up to 225 degrees C and consists of a preheating, a column heating and a cooling unit. Fast cycle times after a temperature gradient can be realized by an internal silicone oil bath which cools down the preheating and column heating unit. Long-term thermal stability of a polybutadiene-coated zirconium dioxide column has been evaluated using a tubular oven in which the column was placed. The packing material was stable after 50h of operation at 185 degrees C. A mixture containing four steroids was separated at ambient conditions using a mobile phase of 25% acetonitrile:75% deionized water and a mobile phase of pure deionized water at 185 degrees C using the specially designed heating system and the PBD column. Analysis time could be drastically reduced from 17 min at ambient conditions and a flow rate of 1 mL/min to only 1.2 min at 185 degrees C and a flow rate of 5 mL/min. At these extreme conditions, no thermal mismatch was observed and peaks were not distorted, thus underlining the performance of the developed heating system. Temperature programming was performed by separating cytostatic and antibiotic drugs with a temperature gradient using only water as the mobile phase. In contrast to an isocratic elution of this mixture at room temperature, overall analysis time could be reduced two-fold from 20 to 10 min.

Distributed control of large space antennas

NASA Technical Reports Server (NTRS)

Cameron, J. M.; Hamidi, M.; Lin, Y. H.; Wang, S. J.

1983-01-01

A systematic way to choose control design parameters and to evaluate performance for large space antennas is presented. The structural dynamics and control properties for a Hoop and Column Antenna and a Wrap-Rib Antenna are characterized. Some results of the effects of model parameter uncertainties to the stability, surface accuracy, and pointing errors are presented. Critical dynamics and control problems for these antenna configurations are identified and potential solutions are discussed. It was concluded that structural uncertainties and model error can cause serious performance deterioration and can even destabilize the controllers. For the hoop and column antenna, large hoop and long meat and the lack of stiffness between the two substructures result in low structural frequencies. Performance can be improved if this design can be strengthened. The two-site control system is more robust than either single-site control systems for the hoop and column antenna.

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

Direct coupling of microbore HPLC columns to MS systems

NASA Technical Reports Server (NTRS)

Mcnair, H. M.

1985-01-01

A detailed investigation using electron microscopy was conducted which examined the conditions of materials used in the construction of stable, high performance microbore liquid chromatography (LC) columns. Small details proved to be important. The effects of temperature on the elution of several homologous series used as probe compounds was examined in reverse phase systems. They showed that accessible temperature changes provide roughly half the increase in solvent strength that would be obtained going from a 100% aqueous to a 100% organic mobile phase, which is sufficient to warrant their use in many analyses requiring the use of gradients. Air circulation temperature control systems provide the easiest means of obtaining rapid, wide range changes in column temperature. However, slow heat transfer from the gas leads to thermal nonuniformity in the column and a decrease in resolution as the temperature program progresses.

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.

Environmental Characterization of Mine Countermeasure Test Ranges: Hydrography and Water Column Optics

DTIC Science & Technology

2015-09-30

changes in near-shore water columns and support companion laser imaging system tests. The physical, biological and optical oceanographic data...developed under this project will be used as input to optical and environmental models to assess the performance characteristics of laser imaging systems...OBJECTIVES We proposed to characterize the physical, biological and optical fields present during deployments of the Streak Tube Imaging Lidar

On the feasibility to conduct gradient liquid chromatography separations in narrow-bore columns at pressures up to 2000bar.

PubMed

De Pauw, Ruben; Swier, Tim; Degreef, Bart; Desmet, Gert; Broeckhoven, Ken

2016-11-18

The limits in operating pressures are extended for narrow-bore columns in gradient elution up to 2000bar. As the required pumps for these pressures are incompatible with common chromatographic solvents and are not suitable to apply a mobile phase composition gradient, a mobile phase delivery and injection system is described and experimentally validated which allows to use any possible chromatographic solvent in isocratic and gradient elution. The mobile phase delivery and injection system also allows to perform multiple separations without the need to depressurize the column. This system consists out of 5 dual on/off valves and two large volume loops in which the gradient and equilibration volume of initial mobile phase are loaded by a commercial liquid chromatography pump. The loops are then flushed toward the column at extreme pressures. The mobile phase delivery and injection system is first evaluated in isocratic elution and shows a comparable performance to a state-of-the-art commercial flow-through-needle injector but with twice the pressure rating. Distortion of the loaded gradient by dispersion in the gradient storage loop is studied. The effect of the most important parameters (such as flow rate, pressure and gradient steepness) is experimentally investigated. Different gradient steepnesses and volumes can be applied at different flow rates and operating pressures with a good repeatability. Due to the isobaric operation of the pumps, the gradient is monitored in real-time by a mass flow meter installed at the detector outlet. The chromatograms are then converted from time to volume-base. A separation of a 19-compound sample is performed on a 300×2.1mm column at 1000bar and on a 600×2.1mm column at 2000bar. The peak capacity was found to increase from 141 to 199 and thus scales with L as is predicted by theory. This allows to conclude that the inlet pressure for narrow-bore columns in gradient elution can be increased up to 2000bar without fundamental pressure-induced limitations. Copyright © 2016 Elsevier B.V. All rights reserved.

Pressurized planar electrochromatography, high-performance thin-layer chromatography and high-performance liquid chromatography--comparison of performance.

PubMed

Płocharz, Paweł; Klimek-Turek, Anna; Dzido, Tadeusz H

2010-07-16

Kinetic performance, measured by plate height, of High-Performance Thin-Layer Chromatography (HPTLC), High-Performance Liquid Chromatography (HPLC) and Pressurized Planar Electrochromatography (PPEC) was compared for the systems with adsorbent of the HPTLC RP18W plate from Merck as the stationary phase and the mobile phase composed of acetonitrile and buffer solution. The HPLC column was packed with the adsorbent, which was scrapped from the chromatographic plate mentioned. An additional HPLC column was also packed with adsorbent of 5 microm particle diameter, C18 type silica based (LiChrosorb RP-18 from Merck). The dependence of plate height of both HPLC and PPEC separating systems on flow velocity of the mobile phase and on migration distance of the mobile phase in TLC system was presented applying test solute (prednisolone succinate). The highest performance, amongst systems investigated, was obtained for the PPEC system. The separation efficiency of the systems investigated in the paper was additionally confirmed by the separation of test component mixture composed of six hormones. 2010 Elsevier B.V. All rights reserved.

Stability and dynamic analysis of a slender column with curved longitudinal stiffeners

NASA Technical Reports Server (NTRS)

Lake, Mark S.

1989-01-01

The results of a stability design study are presented for a slender column with curved longitudinal stiffeners for large space structure applications. Linear stability analyses are performed using a link-plate representation of the stiffeners to determine stiffener local buckling stresses. Results from a set of parametric analyses are used to determine an approximate explicit expression for stiffener local buckling in terms of its geometric parameters. This expression along with other equations governing column stability and mass are assembled into a determinate system describing minimum mass stiffened column design. An iterative solution is determined to solve this system and a computer program incorporating this routine is presented. Example design problems are presented which verify the solution accuracy and illustrate the implementation of the solution routine. Also, observations are made which lead to a greatly simplified first iteration design equation relating the percent increase in column mass to the percent increase in column buckling load. From this, generalizations are drawn as to the mass savings offered by the stiffened column concept. Finally, the percent increase in fundamental column vibration frequency due to the addition of deployable stiffeners is studied.

Miniaturized protein separation using a liquid chromatography column on a flexible substrate

NASA Astrophysics Data System (ADS)

Yang, Yongmo; Chae, Junseok

2008-12-01

We report a prototype protein separator that successfully miniaturizes existing technology for potential use in biocompatible health monitoring implants. The prototype is a liquid chromatography (LC) column (LC mini-column) fabricated on an inexpensive, flexible, biocompatible polydimethylsiloxane (PDMS) enclosure. The LC mini-column separates a mixture of proteins using size exclusion chromatography (SEC) with polydivinylbenzene beads (5-20 µm in diameter with 10 nm pore size). The LC mini-column is smaller than any commercially available LC column by a factor of ~11 000 and successfully separates denatured and native protein mixtures at ~71 psi of the applied fluidic pressure. Separated proteins are analyzed using NuPAGE-gel electrophoresis, high-performance liquid chromatography (HPLC) and an automated electrophoresis system. Quantitative HPLC results demonstrate successful separation based on intensity change: within 12 min, the intensity between large and small protein peaks changed by a factor of ~20. In further evaluation using the automated electrophoresis system, the plate height of the LC mini-column is between 36 µm and 100 µm. The prototype LC mini-column shows the potential for real-time health monitoring in applications that require inexpensive, flexible implant technology that can function effectively under non-laboratory conditions.

Purification and Characteriztion of the Type III Secretion System Protein from Burkholderia mallei

DTIC Science & Technology

2013-08-01

official Department of the Army position unless so designated by other authorizing documents. REPORT DOCUMENTATION PAGE Form Approved OMB No...HP column), the procedure was performed in an automated mode using the following four steps: eluting through a HisTrap crude FF column, desalting

Rapid determination of parabens in seafood sauces by high-performance liquid chromatography: A practical comparison of core-shell particles and sub-2 μm fully porous particles.

PubMed

Ye, Jing; Cao, Xiaoji; Cheng, Zhuo; Qin, Ye; Lu, Yanbin

2015-12-01

In this work, the chromatographic performance of superficially porous particles (Halo core-shell C18 column, 50 mm × 2.1 mm, 2.7 μm) was compared with that of sub-2 μm fully porous particles (Acquity BEH C18 , 50 mm × 2.1 mm, 1.7 μm). Four parabens, methylparaben, ethylparaben, propylparaben, and butylparaben, were used as representative compounds for calculating the plate heights in a wide flow rate range and analyzed on the basis of the Van Deemter and Knox equations. Theoretical Poppe plots were constructed for each column to compare their kinetic performance. Both phases gave similar minimum plate heights when using nonreduced coordinates. Meanwhile, the flat C-term of the core-shell column provided the possibilities for applying high flow rates without significant loss in efficiency. The low backpressure of core-shell particles allowed this kind of column, especially compatible with conventional high-performance liquid chromatography systems. Based on these factors, a simple high-performance liquid chromatography method was established and validated for the determination of parabens in various seafood sauces using the Halo core-shell C18 column for separation. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Full Scale RC Beam-Column Joints Strengthened with Steel Reinforced Polymer Systems

NASA Astrophysics Data System (ADS)

De Vita, Alessandro; Napoli, Annalisa; Realfonzo, Roberto

2017-07-01

This paper presents the results of an experimental campaign performed at the Laboratory of Materials and Structural Testing of the University of Salerno (Italy) in order to investigate the seismic performance of RC beam-column joints strengthened with Steel Reinforced Polymer (SRP) systems. With the aim to represent typical façade frames’ beam-column subassemblies found in existing RC buildings, specimens were provided with two short beam stubs orthogonal to the main beam and were designed with inadequate seismic details. Five members were strengthened by using two different SRP layouts while the remaining ones were used as benchmarks. Once damaged, two specimens were also repaired, retrofitted with SRP and subjected to cyclic test again. The results of cyclic tests performed on SRP strengthened joints are examined through a comparison with the outcomes of the previous experimental program including companion specimens not provided with transverse beam stubs and strengthened by Carbon Fiber Reinforced Polymer (CFRP) systems. In particular, both qualitative and quantitative considerations about the influence of the confining effect provided by the secondary beams on the joint response, the suitability of all the adopted strengthening solutions (SRP/CFRP systems), the performances and the failure modes experienced in the several cases studied are provided.

Toward in situ monitoring of water contamination by nitroenergetic compounds.

PubMed

Johnson, Brandy J; Leska, Iwona A; Medina, Alejandro; Dyson, Norris F; Nasir, Mansoor; Melde, Brian J; Taft, Jenna R; Charles, Paul T

2012-11-06

We have previously described the application of novel porous organosilicate materials to the preconcentration of nitroenergetic targets from aqueous solution prior to HPLC analysis. The performance of the sorbents and the advantages of these types of materials over commercially available solid phase extraction sorbents have been demonstrated. Here, the development of systems for application of those sorbents to in situ monitoring is described. Considerations such as column pressure, particulate filtration, and component durability are discussed. The diameter of selected column housings, the sorbent bed depth, and the frits utilized significantly impact the utility of the sorbent columns in the prototype system. The impact of and necessity for improvements in the morphological characteristics of the sorbents as they relate to reduction in column pressure are detailed. The results of experiments utilizing a prototype system are presented. Data demonstrating feasibility for use of the sorbents in preconcentration prior to ion mobility spectrometry is also presented.

Implications of soil mixing for NAPL source zone remediation: Column studies and modeling of field-scale systems

NASA Astrophysics Data System (ADS)

Olson, Mitchell R.; Sale, Tom C.

2015-06-01

Soil remediation is often inhibited by subsurface heterogeneity, which constrains contaminant/reagent contact. Use of soil mixing techniques for reagent delivery provides a means to overcome contaminant/reagent contact limitations. Furthermore, soil mixing reduces the permeability of treated soils, thus extending the time for reactions to proceed. This paper describes research conducted to evaluate implications of soil mixing on remediation of non-aqueous phase liquid (NAPL) source zones. The research consisted of column studies and subsequent modeling of field-scale systems. For column studies, clean influent water was flushed through columns containing homogenized soils, granular zero valent iron (ZVI), and trichloroethene (TCE) NAPL. Within the columns, NAPL depletion occurred due to dissolution, followed by either column-effluent discharge or ZVI-mediated degradation. Complete removal of TCE NAPL from the columns occurred in 6-8 pore volumes of flow. However, most of the TCE (> 96%) was discharged in the column effluent; less than 4% of TCE was degraded. The low fraction of TCE degraded is attributed to the short hydraulic residence time (< 4 days) in the columns. Subsequently, modeling was conducted to scale up column results. By scaling up to field-relevant system sizes (> 10 m) and reducing permeability by one-or-more orders of magnitude, the residence time could be greatly extended, potentially for periods of years to decades. Model output indicates that the fraction of TCE degraded can be increased to > 99.9%, given typical post-mixing soil permeability values. These results suggest that remediation performance can be greatly enhanced by combining contaminant degradation with an extended residence time.

Compact sieve-tray distillation column for ammonia-water absorption heat pump: Part 1 -- Design methodology

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

Anand, G.; Erickson, D.C.

1999-07-01

The distillation column is a key component of ammonia-water absorption units including advanced generator-absorber heat exchange (GAX) cycle heat pumps. The design of the distillation column is critical to unit performance, size, and cost. The distillation column can be designed with random packing, structured packing, or various tray configurations. A sieve-tray distillation column is the least complicated tray design and is less costly than high-efficiency packing. Substantial literature is available on sieve tray design and performance. However, most of the correlations and design recommendations were developed for large industrial hydrocarbon systems and are generally not directly applicable to the compactmore » ammonia-water column discussed here. The correlations were reviewed and modified as appropriate for this application, and a sieve-tray design model was developed. This paper presents the sieve-tray design methodology for highly compact ammonia-water columns. A conceptual design of the distillation column for an 8 ton vapor exchange (VX) GAX heat pump is presented, illustrating relevant design parameters and trends. The design process revealed several issues that have to be investigated experimentally to design the final optimized rectifier. Validation of flooding and weeping limits and tray/point efficiencies are of primary importance.« less

Practical comparison of 2.7 microm fused-core silica particles and porous sub-2 microm particles for fast separations in pharmaceutical process development.

PubMed

Abrahim, Ahmed; Al-Sayah, Mohammad; Skrdla, Peter; Bereznitski, Yuri; Chen, Yadan; Wu, Naijun

2010-01-05

Fused-core silica stationary phases represent a key technological advancement in the arena of fast HPLC separations. These phases are made by fusing a 0.5 microm porous silica layer onto 1.7 microm nonporous silica cores. The reduced intra-particle flow path of the fused particles provides superior mass transfer kinetics and better performance at high mobile phase velocities, while the fused-core particles provide lower pressure than sub-2 microm particles. In this work, chromatographic performance of the fused-core particles (Ascentis Express) was investigated and compared to that of sub-2 microm porous particles (1.8 microm Zorbax Eclipse Plus C18 and 1.7 microm Acquity BEH C18). Specifically, retention, selectivity, and loading capacity were systematically compared for these two types of columns. Other chromatographic parameters such as efficiency and pressure drop were also studied. Although the fused-core column was found to provide better analyte shape selectivity, both columns had similar hydrophobic, hydrogen bonding, total ion-exchange, and acidic ion-exchange selectivities. As expected, the retention factors and sample loading capacity on the fused-core particle column were slightly lower than those for the sub-2 microm particle column. However, the most dramatic observation was that similar efficiency separations to the sub-2 microm particles could be achieved using the fused-core particles, without the expense of high column back pressure. The low pressure of the fused-core column allows fast separations to be performed routinely on a conventional LC system without significant loss in efficiency or resolution. Applications to the HPLC impurity profiling of drug substance candidates were performed using both types of columns to validate this last point.

Design and Prototype of an Automated Column-Switching HPLC System for Radiometabolite Analysis.

PubMed

Vasdev, Neil; Collier, Thomas Lee

2016-08-17

Column-switching high performance liquid chromatography (HPLC) is extensively used for the critical analysis of radiolabeled ligands and their metabolites in plasma. However, the lack of streamlined apparatus and consequently varying protocols remain as a challenge among positron emission tomography laboratories. We report here the prototype apparatus and implementation of a fully automated and simplified column-switching procedure to allow for the easy and automated determination of radioligands and their metabolites in up to 5 mL of plasma. The system has been used with conventional UV and coincidence radiation detectors, as well as with a single quadrupole mass spectrometer.

Assessing Arsenic Removal by Metal (Hydr)Oxide Adsorptive Media Using Rapid Small Scale Column Tests

EPA Science Inventory

The rapid small scale column test (RSSCT) was use to evaluate the the performance of eight commercially available adsorptive media for the removal of arsenic. Side-by-side tests were conducted using RSSCTs and pilot/full-scale systems either in the field or in the laboratory. ...

Treatment of Copper Contaminated Municipal Wastewater by Using UASB Reactor and Sand-Chemically Carbonized Rubber Wood Sawdust Column

PubMed Central

Biswas, Swarup; Mishra, Umesh

2016-01-01

The performance of a laboratory scale upflow anaerobic sludge blanket (UASB) reactor and its posttreatment unit of sand-chemically carbonized rubber wood sawdust (CCRWSD) column system for the treatment of a metal contaminated municipal wastewater was investigated. Copper ion contaminated municipal wastewater was introduced to a laboratory scale UASB reactor and the effluent from UASB reactor was then followed by treatment with sand-CCRWSD column system. The laboratory scale UASB reactor and column system were observed for a period of 121 days. After the posttreatment column the average removal of monitoring parameters such as copper ion concentration (91.37%), biochemical oxygen demand (BODT) (93.98%), chemical oxygen demand (COD) (95.59%), total suspended solid (TSS) (95.98%), ammonia (80.68%), nitrite (79.71%), nitrate (71.16%), phosphorous (44.77%), total coliform (TC) (99.9%), and fecal coliform (FC) (99.9%) was measured. The characterization of the chemically carbonized rubber wood sawdust was done by scanning electron microscope (SEM), X-ray fluorescence spectrum (XRF), and Fourier transforms infrared spectroscopy (FTIR). Overall the system was found to be an efficient and economical process for the treatment of copper contaminated municipal wastewater. PMID:26904681

Treatment of Copper Contaminated Municipal Wastewater by Using UASB Reactor and Sand-Chemically Carbonized Rubber Wood Sawdust Column.

PubMed

Biswas, Swarup; Mishra, Umesh

2016-01-01

The performance of a laboratory scale upflow anaerobic sludge blanket (UASB) reactor and its posttreatment unit of sand-chemically carbonized rubber wood sawdust (CCRWSD) column system for the treatment of a metal contaminated municipal wastewater was investigated. Copper ion contaminated municipal wastewater was introduced to a laboratory scale UASB reactor and the effluent from UASB reactor was then followed by treatment with sand-CCRWSD column system. The laboratory scale UASB reactor and column system were observed for a period of 121 days. After the posttreatment column the average removal of monitoring parameters such as copper ion concentration (91.37%), biochemical oxygen demand (BODT) (93.98%), chemical oxygen demand (COD) (95.59%), total suspended solid (TSS) (95.98%), ammonia (80.68%), nitrite (79.71%), nitrate (71.16%), phosphorous (44.77%), total coliform (TC) (99.9%), and fecal coliform (FC) (99.9%) was measured. The characterization of the chemically carbonized rubber wood sawdust was done by scanning electron microscope (SEM), X-ray fluorescence spectrum (XRF), and Fourier transforms infrared spectroscopy (FTIR). Overall the system was found to be an efficient and economical process for the treatment of copper contaminated municipal wastewater.

Cool pool development. Quarterly technical report No. 1, April-June 1979

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

Crowther, K.

1979-10-15

The Cool Pool is a passive cooling system consisting of a shaded, evaporating roof pond which thermosiphons cool water into water-filled, metal columns (culvert pipes) located within the building living space. The water in the roof pond is cooled by evaporation, convection and radiation. Because the water in the pool and downcomer is colder and denser than the water in the column a pressure difference is created and the cold water flows from the pool, through the downcomer and into the bottom of the column. The warm column water rises and flows through a connecting pipe into the pool. Itmore » is then cooled and the cycle repeats itself. The system requires no pumps. The water column absorbs heat from the building interior primarily by convection and radiation. Since the column is radiating at a significantly lower temperature than the interior walls it plays a double role in human comfort. Not only does it cool the air by convection but it provides a heat sink to which people can radiate. Since thermal radiation is important to the cooling of people, the cold water column contributes substantially to their feelings of comfort. Research on the Cool Pool system includes the following major tasks: control of biological organisms and debris in the roof pond and water cylinders; development of a heat exchanger; experimental investigation of the system's thermal performance; and development of a predictive computer simulation of the Cool Pool. Progress in these tasks is reported.« less

Evaluation of Structural Robustness against Column Loss: Methodology and Application to RC Frame Buildings.

PubMed

Bao, Yihai; Main, Joseph A; Noh, Sam-Young

2017-08-01

A computational methodology is presented for evaluating structural robustness against column loss. The methodology is illustrated through application to reinforced concrete (RC) frame buildings, using a reduced-order modeling approach for three-dimensional RC framing systems that includes the floor slabs. Comparisons with high-fidelity finite-element model results are presented to verify the approach. Pushdown analyses of prototype buildings under column loss scenarios are performed using the reduced-order modeling approach, and an energy-based procedure is employed to account for the dynamic effects associated with sudden column loss. Results obtained using the energy-based approach are found to be in good agreement with results from direct dynamic analysis of sudden column loss. A metric for structural robustness is proposed, calculated by normalizing the ultimate capacities of the structural system under sudden column loss by the applicable service-level gravity loading and by evaluating the minimum value of this normalized ultimate capacity over all column removal scenarios. The procedure is applied to two prototype 10-story RC buildings, one employing intermediate moment frames (IMFs) and the other employing special moment frames (SMFs). The SMF building, with its more stringent seismic design and detailing, is found to have greater robustness.

OTEC gas desorption studies

NASA Astrophysics Data System (ADS)

Chen, F. C.; Golshani, A.

1982-02-01

Experiments on deaeration in packed columns and barometric intake systems, and with hydraulic air compression for open-cycle OTEC systems are reported. A gas desorption test loop consisting of water storage tanks, a vacuum system, a liquid recirculating system, an air supply, a column test section, and two barometric leg test sections was used to perform the tests. The aerated water was directed through columns filled with either ceramic Raschig rings or plastic pall rings, and the system vacuum pressure, which drives the deaeration process, was found to be dependent on water velocity and intake pipe height. The addition of a barometric intake pipe increased the deaeration effect 10%, and further tests were run with lengths of PVC pipe as potential means for noncondensibles disposal through hydraulic air compression. Using the kinetic energy from the effluent flow to condense steam in the noncondensible stream improved the system efficiency.

Evaluation of layered and mixed passive treatment systems for acid mine drainage.

PubMed

Jeen, Sung-Wook; Mattson, Bruce

2016-11-01

Laboratory column tests for passive treatment systems for mine drainage from a waste rock storage area were conducted to evaluate suitable reactive mixture, system configuration, effects of influent water chemistry, and required residence time. Five columns containing straw, chicken manure, mushroom compost, and limestone (LS), in either layered or mixed configurations, were set up to simulate the treatment system. The results showed that all of the five columns removed metals of concern (i.e. Al, Cd, Co, Cu, Fe, Ni, and Zn) with a residence time of 15 h and greater. Reaction mechanisms responsible for the removal of metals may include sulfate reduction and subsequent sulfide precipitation, precipitation of secondary carbonates and hydroxides, co-precipitation, and sorption on organic substrates and secondary precipitates. The results suggest that the mixed systems containing organic materials and LS perform better than the layered systems, sequentially treated by organic and LS layers, due to the enhanced pH adjustment, which is beneficial to bacterial activity and precipitation of secondary minerals. The column tests provide a basis for the design of a field-scale passive treatment system, such as a reducing and alkalinity producing system or a permeable reactive barrier.

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) (r>0.997) and a system precision of 10 mg L(-1) with a RSD ≤ 1.65%. The high performance of the chromatography process with the RP-Amide column under optimised conditions was highlighted and well documented (HETP values ≤ 10 μm, peak symmetry ≤ 1.33, resolution ≥ 1.87 and time for one analysis <8.0 min). The results of these experiments confirmed the benefits of extending chromatographic selectivity using core-shell particle column technology in a SIC manifold. Copyright © 2012 Elsevier B.V. All rights reserved.

Compact microchannel system

DOEpatents

Griffiths, Stewart

2003-09-30

The present invention provides compact geometries for the layout of microchannel columns through the use of turns and straight channel segments. These compact geometries permit the use of long separation or reaction columns on a small microchannel substrate or, equivalently, permit columns of a fixed length to occupy a smaller substrate area. The new geometries are based in part on mathematical analyses that provide the minimum turn radius for which column performance in not degraded. In particular, we find that straight channel segments of sufficient length reduce the required minimum turn radius, enabling compact channel layout when turns and straight segments are combined. The compact geometries are obtained by using turns and straight segments in overlapped or nested arrangements to form pleated or coiled columns.

Implications of soil mixing for NAPL source zone remediation: Column studies and modeling of field-scale systems.

PubMed

Olson, Mitchell R; Sale, Tom C

2015-01-01

Soil remediation is often inhibited by subsurface heterogeneity, which constrains contaminant/reagent contact. Use of soil mixing techniques for reagent delivery provides a means to overcome contaminant/reagent contact limitations. Furthermore, soil mixing reduces the permeability of treated soils, thus extending the time for reactions to proceed. This paper describes research conducted to evaluate implications of soil mixing on remediation of non-aqueous phase liquid (NAPL) source zones. The research consisted of column studies and subsequent modeling of field-scale systems. For column studies, clean influent water was flushed through columns containing homogenized soils, granular zero valent iron (ZVI), and trichloroethene (TCE) NAPL. Within the columns, NAPL depletion occurred due to dissolution, followed by either column-effluent discharge or ZVI-mediated degradation. Complete removal of TCE NAPL from the columns occurred in 6-8 pore volumes of flow. However, most of the TCE (>96%) was discharged in the column effluent; less than 4% of TCE was degraded. The low fraction of TCE degraded is attributed to the short hydraulic residence time (<4 days) in the columns. Subsequently, modeling was conducted to scale up column results. By scaling up to field-relevant system sizes (>10 m) and reducing permeability by one-or-more orders of magnitude, the residence time could be greatly extended, potentially for periods of years to decades. Model output indicates that the fraction of TCE degraded can be increased to >99.9%, given typical post-mixing soil permeability values. These results suggest that remediation performance can be greatly enhanced by combining contaminant degradation with an extended residence time. Copyright © 2015 Elsevier B.V. All rights reserved.

Shell and small particles; evaluation of new column technology.

PubMed

Fekete, Szabolcs; Fekete, Jeno; Ganzler, Katalin

2009-01-15

The performance of 5 cm long columns packed with shell particles was compared to totally porous sub-2 microm particles in gradient and isocratic elution separations of hormones (dienogest, finasteride, gestodene, levonorgestrel, estradiol, ethinylestradiol, noretistherone acetate, bicalutamide and tibolone). Peak capacities around 140-150 could be achieved in 25 min with the 5 cm long columns. The Ascentis Express column (packed with 2.7 microm shell particles) showed similar efficiency to sub-2 microm particles under gradient conditions. Applying isocratic separation, the column of 2.7 microm shell particles had a reduced plate height minimum of approximately h=1.6. It was much smaller than obtained with totally porous particles (h approximately = 2.8). The impedance time also proved more favorable with 2.7 microm shell particles than with totally porous particles. The influence of extra-column volume on column efficiency was investigated. The extra-column dispersion of the chromatographic system may cause a shift of the HETP curves.

Effect of pressure pulses at the interface valve on the stability of second dimension columns in online comprehensive two-dimensional liquid chromatography.

PubMed

Talus, Eric S; Witt, Klaus E; Stoll, Dwight R

2015-01-23

Users of online comprehensive two-dimensional liquid chromatography (LCxLC) frequently acknowledge that the mechanical instability of HPLC columns installed in these systems, particularly in the second dimension, is a significant impediment to its use. Such instability is not surprising given the strenuous operating environment to which these columns are subjected, including the large number (thousands per day) of fast and large pressure pulses resulting from interface valve switches (on the timescale of tens of milliseconds) associated with very fast second dimension separations. There appear to be no published reports of systematic studies of the relationship between second dimension column lifetime and any of these variables. In this study we focused on the relationship between the lifetimes of commercially available columns and the pressure pulses observed at the inlet of the second dimension column that occur during the switching of the valve that interfaces the two dimensions of a LCxLC system. We find that the magnitude of the pressure drop at the inlet of the second dimension column during the valve switch, which may vary between 10 and 95% of the column inlet pressure, is dependent on valve switching speed and design, and has a dramatic impact on column lifetime. In the worst case, columns fail within the first few hours of use in an LCxLC system. In the best case, using a valve that exhibits much smaller pressure pulses, the same columns exhibit much improved lifetimes and have been used continuously under LCxLC conditions for several days with no degradation in performance. This result represents a first step in understanding the factors that affect second dimension column lifetime, and will significantly improve the usability of the LCxLC technique in general. Copyright © 2014 Elsevier B.V. All rights reserved.

Preparation of a poly(styrene-co-DPHA-co-EDMA) monolith and its application for the separation of small molecules and biomacromolecules by HPLC.

PubMed

Wang, Xixi; Li, Xueying; Jiang, Xiaoya; Dong, Peipei; Liu, Haiyan; Bai, Ligai; Yan, Hongyuan

2017-04-01

A high performance liquid chromatography (HPLC) monolithic column was prepared by redox polymerization of styrene, dipentaerythritol hexaacrylate (DPHA) and ethylene glycol dimethacrylate (EDMA) in a porogen system of n-propanol/PEG400. The monolith was characterized by scanning electron microscopy (SEM), mercury intrusion porosimetry (MIP) and the results indicated that the monolith had a stable and homogeneous structure. The porosity of the monolithic column was 75.86% and average pore diameter was 2.1µm. Several alkylbenzenes and anilines were used to evaluate the column performance in terms of hydrophobicity. Then the column was applied to separate small molecules including phytosterol and BSA tryptic digest. Finally, five standard proteins, egg white and plasma were separated respectively and high separation capacity of protein was obtained. Copyright © 2016 Elsevier B.V. All rights reserved.

Experimental investigation of damage behavior of RC frame members including non-seismically designed columns

NASA Astrophysics Data System (ADS)

Chen, Linzhi; Lu, Xilin; Jiang, Huanjun; Zheng, Jianbo

2009-06-01

Reinforced concrete (RC) frame structures are one of the mostly common used structural systems, and their seismic performance is largely determined by the performance of columns and beams. This paper describes horizontal cyclic loading tests of ten column and three beam specimens, some of which were designed according to the current seismic design code and others were designed according to the early non-seismic Chinese design code, aiming at reporting the behavior of the damaged or collapsed RC frame strctures observed during the Wenchuan earthquake. The effects of axial load ratio, shear span ratio, and transverse and longitudinal reinforcement ratio on hysteresis behavior, ductility and damage progress were incorporated in the experimental study. Test results indicate that the non-seismically designed columns show premature shear failure, and yield larger maximum residual crack widths and more concrete spalling than the seismically designed columns. In addition, longitudinal steel reinforcement rebars were severely buckled. The axial load ratio and shear span ratio proved to be the most important factors affecting the ductility, crack opening width and closing ability, while the longitudinal reinforcement ratio had only a minor effect on column ductility, but exhibited more influence on beam ductility. Finally, the transverse reinforcement ratio did not influence the maximum residual crack width and closing ability of the seismically designed columns.

Transport and degradation of metalaxyl and isoproturon in biopurification columns inoculated with pesticide-primed material.

PubMed

De Wilde, Tineke; Spanoghe, Pieter; Sniegowksi, Kristel; Ryckeboer, Jaak; Jaeken, Peter; Springael, Dirk

2010-01-01

Laboratory column displacement experiments were performed to examine whether addition of pesticide-primed material to the matrix of an on-farm biopurification system (BPS), intended to remove pesticides from agricultural waste water, positively affects the degradation of mobile pesticides in the system. Percolated column microcosms with varying types and amounts of metalaxyl and/or isoproturon-primed material or non-primed material were irrigated with water artificially contaminated with isoproturon and/or metalaxyl. Transport of isoproturon was well described using the convection dispersion equation and no dissipation was observed, even in columns inoculated with isoproturon-primed material. On the other hand, delayed dissipation of metalaxyl, i.e., after an initial lag phase, was encountered in all columns receiving metalaxyl. In all systems, dissipation could be described using the Monod model indicating that a metalaxyl degrading population grew in the systems. There was a clear correlation between the lag phase and the amount of metalaxyl-primed material added to the system, i.e., increasing amounts of added material resulted into shorter lag phases and hence more rapid initiation of growth-associated metalaxyl degradation in the system. Our observations suggest that indeed pesticide-primed material can reduce the start-up phase of degradation of mobile pesticides in a BPS and as such can increase its efficiency. However, the primed material should be chosen carefully and preferentially beforehand tested for its capacity to degrade the pesticide.

Ultrafast UPLC-ESI-MS and HPLC with monolithic column for determination of principal flavor compounds in vanilla pods.

PubMed

Sharma, Upendra K; Sharma, Nandini; Sinha, Arun K; Kumar, Neeraj; Gupta, Ajai P

2009-10-01

In this study, two novel chromatographic methods based on monolithic column high-performance liquid chromatography (HPLC) and ultra-performance liquid chromatography (UPLC) were developed for the ultrafast determination of principal flavor compounds namely vanillin, vanillic acid, p-hydroxybenzoic acid, and p-hydroxybenzaldehyde in ethanolic extracts of Vanilla planifolia pods. Good separation was achieved within 2.5 min using Chromolith RP18e column (100 mm x 4.6 mm) for HPLC and Acquity BEH C-18 (100 mm x 2.1 mm, 1.7 microm) column for UPLC. Both methods were compared in terms of total analysis time, mobile phase consumption, sensitivity, and validation parameters like precision, accuracy, LOD, and LOQ. Further, system suitability test data including resolution, capacity factor, theoretical plates, and tailing factor was determined for both the methods by ten replicate injections. Monolithic column based HPLC gave better results for most of the selected parameters while UPLC was found to be more eco-friendly with low mobile phase consumption and better sensitivity. Both methods may be used conveniently for the high throughput analysis of large number of samples in comparison to traditional particulate column.

Simulation of Unique Pressure Changing Steps and Situations in Psa Processes

NASA Technical Reports Server (NTRS)

Ebner, Armin D.; Mehrotra, Amal; Knox, James C.; LeVan, Douglas; Ritter, James A.

2007-01-01

A more rigorous cyclic adsorption process simulator is being developed for use in the development and understanding of new and existing PSA processes. Unique features of this new version of the simulator that Ritter and co-workers have been developing for the past decade or so include: multiple absorbent layers in each bed, pressure drop in the column, valves for entering and exiting flows and predicting real-time pressurization and depressurization rates, ability to account for choked flow conditions, ability to pressurize and depressurize simultaneously from both ends of the columns, ability to equalize between multiple pairs of columns, ability to equalize simultaneously from both ends of pairs of columns, and ability to handle very large pressure ratios and hence velocities associated with deep vacuum systems. These changes to the simulator now provide for unique opportunities to study the effects of novel pressure changing steps and extreme process conditions on the performance of virtually any commercial or developmental PSA process. This presentation will provide an overview of the cyclic adsorption process simulator equations and algorithms used in the new adaptation. It will focus primarily on the novel pressure changing steps and their effects on the performance of a PSA system that epitomizes the extremes of PSA process design and operation. This PSA process is a sorbent-based atmosphere revitalization (SBAR) system that NASA is developing for new manned exploration vehicles. This SBAR system consists of a 2-bed 3-step 3-layer system that operates between atmospheric pressure and the vacuum of space, evacuates from both ends of the column simultaneously, experiences choked flow conditions during pressure changing steps, and experiences a continuously changing feed composition, as it removes metabolic CO2 and H20 from a closed and fixed volume, i.e., the spacecraft cabin. Important process performance indicators of this SBAR system are size, and the corresponding CO2 and H20 removal efficiencies, and N2 and O2 loss rates. Results of the fundamental behavior of this PSA process during extreme operating conditions will be presented and discussed.

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

Youker, Amanda J.; Krebs, John F.; Quigley, Kevin J.

With funding from the National Nuclear Security Administrations Material Management and Minimization Office, Argonne National Laboratory (Argonne) is providing technical assistance to help accelerate the U.S. production of Mo-99 using a non-highly enriched uranium (non-HEU) source. A potential Mo-99 production pathway is by accelerator-initiated fissioning in a subcritical uranyl sulfate solution containing low enriched uranium (LEU). As part of the Argonne development effort, we are undertaking the AMORE (Argonne Molybdenum Research Experiment) project, which is essentially a pilot facility for all phases of Mo-99 production, recovery, and purification. Production of Mo-99 and other fission products in the subcritical target solutionmore » is initiated by putting an electron beam on a depleted uranium (DU) target; the fast neutrons produced in the DU target are thermalized and lead to fissioning of U-235. At the end of irradiation, Mo is recovered from the target solution and separated from uranium and most of the fission products by using a titania column. The Mo is stripped from the column with an alkaline solution. After acidification of the Mo product solution from the recovery column, the Mo is concentrated (and further purified) in a second titania column. The strip solution from the concentration column is then purified with the LEU Modified Cintichem process. A full description of the process can be found elsewhere [1–3]. The initial commissioning steps for the AMORE project include performing a Mo-99 spike test with pH 1 sulfuric acid in the target vessel without a beam on the target to demonstrate the initial Mo separation-and-recovery process, followed by the concentration column process. All glovebox operations were tested with cold solutions prior to performing the Mo-99 spike tests. Two Mo-99 spike tests with pH 1 sulfuric acid have been performed to date. Figure 1 shows the flow diagram for the remotely operated Mo-recovery system for the AMORE project. There are two separate pumps and flow paths for the acid and base operations. The system contains three sample ladders with eight sample loops per ladder for target mixing; column loading, including acid and water washes; and column stripping, including the final water wash.« less

Pre-disinfection columns to improve the performance of the direct electro-disinfection of highly faecal-polluted surface water.

PubMed

Isidro, J; Llanos, J; Sáez, C; Lobato, J; Cañizares, P; Rodrigo, M A

2018-09-15

This work presents the design and evaluation of a new concept of pre-disinfection treatment that is especially suited for highly polluted surface water and is based on the combination of coagulation-flocculation, lamellar sedimentation and filtration into a single-column unit, in which the interconnection between treatments is an important part of the overall process. The new system, the so-called PREDICO (PRE-DIsinfection Column) system, was built with low-cost consumables from hardware stores (in order to promote in-house construction of the system in poor countries) and was tested with a mixture of 20% raw wastewater and 80% surface water (in order to simulate an extremely bad situation). The results confirmed that the PREDICO system helps to avoid fouling in later electro-disinfection processes and attains a remarkable degree of disinfection (3-4 log units), which supplements the removal of pathogens attained by the electrolytic cell (more than 4 log units). The most important sizing parameters for the PREDICO system are the surface loading rate (SLR) and the hydraulic residence time (HRT); SLR values under 20 cm min -1 and HRT values over 13.6 min in the PREDICO system are suitable to warrant efficient performance of the system. Copyright © 2018 Elsevier Ltd. All rights reserved.

Analysis of Slab-column Shearwall Structure of 6000 Tons Cold Storage

NASA Astrophysics Data System (ADS)

He, Dongqing; Song, Pengwei; Jie, Pengyu

2018-05-01

Combining with the functional requirements, the site conditions and the 6000 tons load characteristics of cold storage, so determine its structure system for the slab-column-shear wall structure. The paper recommends the design of foundation, the settings of column cap, the arrangement of shear wall, the punching shear of floor slab and the analysis and calculation results of main structure. By addition shear wall in slab-column structure to increase the overall stiffness of structure and improve the seismic performance of structure. Take the detached form between the main structure and the external wall insulation, while set anchorage beam between in the main floor and the ring beam along the axis of the column grid to enhance the overall stability of the external wall insulation.

Mitigation of Liquefaction in Sandy Soils Using Stone Columns

NASA Astrophysics Data System (ADS)

Selcuk, Levent; Kayabalı, Kamil

2010-05-01

Soil liquefaction is one of the leading causes of earthquake-induced damage to structures. Soil improvement methods provide effective solutions to reduce the risk of soil liquefaction. Thus, soil ground treatments are applied using various techniques. However, except for a few ground treatment methods, they generally require a high cost and a lot of time. Especially in order to prevent the risk of soil liquefaction, stone columns conctructed by vibro-systems (vibro-compaction, vibro-replacement) are one of the traditional geotechnical methods. The construction of stone columns not only enhances the ability of clean sand to drain excess pore water during an earthquake, but also increases the relative density of the soil. Thus, this application prevents the development of the excess pore water pressure in sand during earthquakes and keeps the pore pressure ratio below a certain value. This paper presents the stone column methods used against soil liquefaction in detail. At this stage, (a) the performances of the stone columns were investigated in different spacing and diameters of columns during past earthquakes, (b) recent studies about design and field applications of stone columns were presented, and (c) a new design method considering the relative density of soil and the capacity of drenage of columns were explained in sandy soil. Furthermore, with this new method, earthquake performances of the stone columns constructed at different areas were investigated before the 1989 Loma Prieta and the 1994 Northbridge earthquakes, as case histories of field applications, and design charts were compiled for suitable spacing and diameters of stone columns with consideration to the different sandy soil parameters and earhquake conditions. Key Words: Soil improvement, stone column, excess pore water pressure

Performance comparison of three types of high-speed counter-current chromatographs for the separation of components of hydrophilic and hydrophobic color additives.

PubMed

Weisz, Adrian; Ito, Yoichiro

2011-09-09

The performance of three types of high-speed counter-current chromatography (HSCCC) instruments was assessed for their use in separating components in hydrophilic and hydrophobic dye mixtures. The HSCCC instruments compared were: (i) a J-type coil planet centrifuge (CPC) system with a conventional multilayer-coil column, (ii) a J-type CPC system with a spiral-tube assembly-coil column, and (iii) a cross-axis CPC system with a multilayer-coil column. The hydrophilic dye mixture consisted of a sample of FD&C Blue No. 2 that contained mainly two isomeric components, 5,5'- and 5,7'-disulfonated indigo, in the ratio of ∼7:1. The hydrophobic dye mixture consisted of a sample of D&C Red No. 17 (mainly Sudan III) and Sudan II in the ratio of ∼4:1. The two-phase solvent systems used for these separations were 1-butanol/1.3M HCl and hexane/acetonitrile. Each of the three instruments was used in two experiments for the hydrophilic dye mixture and two for the hydrophobic dye mixture, for a total of 12 experiments. In one set of experiments, the lower phase was used as the mobile phase, and in the second set of experiments, the upper phase was used as the mobile phase. The results suggest that: (a) use of a J-type instrument with either a multilayer-coil column or a spiral-tube assembly column, applying the lower phase as the mobile phase, is preferable for separating the hydrophilic components of FD&C Blue No. 2; and (b) use of a J-type instrument with multilayer-coil column, while applying either the upper phase or the lower phase as the mobile phase, is preferable for separating the hydrophobic dye mixture of D&C Red No. 17 and Sudan II. Published by Elsevier B.V.

Evaluation of Structural Robustness against Column Loss: Methodology and Application to RC Frame Buildings

PubMed Central

Bao, Yihai; Main, Joseph A.; Noh, Sam-Young

2017-01-01

A computational methodology is presented for evaluating structural robustness against column loss. The methodology is illustrated through application to reinforced concrete (RC) frame buildings, using a reduced-order modeling approach for three-dimensional RC framing systems that includes the floor slabs. Comparisons with high-fidelity finite-element model results are presented to verify the approach. Pushdown analyses of prototype buildings under column loss scenarios are performed using the reduced-order modeling approach, and an energy-based procedure is employed to account for the dynamic effects associated with sudden column loss. Results obtained using the energy-based approach are found to be in good agreement with results from direct dynamic analysis of sudden column loss. A metric for structural robustness is proposed, calculated by normalizing the ultimate capacities of the structural system under sudden column loss by the applicable service-level gravity loading and by evaluating the minimum value of this normalized ultimate capacity over all column removal scenarios. The procedure is applied to two prototype 10-story RC buildings, one employing intermediate moment frames (IMFs) and the other employing special moment frames (SMFs). The SMF building, with its more stringent seismic design and detailing, is found to have greater robustness. PMID:28890599

40 CFR 63.343 - Compliance provisions.

Code of Federal Regulations, 2010 CFR

2010-07-01

... operators of affected sources. (1) Composite mesh-pad systems. (i) During the initial performance test, the... with the emission limitations in § 63.342 through the use of a composite mesh-pad system shall... one performance test and accept ±2 inches of water column from this value as the compliant range. (ii...

40 CFR 63.343 - Compliance provisions.

Code of Federal Regulations, 2012 CFR

2012-07-01

... operators of affected sources. (1) Composite mesh-pad systems. (i) During the initial performance test, the... with the emission limitations in § 63.342 through the use of a composite mesh-pad system shall... one performance test and accept ±2 inches of water column from this value as the compliant range. (ii...

40 CFR 63.343 - Compliance provisions.

Code of Federal Regulations, 2011 CFR

2011-07-01

... operators of affected sources. (1) Composite mesh-pad systems. (i) During the initial performance test, the... with the emission limitations in § 63.342 through the use of a composite mesh-pad system shall... one performance test and accept ±2 inches of water column from this value as the compliant range. (ii...

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).

Microfluidic chip for peptide analysis with an integrated HPLC column, sample enrichment column, and nanoelectrospray tip.

PubMed

Yin, Hongfeng; Killeen, Kevin; Brennen, Reid; Sobek, Dan; Werlich, Mark; van de Goor, Tom

2005-01-15

Current nano-LC/MS systems require the use of an enrichment column, a separation column, a nanospray tip, and the fittings needed to connect these parts together. In this paper, we present a microfabricated approach to nano-LC, which integrates these components on a single LC chip, eliminating the need for conventional LC connections. The chip was fabricated by laminating polyimide films with laser-ablated channels, ports, and frit structures. The enrichment and separation columns were packed using conventional reversed-phase chromatography particles. A face-seal rotary valve provided a means for switching between sample loading and separation configurations with minimum dead and delay volumes while allowing high-pressure operation. The LC chip and valve assembly were mounted within a custom electrospray source on an ion-trap mass spectrometer. The overall system performance was demonstrated through reversed-phase gradient separations of tryptic protein digests at flow rates between 100 and 400 nL/min. Microfluidic integration of the nano-LC components enabled separations with subfemtomole detection sensitivity, minimal carryover, and robust and stable electrospray throughout the LC solvent gradient.

Characterization of new types of stationary phases for fast and ultra-fast liquid chromatography by signal processing based on AutoCovariance Function: a case study of application to Passiflora incarnata L. extract separations.

PubMed

Pietrogrande, Maria Chiara; Dondi, Francesco; Ciogli, Alessia; Gasparrini, Francesco; Piccin, Antonella; Serafini, Mauro

2010-06-25

In this study, a comparative investigation was performed of HPLC Ascentis (2.7 microm particles) columns based on fused-core particle technology and Acquity (1.7 microm particles) columns requiring UPLC instruments, in comparison with Chromolith RP-18e columns. The study was carried out on mother and vegetal tinctures of Passiflora incarnata L. on one single or two coupled columns. The fundamental attributions of the chromatographic profiles are evaluated using a chemometric procedure, based on the AutoCovariance Function (ACVF). Different chromatographic systems are compared in terms of their separation parameters, i.e., number of total chemical components (m(tot)), separation efficiency (sigma), peak capacity (n(c)), overlap degree of peaks and peak purity. The obtained results show the improvements achieved by HPLC columns with narrow size particles in terms of total analysis time and chromatographic efficiency: comparable performance are achieved by Ascentis (2.7 microm particle) column and Acquity (1.7 microm particle) column requiring UPLC instruments. The ACVF plot is proposed as a simplified tool describing the chromatographic fingerprint to be used for evaluating and comparing chemical composition of plant extracts by using the parameters D% - relative abundance of the deterministic component - and c(EACF) - similarity index computed on ACVF. Copyright 2010 Elsevier B.V. All rights reserved.

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.

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.

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

Nano-LC/MALDI-MS using a column-integrated spotting probe for analysis of complex biomolecule samples.

PubMed

Hioki, Yusaku; Tanimura, Ritsuko; Iwamoto, Shinichi; Tanaka, Koichi

2014-03-04

Nanoflow liquid chromatography (nano-LC) is an essential technique for highly sensitive analysis of complex biological samples, and matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) is advantageous for rapid identification of proteins and in-depth analysis of post-translational modifications (PTMs). A combination of nano-LC and MALDI-MS (nano-LC/MALDI-MS) is useful for highly sensitive and detailed analysis in life sciences. However, the existing system does not fully utilize the advantages of each technique, especially in the interface of eluate transfer from nano-LC to a MALDI plate. To effectively combine nano-LC with MALDI-MS, we integrated a nano-LC column and a deposition probe for the first time (column probe) and incorporated it into a nano-LC/MALDI-MS system. Spotting nanoliter eluate droplets directly from the column onto the MALDI plate prevents postcolumn diffusion and preserves the chromatographic resolution. A DHB prespotted plate was prepared to suit the fabricated column probe to concentrate the droplets of nano-LC eluate. The performance of the advanced nano-LC/MALDI-MS system was substantiated by analyzing protein digests. When the system was coupled with multidimensional liquid chromatography (MDLC), trace amounts of glycopeptides that spiked into complex samples were successfully detected. Thus, a nano-LC/MALDI-MS direct-spotting system that eliminates postcolumn diffusion was constructed, and the efficacy of the system was demonstrated through highly sensitive analysis of the protein digests or spiked glycopeptides.

PEROXIDE DESTRUCTION TESTING FOR THE 200 AREA EFFLUENT TREATMENT FACILITY

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

HALGREN DL

2010-03-12

The hydrogen peroxide decomposer columns at the 200 Area Effluent Treatment Facility (ETF) have been taken out of service due to ongoing problems with particulate fines and poor destruction performance from the granular activated carbon (GAC) used in the columns. An alternative search was initiated and led to bench scale testing and then pilot scale testing. Based on the bench scale testing three manganese dioxide based catalysts were evaluated in the peroxide destruction pilot column installed at the 300 Area Treated Effluent Disposal Facility. The ten inch diameter, nine foot tall, clear polyvinyl chloride (PVC) column allowed for the samemore » six foot catalyst bed depth as is in the existing ETF system. The flow rate to the column was controlled to evaluate the performance at the same superficial velocity (gpm/ft{sup 2}) as the full scale design flow and normal process flow. Each catalyst was evaluated on peroxide destruction performance and particulate fines capacity and carryover. Peroxide destruction was measured by hydrogen peroxide concentration analysis of samples taken before and after the column. The presence of fines in the column headspace and the discharge from carryover was generally assessed by visual observation. All three catalysts met the peroxide destruction criteria by achieving hydrogen peroxide discharge concentrations of less than 0.5 mg/L at the design flow with inlet peroxide concentrations greater than 100 mg/L. The Sud-Chemie T-2525 catalyst was markedly better in the minimization of fines and particle carryover. It is anticipated the T-2525 can be installed as a direct replacement for the GAC in the peroxide decomposer columns. Based on the results of the peroxide method development work the recommendation is to purchase the T-2525 catalyst and initially load one of the ETF decomposer columns for full scale testing.« less

Cyclic performance of concrete-filled steel batten built-up columns

NASA Astrophysics Data System (ADS)

Razzaghi, M. S.; Khalkhaliha, M.; Aziminejad, A.

2016-03-01

Steel built-up batten columns are common types of columns in Iran and some other parts of the world. They are economic and have acceptable performance due to gravity loads. Although several researches have been conducted on the behavior of the batten columns under axial loads, there are few available articles about their seismic performance. Experience of the past earthquakes, particularly the 2003 Bam earthquake in Iran, revealed that these structural members are seismically vulnerable. Thus, investigation on seismic performance of steel batten columns due to seismic loads and providing a method for retrofitting them are important task in seismic-prone areas. This study aims to investigate the behavior of concrete-filled batten columns due to combined axial and lateral loads. To this end, nonlinear static analyses were performed using ANSYS software. Herein, the behaviors of the steel batten columns with and without concrete core were compared. The results of this study showed that concrete-filled steel batten columns, particularly those filled with high-strength concrete, may cause significant increases in energy absorption and capacity of the columns. Furthermore, concrete core may improve post-buckling behavior of steel batten columns.

Integrated enzyme reactor and high resolving chromatography in "sub-chip" dimensions for sensitive protein mass spectrometry.

PubMed

Hustoft, Hanne Kolsrud; Brandtzaeg, Ole Kristian; Rogeberg, Magnus; Misaghian, Dorna; Torsetnes, Silje Bøen; Greibrokk, Tyge; Reubsaet, Léon; Wilson, Steven Ray; Lundanes, Elsa

2013-12-16

Reliable, sensitive and automatable analytical methodology is of great value in e.g. cancer diagnostics. In this context, an on-line system for enzymatic cleavage of proteins, subsequent peptide separation by liquid chromatography (LC) with mass spectrometric detection has been developed using "sub-chip" columns (10-20 μm inner diameter, ID). The system could detect attomole amounts of isolated cancer biomarker progastrin-releasing peptide (ProGRP), in a more automatable fashion compared to previous methods. The workflow combines protein digestion using an 20 μm ID immobilized trypsin reactor with a polymeric layer of 2-hydroxyethyl methacrylate-vinyl azlactone (HEMA-VDM), desalting on a polystyrene-divinylbenzene (PS-DVB) monolithic trap column, and subsequent separation of resulting peptides on a 10 μm ID (PS-DVB) porous layer open tubular (PLOT) column. The high resolution of the PLOT columns was maintained in the on-line system, resulting in narrow chromatographic peaks of 3-5 seconds. The trypsin reactors provided repeatable performance and were compatible with long-term storage.

Performance of dead Azolla filiculoides biomass in Biosorption of Au from wastewater.

PubMed

Umali, L J; Duncan, J R; Burgess, J E

2006-01-01

Dried milled biomass of Azolla filiculoides removed up to 98.2% of gold from wastewater from a gold plating factory containing 5 mg gold/l in solution in batch biosorption. The gold uptake capacity of the biomass was 98 mg/g. Whole dried biomass used in a continuous flow column removed up to 100% of gold from diluted wastewater. A similar column was linked to a sulphide precipitation process to provide a two-step system which was able to remove 98% of gold from undiluted wastewater containing 41 mg Au/l. The lifetime of the column was five days.

40 CFR 63.343 - Compliance provisions.

Code of Federal Regulations, 2013 CFR

2013-07-01

.... (1) Composite mesh-pad systems. (i) During the initial performance test, the owner or operator of an... limitations in § 63.342 through the use of a composite mesh-pad system shall determine the outlet chromium... performance test and accept ±2 inches of water column from this value as the compliant range. (ii) On and...

40 CFR 63.343 - Compliance provisions.

Code of Federal Regulations, 2014 CFR

2014-07-01

.... (1) Composite mesh-pad systems. (i) During the initial performance test, the owner or operator of an... limitations in § 63.342 through the use of a composite mesh-pad system shall determine the outlet chromium... performance test and accept ±2 inches of water column from this value as the compliant range. (ii) On and...

Effects of elevated temperature and mobile phase composition on a novel C18 silica column.

PubMed

Lippert, J Andreas; Johnson, Todd M; Lloyd, Jarem B; Smith, Jared P; Johnson, Bryce T; Furlow, Jason; Proctor, Angela; Marin, Stephanie J

2007-05-01

A novel polydentate C18 silica column was evaluated at an elevated temperature under acidic, basic, and neutral mobile phase conditions using ACN and methanol as the mobile phase organic modifier. The temperature range was 40-200 degrees C. The mobile phase compositions were from 0 to 80% organic-aqueous v/v and the mobile phase pH levels were between 2 and 12. The maximum operating temperature of the column was affected by the amount and type of organic modifier used in the mobile phase. Under neutral conditions, the column showed good column thermal stability at temperatures ranging between 120 and 200 degrees C in methanol-water and ACN-water solvent systems. At pH 2 and 3, the column performed well up to about 160 degrees C at two fixed ACN-buffer compositions. Under basic conditions at elevated temperatures, the column material deteriorated more quickly, but still remained stable up to 100 degrees C at pH 9 and 60 degrees C at pH 10. The results of this study indicate that this novel C18 silica-based column represents a significant advancement in RPLC column technology with enhanced thermal and pH stability when compared to traditional bonded phase silica columns.

Investigation of column flotation process on sulphide ore using 2-electrode capacitance sensor: The effect of air flow rate and solid percentage

NASA Astrophysics Data System (ADS)

Haryono, Didied; Harjanto, Sri; Wijaya, Rifky; Oediyani, Soesaptri; Nugraha, Harisma; Huda, Mahfudz Al; Taruno, Warsito Purwo

2018-04-01

Investigation of column flotation process on sulphide ore using 2-electrode capacitance sensor is presented in this paper. The effect of air flow rate and solid percentage on column flotation process has been experimentally investigated. The purpose of this paper is to understand the capacitance signal characteristic affected by the air flow rate and the solid percentage which can be used to determine the metallurgical performance. Experiments were performed using a laboratory column flotation cell which has a diameter of 5 cm and the total height of 140 cm. The sintered ceramic sparger and wash water were installed at the bottom and above of the column. Two-electrode concave type capacitance sensor was also installed at a distance of 50 cm from the sparger. The sensor was attached to the outer wall of the column, connected to data acquisition system, manufactured by CTECH Labs Edwar Technology and personal computer for further data processing. Feed consisting ZnS and SiO2 with the ratio of 3:2 was mixed with some reagents to make 1 litre of slurry. The slurry was fed into the aerated column at 100 cm above the sparger with a constant rate and the capacitance signals were captured during the process. In this paper, 7.5 and 10% of solid and 2-4 L/min of air flow rate with 0.5 L/min intervals were used as independent variables. The results show that the capacitance signal characteristics between the 7.5 and 10% of solid are different at any given air flow rate in which the 10% solid produced signals higher than those of 7.5%. Metallurgical performance and capacitance signal exhibit a good correlation.

Sustainable materials used as stone column filler: A short review

NASA Astrophysics Data System (ADS)

Zukri, Azhani; Nazir, Ramli

2018-04-01

Stone columns (also known as granular piles) are one of the methods for soft soil stabilization and typically used to increase bearing capacity and stability of slope.; Apart from decreasing the compressibility of loose and fine graded soils, it also accelerates the consolidation effect by improving the drainage path for pore water pressure dissipation and reduces the liquefaction potential of soils during earthquake event. Stone columns are probably the most “natural” ground treatment method or foundation system in existence to date. The benefit of stone columns is owing to the partial replacement of compressible soil by more competent materials such as stone aggregate, sand and other granular materials. These substitutes also act as reinforcement material, hence increasing overall strength and stiffness of the soft soil. Nowadays, a number of research has been conducted on the behaviour and performance of stone columns with various materials utilized as column filler replacing the normal aggregate. This paper will review extensively on previously conducted research on some of the materials used as stone column backfill materials, its suitability and the effectiveness as a substitute for regular aggregates in soft soil improvement works.

A composite reactor with wetted-wall column for mineral carbonation study in three-phase systems.

PubMed

Zhu, Chen; Yao, Xizhi; Zhao, Liang; Teng, H Henry

2016-11-01

Despite the availability of various reactors designed to study gas-liquid reactions, no appropriate devices are available to accurately investigate triple-phased mineral carbonation reactions involving CO 2 gas, aqueous solutions (containing divalent cations), and carbonate minerals. This report presents a composite reactor that combines a modified conventional wetted-wall column, a pH control module, and an attachment to monitor precipitation reactions. Our test and calibration experiments show that the absorption column behaved largely in agreement with theoretical predictions and previous observations. Experimental confirmation of CO 2 absorption in NaOH and ethanolamine supported the effectiveness of the column for gas-liquid interaction. A test run in the CO 2 -NH 3 -MgCl 2 system carried out for real time investigation of the relevant carbonation reactions shows that the reactor's performance closely followed the expected reaction path reflected in pH change, the occurrence of precipitation, and the rate of NH 3 addition, indicating the appropriateness of the composite device in studying triple-phase carbonation process.

Multi-Column Experimental Test Bed Using CaSDB MOF for Xe/Kr Separation

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

Welty, Amy Keil; Greenhalgh, Mitchell Randy; Garn, Troy Gerry

Processing of spent nuclear fuel produces off-gas from which several volatile radioactive components must be separated for further treatment or storage. As part of the Off-gas Sigma Team, parallel research at INL and PNNL has produced several promising sorbents for the selective capture of xenon and krypton from these off-gas streams. In order to design full-scale treatment systems, sorbents that are promising on a laboratory scale must be proven under process conditions to be considered for pilot and then full-scale use. To that end, a bench-scale multi-column system with capability to test multiple sorbents was designed and constructed at INL.more » This report details bench-scale testing of CaSDB MOF, produced at PNNL, and compares the results to those reported last year using INL engineered sorbents. Two multi-column tests were performed with the CaSDB MOF installed in the first column, followed with HZ-PAN installed in the second column. The CaSDB MOF column was placed in a Stirling cryocooler while the cryostat was employed for the HZ-PAN column. Test temperatures of 253 K and 191 K were selected for the first column while the second column was held at 191 K for both tests. Calibrated volume sample bombs were utilized for gas stream analyses. At the conclusion of each test, samples were collected from each column and analyzed for gas composition. While CaSDB MOF does appear to have good capacity for Xe, the short time to initial breakthrough would make design of a continuous adsorption/desorption cycle difficult, requiring either very large columns or a large number of smaller columns. Because of the tenacity with which Xe and Kr adhere to the material once adsorbed, this CaSDB MOF may be more suitable for use as a long-term storage solution. Further testing is recommended to determine if CaSDB MOF is suitable for this purpose.« less

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.

The use of One-Dimensional Laboratory Experiments to Assess Hydraulic Processes in Wastewater Soil Absorption Systems

NASA Astrophysics Data System (ADS)

Huntzinger, D. N.; McCray, J. E.; Siegrist, R.; Lowe, K.; VanCuyk, S.

2001-05-01

Sixteen, one-dimensional column lysimeters have been developed to evaluate the influence of loading regime and infiltrative surface character on hydraulic performance in wastewater soil absorption systems. A duplicate design was utilized to evaluate two infiltrative surface conditions (gravel-free vs. gravel-laden) under four hydraulic loading regimes representative of possible field conditions. By loading the columns at rates of 25 to 200 cm/day, the 17 weeks of column operation actually reflect up to approximately 13 yrs of field operation (at 5 cm/day). Therefore, the cumulative mass throughput and infiltrative rate loss for each loading regime can be examined to determine the viability of accelerated loading as a means to compress the time scale of observation, while still producing meaningfully results for the field scale. During operation, the columns were loaded with septic tank effluent at a prescribed rate and routinely monitoring for applied effluent composition, infiltration rate, time-dependant soil water content, water volume throughput, and percolate composition. Bromide tracer tests were completed prior to system startup and at weeks 2, 6, and 17 of system operation. Hydraulic characterization of the columns is based on measurements of the hydraulic loading rate, volumetric throughput, soil water content, and bromide breakthrough curves. Incipient ponding of wastewater developed during the 1st week of operation for columns loaded at the highest hydraulic rate (loading regimes 1 and 2), and during the 3rd and 6th week of operation for loading regimes 3 and 4, respectfully. The bromide breakthrough curves exhibit later breakthrough and tailing as system life increases, indicating the development of spatially variability in hydraulic conductivity within the column and the development of a clogging zone at the infiltrative surface. Throughput is assessed for each loading regime to determine the infiltration rate loss versus days of operation. Loading regimes 1 and 2 approach a comparable long-term throughput rate less than 20 cm/day, while loading regimes 3 and 4 reach a long-term throughput rate of less than 10 cm/day. These one-dimensional columns allow for the analysis of infiltrative rate loss and hydraulic behavior as a result of infiltrative surface character and loading regime.

Enhanced Removal of Nutrients and Trace Organics from Urban Runoff with Novel Capture, Treatment, and Recharge Systems

NASA Astrophysics Data System (ADS)

Ashoori, N.; Planes, M. T.; Lefevre, G.; Sedlak, D.; Luthy, R. G.

2017-12-01

Rapid population growth, urban sprawl and impact of climate change are forcing water-stressed areas to rely on new local sources of water supply. Under this scenario, reclamation of stormwater runoff has emerged as a source for irrigation and replenishing drinking-water groundwater reservoirs. However, urban stormwater can be a significant source of pollutants, including nutrients and organic compounds. In order to overcome the stormwater treatment system limitations, this project has developed a pilot-scale column system for passive treatment of infiltrated water using low-cost, low-energy geomedia. The objective was to provide guidance on the design and operation of systems for controlling nutrient and trace organic contaminant releases to surface waters. The work comprised of replicate column studies in the field to test stormwater treatment modules with various media, such as woodchips and biochar, using urban runoff from a watershed in Sonoma, California. Woodchip bioreactors host an endemic population of microorganisms that can be harnessed to biologically degrade nitrate. The columns amended with biochar enhance removal of organic pollutants present in stormwater through physicochemical processes (i.e., adsorption onto biochar) and biodegradation in the column through increasing retention time. The field columns were conditioned with stormwater for eight months before being spiked weekly with 50 ppb of representative trace organics. The key finding was the successful field demonstration of a novel treatment system for both the removal of nitrate and trace organics. Nitrogen removal was successful in all columns for the thirteen month experiment due to the woodchips being an effective source of carbon for denitrifying microorganisms to convert nitrate to nitrogen gases. As for the trace organics experiments, the results highlight an overall attenuation of the studied trace organic compounds by the columns containing woodchip and biochar throughout the five months of contaminant dosing. By developing a fundamental understanding of the mechanisms of contaminant removal in the laboratory and testing system performance at the test-bed scale, the project advances efforts to improve water quality and augment local water supplies through distributed capture, treatment, and recharge systems.

High growth potential and nitrogen removal performance of marine anammox bacteria in shrimp-aquaculture sediment.

PubMed

Van Duc, Luong; Song, Bongkeun; Ito, Hiroaki; Hama, Takehide; Otani, Masashi; Kawagoshi, Yasunori

2018-04-01

Anaerobic ammonium oxidation (anammox) bacteria were enriched in continuous packed-bed columns with marine sediment. One column (SB-C) was packed with only marine sediment collected from a shrimp-aquaculture pond, and another column (SB-AMX) was inoculated with marine anammox bacteria (MAB) as a control. These columns were continuously fed with natural or artificial seawater including ammonium (NH 4 + ) and nitrite (NO 2 - ). The SB-AMX showed anammox activities from the beginning and continued for over 200 days. However, the SB-C had no nitrogen removal performance for over 170 days. After adding a bicarbonate solution (KHCO 3 ) to the sediment-only packed column, anammox activity was observed within 13 days. The column exhibited a nitrogen removal efficiency (NRE) of 88% at a nitrogen loading rate (NLR) of 1.0 kg-N·m -3 ·day -1 , which was comparable to the control one. A next-generation sequencing analysis revealed the predominance of MAB related to "Candidatus Scalindua spp.". In addition, the co-occurrence of sulfur-oxidizing denitrifiers was observed, which suggests their symbiotic relationship. This study suggests the applicability of MAB for in-situ bioremediation of nitrogen-contaminated marine sediments and reveals a potential microbial interaction between anammox and sulfur-oxidizing communities responsible for nitrogen and sulfur cycling in marine aquaculture systems. Copyright © 2017 Elsevier Ltd. All rights reserved.

A hybrid monolithic column based on boronate-functionalized graphene oxide nanosheets for online specific enrichment of glycoproteins.

PubMed

Zhou, Chanyuan; Chen, Xiaoman; Du, Zhuo; Li, Gongke; Xiao, Xiaohua; Cai, Zongwei

2017-05-19

A hybrid monolithic column based on aminophenylboronic acid (APBA)-functionalized graphene oxide (GO) has been developed and used for selective enrichment of glycoproteins. The APBA/GO composites were homogeneously incorporated into a polymer monolithic column with the help of oligomer matrix and followed by in situ polymerization. The effect of dispersion of APBA/GO composites in the polymerization mixture on the performance of the monolithic column was explored in detail. The presence of graphene oxide not only enlarged the BET surface area from 6.3m 2 /g to 169.4m 2 /g, but also provided abundant boronic acid moieties for glycoprotein extraction, which improved the enrichment selectivity and efficiency for glycoproteins. The APBA/GO hybrid monolithic column was incorporated into a sequential injection system, which facilitated online extraction of proteins. Combining the superior properties of extraordinary surface area of GO and the affinity interaction of APBA to glycoproteins, the APBA/GO hybrid monolithic column showed higher enrichment factors for glycoproteins than other proteins without cis-diol-containing groups. Also, under comparable or even shorter processing time and without the addition of any organic solvent, it showed higher binding capacity toward glycoproteins compared with the conventional boronate affinity monolithic column. The practical applicability of this system was demonstrated by processing of egg white samples for extraction of ovalbumin and ovotransferrin, and satisfactory results were obtained by assay with SDS-PAGE. Copyright © 2017 Elsevier B.V. All rights reserved.

Effects of Cabin Upsets on Adsorption Columns for Air Revitalization

NASA Technical Reports Server (NTRS)

LeVan, M. Douglas

1999-01-01

The National Aeronautics and Space Administration (NASA) utilizes adsorption technology as part of contaminant removal systems designed for long term missions. A variety of trace contaminants can be effectively removed from gas streams by adsorption onto activated carbon. An activated carbon adsorption column meets NASA's requirements of a lightweight and efficient means of controlling trace contaminant levels aboard spacecraft and space stations. The activated carbon bed is part of the Trace Contaminant Control System (TCCS) which is utilized to purify the cabin atmosphere. TCCS designs oversize the adsorption columns to account for irregular fluctuations in cabin atmospheric conditions. Variations in the cabin atmosphere include changes in contaminant concentrations, temperature, and relative humidity. Excessively large deviations from typical conditions can result from unusual crew activity, equipment malfunctions, or even fires. The research carried out under this award focussed in detail on the effects of cabin upsets on the performance of activated carbon adsorption columns. Both experiments and modeling were performed with an emphasis on the roll of a change in relative humidity on adsorption of trace contaminants. A flow through fixed-bed apparatus was constructed at the NASA Ames Research Center, and experiments were performed there by W. Scot Appel under the direction of Dr. John E. Finn. Modeling work was performed at the University of Virginia and at Vanderbilt University by W. Scot Appel under the direction of M. Douglas LeVan. All three participants collaborated in all of the various phases of the research. The most comprehensive document describing the research is the Ph.D. dissertation of W. Scot Appel. Results have been published in several papers and presented in talks at technical conferences. All documents have been transmitted to Dr. John E. Finn.

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

Effect of n-octanol in the mobile phase on lipophilicity determination by reversed-phase high-performance liquid chromatography on a modified silica column.

PubMed

Benhaim, Deborah; Grushka, Eli

2008-10-31

In this study, we show that the addition of n-octanol to the mobile phase improves the chromatographic determination of lipophilicity parameters of xenobiotics (neutral solutes, acidic, neutral and basic drugs) on a Phenomenex Gemini C18 column. The Gemini C18 column is a new generation hybrid silica-based column with an extended pH range capability. The wide pH range (2-12) afforded the examination of basic drugs and acidic drugs in their neutral form. Extrapolated retention factor values, [Formula: see text] , obtained on the above column with the n-octanol-modified mobile phase were very well correlated (1:1 correlation) with literature values of logP (logarithm of the partition coefficient in n-octanol/water) of neutral compounds and neutral drugs (69). In addition, we found good linear correlations between measured [Formula: see text] values and calculated values of the logarithm of the distribution coefficient at pH 7.0 (logD(7.0)) for ionized acidic and basic drugs (r(2)=0.95). The Gemini C18 phase was characterized using the linear solvation energy relationship (LSER) model of Abraham. The LSER system constants for the column were compared to the LSER constants of n-octanol/water extraction system using the Tanaka radar plots. The comparison shows that the two methods are nearly equivalent.

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.

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.

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.

Investigation of Re-X glass ceramic for acceleration insulating columns

NASA Astrophysics Data System (ADS)

Faltens, A.; Rosenblum, S.

1985-05-01

In an induction linac the accelerating voltage appears along a voltage-graded vacuum insulator column which is a performance limiting and major cost component. Re-X glass ceramic insulators have the long-sought properties of allowing cast-in gradient electrodes, good breakdown characteristics, and compatibility with high vacuum systems. Re-X is a glass ceramic developed by General Electric for use in the manufacture of electrical apparatus, such as vacuum arc interrupters. We have examined vacuum outgassing behavior and voltage breakdown in vacuum and find excellent performance. The housings are in the shape of tubes with type 430 stainless steel terminations. Due to a matched coefficient of thermal expansion between metal and insulator, no vacuum leaks have resulted from any welding operation. The components should be relatively inexpensive to manufacture in large sizes and appear to be a very attractive accelerator column. We are planning to use a standard GE housing in our MBE-4 induction linac.

Hydrodynamic chromatography of polystyrene microparticles in micropillar array columns.

PubMed

Op de Beeck, Jeff; De Malsche, Wim; Vangelooven, Joris; Gardeniers, Han; Desmet, Gert

2010-09-24

We report on the possibility to perform HDC in micropillar array columns and the potential advantages of such a system. The HDC performance of a pillar array column with pillar diameter = 5 microm and an interpillar distance of 2.5 microm has been characterized using both a low MW tracer (FITC) and differently sized polystyrene bead samples (100, 200 and 500 nm). The reduced plate height curves that were obtained for the different investigated markers all overlapped very well, and attained a minimum value of about h(min)=0.3 (reduction based on the pillar diameter), corresponding to 1.6 microm in absolute value and giving good prospects for high efficiency separations. The obtained reduced retention time values were in fair agreement with that predicted by the Di Marzio and Guttman model for a flow between flat plates, using the minimal interpillar distance as characteristic interplate distance. Copyright 2010 Elsevier B.V. All rights reserved.

Ion exchange of several radionuclides on the hydrous crystalline silicotitanate, UOP IONSIV IE-911

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

Huckman, M.E.; Latheef, I.M.; Anthony, R.G.

1999-04-01

The crystalline silicotitanate, UOP IONSIV IE-911, is a proven material for removing radionuclides from a wide variety of waste streams. It is superior for removing several radionuclides from the highly alkaline solutions typical of DOE wastes. This laboratory previously developed an equilibrium model applicable to complex solutions for IE-910 (the power form of the granular IE-911), and more recently, the authors have developed several single component ion-exchange kinetic models for predicting column breakthrough curves and batch reactor concentration histories. In this paper, the authors model ion-exchange column performance using effective diffusivities determined from batch kinetic experiments. This technique is preferablemore » because the batch experiments are easier, faster, and cheaper to perform than column experiments. They also extend these ideas to multicomponent systems. Finally, they evaluate the ability of the equilibrium model to predict data for IE-911.« less

Quantification of cyclamate and cyclohexylamine in urine samples using high-performance liquid chromatography with trinitrobenzenesulfonic acid pre-column derivatization.

PubMed

Casals, I; Reixach, M; Amat, J; Fuentes, M; Serra-Majem, L

1996-10-25

An HPLC isocratic method with pre-column derivatization and UV detection for the quantification of cyclamate and cyclohexylamine in urine samples is described. The method requires very little sample preparation. Free cyclohexylamine is analysed in a first run and subsequently cyclamate is analysed as cyclohexylamine, after the simple process of oxidation of the sample by means of hydrogen peroxide. Cycloheptylamine is used as internal standard. Trinitrobenzenesulfonic acid (TNBS) appears to be a good reagent for the pre-column derivatization. The time per run is 15 min; the coefficients of variation of the assays range from 1.1 to 5.5%; the limits of detection are 0.09 and 0.11 ppm for cyclohexylamine and cyclamate anion, respectively. The system described has always performed efficiently, with a high degree of stability, in daily routine work.

LSST (Hoop/Column) Maypole Antenna Development Program, phase 1, part 1

NASA Technical Reports Server (NTRS)

Sullivan, M. R.

1982-01-01

The first of a two-phase program was performed to develop the technology necessary to evaluate, design, manufacture, package, transport and deploy the hoop/column deployable antenna reflector by means of a ground based program. The hoop/column concept consists of a cable stiffened large diameter hoop and central column structure that supports and contours a radio frequency reflective mesh surface. Mission scenarios for communications, radiometer and radio astronomy, were studied. The data to establish technology drivers that resulted in a specification of a point design was provided. The point design is a multiple beam quadaperture offset antenna system wich provides four separate offset areas of illumination on a 100 meter diameter symmetrical parent reflector. The periphery of the reflector is a hoop having 48 segments that articulate into a small stowed volume around a center extendable column. The hoop and column are structurally connected by graphite and quartz cables. The prominence of cables in the design resulted in the development of advanced cable technology. Design verification models were built of the hoop, column, and surface stowage subassemblies. Model designs were generated for a half scale sector of the surface and a 1/6 scale of the complete deployable reflector.

Analysis of Breakthrough Profiles Based on Gamma Ray Emission Along Loaded Packed Bed Columns: Comparative Evaluation of Ionsiv IE-911 and Chabazite Zeolite for the Removal of Radiostrontium and Cesium from Groundwater

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

Bostick, D.T.; DePaoli, S.M.; Lucero, A.J.

1999-10-18

A gamma counting system has been assembled that can profile the breakthrough fronts of gamma-emitting radioisotopes longitudinally and axially along a loaded column. This profiling technique has been particularly useful in columns studies such as those performed with IONSP IE-911, a crystalline silicotitanate (CST) manufactured by UOP, in which unusually long operating times are required to observe cesium breakthrough in column effluent. The length of the mass transfer zone and extent of column saturation can be detected early in a column study by viewing the relative emission of gamma emitters along I the length of the column. In this study,more » gamma scans were used to analyze loaded CST and zeolite columns used in the treatment of process wastewater simulant and actual groundwater. Results indicate good run-to-run reproductibility in acquiring the scans. The longitudinal gamma scans for both {sup 90}Sr and {sup 137}Cs conformed with breakthrough results reported on the basis of column effluent activity. Although not obvious from data obtained by monitoring effluent activity, the gamma scans indicated that both cesium and strontium in the saturated zone of the CST column are slowly displaced by the higher levels of groundwater cations and are then resorbed further down the column. This displacement phenomenon identified by gamma scans was verified using data from a zeolite column, in which both the gamma scan and column effluent data exhibited radionuclide displacement by groundwater cations. The gamma emission intensities from the CST column runs are used to quantitate and compare the distribution coefficient and loading capacity of {sup 137}Cs on CST versus zeolite.« less

Modeling of rotating disc contactor (RDC) column

NASA Astrophysics Data System (ADS)

Ismail, Wan Nurul Aiffah; Zakaria, Siti Aisyah; Noor, Nor Fashihah Mohd; Sulong, Ibrahim; Arshad, Khairil Anuar

2014-12-01

Liquid-liquid extraction is one of the most important separation processes. Different kinds of liquid-liquid extractor such as Rotating Disc Contactor (RDC) Column being used in industries. The study of liquid-liquid extraction in an RDC column has become a very important subject to be discussed not just among chemical engineers but mathematician as well. In this research, the modeling of small diameter RDC column using the chemical system involving cumene/isobutryric asid/water are analyzed by the method of Artificial Neural Network (ANN). In the previous research, we begin the process of analyzed the data using methods of design of the experiments (DOE) to identify which factor and their interaction factor are significant and to determine the percentage of contribution of the variance for each factor. From the result obtained, we continue the research by discussed the development and validation of an artificial neural network model in estimating the concentration of continuous and concentration of dispersed outlet for an RDC column. It is expected that an efficient and reliable model will be formed to predict RDC column performance as an alternative to speed up the simulation process.

Green Chromatographic Separation of Coumarin and Vanillins Using Subcritical Water as the Mobile Phase.

PubMed

Kayan, Berkant; Akay, Sema; Yang, Yu

2016-08-01

Pure water was used as the eluent for separation of coumarin, vanillin and ethyl vanillin at temperatures ranging from 100 to 200°C using a homemade subcritical water chromatography (SBWC) system. Chromatographic separations were performed on five commercial columns including XTerra MS C18, XBridge C18, Zorbax RRHD Eclipse Plus, Zorbax SB-Phenyl and Zorbax SB-C18 columns. The retention time of all three solutes decreased with increasing water temperature. The shortest retention time among all acceptable separations, less than 4 min, was achieved on the Zorbax SB-C18 column at 200°C. While separations on the XTerra MS C18 column resulted in fronting peaks and a degradation peak from ethyl vanillin on the Zorbax RRHD Eclipse Plus column was observed, all three other columns yielded reasonable separations under SBWC conditions. In addition to separation of the standard test mixture, separation of coumarin contained in a skincare cream sample was also carried out using SBWC. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Applying high-throughput methods to develop a purification process for a highly glycosylated protein.

PubMed

Sanaie, Nooshafarin; Cecchini, Douglas; Pieracci, John

2012-10-01

Micro-scale chromatography formats are becoming more routinely used in purification process development because of their ability to rapidly screen large number of process conditions at a time with minimal material. Given the usual constraints that exist on development timelines and resources, these systems can provide a means to maximize process knowledge and process robustness compared to traditional packed column formats. In this work, a high-throughput, 96-well filter plate format was used in the development of the cation exchange and hydrophobic interaction chromatography steps of a purification process designed to alter the glycoform distribution of a small protein. The significant input parameters affecting process performance were rapidly identified for both steps and preliminary operating conditions were identified. These ranges were verified in a packed chromatography column in order to assess the ability of the 96-well plate to predict packed column performance. In both steps, the 96-well plate format consistently led to underestimated glycoform-enrichment levels and to overestimated product recovery rates compared to the column-based approach. These studies demonstrate that the plate format can be used as a screening tool to narrow the operating ranges prior to further optimization on packed chromatography columns. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Anion-exchange high-performance liquid chromatography with post-column detection for the analysis of phytic acid and other inositol phosphates

NASA Technical Reports Server (NTRS)

Rounds, M. A.; Nielsen, S. S.; Mitchell, C. A. (Principal Investigator)

1993-01-01

The use of gradient anion-exchange HPLC, with a simple post-column detection system, is described for the separation of myo-inositol phosphates, including "phytic acid" (myo-inositol hexaphosphate). Hexa-, penta-, tetra-, tri- and diphosphate members of this homologous series are clearly resolved within 30 min. This method should facilitate analysis and quantitation of "phytic acid" and other inositol phosphates in plant, food, and soil samples.

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…

Two-Phase Flow in Packed Columns and Generation of Bubbly Suspensions for Chemical Processing in Space

NASA Technical Reports Server (NTRS)

Motil, Brian J.; Green, R. D.; Nahra, H. K.; Sridhar, K. R.

2000-01-01

For long-duration space missions, the life support and In-Situ Resource Utilization (ISRU) systems necessary to lower the mass and volume of consumables carried from Earth will require more sophisticated chemical processing technologies involving gas-liquid two-phase flows. This paper discusses some preliminary two-phase flow work in packed columns and generation of bubbly suspensions, two types of flow systems that can exist in a number of chemical processing devices. The experimental hardware for a co-current flow, packed column operated in two ground-based low gravity facilities (two-second drop tower and KC- 135 low-gravity aircraft) is described. The preliminary results of this experimental work are discussed. The flow regimes observed and the conditions under which these flow regimes occur are compared with the available co-current packed column experimental work performed in normal gravity. For bubbly suspensions, the experimental hardware for generation of uniformly sized bubbles in Couette flow in microgravity conditions is described. Experimental work was performed on a number of bubbler designs, and the capillary bubble tube was found to produce the most consistent size bubbles. Low air flow rates and low Couette flow produce consistent 2-3 mm bubbles, the size of interest for the "Behavior of Rapidly Sheared Bubbly Suspension" flight experiment. Finally the mass transfer implications of these two-phase flows is qualitatively discussed.

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.

Chromatographic column evaluation for the untargeted profiling of glucosinolates in cauliflower by means of ultra-high performance liquid chromatography coupled to high resolution mass spectrometry.

PubMed

Capriotti, Anna Laura; Cavaliere, Chiara; La Barbera, Giorgia; Montone, Carmela Maria; Piovesana, Susy; Zenezini Chiozzi, Riccardo; Laganà, Aldo

2018-03-01

The untargeted profiling is a promising approach for the characterization of secondary metabolites in biological matrices. Thanks to the recent rapid development of high-resolution mass spectrometry (HRMS) instrumentations, the number of applications by untargeted approaches for biological samples profiling has widely increased in the recent years. Despite the high potentialities of HRMS, however, a major issue in natural products analysis often arises in the upstream process of compounds separation. A separation technique is necessary to avoid phenomena such as signal suppression, and it is especially needed in the presence of isomeric metabolites, which are otherwise indistinguishable. Glucosinolates (GLSs), a group of secondary metabolites widely distributed among plants, resulted to be associated to the prevention of some serious diseases, such as cancer. This led to the development of several methods for the analysis of GLSs in vegetables tissues. The issue of GLSs chromatographic separation has been widely studied in the past because of the difficulty in the analysis of this highly polar and variable class of compounds. Several alternatives to reversed phase (RP) chromatography, sometimes not compatible with the coupling of liquid chromatography with mass spectrometry, have been tested for the analysis of intact GLSs. However, the availability of new stationary phases, in the last years, could allow the re-evaluation of RP chromatography for the analysis of intact GLSs. In this work, a thorough evaluation of four RP chromatographic columns for the analysis of GLSs in cauliflower (Brassica oleracea L. var. botrytis) extracts by an ultra-high performance liquid chromatographic system coupled via electrospray source to a hybrid quadrupole-Orbitrap mass spectrometer is presented. The columns tested were the following: one column Luna Omega polar C 18 , one column Kinetex Biphenyl, one column Kinetex core-shell XB-C 18 , two columns Kinetex core-shell XB-C 18 . After a previous optimization of the extraction method, cauliflower extracts were analyzed testing four different mobile phases onto the four columns for a total of sixteen different chromatographic conditions. The chromatographic systems were evaluated based on the number of detected and tentatively identified GLSs. Luna Polar stationary phase resulted to be the most suitable for the analysis of GLSs compared to Kinetex XB and Kinetex Biphenyl columns stationary phase. However, two in series Kinetex XB columns increased the number of tentatively identified GLSs compared to one Kinetex XB, showing the importance of column length in the analysis of complex mixtures. The data obtained with the best chromatographic system were deeply analyzed by MS/MS investigation for the final identification. Fiflty-one GLSs were tentatively identified, 24 of which have never been identified in cauliflower. Finally the linearity of the analytes response over the analyzed range of concentration was checked, suggesting that the developed method is suitable for both qualitative and quantitative analysis of GLSs in phytochemical mixtures. Copyright © 2017 Elsevier B.V. All rights reserved.

Evaluation of the phase ratio for three C18 high performance liquid chromatographic columns.

PubMed

Caiali, Edvin; David, Victor; Aboul-Enein, Hassan Y; Moldoveanu, Serban C

2016-02-26

For a chromatographic column, phase ratio Φ is defined as the ratio between the volume of the stationary phase Vst and the void volume of the column V0, and it is an important parameter characterizing the HPLC process. Although apparently simple, the evaluation of Φ presents difficulties because there is no sharp boundary between the mobile phase and the stationary phase. In addition, the boundary depends not only on the nature of the stationary phase, but also on the composition of the mobile phase. In spite of its importance, phase ratio is seldom reported for commercially available HPLC columns and the data typically provided by the vendors about the columns do not provide key information that would allow the calculation of Φ based on Vst and V0 values. A different procedure for the evaluation of Φ is based on the following formula: log k'j=a log Kow,j+log Φ, where k'j is the retention factor for a compound j that must be a hydrocarbon, Kow,j is the octanol/water partition coefficient, and a is a proportionality constant. Present study describes the experimental evaluation of Φ based on the measurement of k'j for the compounds in the homologous series between benzene and butylbenzene for three C18 columns: Gemini C18, Luna C18 both with 5 μm particles, and a Chromolith Performance RP-18. The evaluation was performed for two mobile phase systems at different proportions of methanol/water and acetonitrile/water. The octanol/water partition coefficients were obtained from the literature. The results obtained in the study provide further support for the new procedure for the evaluation of phase ratio. Copyright © 2016 Elsevier B.V. All rights reserved.

The Copernicus S5P Mission Performance Centre / Validation Data Analysis Facility for TROPOMI operational atmospheric data products

NASA Astrophysics Data System (ADS)

Compernolle, Steven; Lambert, Jean-Christopher; Langerock, Bavo; Granville, José; Hubert, Daan; Keppens, Arno; Rasson, Olivier; De Mazière, Martine; Fjæraa, Ann Mari; Niemeijer, Sander

2017-04-01

Sentinel-5 Precursor (S5P), to be launched in 2017 as the first atmospheric composition satellite of the Copernicus programme, carries as payload the TROPOspheric Monitoring Instrument (TROPOMI) developed by The Netherlands in close cooperation with ESA. Designed to measure Earth radiance and solar irradiance in the ultraviolet, visible and near infrared, TROPOMI will provide Copernicus with observational data on atmospheric composition at unprecedented geographical resolution. The S5P Mission Performance Center (MPC) provides an operational service-based solution for various QA/QC tasks, including the validation of S5P Level-2 data products and the support to algorithm evolution. Those two tasks are to be accomplished by the MPC Validation Data Analysis Facility (VDAF), one MPC component developed and operated at BIRA-IASB with support from S[&]T and NILU. The routine validation to be ensured by VDAF is complemented by a list of validation AO projects carried out by ESA's S5P Validation Team (S5PVT), with whom interaction is essential. Here we will introduce the general architecture of VDAF, its relation to the other MPC components, the generic and specific validation strategies applied for each of the official TROPOMI data products, and the expected output of the system. The S5P data products to be validated by VDAF are diverse: O3 (vertical profile, total column, tropospheric column), NO2 (total and tropospheric column), HCHO (tropospheric column), SO2 (column), CO (column), CH4 (column), aerosol layer height and clouds (fractional cover, cloud-top pressure and optical thickness). Starting from a generic validation protocol meeting community-agreed standards, a set of specific validation settings is associated with each data product, as well as the appropriate set of Fiducial Reference Measurements (FRM) to which it will be compared. VDAF collects FRMs from ESA's Validation Data Centre (EVDC) and from other sources (e.g., WMO's GAW, NDACC and TCCON). Data manipulations on satellite and FRM data (format conversion, filtering, co-location, regridding and vertical smoothing) are performed by the open source software HARP, while more specific manipulations apply in-house routines. The paper concludes with a short description of expected outputs of the system.

Evaluation of an International Pharmacopoeia method for the analysis of nelfinavir mesilate by liquid chromatography.

PubMed

Yekkala, Raja Satyanarayana; Vandenwayenberg, Stephanie; Hoogmartens, Jos; Adams, Erwin

2006-11-17

A gradient LC method for the determination of related substances in nelfinavir mesilate (NFVM) has been recently published in the International Pharmacopoeia. The method uses a base deactivated reversed phase C18 column (25 cm x 4.6 mm I.D.), 5 microm kept at a temperature of 35 degrees C. The mobile phases consist of acetonitrile, methanol, phosphate buffer pH 3.4 and water. The flow rate is 1.0 ml/min. UV detection is performed at 225 nm. A system suitability test (SST) is described to govern the quality of the separation. The separation towards NFVM components was investigated on 18 C18 columns and correlation was made with the column classification system developed in our laboratory. The method was evaluated using a Hypersil BDS C18 column (25 cm x 4.6 mm I.D.), 5 microm. A two level fractional factorial design was applied to examine the robustness of the method. The method shows good selectivity, precision, linearity and sensitivity. Seven commercial samples were examined using this method.

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.

Development of a 45kpsi ultrahigh pressure liquid chromatography instrument for gradient separations of peptides using long microcapillary columns and sub-2μm particles.

PubMed

Grinias, Kaitlin M; Godinho, Justin M; Franklin, Edward G; Stobaugh, Jordan T; Jorgenson, James W

2016-10-21

Commercial chromatographic instrumentation for bottom-up proteomics is often inadequate to resolve the number of peptides in many samples. This has inspired a number of complex approaches to increase peak capacity, including various multidimensional approaches, and reliance on advancements in mass spectrometry. One-dimensional reversed phase separations are limited by the pressure capabilities of commercial instruments and prevent the realization of greater separation power in terms of speed and resolution inherent to smaller sorbents and ultrahigh pressure liquid chromatography. Many applications with complex samples could benefit from the increased separation performance of long capillary columns packed with sub-2μm sorbents. Here, we introduce a system that operates at a constant pressure and is capable of separations at pressures up to 45kpsi. The system consists of a commercially available capillary liquid chromatography instrument, for sample management and gradient creation, and is modified with a storage loop and isolated pneumatic amplifier pump for elevated separation pressure. The system's performance is assessed with a complex peptide mixture and a range of microcapillary columns packed with sub-2μm C18 particles. Copyright © 2016 Elsevier B.V. All rights reserved.

Reliable prediction of heat transfer coefficient in three-phase bubble column reactor via adaptive neuro-fuzzy inference system and regularization network

NASA Astrophysics Data System (ADS)

Garmroodi Asil, A.; Nakhaei Pour, A.; Mirzaei, Sh.

2018-04-01

In the present article, generalization performances of regularization network (RN) and optimize adaptive neuro-fuzzy inference system (ANFIS) are compared with a conventional software for prediction of heat transfer coefficient (HTC) as a function of superficial gas velocity (5-25 cm/s) and solid fraction (0-40 wt%) at different axial and radial locations. The networks were trained by resorting several sets of experimental data collected from a specific system of air/hydrocarbon liquid phase/silica particle in a slurry bubble column reactor (SBCR). A special convection HTC measurement probe was manufactured and positioned in an axial distance of 40 and 130 cm above the sparger at center and near the wall of SBCR. The simulation results show that both in-house RN and optimized ANFIS due to powerful noise filtering capabilities provide superior performances compared to the conventional software of MATLAB ANFIS and ANN toolbox. For the case of 40 and 130 cm axial distance from center of sparger, at constant superficial gas velocity of 25 cm/s, adding 40 wt% silica particles to liquid phase leads to about 66% and 69% increasing in HTC respectively. The HTC in the column center for all the cases studied are about 9-14% larger than those near the wall region.

Alachlor transformation patterns in aquatic field mesocosms under variable oxygen and nutrient conditions

USGS Publications Warehouse

Graham, D.W.; Miley, M.K.; Denoyelles, F.; Smith, Val H.; Thurman, E.M.; Carter, R.

2000-01-01

Alachlor is one of the most commonly used herbicides in both Europe and North America. Because of its toxic properties, its fate and attenuation in natural waters is practically important. This paper assesses factors that affect alachlor decay rate in aquatic systems using field-scale experimental units. In particular, we used field mesocosms (11.3 m3 outdoor fiberglass tanks) to examine the affect of oxygen level and other factors on decay rate in water columns. This is one of the first studies ever performed where diverse water column conditions have been successfully simulated using common mesocosm-scale facilities. Four treatments were assessed, including aerobic systems (aerobic); low nutrient, oxygen-stratified systems (stratified-LN); moderate nutrient, oxygen-stratified systems (stratified-HN); and anaerobic systems (anaerobic). The lowest half-lives were observed in the anaerobic units (9.7 days) followed by the aerobic (21 days), stratified-HN (22 days), and stratified-LN (46 days) units. Our results indicate that alachlor is transformed most rapidly under anaerobic conditions, although the ambient phosphorus level also appears to influence decay rate. In this study, two common alachlor breakdown products, ethane sulfonic acid (ESA) and oxanilic acid, were also monitored. Oxanilic acid was produced in greater quantities than ESA under all treatments with the highest levels being produced in the stratified-HN units. In general, our results suggest that previous laboratory data, which indicated that high rates of alachlor decay can occur under oxygen-free methanogenic conditions, is translatable to field-scale applications. Copyright (C) 2000 Elsevier Science Ltd.Alachlor is one of the most commonly used herbicides in both Europe and North America. Because of its toxic properties, its fate and attenuation in natural waters is practically important. This paper assesses factors that affect alachlor decay rate in aquatic systems using field-scale experimental units. In particular, we used field mesocosms (11.3 m3 outdoor fiberglass tanks) to examine the affect of oxygen level and other factors on decay rate in water columns. This is one of the first studies ever performed where diverse water column conditions have been successfully simulated using common mesocosm-scale facilities. Four treatments were assessed, including aerobic systems (aerobic); low nutrient, oxygen-stratified systems (stratified-LN); moderate nutrient, oxygen-stratified systems (stratified-HN); and anaerobic systems (anaerobic). The lowest half-lives were observed in the anaerobic units (9.7 days) followed by the aerobic (21 days), stratified-HN (22 days), and stratified-LN (46 days) units. Our results indicate that alachlor is transformed most rapidly under anaerobic conditions, although the ambient phosphorus level also appears to influence decay rate. In this study, two common alachlor breakdown products, ethane sulfonic acid (ESA) and oxanilic acid, were also monitored. Oxanilic acid was produced in greater quantities than ESA under all treatments with the highest levels being produced in the stratified-HN units. In general, our results suggest that previous laboratory data, which indicated that high rates of alachlor decay can occur under oxygen-free methanogenic conditions, is translatable to field-scale applications.Aquatic field mesocosms were used to examine the influence of DO concentration and the presence of nutrients on alachlor transformation. Four treatments were used: wholly aerobic water columns, thermally and oxygen stratified water columns with low nutrient levels, stratified water columns with moderate nutrient levels, and wholly anaerobic water columns. The anaerobic treatment produced the highest rate of alachlor decay, followed by the aerobic and stratified treatments. The lowest decay rate occurred in the aerobic, low-nutrient stratified units.

Information or resolution: Which is required from an SEM to study bulk inorganic materials?: Evaluate SEMs’ practical performance

DOE PAGES

Xing, Q.

2016-07-11

Significant technological advances in scanning electron microscopy (SEM) have been achieved over the past years. Different SEMs can have significant differences in functionality and performance. This work presents the perspectives on selecting an SEM for research on bulk inorganic materials. Understanding materials demands quantitative composition and orientation information, and informative and interpretable images that reveal subtle differences in chemistry, orientation/structure, topography, and electronic structure. The capability to yield informative and interpretable images with high signal-to-noise ratios and spatial resolutions is an overall result of the SEM system as a whole, from the electron optical column to the detection system. Themore » electron optical column determines probe performance. The roles of the detection system are to capture, filter or discriminate, and convert signal electrons to imaging information. The capability to control practical operating parameters including electron probe size and current, acceleration voltage or landing voltage, working distance, detector selection, and signal filtration is inherently determined by the SEM itself. As a platform for various accessories, e.g. an energydispersive spectrometer and an electron backscatter diffraction detector, the properties of the electron optical column, specimen chamber, and stage greatly affect the performance of accessories. Ease-of-use and ease-of-maintenance are of practical importance. It is practically important to select appropriate test specimens, design suitable imaging conditions, and analyze the specimen chamber geometry and dimensions to assess the overall functionality and performance of an SEM. Finally, for an SEM that is controlled/operated with a computer, the stable software and user-friendly interface significantly affect the usability of the SEM.« less

Information or resolution: Which is required from an SEM to study bulk inorganic materials?: Evaluate SEMs’ practical performance

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

Xing, Q.

Significant technological advances in scanning electron microscopy (SEM) have been achieved over the past years. Different SEMs can have significant differences in functionality and performance. This work presents the perspectives on selecting an SEM for research on bulk inorganic materials. Understanding materials demands quantitative composition and orientation information, and informative and interpretable images that reveal subtle differences in chemistry, orientation/structure, topography, and electronic structure. The capability to yield informative and interpretable images with high signal-to-noise ratios and spatial resolutions is an overall result of the SEM system as a whole, from the electron optical column to the detection system. Themore » electron optical column determines probe performance. The roles of the detection system are to capture, filter or discriminate, and convert signal electrons to imaging information. The capability to control practical operating parameters including electron probe size and current, acceleration voltage or landing voltage, working distance, detector selection, and signal filtration is inherently determined by the SEM itself. As a platform for various accessories, e.g. an energydispersive spectrometer and an electron backscatter diffraction detector, the properties of the electron optical column, specimen chamber, and stage greatly affect the performance of accessories. Ease-of-use and ease-of-maintenance are of practical importance. It is practically important to select appropriate test specimens, design suitable imaging conditions, and analyze the specimen chamber geometry and dimensions to assess the overall functionality and performance of an SEM. Finally, for an SEM that is controlled/operated with a computer, the stable software and user-friendly interface significantly affect the usability of the SEM.« less

Effect of bioaugmentation and biostimulation on sulfate-reducing column startup captured by functional gene profiling.

PubMed

Pereyra, Luciana P; Hiibel, Sage R; Perrault, Elizabeth M; Reardon, Kenneth F; Pruden, Amy

2012-10-01

Sulfate-reducing permeable reactive zones (SR-PRZs) depend upon a complex microbial community to utilize a lignocellulosic substrate and produce sulfides, which remediate mine drainage by binding heavy metals. To gain insight into the impact of the microbial community composition on the startup time and pseudo-steady-state performance, functional genes corresponding to cellulose-degrading (CD), fermentative, sulfate-reducing, and methanogenic microorganisms were characterized in columns simulating SR-PRZs using quantitative polymerase chain reaction (qPCR) and denaturing gradient gel electrophoresis (DGGE). Duplicate columns were bioaugmented with sulfate-reducing or CD bacteria or biostimulated with ethanol or carboxymethyl cellulose and compared with baseline dairy manure inoculum and uninoculated controls. Sulfate removal began after ~ 15 days for all columns and pseudo-steady state was achieved by Day 30. Despite similar performance, DGGE profiles of 16S rRNA gene and functional genes at pseudo-steady state were distinct among the column treatments, suggesting the potential to control ultimate microbial community composition via bioaugmentation and biostimulation. qPCR revealed enrichment of functional genes in all columns between the initial and pseudo-steady-state time points. This is the first functional gene-based study of CD, fermentative and sulfate-reducing bacteria and methanogenic archaea in a lignocellulose-based environment and provides new qualitative and quantitative insight into startup of a complex microbial system. © 2012 Federation of European Microbiological Societies. Published by Blackwell Publishing Ltd. All rights reserved.

The separation of flavonoids from Pongamia pinnata using combination columns in high-speed counter-current chromatography with a three-phase solvent system.

PubMed

Yin, Hao; Zhang, Si; Long, Lijuan; Yin, Hang; Tian, Xinpeng; Luo, Xiongming; Nan, Haihan; He, Sha

2013-11-08

The mangrove plant Pongamia pinnata (Leguminosae) is well known as a plant pesticide. Previous studies have indicated that the flavonoids are responsible of the biological activities of the plant. A new high-speed counter-current chromatography (HSCCC) method for the separation of three flavonoids, karanjin (1), pinnatin (2), and pongaflavone (3), from P. pinnata was developed in the present study. The lower and intermediate phase (LP and IP) of a new three-phase solvent system, n-hexane-acetonitrile-dichloromethane-water, at a volume ratio of 5:5:1:5, were used as the stationary phases, while the upper phase (UP) was used as the mobile phase, and the volume ratio between the stationary phases in the CCC column could be tuned by varying the initial pumped volume ratio of the stationary phases. The CCC columns containing all three phases of the solvent system were considered combination columns. According to the theories of combination column, it is possible to optimize the retention time of the target compounds by varying the volume ratio of the stationary phases in the HSCCC combination columns, as well as the suitable volume ratios of the stationary phases for the separation of the target compounds were predicted from the partition coefficients of the compounds in the three-phase solvent system. Then, three HSCCC separations using the combination columns with initial pumped LP:IP volume ratios of 1:0, 0.9:0.1, and 0.7:0.3 were performed separately based on the prediction. Three target compounds were prepared with high purity when the initial pumped volume ratio of the stationary phases was 0.9:0.1. The baseline separation of compounds 2 and 3 was achieved on the combination column with an initial pumped volume ratio of 0.7:0.3. Furthermore, the three experiments clearly demonstrated that the retentions and resolutions of the target compounds increased with an increasing volume ratio of IP, which is consistent with the prediction for the retention times for the solutes on combination columns. The method proposed here reduces the need for solvent selection compared with the conventional method and may have broad potential applicability in the preparation of natural products. Copyright © 2013 Elsevier B.V. All rights reserved.

Field and Laboratory Application of a Gas Chromatograph Low Thermal Mass Resistively Heated Column System in Detecting Traditional and Non-Traditional Chemical Warfare Agents Using Solid Phase Micro-Extraction

DTIC Science & Technology

2005-02-01

followed by extensive sample preparation procedures that are performed in a laboratory. Analysis is typically conducted by injecting a liquid or gas sample...Alfentanil, Remifentanil , Sufentanil, and Carfentanil) in a laboratory. (5) Quantitatively determine a maximum temperature ramping rate at which the LTM...RHT Column combined with a GC-MS can separate and analyze a mixture of non- traditional CWAs (i.e. Fentanyl, Alfentanil, Remifentanil , Sufentanil

Substituted decision making: elder guardianship.

PubMed

Leatherman, Martha E; Goethe, Katherine E

2009-11-01

The goal of this column is to help experienced clinicians navigate the judicial system when they are confronted with requests for capacity evaluations that involve guardianship (conservatorship). The interface between the growing elderly medical population and increasing requests for substituted decision making is becoming more complex. This column will help practicing psychiatrists understand the medical, legal, and societal factors involved in adult guardianship. Such understanding is necessary in order to effectively perform guardianship evaluations and adequately inform courts, patients, and families about the psychiatric diagnoses central to substituted decision making.

A parallel-vector algorithm for rapid structural analysis on high-performance computers

NASA Technical Reports Server (NTRS)

Storaasli, Olaf O.; Nguyen, Duc T.; Agarwal, Tarun K.

1990-01-01

A fast, accurate Choleski method for the solution of symmetric systems of linear equations is presented. This direct method is based on a variable-band storage scheme and takes advantage of column heights to reduce the number of operations in the Choleski factorization. The method employs parallel computation in the outermost DO-loop and vector computation via the 'loop unrolling' technique in the innermost DO-loop. The method avoids computations with zeros outside the column heights, and as an option, zeros inside the band. The close relationship between Choleski and Gauss elimination methods is examined. The minor changes required to convert the Choleski code to a Gauss code to solve non-positive-definite symmetric systems of equations are identified. The results for two large-scale structural analyses performed on supercomputers, demonstrate the accuracy and speed of the method.

A parallel-vector algorithm for rapid structural analysis on high-performance computers

NASA Technical Reports Server (NTRS)

Storaasli, Olaf O.; Nguyen, Duc T.; Agarwal, Tarun K.

1990-01-01

A fast, accurate Choleski method for the solution of symmetric systems of linear equations is presented. This direct method is based on a variable-band storage scheme and takes advantage of column heights to reduce the number of operations in the Choleski factorization. The method employs parallel computation in the outermost DO-loop and vector computation via the loop unrolling technique in the innermost DO-loop. The method avoids computations with zeros outside the column heights, and as an option, zeros inside the band. The close relationship between Choleski and Gauss elimination methods is examined. The minor changes required to convert the Choleski code to a Gauss code to solve non-positive-definite symmetric systems of equations are identified. The results for two large scale structural analyses performed on supercomputers, demonstrate the accuracy and speed of the method.

Phototoxicity testing by online irradiation and HPLC.

PubMed

Schröder, Sven; Surmann, J P

2006-11-01

A high-performance liquid chromatography (HPLC) system was developed for the determination of drug photostability and phototoxicity based on an automated column-switching system with aqueous online UV-A irradiation and hyphenated organic separation of the drug and its photoproducts. The photoreactor is built with an poly(ethylene-co-tetrafluoroethylene) (ETFE) reaction coil knitted around a UV-A light source. The chromatographic separation was performed with two special C18 columns, which are also suitable for using with pure water as eluent. Degradation of chlorpromazine (CPZ) by ultraviolet light was investigated at pH 7 and pH 3. Furthermore chlorpromazine was irradiated in the presence of guanosine-5-monophosphate (GMP) in pH 7 buffered solution, leading to a new photoproduct. In the pH 3 irradiation studies of CPZ and GMP, no reaction was detected between the molecules.

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.

Sugar Determination in Foods with a Radially Compressed High Performance Liquid Chromatography Column.

ERIC Educational Resources Information Center

Ondrus, Martin G.; And Others

1983-01-01

Advocates use of Waters Associates Radial Compression Separation System for high performance liquid chromatography. Discusses instrumentation and reagents, outlining procedure for analyzing various foods and discussing typical student data. Points out potential problems due to impurities and pump seal life. Suggests use of ribose as internal…

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 parameters on the cyclic behavior of UHPCFFT columns. Strong correlations were noted between the initial stiffness and the stiffness index, and between the moment capacity and the reinforcement index. Finally, a thorough analytical study was carried out to investigate the seismic response of the proposed steel-free UHPCFFT columns, which showed their superior earthquake resistance, as compared to their RC counterparts.

A novel octadecylsilane functionalized graphene oxide/silica composite stationary phase for high performance liquid chromatography.

PubMed

Liang, Xiaojing; Wang, Shuai; Liu, Shujuan; Liu, Xia; Jiang, Shengxiang

2012-08-01

An octadecylsilane functionalized graphene oxide/silica stationary phase was fabricated by assembling graphene oxide onto the silica particles through an amide bond and subsequent immobilization of octadecylsilane. The chromatographic properties of the stationary phase were investigated by reversed-phase chromatography with alkylbenzenes, polycyclic aromatic hydrocarbons, amines, and phenolic compounds as the analytes. All the compounds achieved good separation on the column. The comparison between a C18 commercial column and the new stationary phase indicated that the existence of π-electron system of graphene oxide allows π-π interaction between analyte and octadecylsilane functionalized graphene oxide/silica stationary phase except for hydrophobic interaction, while only hydrophobic interaction presented between analyte and C18 commercial column. This suggests that some analytes can be better separated on the octadecylsilane functionalized graphene oxide/silica column. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Effects of expected-value information and display format on recognition of aircraft subsystem abnormalities

NASA Technical Reports Server (NTRS)

Palmer, Michael T.; Abbott, Kathy H.

1994-01-01

This study identifies improved methods to present system parameter information for detecting abnormal conditions and to identify system status. Two workstation experiments were conducted. The first experiment determined if including expected-value-range information in traditional parameter display formats affected subject performance. The second experiment determined if using a nontraditional parameter display format, which presented relative deviation from expected value, was better than traditional formats with expected-value ranges included. The inclusion of expected-value-range information onto traditional parameter formats was found to have essentially no effect. However, subjective results indicated support for including this information. The nontraditional column deviation parameter display format resulted in significantly fewer errors compared with traditional formats with expected-value-ranges included. In addition, error rates for the column deviation parameter display format remained stable as the scenario complexity increased, whereas error rates for the traditional parameter display formats with expected-value ranges increased. Subjective results also indicated that the subjects preferred this new format and thought that their performance was better with it. The column deviation parameter display format is recommended for display applications that require rapid recognition of out-of-tolerance conditions, especially for a large number of parameters.

Behaviour of fibre reinforced polymer confined reinforced concrete columns under fire condition

NASA Astrophysics Data System (ADS)

Chowdhury, Ershad Ullah

In recent years, fibre reinforced polymer (FRP) materials have demonstrated enormous potential as materials for repairing and retrofitting concrete bridges that have deteriorated from factors such as electro-chemical corrosion and increased load requirements. However, concerns associated with fire remain an obstacle to applications of FRP materials in buildings and parking garages due to FRP's sensitivity to high temperatures as compared with other structural materials and to limited knowledge on their thermal and mechanical behaviour in fire. This thesis presents results from an ongoing study on the fire performance of FRP materials, fire insulation materials and systems, and FRP wrapped reinforced concrete columns. The overall goal of the study is to understand the fire behaviour of FRP materials and FRP strengthened concrete columns and ultimately, provide rational fire safety design recommendations and guidelines for FRP strengthened concrete columns. A combined experimental and numerical investigation was conducted to achieve the goals of this research study. The experimental work consisted of both small-scale FRP material testing at elevated temperatures and full-scale fire tests on FRP strengthened columns. A numerical model was developed to simulate the behaviour of unwrapped reinforced concrete and FRP strengthened reinforced concrete square or rectangular columns in fire. After validating the numerical model against test data available in literature, it was determined that the numerical model can be used to analyze the behaviour of concrete axial compressive members in fire. Results from this study also demonstrated that although FRP materials experience considerable loss of their mechanical and bond properties at temperatures somewhat below the glass transition temperature of the resin matrix, externally-bonded FRP can be used in strengthening concrete structural members in buildings, if appropriate supplemental fire protection system is provided over the FRP strengthening system.

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.

Perfluorinated acids as ion-pairing agents in the determination of monoamine transmitters and some prominent metabolites in rat brain by high-performance liquid chromatography with amperometric detection.

PubMed

Patthy, M; Gyenge, R

1988-09-30

The behaviour of trifluoroacetate and heptafluorobutyrate as pairing ions for the reversed-phase ion-pair separation of monoamine transmitters and related metabolites was studied. The performance of systems with the perfluorinated acids was compared with that of systems containing sodium octyl sulphonate and was found to be better in terms of peak resolution combined with total analysis time, day-to-day reproducibility and the time required for attaining initial chromatographic equilibrium. Rat brain samples were deproteinized in the acidified mobile phase, injected directly on to a high-performance liquid chromatographic column and quantitated using an amperometric detector. Sample run times were 6-8 min, at a relatively low flow-rate. The detection limits achieved are fairly uncommon with conventional bore columns. The two perfluorinated acids studied differ in the dominant mechanisms of ion-pair formation and show selectivity differences as a result.

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.

Sol-gel open tubular ODS columns with reversed electroosmotic flow for capillary electrochromatography.

PubMed

Hayes, J D; Malik, A

2001-03-01

Sol-gel chemistry was successfully used for the fabrication of open tubular columns with surface-bonded octadecylsilane (ODS) stationary-phase coating for capillary electrochromatography (OT-CEC). Following column preparations, a series of experiments were performed to investigate the performance of the sol-gel coated ODS columns in OT-CEC. The incorporation of N-octadecyldimethyl[3-(trimethoxysilyl)propyl]ammonium chloride as one of the sol-gel precursors played an important role in the electrochromatographic performance of the prepared columns. This chemical reagent possesses a chromatographically favorable, bonded ODS moiety, in conjunction with three methoxy groups allowing for sol-gel reactivity. In addition, a positively charged nitrogen atom is present in the molecular structure of this reagent and provides a positively charged capillary surface responsible for the reversed electroosmotic flow (EOF) in the columns during CEC operation. Comparative studies involving the EOF within such sol-gel ODS coated and uncoated capillaries were performed using acetonitrile and methanol as the organic modifiers in the mobile phase. The use of a deactivating reagent, phenyldimethylsilane, in the sol-gel solution was evaluated. Efficiency values of over 400,000 theoretical plates per meter were achieved in CEC on a 64 cm x 25 microm i.d. sol-gel ODS open tubular column. Test mixtures of polycyclic aromatic hydrocarbons, benzene derivatives, and aromatic aldehydes and ketones were used to evaluate the CEC performances of both nondeactivated and deactivated open tubular sol-gel columns. The effects of mobile-phase organic modifier contents and pH on EOF in such columns were evaluated. The prepared sol-gel ODS columns are characterized by switchable electroosmotic flow. A pH value of approximately 8.5 was found correspond to the isoelectric point for the prepared sol-gel ODS coatings.

Effects of a malfunctional column on conventional and FeedCol-simulated moving bed chromatography performance.

PubMed

Song, Ji-Yeon; Oh, Donghoon; Lee, Chang-Ha

2015-07-17

The effects of a malfunctional column on the performance of a simulated moving bed (SMB) process were studied experimentally and theoretically. The experimental results of conventional four-zone SMB (2-2-2-2 configuration) and FeedCol operation (2-2-2-2 configuration with one feed column) with one malfunctional column were compared with simulation results of the corresponding SMB processes with a normal column configuration. The malfunctional column in SMB processes significantly deteriorated raffinate purity. However, the extract purity was equivalent or slightly improved compared with the corresponding normal SMB operation because the complete separation zone of the malfunctional column moved to a lower flow rate range in zones II and III. With the malfunctional column configuration, FeedCol operation gave better experimental performance (up to 7%) than conventional SMB operation because controlling product purity with FeedCol operation was more flexible through the use of two additional operating variables, injection time and injection length. Thus, compared with conventional SMB separation, extract with equivalent or slightly better purity could be produced from FeedCol operation even with a malfunctional column, while minimizing the decrease in raffinate purity (less than 2%). Copyright © 2015 Elsevier B.V. All rights reserved.

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 efficiency model is then built to predict the actual performance of real TCRSPs. The experimental and calculated resolution data are found in very good agreement for a change, Δv m =-10cm 3 /mol, of the partial molar volume of the two PAH isomers upon transfer from the acetonitrile-water eluent mixture to the silica-C 18 stationary phase. Copyright © 2017 Elsevier B.V. All rights reserved.

Effects of Irregular Bridge Columns and Feasibility of Seismic Regularity

NASA Astrophysics Data System (ADS)

Thomas, Abey E.

2018-05-01

Bridges with unequal column height is one of the main irregularities in bridge design particularly while negotiating steep valleys, making the bridges vulnerable to seismic action. The desirable behaviour of bridge columns towards seismic loading is that, they should perform in a regular fashion, i.e. the capacity of each column should be utilized evenly. But, this type of behaviour is often missing when the column heights are unequal along the length of the bridge, allowing short columns to bear the maximum lateral load. In the present study, the effects of unequal column height on the global seismic performance of bridges are studied using pushover analysis. Codes such as CalTrans (Engineering service center, earthquake engineering branch, 2013) and EC-8 (EN 1998-2: design of structures for earthquake resistance. Part 2: bridges, European Committee for Standardization, Brussels, 2005) suggests seismic regularity criterion for achieving regular seismic performance level at all the bridge columns. The feasibility of adopting these seismic regularity criterions along with those mentioned in literatures will be assessed for bridges designed as per the Indian Standards in the present study.

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.

MODELING CST ION EXCHANGE FOR CESIUM REMOVAL FROM SCIX BATCHES 1 - 4

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

Smith, F.

2011-04-25

The objective of this work is, through modeling, to predict the performance of Crystalline Silicotitinate (CST) for the removal of cesium from Small Column Ion Exchange (SCIX) Batches 1-4 (as proposed in Revision 16 of the Liquid Waste System Plan). The scope of this task is specified in Technical Task Request (TTR) 'SCIX Feed Modeling', HLE-TTR-2011-003, which specified using the Zheng, Anthony, Miller (ZAM) code to predict CST isotherms for six given SCIX feed compositions and the VErsatile Reaction and SEparation simulator for Liquid Chromatography (VERSE-LC) code to predict ion-exchange column behavior. The six SCIX feed compositions provided in themore » TTR represent SCIX Batches 1-4 and Batches 1 and 2 without caustic addition. The study also investigated the sensitivity in column performance to: (1) Flow rates of 5, 10, and 20 gpm with 10 gpm as the nominal flow; and (2) Temperatures of 25, 35, and 45 C with 35 C as the nominal temperature. The isotherms and column predictions presented in this report reflect the expected performance of engineered CST IE-911. This form of CST was used in experiments conducted at the Savannah River National Laboratory (SRNL) that formed the basis for estimating model parameters (Hamm et al., 2002). As has been done previously, the engineered resin capacity is estimated to be 68% of the capacity of particulate CST without binder.« less

Information or resolution: Which is required from an SEM to study bulk inorganic materials?

PubMed

Xing, Q

2016-11-01

Significant technological advances in scanning electron microscopy (SEM) have been achieved over the past years. Different SEMs can have significant differences in functionality and performance. This work presents the perspectives on selecting an SEM for research on bulk inorganic materials. Understanding materials demands quantitative composition and orientation information, and informative and interpretable images that reveal subtle differences in chemistry, orientation/structure, topography, and electronic structure. The capability to yield informative and interpretable images with high signal-to-noise ratios and spatial resolutions is an overall result of the SEM system as a whole, from the electron optical column to the detection system. The electron optical column determines probe performance. The roles of the detection system are to capture, filter or discriminate, and convert signal electrons to imaging information. The capability to control practical operating parameters including electron probe size and current, acceleration voltage or landing voltage, working distance, detector selection, and signal filtration is inherently determined by the SEM itself. As a platform for various accessories, e.g. an energy-dispersive spectrometer and an electron backscatter diffraction detector, the properties of the electron optical column, specimen chamber, and stage greatly affect the performance of accessories. Ease-of-use and ease-of-maintenance are of practical importance. It is practically important to select appropriate test specimens, design suitable imaging conditions, and analyze the specimen chamber geometry and dimensions to assess the overall functionality and performance of an SEM. For an SEM that is controlled/operated with a computer, the stable software and user-friendly interface significantly improve the usability of the SEM. SCANNING 38:864-879, 2016. © 2016 Wiley Periodicals, Inc. © Wiley Periodicals, Inc.

Excitatory signal flow and connectivity in a cortical column: focus on barrel cortex.

PubMed

Lübke, Joachim; Feldmeyer, Dirk

2007-07-01

A basic feature of the neocortex is its organization in functional, vertically oriented columns, recurring modules of signal processing and a system of transcolumnar long-range horizontal connections. These columns, together with their network of neurons, present in all sensory cortices, are the cellular substrate for sensory perception in the brain. Cortical columns contain thousands of neurons and span all cortical layers. They receive input from other cortical areas and subcortical brain regions and in turn their neurons provide output to various areas of the brain. The modular concept presumes that the neuronal network in a cortical column performs basic signal transformations, which are then integrated with the activity in other networks and more extended brain areas. To understand how sensory signals from the periphery are transformed into electrical activity in the neocortex it is essential to elucidate the spatial-temporal dynamics of cortical signal processing and the underlying neuronal 'microcircuits'. In the last decade the 'barrel' field in the rodent somatosensory cortex, which processes sensory information arriving from the mysticial vibrissae, has become a quite attractive model system because here the columnar structure is clearly visible. In the neocortex and in particular the barrel cortex, numerous neuronal connections within or between cortical layers have been studied both at the functional and structural level. Besides similarities, clear differences with respect to both physiology and morphology of synaptic transmission and connectivity were found. It is therefore necessary to investigate each neuronal connection individually, in order to develop a realistic model of neuronal connectivity and organization of a cortical column. This review attempts to summarize recent advances in the study of individual microcircuits and their functional relevance within the framework of a cortical column, with emphasis on excitatory signal flow.

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. The test results showed the effectiveness of the advanced materials in reducing damage and permanent displacements. The damage was minimal in plastic hinges with SMA/ECC and those with built-in elastomeric pads. Conventional RC plastic hinges were severely damaged due to spalling of concrete and rupture of the longitudinal and transverse reinforcement. Extensive post-test analytical studies were conducted and it was determined that a computational model of the bridge that included bridge-abutment interaction using OpenSees was able to provide satisfactory estimations of key structural parameters such as superstructure displacements and base shears. The analytical model was also used to conduct parametric studies on single-column and bridge-system response under near-fault ground motions. The effects of vertical excitations and transverse shear-keys at the bridge abutments on the superstructure displacement and column drifts were also explored.

Biological nitrogen removal using soil columns for the reuse of reclaimed water: Performance and microbial community analysis.

PubMed

Sun, Jiaji; Chen, Lei; Rene, Eldon R; Hu, Qian; Ma, Weifang; Shen, Zhenyao

2018-07-01

The main aim of this study was to remove nitrogen compounds from reclaimed water and reuse the water in semi-arid riverine lake systems. In order to assess the nitrogen removal efficiencies in different natural environments, laboratory scale column experiments were performed using sterilized soil (SS), silty clay (SC), soil with submerged plant (SSP) and biochar amendment soil (BCS). The initial concentration of NO 3 - -N and the flow rate was maintained constant at 15 mg L -1 and 0.6 ± 0.1 m d -1 , respectively. Among the tested columns, both SSP and BCS were able to achieve NO 3 - -N levels <0.2 mg L -1 in the treated reclaimed water. The results from bacterial community structure analysis, using 454 pyrosequencing of 16s rRNA genes, showed that the dominant denitrifier was Bacillus at the genera level. Copyright © 2018 Elsevier Ltd. All rights reserved.

Experimental study on beam for composite CES structural system

NASA Astrophysics Data System (ADS)

Matsui, Tomoya

2017-10-01

Development study on Concrete Encase Steel (CES) composite structure system has been continuously conducted toward the practical use. CES structure is composed of steel and fiber reinforced concrete. In previous study, it was found that CES structure has good seismic performance from experimental study of columns, beam - column joints, shear walls and a two story two span frame. However, as fundamental study on CES beam could be lacking, it is necessary to understand the structural performance of CES beam. In this study, static loading tests of CES beams were conducted with experimental valuable of steel size, the presence or absence of slab and thickness of slab. And restoring characteristics, failure behavior, deformation behavior, and strength evaluation method of CES beam were investigated. As the results, it was found that CES beam showed stable hysteresis behavior. Furthermore it was found that the flexural strength of the CES beam could be evaluated by superposition strength theory.

Performance of the fixed-bed of granular activated carbon for the removal of pesticides from water supply.

PubMed

Alves, Alcione Aparecida de Almeida; Ruiz, Giselle Louise de Oliveira; Nonato, Thyara Campos Martins; Müller, Laura Cecilia; Sens, Maurício Luiz

2018-02-26

The application of a fixed bed adsorption column of granular activated carbon (FBAC-GAC), in the removal of carbaryl, methomyl and carbofuran at a concentration of 25 μg L -1 for each carbamate, from the public water supply was investigated. For the determination of the presence of pesticides in the water supply, the analytical technique of high-performance liquid chromatography with post-column derivatization was used. Under conditions of constant diffusivity, the FBAC-GAC was saturated after 196 h of operation on a pilot scale. The exhaust rate of the granular activated carbon (GAC) in the FBAC-GAC until the point of saturation was 0.02 kg GAC m -3 of treated water. By comparing a rapid small-scale column test and FBAC-GAC, it was confirmed that the predominant intraparticle diffusivity in the adsorption column was constant diffusivity. Based on the results obtained on a pilot scale, it was possible to estimate the values to be applied in the FBAC-GAC (full scale) to remove the pesticides, which are particle size with an average diameter of 1.5 mm GAC; relationship between the internal diameter of the column and the average diameter of GAC ≥50 in order to avoid preferential flow near the adsorption column wall; surface application rate 240 m 3  m -2  d -1 and an empty bed contact time of 3 min. BV: bed volume; CD: constant diffusivity; EBCT: empty bed contact time; FBAC-GAC: fixed bed adsorption column of granular activated carbon; GAC: granular activated carbon; MPV: maximum permitted values; NOM: natural organic matter; PD: proportional diffusivity; pH PCZ : pH of the zero charge point; SAR: surface application rate; RSSCT: rapid small-scale column test; WTCS: water treated conventional system.

Design of a coil satellite centrifuge and its performance on counter-current chromatographic separation of 4-methylumbelliferyl sugar derivatives with polar organic-aqueous two-phase solvent systems.

PubMed

Shinomiya, Kazufusa; Tokura, Koji; Kimura, Emiru; Takai, Midori; Harikai, Naoki; Yoshida, Kazunori; Yanagidaira, Kazuhiro; Ito, Yoichiro

2015-05-01

A new high-speed counter-current chromatograph, named coil satellite centrifuge (CSC), was designed and fabricated in our laboratory. The CSC apparatus produces the satellite motion such that the coiled column simultaneously rotates around the sun axis (the angular velocity, ω1), the planet axis (ω2) and the satellite axis (the central axis of the column) (ω3). In order to achieve this triplicate rotary motion without twisting of the flow tube, the rotation of each axis was determined by the following formula: ω1=ω2+ω3. This relation enabled to lay out the flow tube without twisting by the simultaneous rotation of three axes. The flow tube was introduced from the bottom side of the apparatus into the sun axis of the first rotary frame reaching the upper side of the planet axis and connected to the column in the satellite axis. The performance of the apparatus was examined on separation of 4-methylumbelliferyl (MU) sugar derivatives as test samples with organic-aqueous two-phase solvent systems composed of ethyl acetate/1-butanol/water (3:2:5, v/v) for lower phase mobile and (1:4:5, v/v) for upper phase mobile. With lower phase mobile, five 4-MU sugar derivatives including β-D-cellobioside (Cel), β-D-glucopyranoside, α-D-mannopyranoside, β-D-fucopyranoside and α-L-fucopyranoside (α-L-Fuc) were separated with the combined rotation around each axis at counterclockwise (CCW) (ω1) - CCW (ω2) - CCW (ω3) by the flow tube distribution. With upper phase mobile, three 4-MU sugar derivatives including α-L-Fuc, β-D-galactopyranoside and Cel were separated with the combined rotation around each axis at clockwise (CW) (ω1) - CW (ω2) - CW (ω3) by the flow tube distribution. A series of experiments on peak resolution and stationary phase retention revealed that better partition efficiencies were obtained at the flow rate of 0.5 mL/min (column 1) and 0.8 mL/min (column 2) for lower phase mobile and 0.2 mL/min (column 1) and 0.4 mL/min (column 2) for upper phase mobile when using the left-handed multilayer coil (total capacity: 57.0 mL for column 1 and 75.0 mL for column 2) under the rotation speeds of approximately ω1=300 rpm, ω2=150 rpm and ω3=150 rpm. Copyright © 2015 Elsevier B.V. All rights reserved.

Systematic evaluation of commercially available ultra-high performance liquid chromatography columns for drug metabolite profiling: optimization of chromatographic peak capacity.

PubMed

Dubbelman, Anne-Charlotte; Cuyckens, Filip; Dillen, Lieve; Gross, Gerhard; Hankemeier, Thomas; Vreeken, Rob J

2014-12-29

The present study investigated the practical use of modern ultra-high performance liquid chromatography (UHPLC) separation techniques for drug metabolite profiling, aiming to develop a widely applicable, high-throughput, easy-to-use chromatographic method, with a high chromatographic resolution to accommodate simultaneous qualitative and quantitative analysis of small-molecule drugs and metabolites in biological matrices. To this end, first the UHPLC system volume and variance were evaluated. Then, a mixture of 17 drugs and various metabolites (molecular mass of 151-749Da, logP of -1.04 to 6.7), was injected on six sub-2μm particle columns. Five newest generation core shell technology columns were compared and tested against one column packed with porous particles. Two aqueous (pH 2.7 and 6.8) and two organic mobile phases were evaluated, first with the same flow and temperature and subsequently at each column's individual limit of temperature and pressure. The results demonstrated that pre-column dead volume had negligible influence on the peak capacity and shape. In contrast, a decrease in post-column volume of 57% resulted in a substantial (47%) increase in median peak capacity and significantly improved peak shape. When the various combinations of stationary and mobile phases were used at the same flow rate (0.5mL/min) and temperature (45°C), limited differences were observed between the median peak capacities, with a maximum of 26%. At higher flow though (up to 0.9mL/min), a maximum difference of almost 40% in median peak capacity was found between columns. The finally selected combination of solid-core particle column and mobile phase composition was chosen for its selectivity, peak capacity, wide applicability and peak shape. The developed method was applied to rat hepatocyte samples incubated with the drug buspirone and demonstrated to provide a similar chromatographic resolution, but a 6 times higher signal-to-noise ratio than a more traditional UHPLC metabolite profiling method using a fully porous particle packed column, within one third of the analysis time. In conclusion, a widely applicable, selective and fast chromatographic method was developed that can be applied to perform drug metabolite profiling in the timeframe of a quantitative analysis. It is envisioned that this method will in future be used for simultaneous qualitative and quantitative analysis and can therefore be considered a first important step in the Quan/Qual workflow. Copyright © 2014 Elsevier B.V. All rights reserved.

Field modeling and ray-tracing of a miniature scanning electron microscope beam column.

PubMed

Loyd, Jody S; Gregory, Don A; Gaskin, Jessica A

2017-08-01

A miniature scanning electron microscope (SEM) focusing column design is introduced and its potential performance assessed through an estimation of parameters that affect the probe radius, to include source size, spherical and chromatic aberration, diffraction and space charge broadening. The focusing column, a critical component of any SEM capable of operating on the lunar surface, was developed by the NASA Marshall Space Flight Center and Advanced Research Systems. The ray-trace analysis presented uses a model of the electrostatic field (within the focusing column) that is first calculated using the boundary element method (BEM). This method provides flexibility in modeling the complex electrode shapes of practical electron lens systems. A Fourier series solution of the lens field is then derived within a cylindrical domain whose boundary potential is provided by the BEM. Used in this way, the Fourier series solution is an accuracy enhancement to the BEM solution, allowing sufficient precision to assess geometric aberrations through direct ray-tracing. Two modes of operation with distinct lens field solutions are described. © The Author 2017. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

Efficient control system for low-concentration inorganic gases from a process vent stream: application of surfactants in spray and packed columns.

PubMed

Chein, Hungmin; Aggarwal, Shankar G; Wu, Hsin-Hsien

2004-11-01

Control of low-concentration pollutants from a semiconductor process vent stream using a wet-scrubbing technique is a challenging task to meet Taiwan environmental emission standards. An efficient wet-scrubber is designed on a pilot scale and tested to control low concentration acid and base waste-gas emission. The scrubber system consisted of two columns, i.e., a fine spray column [cutoff diameter (based on volume), Dv(50) = 15.63 microm; Sauter mean diameter (SMD) = 7.62 microm], which is especially efficient for NH3 removal as the pH of the spraying liquid is approximately 7 followed by a packed column with a scrubbing liquid pH approximately 9.0 mainly for acids removal. It is observed that use of the surfactants in low concentration about 10(-4) M and 10(-7) M in the spray liquid and in the scrubbing liquid, respectively, remarkably enhances the removal efficiency of the system. A traditional packed column (without the spray column and the surfactant) showed that the removal efficiencies of NH3, HF, and HCl for the inlet concentration range 0.2 to 3 ppm were (n = 5) 22.6+/-3.4%, 43.4+/-5.5%, and 40.4+/-7.4%, respectively. The overall efficiencies of the proposed system (the spray column and the packed column) in the presence of the surfactant in the spray liquid and in the scrubbing liquid forthese three species were found to increase significantly (n = 5) from 60.3+/-3.6 to 82.8+/-6.8%, 59.1+/-2.7 to 83.4+/-4.2%, and 56.2+/-7.3 to 81.0+/-6.7%, respectively. In this work, development of charge on the gas-liquid interface due to the surfactants has been measured and discussed. It is concluded that the presence of charge on the gas-liquid interface is the responsible factor for enhancement of the removal efficiency (mass-transfer in liquid phase). The effects of the type of surfactants, their chain length, concentration in liquid, etc. on the removal efficiency are discussed. Since the pilot tests were performed under the operating conditions similar to most of the wet-scrubbers operated in semiconductors manufacturing facilities for inorganic pollutants, this study can be applied to modify the existing wet-scrubbers to enhance the removal efficiencies, especially for low-concentration pollutants.

[Determination of arbutin in apple juice concentrate by ultra performance liquid chromatography with electrospray ionization tandem mass spectrometry].

PubMed

Kong, Xianghong; He, Qiang; Yue, Aishan; Wu, Shuangmin; Li, Jianhua

2010-06-01

An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/ MS) method was developed for the determination of arbutin in apple juice concentrate. Samples were diluted with water, then cleaned-up with a PS-DVB column. Quantitation was carried out using an external standard method. UPLC was performed on an Eclipse Plus C, column (100 mm x 2.1 mm, 1.8 microm) using a gradient solvent system (methanol-water). MS/MS was performed with multiple reaction monitoring (MRM) mode. The detection limit of arbutin was 0.02 mg/L. The method showed good linear relationship at the range of 0.04-2.0 mg/L. The recoveries ranged from 75.2% to 102.7% with relative standard deviations (RSDs) less than 8.9%. The method is simple, fast and sensitive. It's suitable for quantitative and qualitative analysis of arbutin in apple juice concentrate.

An approach to enhance pnetCDF performance in ...

EPA Pesticide Factsheets

Data intensive simulations are often limited by their I/O (input/output) performance, and "novel" techniques need to be developed in order to overcome this limitation. The software package pnetCDF (parallel network Common Data Form), which works with parallel file systems, was developed to address this issue by providing parallel I/O capability. This study examines the performance of an application-level data aggregation approach which performs data aggregation along either row or column dimension of MPI (Message Passing Interface) processes on a spatially decomposed domain, and then applies the pnetCDF parallel I/O paradigm. The test was done with three different domain sizes which represent small, moderately large, and large data domains, using a small-scale Community Multiscale Air Quality model (CMAQ) mock-up code. The examination includes comparing I/O performance with traditional serial I/O technique, straight application of pnetCDF, and the data aggregation along row and column dimension before applying pnetCDF. After the comparison, "optimal" I/O configurations of this application-level data aggregation approach were quantified. Data aggregation along the row dimension (pnetCDFcr) works better than along the column dimension (pnetCDFcc) although it may perform slightly worse than the straight pnetCDF method with a small number of processors. When the number of processors becomes larger, pnetCDFcr outperforms pnetCDF significantly. If the number of proces

Use of mesophilic and thermophilic bacteria for the improvement of copper extraction from a low-grade ore

NASA Astrophysics Data System (ADS)

Darezereshki, E.; Schaffie, M.; Lotfalian, M.; Seiedbaghery, S. A.; Ranjbar, M.

2011-04-01

Bioleaching was examined for copper extraction from a low grade ore using mesophilic and moderate thermophilic bacteria. Five equal size columns were used for the leaching of the ore. Sulfuric acid solution with a flow rate of 3.12 L·m-2·h-1 and pH 1.5 passed through each column continuously for 90 d. In the first and the second column, bioleaching was performed without agglomeration of the ore and on the agglomerated ore, respectively. 28wt% of the copper was extracted in the first column after 40 d, while this figure was 38wt% in the second column. After 90 d, however, the overall extractions were almost the same for both of them. Bioleaching with mesophilic bacteria was performed in the third column without agglomeration of the ore and in the fourth column on the agglomerated ore. After 40 d, copper extractions in the third and the fourth columns were 62wt% and 70wt%, respectively. Copper extractions were 75wt% for both the columns after 90 d. For the last column, bioleaching was performed with moderate thermophilic bacteria and agglomerated ore. Copper extractions were 80wt% and 85wt% after 40 and 90 d, respectively. It was concluded that crushing and agglomeration of the ore using bacteria could enhance the copper extraction considerably.

On-Line 1D and 2D PLOT/LC-ESI-MS Using 10 μm i.d. Poly(styrene–divinylbenzene) Porous Layer Open Tubular (PLOT) Columns For Ultrasensitive Proteomic Analysis

PubMed Central

Luo, Quanzhou; Yue, Guihua; Valaskovic, Gary A; Gu, Ye; Wu, Shiaw-Lin; Karger, Barry L.

2008-01-01

Following on our recent work, on-line one dimensional (1D) and two dimensional (2D) PLOT/LC-ESI-MS platforms using 3.2 m × 10 μm i.d. poly(styrenedivinylbenzene) (PS-DVB) porous layer open tubular (PLOT) columns have been developed to provide robust, high performance and ultrasensitive proteomic analysis. Using a PicoClear tee, the dead volume connection between a 50 μm i.d. PS-DVB monolithic microSPE column and the PLOT column was minimized. The microSPE/PLOT column assembly provided a separation performance similar to that obtained with direct injection onto the PLOT column at a mobile phase flow rate of 20 nL/min. The trace analysis potential of the platform was evaluated using an in-gel tryptic digest sample of a gel fraction (15 to 40 kDa) of a cervical cancer (SiHa) cell line. As an example of the sensitivity of the system, ∼2.5 ng of protein in 2 μL solution, an amount corresponding to 20 SiHa cells, was subjected to on-line microSPE-PLOT/LC-ESIMS/MS analysis using a linear ion trap MS. 237 peptides associated with 163 unique proteins were identified from a single analysis when using stringent criteria associated with a false positive rate less than 1% . The number of identified peptides and proteins increased to 638 and 343, respectively, as the injection amount was raised to ∼45 ng of protein, an amount corresponding to 350 SiHa cells. In comparison, only 338 peptides and 231 unique proteins were identified (false positive rate again less than 1%) from 750 ng of protein from the identical gel fraction, an amount corresponding to 6000 SiHa cells, using a typical 15 cm × 75 μm i.d. packed capillary column. The greater sensitivity, higher recovery, and higher resolving power of the PLOT column resulted in the increased number of identifications from only ∼5% of the injected sample amount. The resolving power of the microSPE/PLOT assembly was further extended by 2D chromatography via combination of the high-efficiency reversed phase PLOT column with strong cation exchange chromatography (SCX). As an example, 1071 peptides associated with 536 unique proteins were identified from 75 ng of protein from the same gel fraction, an amount corresponding to 600 cells, using 5 ion exchange fractions in online 2D SCX-PLOT/LC-MS. The 2D system, implemented in an automated format, led to simple and robust operation for proteomic analysis. These promising results demonstrate the potential of the PLOT column for ultratrace analysis. PMID:17625912

Evolution of the locomotory system in eels (Teleostei: Elopomorpha).

PubMed

Pfaff, Cathrin; Zorzin, Roberto; Kriwet, Jürgen

2016-08-11

Living anguilliform eels represent a distinct clade of elongated teleostean fishes inhabiting a wide range of habitats. Locomotion of these fishes is highly influenced by the elongated body shape, the anatomy of the vertebral column, and the corresponding soft tissues represented by the musculotendinous system. Up to now, the evolution of axial elongation in eels has been inferred from living taxa only, whereas the reconstruction of evolutionary patterns and functional ecology in extinct eels still is scarce. Rare but excellently preserved fossil eels from the Late Cretaceous and Cenozoic were investigated here to gain a better understanding of locomotory system evolution in anguilliforms and, consequently, their habitat occupations in deep time. The number of vertebrae in correlation with the body length separates extinct and extant anguilliforms. Even if the phylogenetic signal cannot entirely be excluded, the analyses performed here reveal a continuous shortening of the vertebral column with a simultaneous increase in vertebral numbers in conjunction with short lateral tendons throughout the order. These anatomical changes contradict previous hypotheses based on extant eels solely. The body curvatures of extant anguilliforms are highly flexible and can be clearly distinguished from extinct species. Anatomical changes of the vertebral column and musculotendinous system through time and between extinct and extant anguilliforms correlate with changes of the body plan and swimming performance and reveal significant shifts in habitat adaptation and thus behaviour. Evolutionary changes in the skeletal system of eels established here also imply that environmental shifts were triggered by abiotic rather than biotic factors (e.g., K/P boundary mass extinction event).

Experimental framework to study tip vortex interactions in multirotor wakes

NASA Astrophysics Data System (ADS)

Yao, Rongnan; Araya, Daniel

2017-11-01

We present an experimental study to compare the dynamic characteristics of tip vortices shed from a propeller in a crossflow to similar characteristics of an isolated vortex column generated in a closed system. Our aim is to evaluate the feasibility of using this simple isolated system to study the more complicated three-dimensional vortex interactions inherent to multirotor wakes, where the local unsteadiness generated by one rotor can strongly impact the performance of nearby rotors. Time-resolved particle image velocimetry is used to measure the velocity field of the propeller wake flow in a wind tunnel and the vortex column in a water tank. Specific attention is placed on analyzing the observed vortex core precession in the isolated system and comparing this to characteristic tip-vortex wandering phenomenon.

Characterization of new types of stationary phases for fast liquid chromatographic applications.

PubMed

Fekete, Szabolcs; Fekete, Jeno; Ganzler, Katalin

2009-12-05

The performance of a narrow bore silica based monolith column (5 cm x 2 mm) was compared to 5 cm long narrow bore (internal diameter < or = 2.1 mm) columns, packed with shell particles (2.7 microm) and totally porous sub-2 microm particles (1.5 microm, 1.7 microm and 1.9 microm) in gradient and isocratic elution separations of steroids. The highest peak capacity could be achieved with the column packed with 1.5 microm totally porous particles. The columns packed with porous 1.7 microm and shell 2.7 microm particles showed very similar capacity. The monolith column provided the lowest capacity during gradient elution. The plate height (HETP) of the 2.7 microm Ascentis Express column was very similar to the HETP obtained with 1.5 microm and 1.7 microm totally porous particles. The Chromolith monolithic column displayed an efficiency that is comparable to that of columns packed with spherical particles having their diameter between 3 microm and 4 microm. A kinetic plot analysis is presented to compare the theoretical analysis speed of different separation media. At 200 bar, the monolith column provided the highest performance when the required plate number was higher than 5000 (N>5000), however the efficiency drifted off faster in the range of N<5000 than in the case of packed columns. If the possibility of maximum performance was utilized (1000 bar for sub-2 microm particles, 600 bar for shell particles and 200 bar for monolith column) the monolith column would provide the poorest efficiency, while the column, packed with 1.5 microm particles offered the shortest impedance time.

Preparation of open tubular capillary columns by in situ ring-opening polymerization and their applications in cLC-MS/MS analysis of tryptic digest.

PubMed

Wang, Hongwei; Yao, Yating; Li, Ya; Ma, Shujuan; Peng, Xiaojun; Ou, Junjie; Ye, Mingliang

2017-08-01

An open tubular (OT) column (25 μm i.d.) was prepared by in situ ring-opening polymerization of octaglycidyldimethylsilyl polyhedral oligomeric silsesquioxanes (POSS-epoxy) with 4-aminophenyl disulfide (APDS) in a binary porogenic system of ethanol/H 2 O. It was found that porogenic composition played an important role in the formation of OT stationary phases. The ratio of ethanol/H 2 O at 6/1 (v/v) would lead to the fabrication of hybrid monoliths, while the ratio of ethanol/H 2 O at 13/1 (v/v) would result in the synthesis of OT phases. In addition, the effects of precursor content and reaction duration on the thickness of OT stationary phases were investigated. Either lower precursor content or shorter reaction duration would produce thinner layer of OT column. The repeatability of OT columns was evaluated through relative standard deviation (RSD%) with benzene as the analyte. The run-to-run, column-to-column and batch-to-batch repeatabilities were 1.7%, 4.8% and 5.6%, respectively, exhibiting satisfactory repeatability of the OT column. Then tryptic digest of mouse liver proteins was used to evaluate the performance of the resulting OT columns (25 μm i.d. × 2.5 m in length) by cLC-MS/MS analysis, demonstrating their potential in proteome analysis. Copyright © 2017 Elsevier B.V. All rights reserved.

Comparison of monolithic and microparticulate columns for reversed-phase liquid chromatography of tryptic digests of industrial enzymes in cleaning products.

PubMed

Beneito-Cambra, M; Herrero-Martínez, J M; Ramis-Ramos, G; Lindner, W; Lämmerhofer, M

2011-10-14

Enzymes of several classes used in the formulations of cleaning products were characterized by trypsin digestion followed by HPLC with UV detection. A polymeric monolithic column (ProSwift) was used to optimize the separation of both the intact enzymes and their tryptic digests. This column was adequate for the quality control of raw industrial enzyme concentrates. Then, monolithic and microparticulate columns were compared for peptide analysis. Under optimized conditions, the analysis of tryptic digests of enzymes of different classes commonly used in the formulation of cleaning products was carried out. Number of peaks, peak capacity and global resolution were obtained in order to evaluate the chromatographic performance of each column. Particulate shell-core C18 columns (Kinetex, 2.6 μm) showed the best performance, followed by a silica monolithic column (Chromolith RP-18e) and the conventional C18 packings (Gemini, 5 μm or 3 μm). A polymeric monolithic column (ProSwift) gave the worst performances. The proposed method was satisfactorily applied to the characterization of the enzymes present in spiked detergent bases and commercial cleaners. Copyright © 2011 Elsevier B.V. All rights reserved.

The Fire Resistance Performance of Recycled Aggregate Concrete Columns with Different Concrete Compressive Strengths

PubMed Central

Dong, Hongying; Cao, Wanlin; Bian, Jianhui; Zhang, Jianwei

2014-01-01

In order to ascertain the fire resistance performance of recycled aggregate concrete (RAC) components with different concrete compressive strengths, four full-scaled concrete columns were designed and tested under high temperature. Two of the four specimens were constructed by normal concrete with compressive strength ratings of C20 and C30, respectively, while the others were made from recycled coarse aggregate (RCA) concrete of C30 and C40, respectively. Identical constant axial forces were applied to specimens while being subjected to simulated building fire conditions in a laboratory furnace. Several parameters from the experimental results were comparatively analyzed, including the temperature change, vertical displacement, lateral deflection, fire endurance, and failure characteristics of specimens. The temperature field of specimens was simulated with ABAQUS Software (ABAQUS Inc., Provindence, RI, USA) and the results agreed quite well with those from the experiments. Results show that the rate of heat transfer from the surface to the interior of the column increases with the increase of the concrete’s compressive strength for both RAC columns and normal concrete columns. Under the same initial axial force ratio, for columns with the same cross section, those with lower concrete compressive strengths demonstrate better fire resistance performance. The fire resistance performance of RAC columns is better than that of normal concrete columns, with the same concrete compressive strength. PMID:28788279

The Fire Resistance Performance of Recycled Aggregate Concrete Columns with Different Concrete Compressive Strengths.

PubMed

Dong, Hongying; Cao, Wanlin; Bian, Jianhui; Zhang, Jianwei

2014-12-08

In order to ascertain the fire resistance performance of recycled aggregate concrete (RAC) components with different concrete compressive strengths, four full-scaled concrete columns were designed and tested under high temperature. Two of the four specimens were constructed by normal concrete with compressive strength ratings of C20 and C30, respectively, while the others were made from recycled coarse aggregate (RCA) concrete of C30 and C40, respectively. Identical constant axial forces were applied to specimens while being subjected to simulated building fire conditions in a laboratory furnace. Several parameters from the experimental results were comparatively analyzed, including the temperature change, vertical displacement, lateral deflection, fire endurance, and failure characteristics of specimens. The temperature field of specimens was simulated with ABAQUS Software (ABAQUS Inc., Provindence, RI, USA) and the results agreed quite well with those from the experiments. Results show that the rate of heat transfer from the surface to the interior of the column increases with the increase of the concrete's compressive strength for both RAC columns and normal concrete columns. Under the same initial axial force ratio, for columns with the same cross section, those with lower concrete compressive strengths demonstrate better fire resistance performance. The fire resistance performance of RAC columns is better than that of normal concrete columns, with the same concrete compressive strength.

Acoustic mapping of shallow water gas releases using shipborne multibeam systems

NASA Astrophysics Data System (ADS)

Urban, Peter; Köser, Kevin; Weiß, Tim; Greinert, Jens

2015-04-01

Water column imaging (WCI) shipborne multibeam systems are effective tools for investigating marine free gas (bubble) release. Like single- and splitbeam systems they are very sensitive towards gas bubbles in the water column, and have the advantage of the wide swath opening angle, 120° or more allowing a better mapping and possible 3D investigations of targets in the water column. On the downside, WCI data are degraded by specific noise from side-lobe effects and are usually not calibrated for target backscattering strength analysis. Most approaches so far concentrated on manual investigations of bubbles in the water column data. Such investigations allow the detection of bubble streams (flares) and make it possible to get an impression about the strength of detected flares/the gas release. Because of the subjective character of these investigations it is difficult to understand how well an area has been investigated by a flare mapping survey and subjective impressions about flare strength can easily be fooled by the many acoustic effects multibeam systems create. Here we present a semi-automated approach that uses the behavior of bubble streams in varying water currents to detect and map their exact source positions. The focus of the method is application of objective rules for flare detection, which makes it possible to extract information about the quality of the seepage mapping survey, perform automated noise reduction and create acoustic maps with quality discriminators indicating how well an area has been mapped.

High-throughput determination of faropenem in human plasma and urine by on-line solid-phase extraction coupled to high-performance liquid chromatography with UV detection and its application to the pharmacokinetic study.

PubMed

Xie, Rui; Wen, Jun; Wei, Hua; Fan, Guorong; Zhang, Dabing

2010-05-01

An automated system using on-line solid-phase extraction and HPLC with UV detection was developed for the determination of faropenem in human plasma and urine. Analytical process was performed isocratically with two reversed-phase columns connected by a switching valve. After simple pretreatment for plasma and urine with acetonitrile, a volume of 100microl upper layer of the plasma or urine samples was injected for on-line SPE column switching HPLC-UV analysis. The analytes were retained on the self-made trap column (Lichrospher C(18), 4.6mmx37mm, 25microm) with the loading solvent (20mM NaH(2)PO(4) adjusted pH 3.5) at flow rate of 2mlmin(-1), and most matrix materials were removed from the column to waste. After 0.5min washing, the valve was switched to another position so that the target analytes could be eluted from trap column to analytical column in the back-flush mode by the mobile phase (acetonitrile-20mM NaH(2)PO(4) adjusted pH 3.5, 16:84, v/v) at flow rate of 1.5mlmin(-1), and then separated on the analytical column (Ultimate XB-C(18), 4.6mmx50mm, 5microm).The complete cycle of the on-line SPE preconcentration purification and HPLC separation of the analytes was 5min. Calibration curves with good linearities (r=0.9994 for plasma sample and r=0.9988 for urine sample) were obtained in the range 0.02-5microgml(-1) in plasma and 0.05-10microg ml(-1) in urine for faropenem. The optimized method showed good performance in terms of specificity, linearity, detection and quantification limits, precision and accuracy. The method was successfully utilized to quantify faropenem in human plasma and urine to support the clinical pharmacokinetic studies. Copyright 2009 Elsevier B.V. All rights reserved.

Parametric study on the vortex-induced motions of semi-submersibles: Effect of rounded ratios of the column and pontoon

NASA Astrophysics Data System (ADS)

Liu, Mingyue; Xiao, Longfei; Yang, Jianmin; Tian, Xinliang

2017-05-01

The vortex-induced motions (VIMs) of semi-submersibles have emerged as an important issue in offshore engineering, as they pose a threat to safe and reliable operations and severely affect the fatigue lives of risers and mooring systems. The VIM response depends on the shape of the submerged structure and thus is significantly influenced by the design parameters related to the columns and pontoons. Numerical simulations by the detached Eddy simulation method are validated by experimental data and then used for parametric analysis of the VIM performance of various semi-submersibles with different column rounded ratios (Rc/L ) and pontoon rounded ratios (Rp/Lp ). The results show that the transverse amplitudes of a semi-submersible with circular columns at a 0° current heading are twice as large as those at a 45° current heading. However, the semi-submersible with rounded square columns shows more significant transverse motions at a 45° current heading than at a 0° current heading. Furthermore, at the 45° current heading, the transverse amplitudes of the semi-submersibles show a rapid increase as the column radius increases in the range of Rc/L <0.1 . The peak values remain roughly the same for 0.1 ≤Rc/L ≤0.2 and then decrease as the column radius increases (Rc/L ≥0.3 ). In addition, the effect of the pontoon shape on the transverse response is negligible for semi-submersibles with sharp square columns, while for semi-submersibles with rounded square columns or circular columns, the sharp rectangular pontoons greatly mitigate the VIM response.

Reactive barrier system for nitrate removal from mine effluents in northern Sweden: Laboratory experiments

NASA Astrophysics Data System (ADS)

Herbert, Roger

2010-05-01

Laboratory column experiments have been conducted to determine nitrate removal rates from mine effluents by denitrification, with the purpose of providing initial data for the construction of a pilot scale reactive barrier system at the Malmberget iron mine, Sweden. Experiments were conducted at several different flow rates at 5C, 10C and room temperature; annual mean temperatures at the Malmberget site lie close to 0C. Columns were filled with an organic substrate consisting of sawdust mixed with sewage sludge, the source of denitrifying bacteria, supported by oven-dried clay pellets. Apparent denitrification rates, calculated from inflow and outflow nitrate concentrations and column hydraulic residence time, ranged from 5 to 13 mg N/L/d, with the lowest rates corresponding to the 5C experiments. These rates are, however, limited to a certain degree by the low flow rate and the supply of electrons acceptors (i.e. nitrate) to denitrifying bacteria. Results from the column experiment have been used to construct a barrier system in Malmberget, Sweden. Trial runs with the pilot-scale barrier will be conducted during 2010, with the purpose of determining the performance of the barrier as mean air temperatures increase from below to above 0C and saturated flow commences in the barrier. The barrier system is constructed as a rectangular container with steel sheet walls (9m length in flow direction, 1.5m deep), and the flow rate will be adjusted to a hydraulic residence time of 1 day. The pilot-scale barrier system currently lies above ground, but a permanent barrier system would be installed below the ground surface so that the system can be maintained at positive temperatures throughout the year.

Separation and purification of astaxanthin from Phaffia rhodozyma by preparative high-speed counter-current chromatography.

PubMed

Du, Xiping; Dong, Congcong; Wang, Kai; Jiang, Zedong; Chen, Yanhong; Yang, Yuanfan; Chen, Feng; Ni, Hui

2016-09-01

An effective high-speed counter-current chromatography (HSCCC) method was established for the preparative isolation and purification of astaxanthin from Phaffia rhodozyma. With a two-phase solvent system composed of n-hexane-acetone-ethanol-water (1:1:1:1, v/v/v/v), 100mg crude extract of P. rhodozyma was separated to yield 20.6mg of astaxanthin at 92.0% purity. By further one step silica gel column chromatography, the purity reached 99.0%. The chemical structure of astaxanthin was confirmed by thin layer chromatography (TLC), UV spectroscopy scanning, high performance liquid chromatography with a ZORBAX SB-C18 column and a Waters Nova-pak C18 column, and ESI/MS/MS. Copyright © 2016 Elsevier B.V. All rights reserved.

Developing the Pulsed Fission-Fusion (PuFF) Engine

NASA Technical Reports Server (NTRS)

Adams, Robert B.; Cassibry, Jason; Bradley, David; Fabisinski, Leo; Statham, Geoffrey

2014-01-01

In September 2013 the NASA Innovative Advanced Concept (NIAC) organization awarded a phase I contract to the PuFF team. Our phase 1 proposal researched a pulsed fission-fusion propulsion system that compressed a target of deuterium (D) and tritium (T) as a mixture in a column, surrounded concentrically by Uranium. The target is surrounded by liquid lithium. A high power current would flow down the liquid lithium and the resulting Lorentz force would compress the column by roughly a factor of 10. The compressed column would reach criticality and a combination of fission and fusion reactions would occur. Our Phase I results, summarized herein, review our estimates of engine and vehicle performance, our work to date to model the fission-fusion reaction, and our initial efforts in experimental analysis.

Hormone Purification by Isoelectric Focusing

NASA Technical Reports Server (NTRS)

Bier, M.

1985-01-01

Various ground-based research approaches are being applied to a more definitive evaluation of the natures and degrees of electroosmosis effects on the separation capabilities of the Isoelectric Focusing (IEF) process. A primary instrumental system for this work involves rotationally stabilized, horizontal electrophoretic columns specially adapted for the IEF process. Representative adaptations include segmentation, baffles/screens, and surface coatings. Comparative performance and development testing are pursued against the type of column or cell established as an engineering model. Previously developed computer simulation capabilities are used to predict low-gravity behavior patterns and performance for IEF apparatus geometries of direct project interest. Three existing mathematical models plus potential new routines for particular aspects of simulating instrument fluid patterns with varied wall electroosmosis influences are being exercised.

High-performance liquid chromatography method for the simultaneous determination of sulfamethoxazole and trimethoprim in bovine milk using an on-line clean-up column.

PubMed

Pereira, A V; Cass, Q B

2005-11-05

A bidimensional HPLC method for the simultaneous determination of sulfamethoxazole (SMX) and trimethoprim (TMP) in bovine milk has been developed and validated. After centrifugation, aliquots (150 microl) of milk samples were directly injected to a column-switching HPLC system. At the first step a RAM octyl-BSA column was employed to automatically remove proteins that otherwise would interfere with milk analysis. The mobile phase 0.01 M phosphate buffer pH 6.0:acetonitrile (95:5, v/v) was used in the first 5 min for the elution of milk proteins and then 0.01 M phosphate buffer pH 6.0:acetonitrile (83:17, v/v) for transfer SMX and TMP to the analytical column. The separation of SMX and TMP from one another and from other remaining milk components was performed on an octyl column using the mobile phase 0.01 M phosphate buffer pH 5.0:acetonitrile (82:18, v/v), which were detected by UV at 265 nm. The calibration graphs were linear in the concentration ranges of 25-800 ng/ml and 50-400 ng/ml for SMX and TMP, respectively. The intra- and inter-assay coefficients of variation were less than 15% for both drugs. The validated method was applied to the analysis of milk samples of twelve (two groups of six) cows after administration (intramuscular or subcutaneous) of a single recommended therapeutic dose of the SMX-TMP combination.

Biological conversion system

DOEpatents

Scott, C.D.

A system for bioconversion of organic material comprises a primary bioreactor column wherein a biological active agent (zymomonas mobilis) converts the organic material (sugar) to a product (alcohol), a rejuvenator column wherein the biological activity of said biological active agent is enhanced, and means for circulating said biological active agent between said primary bioreactor column and said rejuvenator column.

A bridge column with superelastic NiTi SMA and replaceable rubber hinge for earthquake damage mitigation

NASA Astrophysics Data System (ADS)

Varela, Sebastian; ‘Saiid' Saiidi, M.

2016-07-01

This paper reports a unique concept for resilient bridge columns that can undergo intense earthquake loading and remain functional with minimal damage and residual drift. In this concept, the column is designed so that its components can be easily disassembled and reassembled to facilitate material recycling and component reuse. This is meant to foster sustainability of bridge systems while minimizing monetary losses from earthquakes. Self-centering and energy dissipation in the column were provided by unbonded superelastic nickel-titanium (NiTi) shape memory alloy bars placed inside a plastic hinge element made of rubber. This replaceable plastic hinge was in turn attached to a concrete-filled carbon fiber-reinforced polymer tube and a precast concrete footing that were designed to behave elastically. The proposed concept was evaluated experimentally by testing a ¼-scale column model under simulated near-fault earthquake motions on a shake table. After testing, the model was disassembled, reassembled and tested again. The seismic performance of the reassembled model was found to be comparable to that of the ‘virgin’ model. A relatively simple computational model of the column tested that was developed in OpenSees was able to match some of the key experimental response parameters.

An automated HPLC method for the fractionation of polychlorinated biphenyls, polychlorinated dibenzo-p-dioxins, and polychlorinated dibenzofurans in fish tissue on a porous graphitic carbon column

USGS Publications Warehouse

Echols, Kathy R.; Gale, Robert W.; Tillitt, Donald E.; Schwartz, Ted R.; O'Laughlin, Jerome

1997-01-01

The Ah (aryl-hydrocarbon) hydroxylase-receptor active polychlorinated biphenyls (PCBs), polychlorinated dibenzo-p-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs) were fractionated by an automated high-performance liquid chromatography (HPLC) system using the Hypercarb™ porous graphitic carbon (PGC) column. This commercially available column was used to fractionate the di-, mono-, and non-ortho PCBs into three fractions for gas chromatography (GC)/electron capture detection analysis, and a fourth fraction containing the PCDDs/PCDFs for GC/mass spectrometry analysis. The recoveries of the PCBs ranged from 68 to 96%, and recoveries of the PCDDs/PCDFs ranged from 74 to 123%. The PGC column has the advantage of faster separations (110 min versus 446 min) and less solvent use (275 ml versus 1,100 ml) compared with automated fractionation of these compounds on activated carbon (PX-21), while still affording good separation of the classes. The PGC column may have an advantage over the pyrenyl-based HPLC method because it has a greater loading capacity (400 μg total PCBs versus 250 μg). Overall, the PGC is a standard column that provides reproducible fractionation of PCDD/PCDFs and PCBs for analytical measurement in environmental samples.

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.

Validation of GC and HPLC systems for residue studies

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

Williams, M.

1995-12-01

For residue studies, GC and HPLC system performance must be validated prior to and during use. One excellent measure of system performance is the standard curve and associated chromatograms used to construct that curve. The standard curve is a model of system response to an analyte over a specific time period, and is prima facia evidence of system performance beginning at the auto sampler and proceeding through the injector, column, detector, electronics, data-capture device, and printer/plotter. This tool measures the performance of the entire chromatographic system; its power negates most of the benefits associated with costly and time-consuming validation ofmore » individual system components. Other measures of instrument and method validation will be discussed, including quality control charts and experimental designs for method validation.« less

Fast preparation of hybrid monolithic columns via photo-initiated thiol-yne polymerization for capillary liquid chromatography.

PubMed

Ma, Shujuan; Zhang, Haiyang; Li, Ya; Li, Yanan; Zhang, Na; Ou, Junjie; Ye, Mingliang; Wei, Yinmao

2018-02-23

Although several approaches have been developed to fabricate hybrid monoliths, it would still take a few hours to finish the formation of monoliths. Herein, photo-initiated thiol-yne polymerization was first adopted to in situ fabricate hybrid monoliths within the confines of UV-transparent fused-silica capillary. A silicon-containing diyne (1,3-diethynyltetramethyl-disiloxane, DYDS) was copolymerized with three multithiols, 1,6-hexanedithiol, trimethylolpropane tris(3-mercaptopropionate) and pentaerythriol tetrakis(3-mercaptopropionate), by using a binary porogenic system of diethylene glycol diethyl ether (DEGDE)/poly(ethylene glycol) (PEG200) within 10 min. Several characterizations of three hybrid monoliths (assigned as I, II and III, respectively) were performed. The results showed that these hybrid monoliths possessed bicontinuous porous structure, which was remarkably different from that via typical free-radical polymerization. The highest column efficiency of 76,000 plates per meter for butylbenzene was obtained on the column I in reversed-phase liquid chromatography (RPLC). It was observed that the efficiencies for strong-retained butylbenzene were almost close to those of weak-retained benzene, indicating a retention-independent efficient performance of small molecules on hybrid column I. The surface area of this hybrid monolith was very small in the dry state (less than 10.0 m 2 /g), and the chromatographic behavior of hybrid monolithic columns would be possibly explained by radical-mediated step-growth process of thiol-yne polymerization. Finally, the column I was applied for separation of BSA tryptic digest by cLC-MS/MS, indicating satisfactory separation ability for complicated samples. Copyright © 2018 Elsevier B.V. All rights reserved.

Recent advances in micro-scale and nano-scale high-performance liquid-phase chromatography for proteome research.

PubMed

Tao, Dingyin; Zhang, Lihua; Shan, Yichu; Liang, Zhen; Zhang, Yukui

2011-01-01

High-performance liquid chromatography-electrospray ionization tandem mass spectrometry (HPLC-ESI-MS-MS) is regarded as one of the most powerful techniques for separation and identification of proteins. Recently, much effort has been made to improve the separation capacity, detection sensitivity, and analysis throughput of micro- and nano-HPLC, by increasing column length, reducing column internal diameter, and using integrated techniques. Development of HPLC columns has also been rapid, as a result of the use of submicrometer packing materials and monolithic columns. All these innovations result in clearly improved performance of micro- and nano-HPLC for proteome research.

Technetium-99m generator system

DOEpatents

Mirzadeh, Saed; Knapp, Jr., Furn F.; Collins, Emory D.

1998-01-01

A .sup.99 Mo/.sup.99m Tc generator system includes a sorbent column loaded with a composition containing .sup.99 Mo. The sorbent column has an effluent end in fluid communication with an anion-exchange column for concentrating .sup.99m Tc eluted from the sorbent column. A method of preparing a concentrated solution of .sup.99m Tc includes the general steps of: a. providing a sorbent column loaded with a composition containing .sup.99 Mo, the sorbent column having an effluent end in fluid communication with an anion-exchange column; b. eluting the sorbent column with a salt solution to elute .sup.99m Tc from the sorbent and to trap and concentrate the eluted .sup.99m Tc on the ion-exchange column; and c. eluting the concentrated .sup.99m Tc from the ion-exchange column with a solution comprising a reductive complexing agent.

Technetium-99m generator system

DOEpatents

Mirzadeh, S.; Knapp, F.F. Jr.; Collins, E.D.

1998-06-30

A {sup 99}Mo/{sup 99m}Tc generator system includes a sorbent column loaded with a composition containing {sup 99}Mo. The sorbent column has an effluent end in fluid communication with an anion-exchange column for concentrating {sup 99m}Tc eluted from the sorbent column. A method of preparing a concentrated solution of {sup 99m}Tc includes the general steps of: (a) providing a sorbent column loaded with a composition containing {sup 99}Mo, the sorbent column having an effluent end in fluid communication with an anion-exchange column; (b) eluting the sorbent column with a salt solution to elute {sup 99m}Tc from the sorbent and to trap and concentrate the eluted {sup 99m}Tc on the ion-exchange column; and (c) eluting the concentrated {sup 99m}Tc from the ion-exchange column with a solution comprising a reductive complexing agent. 1 fig.

Effect of vertical active vibration isolation on tracking performance and on ride qualities

NASA Technical Reports Server (NTRS)

Dimasi, F. P.; Allen, R. E.; Calcaterra, P. C.

1972-01-01

An investigation to determine the effect on pilot performance and comfort of an active vibration isolation system for a commercial transport pilot seat is reported. The test setup consisted of: a hydraulic shaker which produced random vertical vibration inputs; the active vibration isolation system; the pilot seat; the pilot control wheel and column; the side-arm controller; and a two-axis compensatory tracking task. The effects of various degrees of pilot isolation on short-term (two-minute) tracking performance and comfort were determined.

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

Duignan, M. R.; Herman, D. T.; Restivo, M. L.

Experiments at several different scales were performed to understand the removal of spherical resorcinol formaldehyde (sRF) ion exchange resin using a gravity drain system with a valve located above the resin screen in the ion exchange column (IXC). This is being considered as part of the design for the Low Activity Waste Pretreatment System (LAWPS) to be constructed at the DOE Hanford Site.

Extending the upper temperature range of gas chromatography with all-silicon microchip columns using a heater/clamp assembly.

PubMed

Ghosh, Abhijit; Johnson, Jacob E; Nuss, Johnathan G; Stark, Brittany A; Hawkins, Aaron R; Tolley, Luke T; Iverson, Brian D; Tolley, H Dennis; Lee, Milton L

2017-09-29

Miniaturization of gas chromatography (GC) instrumentation is of interest because it addresses current and future issues relating to compactness, portability and field application. While incremental advancements continue to be reported in GC with columns fabricated in microchips (referred to in this paper as "microchip columns"), the current performance is far from acceptable. This lower performance compared to conventional GC is due to factors such as pooling of the stationary phase in corners of non-cylindrical channels, adsorption of sensitive compounds on incompletely deactivated surfaces, shorter column lengths and less than optimum interfacing to injector and detector. In this work, a GC system utilizing microchip columns was developed that solves the latter challenge, i.e., microchip interfacing to injector and detector. A microchip compression clamp was constructed to heat the microchip (i.e., primary heater), and seal the injector and detector fused silica interface tubing to the inlet and outlet ports of the microchip channels with minimum extra-column dead volume. This clamp allowed occasional operation up to 375°C and routine operation up to 300°C. The compression clamp was constructed of a low expansion alloy, Kovar™, to minimize leaking due to thermal expansion mismatch at the interface during repeated thermal cycling, and it was tested over several months for more than one hundred injections without forming leaks. A 5.9m long microcolumn with rectangular cross section of 158μm×80μm, which approximately matches a 100μm i.d. cylindrical fused silica column, was fabricated in a silicon wafer using deep reactive ion etching (DRIE) and high temperature fusion bonding; finally, the channel was coated statically with a 1% vinyl, 5% phenyl, 94% methylpolysiloxane stationary phase. High temperature separations of C10-C40 n-alkanes and a commercial diesel sample were demonstrated using the system under both temperature programmed GC (TPGC) and thermal gradient GC (TGGC) conditions. TGGC analysis of a complex essential oil sample was also demonstrated. Addition of a secondary heater and polyimide insulation proved to be helpful in achieving the desired elution temperature without having to raise the primary heater temperature above 300°C for high boiling point compounds. Copyright © 2017 Elsevier B.V. All rights reserved.

Seismic performance of circular reinforced concrete bridge columns constructed with grade 80 reinforcement.

DOT National Transportation Integrated Search

2014-08-01

This project assessed the use of ASTM A706 Grade 80 reinforcing bars in reinforced concrete columns. : Grade 80 is not currently allowed in reinforced concrete columns due to lack of information on the : material characteristics and column performanc...

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.

Research on the Influence of Size Effect for the mechanical Performance of GFRP tube concrete steel tube composite column under axial compression

NASA Astrophysics Data System (ADS)

Li, Wen; Wang, Tong; Na, Yu

2017-08-01

FRP tube-concrete-steel tube composite column (DSTC) was a new type of composite structures. The column consists of FRP outer tube and steel tube and concrete. Concrete was filled between FRP outer tube and steel tube. This column has the character of light and high strength and corrosion resistance. In this paper, properties of DSTC axial compression were studied in depth. The properties were studied by two groups DSTC short columns under axial compression performance experiment. The different size of DSTC short columns was importantly considered. According to results of the experiment, we can conclude that with the size of the column increases the ability of it to resist deformation drops. On the other hand, the size effect influences on properties of different concrete strength DSTC was different. The influence of size effect on high concrete strength was less than that of low concrete.

Ruggedness/robustness evaluation and system suitability test on United States Pharmacopoeia XXVI assay ginsenosides in Asian and American ginseng by high-performance liquid chromatography.

PubMed

Li, Yong-Guo; Chen, Ming; Chou, Gui-Xin; Wang, Zheng-Tao; Hu, Zhi-Bi

2004-09-03

The work of the ruggedness/robustness evaluation and system suitability tests was oriented to profound understand the practicability of using assay methods issued by United States Pharmacopoeia (USP XXVI and XXVII) for ginsenosides in Asian ginseng and American ginseng. The items chosen for the method validation included quantitative related items such as recovery of Rg(1) and Rb(1), respectively, and qualitative related items such as resolution, theoretical plate number, relative retention time of two critical-band-pairs, Rg(1)/Re and Rb(1) with its neighboring peak, respectively. Totally, 16 column types were used for comparison of different vendors, different packing materials, different size, etc. and five sets of LC systems and two laboratories were involved in comparing the data of both quantitative and qualitative items. The results showed that different packing materials of columns used might significantly alters separation. The column packing material Hypersil afforded the preferable separating for the ginsenosides. No significant difference was observed from the different instrumentations and inter-laboratories. Our results suggest a modification of the system suitability test as given in USP26-NF21 and the latest version of USP27-NF22, which was not suitable for most systems. Using resolutions of Rg(1)/Re and Rb(1) with its neighboring peak as critical parameters for the ginsenosides assay and omitting the relative retention time of both Rg(1)/Re and Rb(1) with its neighboring peak is our suggestion for a more reasonable, yet practicable system suitability. Six typical chromatograms gain from different columns were figured out as well.

Identification and control of plasma vertical position using neural network in Damavand tokamak.

PubMed

Rasouli, H; Rasouli, C; Koohi, A

2013-02-01

In this work, a nonlinear model is introduced to determine the vertical position of the plasma column in Damavand tokamak. Using this model as a simulator, a nonlinear neural network controller has been designed. In the first stage, the electronic drive and sensory circuits of Damavand tokamak are modified. These circuits can control the vertical position of the plasma column inside the vacuum vessel. Since the vertical position of plasma is an unstable parameter, a direct closed loop system identification algorithm is performed. In the second stage, a nonlinear model is identified for plasma vertical position, based on the multilayer perceptron (MLP) neural network (NN) structure. Estimation of simulator parameters has been performed by back-propagation error algorithm using Levenberg-Marquardt gradient descent optimization technique. The model is verified through simulation of the whole closed loop system using both simulator and actual plant in similar conditions. As the final stage, a MLP neural network controller is designed for simulator model. In the last step, online training is performed to tune the controller parameters. Simulation results justify using of the NN controller for the actual plant.

Comprehensive two-dimensional HPLC to study the interaction of multiple components in Rheum palmatum L. with HSA by coupling a silica-bonded HSA column to a silica monolithic ODS column.

PubMed

Hu, Lianghai; Li, Xin; Feng, Shun; Kong, Liang; Su, Xingye; Chen, Xueguo; Qin, Feng; Ye, Mingliang; Zou, Hanfa

2006-04-01

A mode of comprehensive 2-D LC was developed by coupling a silica-bonded HSA column to a silica monolithic ODS column. This system combined the affinity property of the HSA column and the high-speed separation ability of the monolithic ODS column. The affinity chromatography with HSA-immobilized stationary phase was applied to study the interaction of multiple components in traditional Chinese medicines (TCMs) with HSA according to their affinity to protein in the first dimension. Then the unresolved components retained on the HSA column were further separated on the silica monolithic ODS column in the second dimension. By hyphenating the 2-D separation system to diode array detector and MS detectors, the UV and molecular weight information of the separated compounds can also be obtained. The developed separation system was applied to analysis of the extract of Rheum palmatum L., a number of low-abundant components can be separated on a single peak from the HSA column after normalization of peak heights. Six compounds were preliminarily identified according to their UV and MS spectra. It showed that this system was very useful for biological fingerprinting analysis of the components in TCMs and natural products.

Two-dimensional liquid chromatography consisting of twelve second-dimension columns for comprehensive analysis of intact proteins.

PubMed

Ren, Jiangtao; Beckner, Matthew A; Lynch, Kyle B; Chen, Huang; Zhu, Zaifang; Yang, Yu; Chen, Apeng; Qiao, Zhenzhen; Liu, Shaorong; Lu, Joann J

2018-05-15

A comprehensive two-dimensional liquid chromatography (LCxLC) system consisting of twelve columns in the second dimension was developed for comprehensive analysis of intact proteins in complex biological samples. The system consisted of an ion-exchange column in the first dimension and the twelve reverse-phase columns in the second dimension; all thirteen columns were monolithic and prepared inside 250 µm i.d. capillaries. These columns were assembled together through the use of three valves and an innovative configuration. The effluent from the first dimension was continuously fractionated and sequentially transferred into the twelve second-dimension columns, while the second-dimension separations were carried out in a series of batches (six columns per batch). This LCxLC system was tested first using standard proteins followed by real-world samples from E. coli. Baseline separation was observed for eleven standard proteins and hundreds of peaks were observed for the real-world sample analysis. Two-dimensional liquid chromatography, often considered as an effective tool for mapping proteins, is seen as laborious and time-consuming when configured offline. Our online LCxLC system with increased second-dimension columns promises to provide a solution to overcome these hindrances. Copyright © 2018 Elsevier B.V. All rights reserved.

Implementation of an MgO-based metal removal step in the passive treatment system of Shilbottle, UK: column experiments.

PubMed

Caraballo, Manuel A; Rötting, Tobias S; Silva, Verónica

2010-09-15

Three laboratory column experiments were performed to test the suitability of two different MgO-rich reagents for removal of Mn and Al from the out-flowing waters of Shilbottle passive treatment system (Northumberland, UK). The input water was doped with 100 mg/L Zn in order to extrapolate results to waters in sulphide mining districts. One column was filled with a Dispersed Alkaline Substrate (DAS) containing 12.5% (v/v) caustic magnesia precipitator dust (CMPD) from Spain mixed with wood shavings, two columns were filled with DAS containing wood shavings and 12.5% or 25% (v/v), respectively, of dolomitic lime precipitator dust (DLPD) from Thrislington, UK. The two columns containing 12.5% of CMPD or DLPD completely removed the contaminants from the inflow water during the first 6 weeks of the experiment (mean removal of 88 mg/L Al, 96 mg/L Zn and 37 mg/L Mn), operating at an acidity load of 140 g acidity/m(2)day. At this moment, a substantial increase of the Al and Mn water concentration in the out-flowing waters of Shilbottle occurred (430 g acidity/m(2)day), leading to passivation of the reactive material and to the development of preferential flow paths within less than another 6 weeks, probably mainly due to Al precipitates. Al should be removed prior to MgO treatment. Copyright 2010 Elsevier B.V. All rights reserved.

Comparison and Analysis of Steel Frame Based on High Strength Column and Normal Strength Column

NASA Astrophysics Data System (ADS)

Liu, Taiyu; An, Yuwei

2018-01-01

The anti-seismic performance of high strength steel has restricted its industrialization in civil buildings. In order to study the influence of high strength steel column on frame structure, three models are designed through MIDAS/GEN finite element software. By comparing the seismic performance and economic performance of the three models, the three different structures are comprehensively evaluated to provide some references for the development of high strength steel in steel structure.

Mathematical analysis of frontal affinity chromatography in particle and membrane configurations.

PubMed

Tejeda-Mansir, A; Montesinos, R M; Guzmán, R

2001-10-30

The scaleup and optimization of large-scale affinity-chromatographic operations in the recovery, separation and purification of biochemical components is of major industrial importance. The development of mathematical models to describe affinity-chromatographic processes, and the use of these models in computer programs to predict column performance is an engineering approach that can help to attain these bioprocess engineering tasks successfully. Most affinity-chromatographic separations are operated in the frontal mode, using fixed-bed columns. Purely diffusive and perfusion particles and membrane-based affinity chromatography are among the main commercially available technologies for these separations. For a particular application, a basic understanding of the main similarities and differences between particle and membrane frontal affinity chromatography and how these characteristics are reflected in the transport models is of fundamental relevance. This review presents the basic theoretical considerations used in the development of particle and membrane affinity chromatography models that can be applied in the design and operation of large-scale affinity separations in fixed-bed columns. A transport model for column affinity chromatography that considers column dispersion, particle internal convection, external film resistance, finite kinetic rate, plus macropore and micropore resistances is analyzed as a framework for exploring further the mathematical analysis. Such models provide a general realistic description of almost all practical systems. Specific mathematical models that take into account geometric considerations and transport effects have been developed for both particle and membrane affinity chromatography systems. Some of the most common simplified models, based on linear driving-force (LDF) and equilibrium assumptions, are emphasized. Analytical solutions of the corresponding simplified dimensionless affinity models are presented. Particular methods for estimating the parameters that characterize the mass-transfer and adsorption mechanisms in affinity systems are described.

Tungsten-188/carrier-free rhenium-188 perrhenic acid generator system

DOEpatents

Knapp, Jr., Furn F.; Lisic, Edward C.; Mirzadeh, Saed; Callahan, Alvin P.

1993-01-01

A generator system for providing a carrier-free radioisotope in the form of an acid comprises a chromatography column in tandem fluid connection with an ion exchange column, the chromatography column containing a charge of a radioactive parent isotope. The chromatography column, charged with a parent isotope, is eluted with an alkali metal salt solution to generate the radioisotope in the form of an intermediate solution, which is passed through the ion-exchange column to convert the radioisotope to a carrier-free acid form.

Tungsten-188/carrier-free rhenium-188 perrhenic acid generator system

DOEpatents

Knapp, F.F. Jr.; Lisic, E.C.; Mirzadeh, S.; Callahan, A.P.

1993-02-16

A generator system for providing a carrier-free radioisotope in the form of an acid comprises a chromatography column in tandem fluid connection with an ion exchange column, the chromatography column containing a charge of a radioactive parent isotope. The chromatography column, charged with a parent isotope, is eluted with an alkali metal salt solution to generate the radioisotope in the form of an intermediate solution, which is passed through the ion-exchange column to convert the radioisotope to a carrier-free acid form.

Tungsten-188/carrier-free rhenium-188 perrhenic acid generator system

DOEpatents

Knapp, Jr., Furn F.; Lisic, Edward C.; Mirzadeh, Saed; Callahan, Alvin P.

1994-01-01

A generator system for providing a carrier-free radioisotope in the form of an acid comprises a chromatography column in tandem fluid connection with an ion exchange column, the chromatography column containing a charge of a radioactive parent isotope. The chromatography column, charged with a parent isotope, is eluted with an alkali metal salt solution to generate the radioisotope in the form of an intermediate solution, which is passed through the ion-exchange column to convert the radioisotope to a carrier-free acid form.

Microscale depletion of high abundance proteins in human biofluids using IgY14 immunoaffinity resin: analysis of human plasma and cerebrospinal fluid.

PubMed

Hyung, Seok-Won; Piehowski, Paul D; Moore, Ronald J; Orton, Daniel J; Schepmoes, Athena A; Clauss, Therese R; Chu, Rosalie K; Fillmore, Thomas L; Brewer, Heather; Liu, Tao; Zhao, Rui; Smith, Richard D

2014-11-01

Removal of highly abundant proteins in plasma is often carried out using immunoaffinity depletion to extend the dynamic range of measurements to lower abundance species. While commercial depletion columns are available for this purpose, they generally are not applicable to limited sample quantities (<20 μL) due to low yields stemming from losses caused by nonspecific binding to the column matrix and concentration of large eluent volumes. Additionally, the cost of the depletion media can be prohibitive for larger-scale studies. Modern LC-MS instrumentation provides the sensitivity necessary to scale-down depletion methods with minimal sacrifice to proteome coverage, which makes smaller volume depletion columns desirable for maximizing sample recovery when samples are limited, as well as for reducing the expense of large-scale studies. We characterized the performance of a 346 μL column volume microscale depletion system, using four different flow rates to determine the most effective depletion conditions for ∼6-μL injections of human plasma proteins and then evaluated depletion reproducibility at the optimum flow rate condition. Depletion of plasma using a commercial 10-mL depletion column served as the control. Results showed depletion efficiency of the microscale column increased as flow rate decreased, and that our microdepletion was reproducible. In an initial application, a 600-μL sample of human cerebrospinal fluid (CSF) pooled from multiple sclerosis patients was depleted and then analyzed using reversed phase liquid chromatography-mass spectrometry to demonstrate the utility of the system for this important biofluid where sample quantities are more commonly limited.

Development of at-line assay to monitor charge variants of MAbs during production.

PubMed

St Amand, M M; Ogunnaike, B A; Robinson, A S

2014-01-01

One major challenge currently facing the biopharmaceutical industry is to understand how MAb microheterogeneity affects therapeutic efficacy, potency, immunogenicity, and clearance. MAb micro-heterogeneity can result from post-translational modifications such as sialylation, galactosylation, C-terminal lysine cleavage, glycine amidation, and tryptophan oxidation, each of which can generate MAb charge variants; such heterogeneity can affect pharmacokinetics (PK) considerably. Implementation of appropriate on-line quality control strategies may help to regulate bioprocesses, thus enabling more homogenous material with desired post-translational modifications and PK behavior. However, one major restriction to implementation of quality control strategies is the availability of techniques for obtaining on-line or at-line measurements of these attributes. In this work, we describe the development of an at-line assay to separate MAb charge variants in near real-time, which could ultimately be used to implement on-line quality control strategies for MAb production. The assay consists of a 2D-HPLC method with sequential in-line Protein A and WCX-10 HPLC column steps. To perform the 2D-HPLC assay at-line, the two columns steps were integrated into a single method using a novel system configuration that allowed parallel flow over column 1 or column 2 or sequential flow from column 1 to column 2. A bioreactor system was also developed such that media samples could be removed automatically from bioreactor vessels during production and delivered to the 2D-HPLC for analysis. With this at-line HPLC assay, we have demonstrated that MAb microheterogeneity occurs throughout the cell cycle whether the host cell line is grown under different or the same nominal culture conditions. © 2013 American Institute of Chemical Engineers.

Microscale depletion of high abundance proteins in human biofluids using IgY14 immunoaffinity resin: Analysis of human plasma and cerebrospinal fluid

DOE PAGES

Hyung, Seok Won; Piehowski, Paul D.; Moore, Ronald J.; ...

2014-09-06

Removal of highly abundant proteins in plasma is often carried out using immunoaffinity depletion to extend the dynamic range of measurements to lower abundance species. While commercial depletion columns are available for this purpose, they generally are not applicable to limited sample quantities (<20 µL) due to low yields stemming from losses caused by nonspecific binding to the column matrix. Additionally, the cost of the depletion media can be prohibitive for larger scale studies. Modern LC-MS instrumentation provides the sensitivity necessary to scale-down depletion methods with minimal sacrifice to proteome coverage, which makes smaller volume depletion columns desirable for maximizingmore » sample recovery when samples are limited, as well as for reducing the expense of large scale studies. We characterized the performance of a 346 µL column volume micro-scale depletion system, using four different flow rates to determine the most effective depletion conditions for ~6 μL injections of human plasma proteins and then evaluated depletion reproducibility at the optimum flow rate condition. Depletion of plasma using a commercial 10 mL depletion column served as the control. Results showed depletion efficiency of the micro-scale column increased as flow rate decreased, and that our micro-depletion was reproducible. We found, in an initial application, a 600 µL sample of human cerebral spinal fluid (CSF) pooled from multiple sclerosis patients was depleted and then analyzed using reversed phase liquid chromatography-mass spectrometry to demonstrate the utility of the system for this important biofluid where sample quantities are more commonly limited.« less

High-performance liquid chromatographic determination of the beta2-selective adrenergic agonist fenoterol in human plasma after fluorescence derivatization.

PubMed

Kramer, S; Blaschke, G

2001-02-10

A sensitive high-performance liquid chromatographic method has been developed for the determination of the beta2-selective adrenergic agonist fenoterol in human plasma. To improve the sensitivity of the method, fenoterol was derivatized with N-(chloroformyl)-carbazole prior to HPLC analysis yielding highly fluorescent derivatives. The assay involves protein precipitation with acetonitrile, liquid-liquid-extraction of fenoterol from plasma with isobutanol under alkaline conditions followed by derivatization with N-(chloroformyl)-carbazole. Reversed-phase liquid chromatographic determination of the fenoterol derivative was performed using a column-switching system consisting of a LiChrospher 100 RP 18 and a LiChrospher RP-Select B column with acetonitrile, methanol and water as mobile phase. The limit of quantitation in human plasma was 376 pg fenoterol/ml. The method was successfully applied for the assay of fenoterol in patient plasma.

Upgrade to Ion Exchange Modeling for Removal of Technetium from Hanford Waste Using SuperLig® 639 Resin

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

Hamm, L.; Smith, F.; Aleman, S.

2013-05-16

This report documents the development and application of computer models to describe the sorption of pertechnetate [TcO₄⁻], and its surrogate perrhenate [ReO₄⁻], on SuperLig® 639 resin. Two models have been developed: 1) A thermodynamic isotherm model, based on experimental data, that predicts [TcO₄⁻] and [ReO₄⁻] sorption as a function of solution composition and temperature and 2) A column model that uses the isotherm calculated by the first model to simulate the performance of a full-scale sorption process. The isotherm model provides a synthesis of experimental data collected from many different sources to give a best estimate prediction of the behaviormore » of the pertechnetate-SuperLig® 639 system and an estimate of the uncertainty in this prediction. The column model provides a prediction of the expected performance of the plant process by determining the volume of waste solution that can be processed based on process design parameters such as column size, flow rate and resin physical properties.« less

Aflatoxin evaluation in ready-to-eat brazil nuts using reversed-phase liquid chromatography and post-column derivatisation.

PubMed

Iamanaka, Beatriz Thie; Nakano, Felipe; Lemes, Daniel Ponciano; Ferranti, Larissa Souza; Taniwaki, Marta Hiromi

2014-01-01

A high-performance liquid chromatography-fluorescence (HPLC-FD) method for aflatoxin quantification in brazil nuts was developed. Samples of brazil nuts collected in Brazilian markets were extracted with methanol:water and cleaned using an immunoaffinity column. Aflatoxins were eluted with methanol and a post-column derivatisation was performed with bromine, using a Kobra Cell system. The optimised method for total aflatoxins was sensitive, with detection and quantification limits of 0.05 and 0.25 µg kg⁻¹, respectively. The method was accurate, with recovery values of 87.6%; 85.3% and 85.0% for 0.5, 5.0 and 14.6 µg kg⁻¹ spiked levels, respectively. It was shown that the method was applicable to brazil nuts. From a total of 95 brazil nut samples analysed from 21 São Paulo supermarket samples and 51 Manaus and 23 Belém street markets samples, 37.9% showed detectable levels of aflatoxins and three exceeded the recommended Codex Alimentarius limit of 10 µg kg⁻¹ for ready-to-eat brazil nuts.

Hydrodynamics, mass transfer, and yeast culture performance of a column bioreactor with ejector.

PubMed

Prokop, A; Janík, P; Sobotka, M; Krumphanzl, V

1983-04-01

A bubble column fitted with an ejector has been tested for its physical and biological performance. The axial diffusion coefficient of the liquid phase in the presence of electrolytes and ethanol was measured by a stimulus-response technique with subsequent evaluation by means of a diffusion model. In contrast to ordinary bubble columns, the coefficient of axial mixing is inversely dependent on the superficial air velocity. The liquid velocity acts in an opposite direction to the backmixing flow in the column. The measurement of volumetric oxygen transfer coefficient in the presence of electrolytes and ethanol was performed using a dynamic gassing-in method adapted for a column. The data were correlated with the superficial air and liquid velocities, total power input, and power for aeration and mixing; the economy coefficient of oxygen transfer was used for finding an optimum ratio of power for aeration and pumping. Growth experiments with Candida utilis on ethanol confirmed some of the above results. Biomass productivity of 2.5 g L(-1) h(-1) testifies about a good transfer capability of the column. Columns fitted with pneumatic and/or hydraulic energy input may be promising for aerobic fermentations considering their mass transfer and mixing characteristics.

Countercurrent Chromatographic Separation of Proteins Using an Eccentric Coiled Column with Synchronous and Nonsynchronous Type-J Planetary Motions

PubMed Central

SHINOMIYA, Kazufusa; YOSHIDA, Kazunori; TOKURA, Koji; TSUKIDATE, Etsuhiro; YANAGIDAIRA, Kazuhiro; ITO, Yoichiro

2015-01-01

Protein separation was performed using the high-speed counter-current chromatograph (HSCCC) at both synchronous and nonsynchronous type-J planetary motions. The partition efficiency was evaluated with two different column configurations, eccentric coil and toroidal coil, on the separation of a set of stable protein samples including cytochrome C, myoglobin and lysozyme with a polymer phase system composed of 12.5% (w/w) polyethylene glycol 1000 and 12.5% (w/w) dibasic potassium phosphate. Better peak resolution was obtained by the eccentric coil than by the toroidal coil using either lower or upper phase as the mobile phase. The peak resolution was further improved using the eccentric coil by the nonsynchronous type-J planetary motion with the combination of 1066 rpm of column rotation and 1000 rpm of revolution. PMID:25765276

Countercurrent chromatographic separation of proteins using an eccentric coiled column with synchronous and nonsynchronous type-J planetary motions.

PubMed

Shinomiya, Kazufusa; Yoshida, Kazunori; Tokura, Koji; Tsukidate, Etsuhiro; Yanagidaira, Kazuhiro; Ito, Yoichiro

2015-01-01

Protein separation was performed using the high-speed countercurrent chromatograph (HSCCC) at both synchronous and nonsynchronous type-J planetary motions. The partition efficiency was evaluated with two different column configurations, eccentric coil and toroidal coil, on the separation of a set of stable protein samples including cytochrome C, myoglobin and lysozyme with a polymer phase system composed of 12.5% (w/w) polyethylene glycol 1000 and 12.5% (w/w) dibasic potassium phosphate. Better peak resolution was obtained by the eccentric coil than by the toroidal coil using either lower or upper phase as the mobile phase. The peak resolution was further improved using the eccentric coil by the nonsynchronous type-J planetary motion with the combination of 1066 rpm of column rotation and 1000 rpm of revolution.

Hand-Portable Gradient Capillary Liquid Chromatography Pumping System.

PubMed

Sharma, Sonika; Plistil, Alex; Barnett, Hal E; Tolley, H Dennis; Farnsworth, Paul B; Stearns, Stanley D; Lee, Milton L

2015-10-20

In this work, a novel splitless nanoflow gradient generator integrated with a stop-flow injector was developed and evaluated using an on-column UV-absorption detector. The gradient pumping system consisted of two nanoflow pumps controlled by micro stepper motors, a mixer connected to a serpentine tube, and a high-pressure valve. The gradient system weighed only 4 kg (9 lbs) and could generate up to 55 MPa (8000 psi) pressure. The system could operate using a 24 V DC battery and required 1.2 A for operation. The total volume capacity of the pump was 74 μL, and a sample volume of 60 nL could be injected. The system provided accurate nanoflow rates as low as 10 nL/min without employing a splitter, making it ideal for capillary column use. The gradient dwell volume was calculated to be 1.3 μL, which created a delay of approximately 4 min with a typical flow rate of 350 nL/min. Gradient performance was evaluated for gradient step accuracy, and excellent reproducibility was obtained in day-to-day experiments (RSD < 1.2%, n = 4). Linear gradient reproducibility was tested by separating a three-component pesticide mixture on a poly(ethylene glycol) diacrylate (PEGDA) monolithic column. The retention time reproducibility was very good in run-to-run experiments (RSD < 1.42%, n = 4). Finally, excellent separation of five phenols was demonstrated using the nanoflow gradient system.

The separation of leukotrienes and hydroxyeicosatetraenoic acid metabolites of arachidonic acid by high performance liquid chromatography (HPLC).

PubMed

Osborne, D J; Peters, B J; Meade, C J

1983-11-01

The following high performance liquid chromatography system was found suitable for separating most lipoxygenase metabolites of arachidonic acid: Techsphere 5-C18 column, eluting solvent methanol:water:acetic acid (65:35:0.06 v/v), pH 5.3. Comparisons with other packing materials and solvent systems are described. The method could be used to identify lipoxygenase products released from mouse macrophage cells stimulated with gamma-hexachlorocyclohexane. Detection limits between 1 and 10 ng were obtained.

Development of an Exhaled Breath Monitoring System with Semiconductive Gas Sensors, a Gas Condenser Unit, and Gas Chromatograph Columns

PubMed Central

Itoh, Toshio; Miwa, Toshio; Tsuruta, Akihiro; Akamatsu, Takafumi; Izu, Noriya; Shin, Woosuck; Park, Jangchul; Hida, Toyoaki; Eda, Takeshi; Setoguchi, Yasuhiro

2016-01-01

Various volatile organic compounds (VOCs) in breath exhaled by patients with lung cancer, healthy controls, and patients with lung cancer who underwent surgery for resection of cancer were analyzed by gas condenser-equipped gas chromatography-mass spectrometry (GC/MS) for development of an exhaled breath monitoring prototype system involving metal oxide gas sensors, a gas condenser, and gas chromatography columns. The gas condenser-GC/MS analysis identified concentrations of 56 VOCs in the breath exhaled by the test population of 136 volunteers (107 patients with lung cancer and 29 controls), and selected four target VOCs, nonanal, acetoin, acetic acid, and propanoic acid, for use with the condenser, GC, and sensor-type prototype system. The prototype system analyzed exhaled breath samples from 101 volunteers (74 patients with lung cancer and 27 controls). The prototype system exhibited a level of performance similar to that of the gas condenser-GC/MS system for breath analysis. PMID:27834896

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.

Mobility of engineered inorganic nanoparticles in porous media

NASA Astrophysics Data System (ADS)

Metreveli, George; Heidmann, Ilona; Schaumann, Gabriele Ellen

2013-04-01

Besides the excellent properties and great potential for various industrial, medical, pharmaceutical, cosmetic, and life science applications, engineered inorganic nanoparticles (EINP) can show also disadvantages concerning increasing risk potential with increasing application, if they are released in the environmental systems. EINP can influence microbial activity and can show toxic effects (Fabrega et al., 2009). Similar to the inorganic natural colloids, EINP can be transported in soil and groundwater systems (Metreveli et al., 2005). Furthermore, due to the large surface area and high sorption and complex formation capacity, EINP can facilitate transport of different contaminants. In this study the mobility behaviour of EINP and their effect on the transport of different metal(loid) species in water saturated porous media was investigated. For these experiments laboratory column system was used. The column was filled with quartz sand. The interactions between EINP and metal(loid)s were characterised by coupling of asymmetrical flow field flow fractionation (AF4) with inductively coupled plasma mass spectrometer (ICP-MS). As EINP laponite (synthetic three layer clay mineral), and as metal(loid)s Cu, Pb, Zn, Pt and As were used. In AF4 experiments sorption of metal(loid)s on the surface of EINP could be observed. The extent of interactions was influenced by pH value and was different for different metal(loid)s. Laboratory column experiments showed high mobility of EINP, which facilitated transport of most of metal(loid)s in water saturated porous media. Furthermore the migration of synthetic silver nanoparticles in natural soil columns was determined in leaching experiments. Acknowledgement Financial support by German Research Council (DFG) and Max-Buchner-Research Foundation (MBFSt) is gratefully acknowledged. We thank Karlsruhe Institute of Technology (KIT) for the opportunity to perform the column and AF4 experiments. References: Fabrega, J., Fawcett, S. R., Renshaw, J. C. Lead, J. R. 2009. Silver nanoparticle impact on bacterial growth: Effect of pH, concentration, and organic matter. Environ. Sci. Technol. 43 (19): 7285-7290 Metreveli, G., Kaulisch, E.-M., Frimmel, F. H. 2005. Coupling of a column system with ICP-MS for the characterisation of colloid mediated metal(loid) transport in porous media. Acta Hydrochim. Hydrobiol. 33 (4): 337-345

Development of Hplc Techniques for the Analysis of Trace Metal Species in the Primary Coolant of a Pressurised Water Reactor.

NASA Astrophysics Data System (ADS)

Barron, Keiron Robert Philip

Available from UMI in association with The British Library. The need to monitor corrosion products in the primary circuit of a pressurised water reactor (PWR), at a concentration of 10pg ml^{-1} is discussed. A review of trace and ultra-trace metal analysis, relevant to the specific requirements imposed by primary coolant chemistry, indicated that high performance liquid chromatography (HPLC), coupled with preconcentration of sample was an ideal technique. A HPLC system was developed to determine trace metal species in simulated PWR primary coolant. In order to achieve the desired detection limit an on-line preconcentration system had to be developed. Separations were performed on Aminex A9 and Benson BC-X10 analytical columns. Detection was by post column reaction with Eriochrome Black T and Calmagite Linear calibrations of 2.5-100ng of cobalt (the main species of interest), were achieved using up to 200ml samples. The detection limit for a 200ml sample was 10pg ml^{-1}. In order to achieve the desired aim of on-line collection of species at 300^circ C, the use of inorganic ion-exchangers is essential. A novel application, utilising the attractive features of the inorganic ion-exchangers titanium dioxide, zirconium dioxide, zirconium arsenophosphate and pore controlled glass beads, was developed for the preconcentration of trace metal species at temperature and pressure. The performance of these exchangers, at ambient and 300^ circC was assessed by their inclusion in the developed analytical system and by the use of radioisotopes. The particular emphasis during the development has been upon accuracy, reproducibility of recovery, stability of reagents and system contamination, studied by the use of radioisotopes and response to post column reagents. This study in conjunction with work carried out at Winfrith, resulted in a monitoring system that could follow changes in coolant chemistry, on deposition and release of metal species in simulated PWR water loops. On -line detection of cobalt at 11pg ml^{ -1} was recorded, something which previously could not be performed by other techniques.

Theoretical modelling and optimization of bubble column dehumidifier for a solar driven humidification-dehumidification system

NASA Astrophysics Data System (ADS)

Ranjitha, P. Raj; Ratheesh, R.; Jayakumar, J. S.; Balakrishnan, Shankar

2018-02-01

Availability and utilization of energy and water are the top most global challenges being faced by the new millennium. At the present state water scarcity has become a global as well as a regional challenge. 40 % of world population faces water shortage. Challenge of water scarcity can be tackled only with increase in water supply beyond what is obtained from hydrological cycle. This can be achieved either by desalinating the sea water or by reusing the waste water. High energy requirement need to be overcome for either of the two processes. Of many desalination technologies, humidification dehumidification (HDH) technology powered by solar energy is widely accepted for small scale production. Detailed optimization studies on system have the potential to effectively utilize the solar energy for brackish water desalination. Dehumidification technology, specifically, require further study because the dehumidifier effectiveness control the energetic performance of the entire HDH system. The reason attributes to the high resistance involved to diffuse dilute vapor through air in a dehumidifier. The present work intends to optimize the design of a bubble column dehumidifier for a solar energy driven desalination process. Optimization is carried out using Matlab simulation. Design process will identify the unique needs of a bubble column dehumidifier in HDH system.

Optimising resolution for a preparative separation of Chinese herbal medicine using a surrogate model sample system.

PubMed

Ye, Haoyu; Ignatova, Svetlana; Peng, Aihua; Chen, Lijuan; Sutherland, Ian

2009-06-26

This paper builds on previous modelling research with short single layer columns to develop rapid methods for optimising high-performance counter-current chromatography at constant stationary phase retention. Benzyl alcohol and p-cresol are used as model compounds to rapidly optimise first flow and then rotational speed operating conditions at a preparative scale with long columns for a given phase system using a Dynamic Extractions Midi-DE centrifuge. The transfer to a high value extract such as the crude ethanol extract of Chinese herbal medicine Millettia pachycarpa Benth. is then demonstrated and validated using the same phase system. The results show that constant stationary phase modelling of flow and speed with long multilayer columns works well as a cheap, quick and effective method of optimising operating conditions for the chosen phase system-hexane-ethyl acetate-methanol-water (1:0.8:1:0.6, v/v). Optimum conditions for resolution were a flow of 20 ml/min and speed of 1200 rpm, but for throughput were 80 ml/min at the same speed. The results show that 80 ml/min gave the best throughputs for tephrosin (518 mg/h), pyranoisoflavone (47.2 mg/h) and dehydrodeguelin (10.4 mg/h), whereas for deguelin (100.5 mg/h), the best flow rate was 40 ml/min.

A Comparative Study of Alternative Controls and Displays for by the Severely Physically Handicapped

NASA Technical Reports Server (NTRS)

Williams, D.; Simpson, C.; Barker, M.

1984-01-01

A modification of a row/column scanning system was investigated in order to increase the speed and accuracy with which communication aids can be accessed with one or two switches. A selection algorithm was developed and programmed in BASIC to automatically select individuals with the characteristic difficulty in controlling time dependent control and display systems. Four systems were compared: (1) row/column directed scan (2 switches); (2) row/column auto scan (1 switch); (3) row auto scan (1 switch); and (4) column auto scan (1 switch). For this sample population, there were no significant differences among systems for scan time to select the correct target. The row/column auto scan system resulted in significantly more errors than any of the other three systems. Thus, the most widely prescribed system for severely physically disabled individuals turns out for this group to have a higher error rate and no faster communication rate than three other systems that have been considered inappropriate for this group.

Electrophoretic Separation of Single Particles Using Nanoscale Thermoplastic Columns.

PubMed

Weerakoon-Ratnayake, Kumuditha M; Uba, Franklin I; Oliver-Calixte, Nyoté J; Soper, Steven A

2016-04-05

Phenomena associated with microscale electrophoresis separations cannot, in many cases, be applied to the nanoscale. Thus, understanding the electrophoretic characteristics associated with the nanoscale will help formulate relevant strategies that can optimize the performance of separations carried out on columns with at least one dimension below 150 nm. Electric double layer (EDL) overlap, diffusion, and adsorption/desorption properties and/or dielectrophoretic effects giving rise to stick/slip motion are some of the processes that can play a role in determining the efficiency of nanoscale electrophoretic separations. We investigated the performance characteristics of electrophoretic separations carried out in nanoslits fabricated in poly(methyl methacrylate), PMMA, devices. Silver nanoparticles (AgNPs) were used as the model system with tracking of their transport via dark field microscopy and localized surface plasmon resonance. AgNPs capped with citrate groups and the negatively charged PMMA walls (induced by O2 plasma modification of the nanoslit walls) enabled separations that were not apparent when these particles were electrophoresed in microscale columns. The separation of AgNPs based on their size without the need for buffer additives using PMMA nanoslit devices is demonstrated herein. Operational parameters such as the electric field strength, nanoslit dimensions, and buffer composition were evaluated as to their effects on the electrophoretic performance, both in terms of efficiency (plate numbers) and resolution. Electrophoretic separations performed at high electric field strengths (>200 V/cm) resulted in higher plate numbers compared to lower fields due to the absence of stick/slip motion at the higher electric field strengths. Indeed, 60 nm AgNPs could be separated from 100 nm particles in free solution using nanoscale electrophoresis with 100 μm long columns.

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.

Extending the limits of operating pressure of narrow-bore column liquid chromatography instrumentation.

PubMed

Pauw, Ruben De; Degreef, Bart; Ritchie, Harald; Eeltink, Sebastiaan; Desmet, Gert; Broeckhoven, Ken

2014-06-20

The increase of the operating pressure in Liquid Chromatography, has been one of the crucial steps toward faster and more efficient separations. In the present contribution, it was investigated if the pressure limits for narrow-bore columns (2.1mm ID) could be increased beyond those of commercially available (1300bar) instrumentation without performance loss. Whereas previous studies applying pressures higher than 2000bar were limited to the use of columns with a diameter smaller or equal to 1mm, it is a difficult feat to expand this to 2.1mm ID given that viscous-heating effects increase according to the fifth power of the column radius. A prototype LC set-up was realized, allowing to operate at pressures up to 2600bar (260MPa) for large separation volumes (>5mL). The performance of an in-house-built injector was compared at 800bar to commercially available injectors, yielding equal performance but twice the maximum pressure rating. The performance of (coupled) custom columns packed with fully porous and superficially porous particles were assessed at ultra-high-pressure conditions. Increasing the inlet pressure from 800 to 2400bar and scaling the column length proportionally (from 150mm to 450mm), resulted in the theoretically expected linear increase in plate count from 20,000 to 59,000. A maximum plate number of 81,000 was realized using a 600mm long (coupled) column at 2600bar. Viscous-heating effects were diminished by insulating coupled columns and applying an intermediate-cooling strategy in a forced-air oven. Copyright © 2014 Elsevier B.V. All rights reserved.

An on-line coupling of nanofibrous extraction with column-switching high performance liquid chromatography - A case study on the determination of bisphenol A in environmental water samples.

PubMed

Háková, Martina; Chocholoušová Havlíková, Lucie; Chvojka, Jiří; Solich, Petr; Šatínský, Dalibor

2018-02-01

Polyamide 6 nanofiber polymers were used as modern sorbents for on-line solid phase extraction (SPE) coupled with liquid chromatography. The on-line SPE system was tested for the determination of bisphenol A in river water samples. Polyamide nanofibers were prepared using needleless electrospinning, inserted into a mini-column cartridge (5 × 4.6mm) and coupled with HPLC. The effect of column packing and the amount of polyamide 6 on extraction efficiency was tested and the packing process was optimized. The proposed method was performed using a 50-µL sample injection followed by an on-line nanofibrous extraction procedure. The influence of the washing mobile phase on the retention of bisphenol A during the extraction procedure was evaluated. Ascentis ® Express C18 (10cm × 4.6mm) core-shell column was used as an analytical column. Fluorescence detection wavelengths (λ ex = 225nm and λ em = 320nm) were used for identification and quantification of Bisphenol A in river waters. The linearity was tested in the range from 2 to 500µgL -1 (using nine calibration points). The limits of detection and quantification were 0.6 and 2µgL -1 , respectively. The developed method was successfully used for the determination of bisphenol A in various samples of river waters in the Czech Republic (The Ohře, Labe, Nisa, Úpa, and Opava Rivers). Copyright © 2017 Elsevier B.V. All rights reserved.

Preparation of quaternary amine monolithic column for strong anion-exchange chromatography and its application to the separation of Enterovirus 71.

PubMed

Gu, Huimin; Yin, Dezhong; Ren, Jie; Zhang, Baoliang; Zhang, Qiuyu

2016-10-15

Large size virion is unable to diffuse into pores of conventional porous chromatography particles. Therefore, separation of virion by conventional column-packing materials is not quite efficient. To solve this problem, a monolithic column with large convective pores and quaternary amine groups was prepared and was applied to separate Enterovirus 71 (EV71, ≈5700-6000kDa). Cross-section, pore structure, hydrodynamic performance, adsorption property and dynamic binding capacity of prepared monolithic column were determined. Double-pore structures, macropore at 2472nm and mesopore at 5-60nm, were formed. The porosity was up to 63.3%, which enable higher permeability and lower back pressure of the monolithic column than commercial UNO™ Q1 column. Based on the breakthrough curves, the loading capacity of bovine serum albumin was calculated to be 42.0mg per column. In addition, prepared quaternary amine monolithic column was proved to be suitable for the separation of protein mixture by strong anion-exchange chromatography. As a practical application, prepared monolith column presents excellent performance to the separation of EV71 from virus-proteins mixture. Copyright © 2016 Elsevier B.V. All rights reserved.

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.

Tungsten-188/carrier-free rhenium-188 perrhenic acid generator system

DOEpatents

Knapp, F.F. Jr.; Lisic, E.C.; Mirzadeh, S.; Callahan, A.P.

1994-01-04

A generator system has been invented for providing a carrier-free radioisotope in the form of an acid comprises a chromatography column in tandem fluid connection with an ion exchange column, the chromatography column containing a charge of a radioactive parent isotope. The chromatography column, charged with a parent isotope, is eluted with an alkali metal salt solution to generate the radioisotope in the form of an intermediate solution, which is passed through the ion-exchange column to convert the radioisotope to a carrier-free acid form. 1 figure.

Parametric Study of Fire Performance of Concrete Filled Hollow Steel Section Columns with Circular and Square Cross-Section

NASA Astrophysics Data System (ADS)

Nurfaidhi Rizalman, Ahmad; Tahir, Ng Seong Yap Mahmood Md; Mohammad, Shahrin

2018-03-01

Concrete filled hollow steel section column have been widely accepted by structural engineers and designers for high rise construction due to the benefits of combining steel and concrete. The advantages of concrete filled hollow steel section column include higher strength, ductility, energy absorption capacity, and good structural fire resistance. In this paper, comparison on the fire performance between circular and square concrete filled hollow steel section column is established. A three-dimensional finite element package, ABAQUS, was used to develop the numerical model to study the temperature development, critical temperature, and fire resistance time of the selected composite columns. Based on the analysis and comparison of typical parameters, the effect of equal cross-sectional size for both steel and concrete, concrete types, and thickness of external protection on temperature distribution and structural fire behaviour of the columns are discussed. The result showed that concrete filled hollow steel section column with circular cross-section generally has higher fire resistance than the square section.

Automated in-line gel filtration for native state mass spectrometry.

PubMed

Waitt, Greg M; Xu, Robert; Wisely, G Bruce; Williams, Jon D

2008-02-01

Characterization of protein-ligand complexes by nondenaturing mass spectrometry provides direct evidence of drug-like molecules binding with potential therapeutic targets. Typically, protein-ligand complexes to be analyzed contain buffer salts, detergents, and other additives to enhance protein solubility, all of which make the sample unable to be analyzed directly by electrospray ionization mass spectrometry. This work describes an in-line gel-filtration method that has been automated and optimized. Automation was achieved using commercial HPLC equipment. Gel column parameters that were optimized include: column dimensions, flow rate, packing material type, particle size, and molecular weight cut-off. Under optimal conditions, desalted protein ions are detected 4 min after injection and the analysis is completed in 20 min. The gel column retains good performance even after >200 injections. A demonstration for using the in-line gel-filtration system is shown for monitoring the exchange of fatty acids from the pocket of a nuclear hormone receptor, peroxisome proliferator activator-delta (PPARdelta) with a tool compound. Additional utilities of in-line gel-filtration mass spectrometry system will also be discussed.

Design and Performance of the Sorbent-Based Atmosphere Revitalization System for Orion

NASA Technical Reports Server (NTRS)

Ritter, James A.; Reynolds, Steven P.; Ebner, Armin D.; Knox, James C.; LeVan, M. Douglas

2007-01-01

Validation and simulations of a real-time dynamic cabin model were conducted on the sorbent-based atmosphere revitalization system for Orion. The dynamic cabin model, which updates the concentration of H2O and CO2 every second during the simulation, was able to predict the steady state model values for H2O and CO2 for long periods of steady metabolic production for a 4-person crew. It also showed similar trends for the exercise periods, where there were quick changes in production rates. Once validated, the cabin model was used to determine the effects of feed flow rate, cabin volume and column volume. A higher feed flow rate reduced the cabin concentrations only slightly over the base case, a larger cabin volume was able to reduce the cabin concentrations even further, and the lower column volume led to much higher cabin concentrations. Finally, the cabin model was used to determine the effect of the amount of silica gel in the column. As the amount increased, the cabin concentration of H2O decreased, but the cabin concentration of CO2 increased.

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.

Optimal performance of single-column chromatography and simulated moving bed processes for the separation of optical isomers

NASA Astrophysics Data System (ADS)

Medi, Bijan; Kazi, Monzure-Khoda; Amanullah, Mohammad

2013-06-01

Chromatography has been established as the method of choice for the separation and purification of optically pure drugs which has a market size of about 250 billion USD. Single column chromatography (SCC) is commonly used in the development and testing phase of drug development while multi-column Simulated Moving Bed (SMB) chromatography is more suitable for large scale production due to its continuous nature. In this study, optimal performance of SCC and SMB processes for the separation of optical isomers under linear and overloaded separation conditions has been investigated. The performance indicators, namely productivity and desorbent requirement have been compared under geometric similarity for the separation of a mixture of guaifenesin, and Tröger's base enantiomers. SCC process has been analyzed under equilibrium assumption i.e., assuming infinite column efficiency, and zero dispersion, and its optimal performance parameters are compared with the optimal prediction of an SMB process by triangle theory. Simulation results obtained using actual experimental data indicate that SCC may compete with SMB in terms of productivity depending on the molecules to be separated. Besides, insights into the process performances in terms of degree of freedom and relationship between the optimal operating point and solubility limit of the optical isomers have been ascertained. This investigation enables appropriate selection of single or multi-column chromatographic processes based on column packing properties and isotherm parameters.

Maximizing performance in supercritical fluid chromatography using low-density mobile phases.

PubMed

Gritti, Fabrice; Fogwill, Michael; Gilar, Martin; Jarrell, Joseph A

2016-10-14

The performance of a 3.0mm×150mm column packed with 1.8μm fully porous HSS-SB-C 18 particles was investigated in supercritical fluid chromatography (SFC) with low-density, highly expansible carbon dioxide. These conditions are selected for the analysis of semi-volatile compounds. Elevated temperatures (>100°C) were then combined with low column back pressures (<100bar). In this work, the inlet temperature of pure carbon dioxide was set at 107°C, the active back pressure regulator (ABPR) pressure was fixed at 100bar, and the flow rate was set at 2.1mL/min at 12°C (liquefied carbon dioxide) and at an inlet column pressure close to 300bar. Nine n-alkylbenzenes (from benzene to octadecylbenzene) were injected under linear (no sample overload) conditions. The severe steepness of the temperature gradients across the column diameter were predicted from a simplified heat transfer model. Such conditions dramatically lower the column performance by affecting the symmetry of the peak shape. In order to cope with this problem, three different approaches were experimentally tested. They include (1) the decoupling and the proper selection of the inlet eluent temperature with respect to the oven temperature, (2) the partial thermal insulation of the column using polyethylene aerogel, and (3) the application of a high vacuum (10 -5 Torr provided by a turbo-molecular pump) in a housing chamber surrounding the whole column body. The results reveal that (1) the column efficiency can be maximized by properly selecting the difference between the eluent and the oven temperatures, (2) the mere wrapping of the column with an excellent insulating material is insufficient to fully eliminate heat exchanges by conduction and the undesirable radial density gradients across the column i.d., and (3) the complete thermal insulation of the SFC column under high vacuum allows to maximize the column efficiency by maintaining the integrity of the peak shape. Copyright © 2016 Elsevier B.V. All rights reserved.

Design concept of a cryogenic distillation column cascade for a ITER scale fusion reactor

NASA Astrophysics Data System (ADS)

Yamanishi, Toshihiko; Enoeda, Mikio; Okuno, Kenji

1994-07-01

A column cascade has been proposed for the fuel cycle of a ITER scale fusion reactor. The proposed cascade consists of three columns and has significant features: either top or bottom product is prior to the other for each column; it is avoided to withdraw side streams as products or feeds of down stream columns; and there is no recycle steam between the columns. In addition, the product purity of the cascade can be maintained against the changes of flow rates and compositions of feed streams just by adjusting the top and bottom flow rates. The control system has been designed for each column in the cascade. A key component in the prior product stream was selected, and the analysis method of this key component was proposed. The designed control system never brings instability as long as the concentration of the key component is measured with negligible time lag. The time lag for the measurement considerably affects the stability of the control system. A significant conclusion by the simulation in this work is that permissible time for the measurement is about 0.5 hour to obtain stable control. Hence, the analysis system using the gas chromatography is valid for control of the columns.

Active buckling control of a beam-column with circular cross-section using piezo-elastic supports and integral LQR control

NASA Astrophysics Data System (ADS)

Schaeffner, Maximilian; Götz, Benedict; Platz, Roland

2016-06-01

Buckling of slender beam-columns subject to axial compressive loads represents a critical design constraint for light-weight structures. Active buckling control provides a possibility to stabilize slender beam-columns by active lateral forces or bending moments. In this paper, the potential of active buckling control of an axially loaded beam-column with circular solid cross-section by piezo-elastic supports is investigated experimentally. In the piezo-elastic supports, lateral forces of piezoelectric stack actuators are transformed into bending moments acting in arbitrary directions at the beam-column ends. A mathematical model of the axially loaded beam-column is derived to design an integral linear quadratic regulator (LQR) that stabilizes the system. The effectiveness of the stabilization concept is investigated in an experimental test setup and compared with the uncontrolled system. With the proposed active buckling control it is possible to stabilize the beam-column in arbitrary lateral direction for axial loads up to the theoretical critical buckling load of the system.

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.

Automated protein hydrolysis delivering sample to a solid acid catalyst for amino acid analysis.

PubMed

Masuda, Akiko; Dohmae, Naoshi

2010-11-01

In this study, we developed an automatic protein hydrolysis system using strong cation-exchange resins as solid acid catalysts. Examining several kinds of inorganic solid acids and cation-exchange resins, we found that a few cation-exchange resins worked as acid catalysts for protein hydrolysis when heated in the presence of water. The most efficient resin yielded amounts of amino acids that were over 70% of those recovered after conventional hydrolysis with hydrochloric acid and resulted in amino acid compositions matching the theoretical values. The solid-acid hydrolysis was automated by packing the resin into columns, combining the columns with a high-performance liquid chromatography system, and heating them. The amino acids that constitute a protein can thereby be determined, minimizing contamination from the environment.

Quantitative determination of p-aminosalicylic acid and its degradation product m-aminophenol in pellets by ion-pair high-performance liquid chromatography applying the monolithic Chromolith Speedrod RP-18e column.

PubMed

Vasbinder, E; Van der Weken, G; Vander Heyden, Y; Baeyens, W R G; Debunne, A; Remon, J P; García-Campaña, A M

2004-01-01

An ion-pair high performance liquid chromatographic method was developed for the simultaneous determination of p-aminosalicylic acid (PAS) and its degradation product m-aminophenol (MAP) in a newly developed multiparticular drug delivery system. Owing to the concentration differences of PAS and MAP, acetanilide and sulfanilic acid were used as internal standards, respectively. The separation was performed on a Chromolith SpeedROD RP-18e column, a new packing material consisting of monolithic rods of highly porous silica. The mobile phase composition was of 20 mm phosphate buffer, 20 mm tetrabutylammonium hydrogen sulphate and 16% (v/v) methanol adjusted to pH 6.8, at a flow-rate of 1.0 mL/min, resulting in a run-time of about 6 min. Detection was by UV at 233 nm. The method was validated and proved to be useful for stability testing of the new dosage form. Separation efficiency was compared between the new packing material Chromolith SpeedROD RP-18e and the conventional reversed-phase cartridge LiChroCART 125-4 (5 microm). A robustness test was carried out on both columns and different separation parameters (retention, resolution, run time, temperature) were determined. Copyright 2004 John Wiley & Sons, Ltd.

The importance of system band broadening in modern size exclusion chromatography.

PubMed

Goyon, Alexandre; Guillarme, Davy; Fekete, Szabolcs

2017-02-20

In the last few years, highly efficient UHP-SEC columns packed with sub-3μm particles were commercialized by several providers. Besides the particle size reduction, the dimensions of modern SEC stationary phases (150×4.6mm) was also modified compared to regular SEC columns (300×6 or 300×8mm). Because the analytes are excluded from the pores in SEC, the retention factors are very low, ranging from -1

Rapid determination of five antibiotic residues in swine wastewater by online solid-phase extraction-high performance liquid chromatography-tandem mass spectrometry.

PubMed

Tagiri-Endo, Misako; Suzuki, Shigeru; Nakamura, Tomoyuki; Hatakeyama, Takashi; Kawamukai, Kazuo

2009-02-01

A simple and quick online solid-phase extraction (SPE) coupled to liquid chromatography (LC)/tandem mass spectrometry (MS/MS) for the determination of the five antibiotics (florfenicol, FF; lincomycin, LCM; oxytetracyclin, OTC; tylosin, TS; valnemulin, VLM) in swine wastewater has been developed. After filtration, aliquots (100 microl) of wastewater samples were directly injected to a column-switching LC system. Some matrix interference was removed by washing up SPE column with 0.2% formic acid solution and acetonitrile. Antibiotics eluted from SPE column were separated on analytical column by converting switching valve and were detected by MS/MS. Calibration curves using the method of standard addition had very good correlation coefficients (r > 0.99) in the range of 0.1 to 2 ng/ml. The intra-day precision of the method was less than 12% and the inter-day precision was between 6 to 17%. The detection limits were 0.01-0.1 ng/ml. When this method was applied to wastewater samples in swine facilities, four compounds (LCM, OTC, TS, and VLM) were detected.

Polyether ether ketone encased monolith frits made of polyether ether ketone tubing with a 0.25 mm opening resulting in an improved separation performance in liquid chromatography.

PubMed

Park, Sin Young; Cheong, Won Jo

2016-05-01

Tiny polyether ether ketone encased monolith frits have been prepared by modified catalytic sulfonation of the inner surface of polyether ether tubing (1.6 mm od, 0.25 mm id) followed by modified formation of organic monolith and cutting of the tubing into slices. The frit was placed below the central hole of the column outlet union and supported by a combination of a silica capillary (0.365 mm od, 0.05 mm id) and a polyether ether ketone sleeve (1.6 mm od, 0.38 mm id) tightened with a nut and a ferrule when the column was packed to prevent sinking of the frit element into the union hole (0.25 mm opening) otherwise. The column packed this way with the frits investigated in this study has shown better separation performance owing to the reduced frit volume in comparison to the column packed with a commercial stainless-steel screen frit. This study establishes the strategy of disposable microcolumns in which cheap disposable frits are used whenever the column is re-packed to yield columns of even better chromatographic performance than the columns with commercial frits. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Increasing phytoplankton-available phosphorus and inhibition of macrophyte on phytoplankton bloom.

PubMed

Dai, Yanran; Wu, Juan; Ma, Xiaohang; Zhong, Fei; Cui, Naxin; Cheng, Shuiping

2017-02-01

We assembled mesocosms to address the coherent mechanisms that an increasing phosphorus (P) concentration in water columns coupled with the phytoplankton bloom and identify the performance gap of regulating phytoplankton growth between two macrophyte species, Ceratophyllum demersum L. and Vallisneria spiralis L. Intense alkaline phosphatase activities (APA) were observed in the unplanted control, with their predominant part, phytoplankton APA (accounting for up to 44.7% of the total APA), and another large share, bacterial APA. These correspond with the large average concentration of total phosphorus (TP), total dissolved phosphorus (TDP) and soluble reactive (SRP) as well as high phytoplankton density in the water column. The consistency among P concentrations, phytoplankton density and APA, together with the positive impact of phytoplankton density on total APA revealed by the structural equation modelling (SEM), indicates that facilitated APA levels in water is an essential strategy for phytoplankton to enhance the available P. Furthermore, a positive interaction between phytoplankton APA and bacteria APA was detected, suggesting a potential collaboration between phytoplankton and bacteria to boost available P content in the water column. Both macrophyte species had a prominent performance on regulating phytoplankton proliferation. The phytoplankton density and quantum yield in C. demersum systems were all significantly lower (33.8% and 24.0%) than those in V. spiralis systems. Additionally, a greater decoupling effect of C. demersum on the relationship between P, APA, phytoplankton density, bacteria dynamic and quantum yield was revealed by SEM. These results imply that the preferred tactic of different species could lead to the performance gap. Copyright © 2016 Elsevier B.V. All rights reserved.

Determination of josamycin residues in porcine tissues using high-performance liquid chromatography with pre-column derivatization and spectrofluorimetric detection.

PubMed

Leroy, P; Decolin, D; Nicolas, A; Archimbault, P

1994-12-01

A simple, selective and sensitive high-performance liquid chromatographic (HPLC) method has been developed for the measurement of josamycin residues in four porcine tissues (i.e., muscle, liver, kidney and fat). The sample preparation consisted of a homogenization step in an acetonitrile-10 mmol l-1 phosphate buffer mixture, pH 6.0 (35 + 65), centrifugation and a liquid-liquid extractive clean-up of the resulting supernatant with isooctane. Pre-column derivatization of josamycin was performed using cyclohexa-1,3-dione in ammonium acetate buffer, pH 5.0 (90 degrees C for 2 h). The derivative was chromatographed in an isocratic reversed-phase HPLC system. A LiChrospher RP 18 end-capped (5 microns) column was eluted with an acetonitrile-methanol-10 mmol l-1 phosphate buffer mixture, pH 6.0 (45 + 5 + 50). The capacity factor of the josamycin derivative was 17.5. Detection was achieved using spectrofluorimetry (lambda ex = 375 nm; lambda em = 450 nm). The structure of the derivative was assessed by using mass spectrometry. Full selectivity was obtained in the HPLC system versus other macrolide antibiotics (tylosin, spiramycin and erythromycin), aldehydes (formaldehyde, acetaldehyde and benzaldehyde) and endogenous compounds. Linearity and repeatability were tested. Correlation coefficients, for calibration curves in the range of 0.1-3.2 micrograms g-1, were greater than 0.999 for all tissues and the relative standard deviation (S(r)) was 4.9% (1.6 micrograms g-1; n = 6); recovery was higher than 88%.

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%.

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.

Analysis on the optical aberration effect on spectral resolution of coded aperture spectroscopy

NASA Astrophysics Data System (ADS)

Hao, Peng; Chi, Mingbo; Wu, Yihui

2017-10-01

The coded aperture spectrometer can achieve high throughput and high spectral resolution by replacing the traditional single slit with two-dimensional array slits manufactured by MEMS technology. However, the sampling accuracy of coding spectrum image will be distorted due to the existence of system aberrations, machining error, fixing errors and so on, resulting in the declined spectral resolution. The influence factor of the spectral resolution come from the decode error, the spectral resolution of each column, and the column spectrum offset correction. For the Czerny-Turner spectrometer, the spectral resolution of each column most depend on the astigmatism, in this coded aperture spectroscopy, the uncorrected astigmatism does result in degraded performance. Some methods must be used to reduce or remove the limiting astigmatism. The curvature of field and the spectral curvature can be result in the spectrum revision errors.

Characterizing pressure issues due to turbulent flow in tubing, in ultra-fast chiral supercritical fluid chromatography at up to 580bar.

PubMed

Berger, Terry A

2016-12-02

It has been widely suggested that the outlet pressure be changed to maintain constant density ("isopycnic" conditions) when comparing the kinetic performance of different columns in supercritical fluid chromatography (SFC). However, at high flow rates, flow in the tubing is turbulent, causing large extra-column pressure drops that limit options for changing outlet pressure. Some of these pressure drops occur before and some after the column, obscuring the actual column inlet and outlet pressures. In this work, a 4.6×100mm, 1.8μm R,R-Whelk-O1 column was used with low dispersion LD (120μm) plumbing to generate sub-1min chiral separations. However, the optimum, or near optimum, flow rate was 5mL-min -1 , producing a system pressure of 580bar (with 40% methanol, outlet pressure 120bar). Both the flow rate and pump pressure required were near the limits of the instrument, and significantly exceeded the capability of many other SFC's. Extra-column pressure drops (ΔP ec ) were as high as 200bar, caused mostly by turbulent flow in the tubing. The ΔP ec increased by more than the square of the flow rate. Reynolds Numbers (Re) were calculated for tubing as a function of flow rate between 100 and 400bar and 5-20% methanol in CO 2 , and 40°-60°C. This represents the most extensive analysis of turbulence in tubing in the SFC literature. Flow in 120μm ID tubing was calculated to be laminar below 1.0mL-min -1 , mostly transitional up to 2.5mL-min -1 and virtually always turbulent at 3mL-min -1 and higher. Flow in 170μm tubing is turbulent at lower flows but generates half the ΔP ec due to the lower mobile phase linear velocity. The results suggest that, while sub-minute chromatograms are easily generated, 4.6mm columns are not very user friendly for use with sub-2μm packings. The high flow rates required just to reach optimum result in high ΔP ec generated by the tubing, causing uncertainty in the true column inlet, outlet, and average column pressure/density. When comparing kinetic performance of columns with different dimensions, the pressure drops in the tubing must be considered. Copyright © 2016 Elsevier B.V. All rights reserved.

Tuning preparation conditions towards optimized separation performance of thermally polymerized organo-silica monolithic columns in capillary liquid chromatography.

PubMed

Gharbharan, Deepa; Britsch, Denae; Soto, Gabriela; Weed, Anna-Marie Karen; Svec, Frantisek; Zajickova, Zuzana

2015-08-21

Tuning of preparation conditions, such as variations in the amount of a porogen, concentration of an aqueous acid catalyst, and adjustment in polymerization temperature and time, towards optimized chromatographic performance of thermally polymerized monolithic capillaries prepared from 3-(methacryloyloxy)propyltrimethoxysilane has been carried out. Performance of capillary columns in reversed-phase liquid chromatography was assessed utilizing various sets of solutes. Results describing hydrophobicity, steric selectivity, and extent of hydrogen bonding enabled comparison of performance of hybrid monolithic columns prepared under thermal (TSG) and photopolymerized (PSG) conditions. Reduced amounts of porogen in the polymerization mixture, and prolonged reaction times were necessary for the preparation of monolithic columns with enhanced retention and column efficiency that reached to 111,000 plates/m for alkylbenzenes with shorter alkyl chains. Both increased concentration of catalyst and higher temperature resulted in faster polymerization but inevitably in insufficient time for pore formation. Thermally polymerized monoliths produced surfaces, which were slightly more hydrophobic (a methylene selectivity of 1.28±0.002 TSG vs 1.20±0.002 PSG), with reduced number of residual silanols (a caffeine/phenol selectivity of 0.13±0.001 TSG vs 0.17±0.003 PSG). However, steric selectivity of 1.70±0.01 was the same for both types of columns. The batch-to-batch repeatability was better using thermal initiation compared to monolithic columns prepared under photopolymerized conditions. RSD for retention factor of benzene was 3.7% for TSG capillaries (n=42) vs. 6.6% for PSG capillaries (n=18). A similar trend was observed for columns prepared within the same batch. Copyright © 2015 Elsevier B.V. All rights reserved.

Zero-valent iron/biotic treatment system for perchlorate-contaminated water: lab-scale performance, modeling, and full-scale implications

EPA Science Inventory

The computer program AQUASIM was used to model biological treatment of perchlorate-contaminated water using zero-valent iron corrosion as the hydrogen gas source. The laboratory-scale column was seeded with an autohydrogenotrophic microbial consortium previously shown to degrade ...

SCALE-UP OF RAPID SMALL-SCALE ADSORPTION TESTS TO FIELD-SCALE ADSORBERS: THEORETICAL AND EXPERIMENTAL BASIS

EPA Science Inventory

Design of full-scale adsorption systems typically includes expensive and time-consuming pilot studies to simulate full-scale adsorber performance. Accordingly, the rapid small-scale column test (RSSCT) was developed and evaluated experimentally. The RSSCT can simulate months of f...

Column dynamic studies and breakthrough curve analysis for Cd(II) and Cu(II) ions adsorption onto palm oil boiler mill fly ash (POFA).

PubMed

Aziz, Abdul Shukor Abdul; Manaf, Latifah Abd; Man, Hasfalina Che; Kumar, Nadavala Siva

2014-01-01

This paper investigates the adsorption characteristics of palm oil boiler mill fly ash (POFA) derived from an agricultural waste material in removing Cd(II) and Cu(II) from aqueous solution via column studies. The performance of the study is described through the breakthrough curves concept under relevant operating conditions such as column bed depths (1, 1.5, and 2 cm) and influent metal concentrations (5, 10, and 20 mg/L). The Cd(II) and Cu(II) uptake mechanism is particularly bed depth- and concentration-dependant, favoring higher bed depth and lower influent metal concentration. The highest bed capacity of 34.91 mg Cd(II)/g and 21.93 mg Cu(II)/g of POFA was achieved at 20 mg/L of influent metal concentrations, column bed depth of 2 cm, and flow rate of 5 mL/min. The whole breakthrough curve simulation for both metal ions were best described using the Thomas and Yoon–Nelson models, but it is apparent that the initial region of the breakthrough for Cd(II) was better described using the BDST model. The results illustrate that POFA could be utilized effectively for the removal of Cd(II) and Cu(II) ions from aqueous solution in a fixed-bed column system.

Tube and column agglutination technology for autocontrol testing.

PubMed

Courtney, J E; Vincent, J L; Indrikovs, A J

2001-01-01

The incidence of positive autocontrol test results with column agglutination technology is a concern. This study investigates the incidence and significance of positive autocontrols in the ID Micro Typing System (gel) and the Gamma ReACT (ReACT). The study encompassed a total of 1021 randomly selected samples from patients and 95 samples from donors collected during 1 month. The autocontrol testing was carried out according to the manufacturer's instructions for the column agglutination tests. The tube method was carried out using low-ionic-strength solution (LISS). The direct antiglobulin test (DAT) was performed using the tube method, and further investigated with elution studies if warranted. Seventy-nine patient's samples (7.74%) had a positive autocontrol: the gel test, 72 (91.13%); ReACT, 21 (26.58%); and the tube method, 27 (34.18%). Of the 79 positive autocontrols, 44 samples had a negative DAT. Of the samples with positive DAT results, only one possessed a clinically significant antibody, anti-D. Moreover, the same sample also tested positive in all three methods. Column agglutination techniques have increased sensitivity for a positive autocontrol beyond the conventional tube method. However, ReACT and gel tests differ significantly in their frequency of positives. Investigation of the significance of a positive autocontrol in column agglutination technology when the conventional tube method is also positive is suggested.

High-performance liquid chromatography coupled with post-column dual-bioactivity assay for simultaneous screening of xanthine oxidase inhibitors and free radical scavengers from complex mixture.

PubMed

Li, D Q; Zhao, J; Li, S P

2014-06-06

Xanthine oxidase (XO) can catalyze hypoxanthine and xanthine to generate uric acid and reactive oxygen species (ROS), including superoxide anion radical (O₂(•-)) and hydrogen peroxide. XO inhibitors and free radical scavengers are beneficial to the treatment of gout and many related diseases. In the present study, an on-line high-performance liquid chromatography (HPLC) coupled with post-column dual-bioactivity assay was established and successfully applied to simultaneously screening of XO inhibitors and free radical scavengers from a complex mixture, Oroxylum indicum extract. The integrated system of HPLC separation, bioactivity screening and mass spectrometry identification was proved to be simple and effective for rapid and sensitive screening of individual bioactive compounds in complex mixtures. Copyright © 2014 Elsevier B.V. All rights reserved.

Separation of amino acids and antibiotics by narrow-bore and normal-bore high-performance liquid chromatography with pre-column derivatization.

PubMed

Fiedler, H P; Plaga, A

1987-01-16

The selectivity, efficiency and lifetime of normal- and narrow-bore columns for high-performance liquid chromatography were investigated for the separation and quantification of amino acids and the amino acid-like antibiotics phosphinothricin and phosphinothricylalanylalanine in biological samples. These compounds were determined by an automated pre-column derivatization with o-phthalaldehyde-2-mercaptoethanol reagent and UV detection at 338 nm.

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

[Synchronous extraction and determination of phenoxy acid herbicides in water by on-line monolithic solid phase microextraction-high performance liquid chromatography].

PubMed

Wang, Jiabin; Wu, Fangling; Zhao, Qi

2015-08-01

A C18 monolithic capillary column was utilized as the solid phase microextraction column to construct an in-tube SPME-HPLC system which was used to simultaneously extract and detect five phenoxy acid herbicides, including 2,4-dichlorophenoxyacetic acid (2,4-D), 2- (2-chloro)-phenoxy propionic acid (2,2-CPPA), 2-(3-chloro)-phenoxy propionic acid (2,3- CPPA), phenoxy propionic acid (PPA) and 2-(2,4-dichlorophenoxy) propionic acid (2,4-DP). The operating parameters of the in-tube SPME-HPLC system, including the length of the monolithic column, the sampling flow rate, the sampling time, the elution flow rate and the elution time, had been investigated in detail. The optimized operating parameters of the in-tube SPME-HPLC system were as follow: the length of the monolithic column was 20 cm, the sampling flow rate was 0. 04 mL/min, sampling time was 13 min; the elution flow rate was 0.02 mL/min, elution time was 5 min. Under the optimized conditions, the detection limits of the five phenoxy acid herbicides were as follows: 9 µg/L for PPA, 4 µg/L for 2,2-CPPA, 4 µg/L for 2,3-CPPA, 5 µg/L for 2,4-D, 5 µg/L for 2,4-DP. Compared with the HPLC method with direct injection, the combined system showed a good enrichment factors to the analytes. The recoveries of the five phenoxy acid herbicides were between 79.0% and 98.0% (RSD ≤ 3.9%). This method was successfully used to detect the five phenoxy acid herbicides in water samples with satisfactory results.

An Engineering Evaluation of Spherical Resorcinol Formaldehyde Resin

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

Birdwell Jr, Joseph F; Lee, Denise L; Taylor, Paul Allen

2010-09-01

A small column ion exchange (SCIX) system has been proposed for removal of cesium from caustic, supernatant, and dissolved salt solutions stored or generated from high-level tank wastes at the US Department of Energy (DOE) Hanford Site and Savannah River Sites. In both instances, deployment of SCIX systems, either in-tank or near-tank, is a means of expediting waste pretreatment and dispositioning with minimal or no new infrastructure requirements. Conceptually, the treatment approach can utilize a range of ion exchange media. Previously, both crystalline silicotitanate (CST), an inorganic, nonelutable sorbent, and resorcinol-formaldehyde (RF), an organic, elutable resin, have been considered formore » cesium removal from tank waste. More recently, Pacific Northwest National Laboratory (PNNL) evaluated use of SuperLig{reg_sign} 644, an elutable ion exchange medium, for the subject application. Results of testing indicate hydraulic limitations of the SuperLig{reg_sign} resin, specifically a high pressure drop through packed ion exchange columns. This limitation is likely the result of swelling and shrinkage of the irregularly shaped (granular) resin during repeated conversions between sodium and hydrogen forms as the resin is first loaded then eluted. It is anticipated that a similar flow limitation would exist in columns packed with conventional, granular RF resin. However, use of spherical RF resin is a likely means of mitigating processing limitations due to excessive pressure drop. Although size changes occur as the spherical resin is cycled through loading and elution operations, the geometry of the resin is expected to effectively mitigate the close packing that leads to high pressure drops across ion exchange columns. Multiple evaluations have been performed to determine the feasibility of using spherical RF resin and to obtain data necessary for design of an SCIX process. The work performed consisted of examination of radiation effects on resin performance, quantification of cesium adsorption performance as a function of operating temperature and pH, and evaluation of sodium uptake (titration) as function of pH and counteranion concentration. The results of these efforts are presented in this report. Hydraulic performance of the resin and the use of eluant alternatives to nitric acid have also been evaluated and have been reported elsewhere (Taylor 2009, Taylor and Johnson 2009).« less

Numerical analysis of dynamic behavior of pre-stressed shape memory alloy concrete beam-column joints

NASA Astrophysics Data System (ADS)

Yan, S.; Xiao, Z. F.; Lin, M. Y.; Niu, J.

2018-04-01

Beam-column joints are important parts of a main frame structure. Mechanical properties of beam-column joints have a great influence on dynamic performances of the frame structure. Shape memory alloy (SMA) as a new type of intelligent metal materials has wide applications in civil engineering. The paper aims at proposing a novel beam-column joint reinforced with pre-stressed SMA tendons to increase its dynamic performance. Based on the finite element analysis (FEA) software ABAQUS, a numerical simulation for 6 beam-column scaled models considering different SMA reinforcement ratios and pre-stress levels was performed, focusing on bearing capacities, energy-dissipation and self-centering capacities, etc. These models were numerically tested under a pseudo-static load on the beam end, companying a constant vertical compressive load on the top of the column. The numerical results show that the proposed SMA-reinforced joint has a significantly increased bearing capacity and a good self-centering capability after unloading even though the energy-dissipation capacity becomes smaller due the less residual deformation. The concept and mechanism of the novel joint can be used as an important reference for civil engineering applications.

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.

Tunnel frit: a nonmetallic in-capillary frit for nanoflow ultra high-performance liquid chromatography-mass spectrometryapplications.

PubMed

Chen, Chao-Jung; Chen, Wei-Yun; Tseng, Mei-Chun; Chen, Yet-Ran

2012-01-03

In this study, an easy method to fabricate a durable in-capillary frit was developed for use in nanoflow liquid chromatography (nanoLC). A small orifice was tunneled into the sol-gel frit during the polymerization process resulting in the simple fabrication of a tunnel frit. A short packing tunnel frit column (2 cm, C(18) particles) was able to sustain over 10,000 psi continuous liquid flow for 10 days without observation of particle loss, and back pressure variation was less than 5%. The tunnel frit was successfully applied to the fabrication of nanoflow ultra high-performance liquid chromatography (nano-UHPLC) trap and analytical columns. In the analysis of tryptic peptides, the tunnel frit trap and analytical columns were demonstrated to have high separation efficiency and sensitivity. In analysis of phosphopeptides, the use of the nonmetallic tunnel frit column showed better sensitivity than the metallic frit column. This design can facilitate the preparation of nano-HPLC and nano-UHPLC columns and the packing material can easily be refilled when the column is severely contaminated or clogged. © 2011 American Chemical Society

Behavior of macroporous vinyl silica and silica monolithic columns in high pressure gas chromatography.

PubMed

Maniquet, Adrien; Bruyer, Nicolas; Raffin, Guy; Baco-Antionali, Franck; Demesmay, Claire; Dugas, Vincent; Randon, Jérôme

2017-06-30

80% vinyltrimethoxysilane-based hybrid silica monoliths (80-VTMS), which have been initially developed for separation in reversed-phase liquid chromatography, have been investigated in high pressure gas chromatography separations (carrier gas pressure up to 60bar) and compared to silica monolithic columns. The behavior of both silica and 80-VTMS monolithic columns was investigated using helium, nitrogen and carbon dioxide as carrier gas. The efficiency of 80-VTMS monolithic columns was shown to vary differently than silica monolithic columns according to the temperature and the carrier gas used. Carrier gas nature was a significant parameter on the retention for both silica and vinyl columns in relation to its adsorption onto the stationary phase in such high pressure conditions. The comparison of retention and selectivity between 80-VTMS monoliths and silica was performed under helium using the logarithm of the retention factor according to the number of carbon atoms combined to Kovats indexes. The very good performances of these columns were demonstrated, allowing the separation of 8 compounds in less than 1min. Copyright © 2017 Elsevier B.V. All rights reserved.

Tuning a Parallel Segmented Flow Column and Enabling Multiplexed Detection.

PubMed

Pravadali-Cekic, Sercan; Kocic, Danijela; Hua, Stanley; Jones, Andrew; Dennis, Gary R; Shalliker, R Andrew

2015-12-15

Active flow technology (AFT) is new form of column technology that was designed to overcome flow heterogeneity to increase separation performance in terms of efficiency and sensitivity and to enable multiplexed detection. This form of AFT uses a parallel segmented flow (PSF) column. A PSF column outlet end-fitting consists of 2 or 4 ports, which can be multiplexed to connect up to 4 detectors. The PSF column not only allows a platform for multiplexed detection but also the combination of both destructive and non-destructive detectors, without additional dead volume tubing, simultaneously. The amount of flow through each port can also be adjusted through pressure management to suit the requirements of a specific detector(s). To achieve multiplexed detection using a PSF column there are a number of parameters which can be controlled to ensure optimal separation performance and quality of results; that is tube dimensions for each port, choice of port for each type of detector and flow adjustment. This protocol is intended to show how to use and tune a PSF column functioning in a multiplexed mode of detection.

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

Rocket-borne observation of singly ionized carbon 158 micron emission from the diffuse interstellar medium

NASA Astrophysics Data System (ADS)

Bock, James Joseph

1994-01-01

We report an observation of 158 micron line emission from singly ionized carbon from the diffuse interstellar medium at high galactic latitude. The integrated line intensity is measured in a 36 arcmin field-of-view along a triangular scan path in a 5 deg x 20 deg region in Ursa Major using a rocket-borne, liquid helium cooled spectrophotometer. The scan includes high latitude infrared cirrus, molecular clouds, a bright external galaxy, M82, and the HI Hole, which is a region of uniquely low neutral hydrogen column density. Emission from (CII) is observed in all regions and, in the absence of appreciable CO emission, is well correlated with neutral hydrogen column density. We observe a (CII) gas cooling rate which varies from (3.25 +/- 0.8 to 1.18 +/- 0.4) x 10-26 ergs-1 H-atom-1, in good agreement with recent observations of UV absorption lines at high galactic latitude. Regions with CO emission have enhanced (CII) line emission over that expected from the correlation with neutral hydrogen column density. The line-to-continuum ratio varies from I(CII)/lambda Ilambda = 0.002 to 0.008 in comparison with the all sky average of 0.0082 reported by FIRAS, which is heavily weighted towards the Galactic plane. The far-infrared continuum intensity, measured at 134 microns, 154 microns, and 186 microns, correlates with the 100 micron brightness measured by IRAS, and in regions excluding molecular clouds, with HI column density. The far-infrared brightness correlated with HI column density is fit by a thermal spectrum with a temperature T = 16.4 (+2.3/-1.8) K assuming an index of emissivity n = 2. The residual brightness after subtracting the emission correlated with neutral hydrogen column density yields an upper limit to the far-infrared extra-galactic background radiation of lambda Ilambda (154 microns) less than 2.6 x 10-12 W cm-2 sr-1. The observation of M82 confirms the laboratory calibration of the instrument. Unique instrumentation was developed to realize the instrument. A high sensitivity detection system consisting of stressed Ge:Ga photoconductors coupled to charge integrating amplifiers is described. We developed a compact, miniature He-4 refrigerator suitable for spaceborne operation. A silicon-gap Fabry-Perot filter, designed for use in high-throughput, compact optical systems, was developed. The performance of a far-infrared low-pass filter stack with high out-of-band rejection is reported. We tested the performance of a telescope baffle system with high-off axis rejection in a combination of ground-based and rocket-borne experiments. A submillimeter-black coating suitable for use in spaceborne telescopes is described. We report the laboratory testing of the instrument and the performance during the flight, and discuss the scientific implications of the observations.

Evaluation of the separation characteristics of application-specific (volatile organic compounds) open-tubular columns for gas chromatography.

PubMed

Poole, Colin F; Qian, Jing; Kiridena, Waruna; Dekay, Colleen; Koziol, Wladyslaw W

2006-11-17

The solvation parameter model is used to characterize the separation characteristics of two application-specific open-tubular columns (Rtx-Volatiles and Rtx-VGC) and a general purpose column for the separation of volatile organic compounds (DB-WAXetr) at five equally spaced temperatures over the range 60-140 degrees C. System constant differences and retention factor correlation plots are then used to determine selectivity differences between the above columns and their closest neighbors in a large database of system constants and retention factors for forty-four open-tubular columns. The Rtx-Volatiles column is shown to have separation characteristics predicted for a poly(dimethyldiphenylsiloxane) stationary phase containing about 16% diphenylsiloxane monomer. The Rtx-VGC column has separation properties similar to the poly(cyanopropylphenyldimethylsiloxane) stationary phase containing 14% cyanopropylphenylsiloxane monomer DB-1701 for non-polar and dipolar/polarizable compounds but significantly different characteristics for the separation of hydrogen-bond acids. For all practical purposes the DB-WAXetr column is shown to be selectivity equivalent to poly(ethylene glycol) columns prepared using different chemistries for bonding and immobilizing the stationary phase. Principal component analysis and cluster analysis are then used to classify the system constants for the above columns and a sub-database of eleven open-tubular columns (DB-1, HP-5, DB-VRX, Rtx-20, DB-35, Rtx-50, Rtx-65, DB-1301, DB-1701, DB-200, and DB-624) commonly used for the separation of volatile organic compounds. A rationale basis for column selection based on differences in intermolecular interactions is presented as an aid to method development for the separation of volatile organic compounds.

Development of an achiral supercritical fluid chromatography method with ultraviolet absorbance and mass spectrometric detection for impurity profiling of drug candidates. Part II. Selection of an orthogonal set of stationary phases.

PubMed

Lemasson, Elise; Bertin, Sophie; Hennig, Philippe; Boiteux, Hélène; Lesellier, Eric; West, Caroline

2015-08-21

Impurity profiling of organic products that are synthesized as possible drug candidates requires complementary analytical methods to ensure that all impurities are identified. Supercritical fluid chromatography (SFC) is a very useful tool to achieve this objective, as an adequate selection of stationary phases can provide orthogonal separations so as to maximize the chances to see all impurities. In this series of papers, we have developed a method for achiral SFC-MS profiling of drug candidates, based on a selection of 160 analytes issued from Servier Research Laboratories. In the first part of this study, focusing on mobile phase selection, a gradient elution with carbon dioxide and methanol comprising 2% water and 20mM ammonium acetate proved to be the best in terms of chromatographic performance, while also providing good MS response [1]. The objective of this second part was the selection of an orthogonal set of ultra-high performance stationary phases, that was carried out in two steps. Firstly, a reduced set of analytes (20) was used to screen 23 columns. The columns selected were all 1.7-2.5μm fully porous or 2.6-2.7μm superficially porous particles, with a variety of stationary phase chemistries. Derringer desirability functions were used to rank the columns according to retention window, column efficiency evaluated with peak width of selected analytes, and the proportion of analytes successfully eluted with good peak shapes. The columns providing the worst performances were thus eliminated and a shorter selection of columns (11) was obtained. Secondly, based on 160 tested analytes, the 11 columns were ranked again. The retention data obtained on these columns were then compared to define a reduced set of the best columns providing the greatest orthogonality, to maximize the chances to see all impurities within a limited number of runs. Two high-performance columns were thus selected: ACQUITY UPC(2) HSS C18 SB and Nucleoshell HILIC. Copyright © 2015 Elsevier B.V. All rights reserved.

High-throughput NGL electron-beam direct-write lithography system

NASA Astrophysics Data System (ADS)

Parker, N. William; Brodie, Alan D.; McCoy, John H.

2000-07-01

Electron beam lithography systems have historically had low throughput. The only practical solution to this limitation is an approach using many beams writing simultaneously. For single-column multi-beam systems, including projection optics (SCALPELR and PREVAIL) and blanked aperture arrays, throughput and resolution are limited by space-charge effects. Multibeam micro-column (one beam per column) systems are limited by the need for low voltage operation, electrical connection density and fabrication complexities. In this paper, we discuss a new multi-beam concept employing multiple columns each with multiple beams to generate a very large total number of parallel writing beams. This overcomes the limitations of space-charge interactions and low voltage operation. We also discuss a rationale leading to the optimum number of columns and beams per column. Using this approach we show how production throughputs >= 60 wafers per hour can be achieved at CDs

Compensated Row-Column Ultrasound Imaging System Using Fisher Tippett Multilayered Conditional Random Field Model

PubMed Central

Ben Daya, Ibrahim; Chen, Albert I. H.; Shafiee, Mohammad Javad; Wong, Alexander; Yeow, John T. W.

2015-01-01

3-D ultrasound imaging offers unique opportunities in the field of non destructive testing that cannot be easily found in A-mode and B-mode images. To acquire a 3-D ultrasound image without a mechanically moving transducer, a 2-D array can be used. The row column technique is preferred over a fully addressed 2-D array as it requires a significantly lower number of interconnections. Recent advances in 3-D row-column ultrasound imaging systems were largely focused on sensor design. However, these imaging systems face three intrinsic challenges that cannot be addressed by improving sensor design alone: speckle noise, sparsity of data in the imaged volume, and the spatially dependent point spread function of the imaging system. In this paper, we propose a compensated row-column ultrasound image reconstruction system using Fisher-Tippett multilayered conditional random field model. Tests carried out on both simulated and real row-column ultrasound images show the effectiveness of our proposed system as opposed to other published systems. Visual assessment of the results show our proposed system’s potential at preserving detail and reducing speckle. Quantitative analysis shows that our proposed system outperforms previously published systems when evaluated with metrics such as Peak Signal to Noise Ratio, Coefficient of Correlation, and Effective Number of Looks. These results show the potential of our proposed system as an effective tool for enhancing 3-D row-column imaging. PMID:26658577

Motion systems providing three or four degrees of freedom

NASA Technical Reports Server (NTRS)

Chou, Richard C. (Inventor)

1982-01-01

A motion system is provided by a platform generally parallel to a base and connected thereto by a column and powered and controlled extensible members, at least three of which are connected between distributed points around the column. In a three degree of freedom device, the column is conical, rigidly supported at its base with a universal joint at its top. The points of attachment define triangles in the base and in the platform surrounding the column with one extensible member connected between each. In the four degree of freedom version, the column is modified by making it effectively a column which is pivoted or guided at the base or contains an extensible member, preferably retains its triangular shape and its universal joint connection to the platform at its apex. For stability four powered and controlled extensible members are provided between points in the base and platform distributed around the column, a preferred pattern of arrangement being a square with the column at the center.

Simple equations to simulate closed-loop recycling liquid-liquid chromatography: Ideal and non-ideal recycling models.

PubMed

Kostanyan, Artak E

2015-12-04

The ideal (the column outlet is directly connected to the column inlet) and non-ideal (includes the effects of extra-column dispersion) recycling equilibrium-cell models are used to simulate closed-loop recycling counter-current chromatography (CLR CCC). Simple chromatogram equations for the individual cycles and equations describing the transport and broadening of single peaks and complex chromatograms inside the recycling closed-loop column for ideal and non-ideal recycling models are presented. The extra-column dispersion is included in the theoretical analysis, by replacing the recycling system (connecting lines, pump and valving) by a cascade of Nec perfectly mixed cells. To evaluate extra-column contribution to band broadening, two limiting regimes of recycling are analyzed: plug-flow, Nec→∞, and maximum extra-column dispersion, Nec=1. Comparative analysis of ideal and non-ideal models has shown that when the volume of the recycling system is less than one percent of the column volume, the influence of the extra-column processes on the CLR CCC separation may be neglected. Copyright © 2015 Elsevier B.V. All rights reserved.

Study on bamboo gluing performance numerical simulation

NASA Astrophysics Data System (ADS)

Zhao, Z. R.; Sun, W. H.; Sui, X. M.; Zhang, X. F.

2018-01-01

Bamboo gluing timber is a green building materials, can be widely used as modern building beams and columns. The existing bamboo gluing timber is usually produced by bamboo columns or bamboo bundle rolled into by bamboo columns. The performance of new bamboo gluing timber is decided by bamboo adhesion character. Based on this, the cohesive damage model of bamboo gluing is created, experiment results are used to validate the model. The model proposed in the work is agreed on the experimental results. Different bamboo bonding length and bamboo gluing performance is analysed. The model is helpful to bamboo integrated timber application.

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.

Achieving the full performance of highly efficient columns by optimizing conventional benchmark high-performance liquid chromatography instruments.

PubMed

Gritti, Fabrice; Sanchez, Carl A; Farkas, Tivadar; Guiochon, Georges

2010-04-30

A series of experiments and measurements demonstrate the importance of minimizing the extra-column band broadening contribution of the instrument used. The combination of several measures allowed the achievement of the full potential efficiency of three Kinetex-C(18) columns, using a conventional liquid chromatograph. The first measure consists in minimizing the extra-column volume of the instrument, without increasing much its back pressure contribution, by changing the needle seat volume, the inner diameter and length of the capillary connectors, and the volume of the detector cell of a standard instrument (Agilent 1100). The second measure consists in injecting a volume of weak eluent (less than half the elution strength of the mobile phase) right after the sample, before the sample had time to reach the column. Experimental results show that these changes could provide most of the resolution expected from the true column performance. After the changes were made, the resolutions of the 2.1 mm x 50 mm, 4.6 mm x 50 mm, and 4.6 mm x 100 mm Kinetex-C(18) columns for compounds having retention factors close to 1 were increased by about 180, 35, and 30%, respectively. The resolutions obtained are then similar to those measured with advanced instruments like the Agilent 1200, the Agilent 1290 Infinity HPLC, and the Acquity chromatographs. 2010 Elsevier B.V. All rights reserved.

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.

Trypsin coatings on electrospun and alcohol-dispersed polymer nanofibers for trypsin digestion column

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

Jun, Seung-Hyun; Chang, Mun Seock; Kim, Byoung Chan

2010-09-15

The construction of a trypsin reactor in a chromatography column for rapid and efficient protein digestion in proteomics is described. Electrospun and alcohol-dispersed polymer nanofibers were used for the fabrication of highly stable trypsin coating, which was prepared by a two-step process of covalent attachment and enzyme crosslinking. In a comparative study with the trypsin coatings on asspun and non-dispersed nanofibers, it has been observed that a simple step of alcohol dispersion improved not only the enzyme loading but also the performance of protein digestion. In-column digestion of enolase was successfully performed in less than twenty minutes. By applying themore » alcohol dispersion of polymer nanofibers, the bypass of samples was reduced by filling up the column with well-dispersed nanofibers, and subsequently, interactions between the protein and the enzymes were improved yielding more complete and reproducible digestions. Regardless of alcohol-dispersion or not, trypsin coating showed better digestion performance and improved performance stability under recycled uses than covalently-attached trypsin. The combination of highly stable trypsin coating and alcoholdispersion of polymer nanofibers has opened up a new potential to develop a trypsin column for on-line and automated protein digestion.« less

Seismic performance of square RC bridge columns under combined loading including torsion with low shear.

DOT National Transportation Integrated Search

2009-12-01

During earthquake excitations, reinforced concrete bridge columns can be subjected to a combination of axial load, shear force, : flexural moments, and torsional moments. The torsional moment can be much more significant in columns of bridges that ar...

Methacrylate-bonded covalent-organic framework monolithic columns for high performance liquid chromatography.

PubMed

Liu, Li-Hua; Yang, Cheng-Xiong; Yan, Xiu-Ping

2017-01-06

Covalent-organic frameworks (COFs) are a newfangled class of intriguing microporous materials. Considering their unique properties, COFs should be promising as packing materials for high performance liquid chromatography (HPLC). However, the irregular shape and sub-micrometer size of COFs synthesized via the traditional methods render the main obstacles for the application of COFs in HPLC. Herein, we report the preparation of methacrylate-bonded COF monolithic columns for HPLC to overcome the above obstacles. The prepared COF bonded monolithic columns not only show good homogeneity and permeability, but also give high column efficiency, good resolution and precision for HPLC separation of small molecules including polycyclic aromatic hydrocarbons, phenols, anilines, nonsteroidal anti-inflammatory drugs and benzothiophenes. Compared with the bare polymer monolithic column, the COF bonded monolithic columns show enhanced hydrophobic, π-π and hydrogen bond interactions in reverse phase HPLC. The results reveal the great potential of COF bonded monoliths for HPLC and COFs in separation sciences. Copyright © 2016 Elsevier B.V. All rights reserved.

A high-performance liquid chromatography micromethod for the simultaneous determination of vigabatrin and gabapentin in serum.

PubMed

Ratnaraj, N; Patsalos, P N

1998-08-01

A gradient high-performance liquid chromatography micromethod is described for the simultaneous quantitation of vigabatrin and gabapentin in human serum. Chromatography was performed using a 125- x 3-mm ID Hypersil BDS C-18 column with a 3-microm mini-bore, eluted with a gradient system comprised of phosphate buffer (pH 6.5)-acetonitrile-methanol-water at a flow rate of 0.45 ml/minute. The column eluent was monitored on a fluorescence detector using excitation and emission wavelengths of 340 and 440 nm, respectively. The lower limit of quantitation for vigabatrin and for gabapentin was 5 micromol/l, and the within-batch and between-batch coefficients of variation were <5%. No interference from commonly prescribed antiepileptic drugs (carbamazepine and its metabolite carbamazepine epoxide, oxcarbazepine and its metabolite 10-hydroxycarbazepine, ethosuximide, lamotrigine, phenobarbitone, phenytoin, primidone, and valproic acid) was observed; thus, the method can be used to monitor vigabatrin and gabapentin in patients on polytherapy antiepileptic drug regimens.

Experimental Evaluation of Beam to Diamond Box Column Connection with Through Plate in Moment Frames

NASA Astrophysics Data System (ADS)

Keshavarzi, Farhad; Mirghaderi, Rasoul; Torabian, Shahabeddin; Imanpour, Ali

2008-07-01

Moment resisting frames with built up section have very enhanced features due to high bending stiffness and strength characteristics in two principal axes and access to column faces for beam to column easy connections. But due to proper transfer of beam stresses to column faces there were always some specific controvertibly issues that how to make the load transfer through and in plane manner in order to mobilize the forces in column faces. Using diamond column instead of box column provide possibility to mobilize the load transfer mechanism in column faces. This section as a column has considerable benefit such as high plastic to elastic section modulus ratio which is an effective factor for force controlled components. Typical connection has no chance to be applied with diamond column. This paper elucidates the seismic behavior of through-plates moment connections to diamond box columns for use in steel moment resisting frames. This connection has a lot of economical benefits such as no need to horizontal continuity plates and satisfying the weak beam—strong column criteria in the connection region. They might serve as panel zone plates as well. According to high shear demand in panel zone of beam to column joint one should use the doublers plates in order to decrease the shear strength demand in this sensitive part of structure but these plates have no possibility to mobilize the load transfer mechanism in column web and transfer them to column flanges. In this type of connection, column faces have effective role in order to decrease the demands on through plate and they are impressive factors for improving the performance of the connection. Experimental analysis was conducted to elucidate the seismic behavior of this connection. The results of Experimental analysis established the effectiveness of the through plate in mitigating local stress concentrations and forming the plastic hinge zone in the beam away from the beam to column interface. The moment-rotation graphs form sub-assemblage show a desirable seismic performance of this connection

Performance of Goddard Earth Observing System GCM Column Radiation Models under Heterogeneous Cloud Conditions

NASA Technical Reports Server (NTRS)

Oreopoulos, L.; Chou, M.-D.; Khairoutdinov, M.; Barker, H. W.; Cahalan, R. F.

2003-01-01

We test the performance of the shortwave (SW) and longwave (LW) Column Radiation Models (CORAMs) of Chou and collaborators with heterogeneous cloud fields from a global single-day dataset produced by NCAR's Community Atmospheric Model with a 2-D CRM installed in each gridbox. The original SW version of the CORAM performs quite well compared to reference Independent Column Approximation (ICA) calculations for boundary fluxes, largely due to the success of a combined overlap and cloud scaling parameterization scheme. The absolute magnitude of errors relative to ICA are even smaller for the LW CORAM which applies similar overlap. The vertical distribution of heating and cooling within the atmosphere is also simulated quite well with daily-averaged zonal errors always below 0.3 K/d for SW heating rates and 0.6 K/d for LW cooling rates. The SW CORAM's performance improves by introducing a scheme that accounts for cloud inhomogeneity. These results suggest that previous studies demonstrating the inaccuracy of plane-parallel models may have unfairly focused on worst scenario cases, and that current radiative transfer algorithms of General Circulation Models (GCMs) may be more capable than previously thought in estimating realistic spatial and temporal averages of radiative fluxes, as long as they are provided with correct mean cloud profiles. However, even if the errors of the particular CORAMs are small, they seem to be systematic, and the impact of the biases can be fully assessed only with GCM climate simulations.

Computer simulation of two electrophoretic columns coupled for isoelectric focusing in simple buffers

NASA Technical Reports Server (NTRS)

Tsai, Amos; Mosher, Richard A.; Bier, Milan

1986-01-01

Computer simulation is used to analyze a system of two electrophoretic columns coupled by mixing the anolyte of one with the catholyte of the other. A mathematical model is presented which is used to predict the pH gradients formed by monovalent buffers in this system, when the currents in the columns are unequal. In the column with the higher current a pH gradient is created which increases from anode to cathode and is potentially useful for isoelectric focusing. The breadth of this gradient is dependent upon the ratio of the currents. The function of the second column is the compensation of buffer migration which occurs in the first column, thereby maintaining constant electrolyte composition. The effects of buffer pKs and mobilities are evaluated.

Performance of a Single Liquid Column Damper for the Control of Dynamic Responses of a Tension Leg Platform

NASA Astrophysics Data System (ADS)

Jaksic, V.; Wright, C.; Chanayil, Afeef; Faruque Ali, Shaikh; Murphy, Jimmy; Pakrashi, Vikram

2015-07-01

Tuned liquid column dampers have been proved to be successful in mitigating the dynamic responses of civil infrastructure. There have been some recent applications of this concept on wind turbines and this passive control system can help to mitigate responses of offshore floating platforms and wave devices. The control of dynamic responses of these devices is important for reducing loads on structural elements and facilitating operations and maintenance (O&M) activities. This paper outlines the use of a tuned single liquid column damper for the control of a tension leg platform supported wind turbine. Theoretical studies were carried out and a scaled model was tested in a wave basin to assess the performance of the damper. The tests on the model presented in this paper correspond to a platform with a very low natural frequency for surge, sway and yaw motions. For practical purposes, it was not possible to tune the liquid damper exactly to this frequency. The consequent approach taken and the efficiency of such approach are presented in this paper. Responses to waves of a single frequency are investigated along with responses obtained from wave spectra characterising typical sea states. The extent of control is quantified using peak and root mean squared dynamic responses respectively. The tests present some guidelines and challenges for testing scaled devices in relation to including response control mechanisms. Additionally, the results provide a basis for dictating future research on tuned liquid column damper based control on floating platforms.

Comparison of GOME-2/Metop total column water vapour with ground-based and in situ measurements

NASA Astrophysics Data System (ADS)

Kalakoski, N.; Kujanpää, J.; Sofieva, V.; Tamminen, J.; Grossi, M.; Valks, P.

2014-12-01

Total column water vapour product from the Global Ozone Monitoring Experiment-2 on board Metop-A and Metop-B satellites (GOME-2/Metop-A and GOME-2/Metop-B) produced by the Satellite Application Facility on Ozone and Atmospheric Chemistry Monitoring (O3M SAF) is compared with co-located radiosonde and Global Positioning System (GPS) observations. The comparisons are performed using recently reprocessed data by the GOME Data Processor (GDP) version 4.7. The comparisons are performed for the period of January 2007-July 2013 (GOME-2A) and from December 2012 to July 2013 (GOME-2B). Radiosonde data are from the Integrated Global Radiosonde Archive (IGRA) maintained by National Climatic Data Center (NCDC) and screened for soundings with incomplete tropospheric column. Ground-based GPS observations from COSMIC/SuomiNet network are used as the second independent data source. Good general agreement between GOME-2 and the ground-based observations is found. The median relative difference of GOME-2 to radiosonde observations is -2.7% for GOME-2A and -0.3% for GOME-2B. Against GPS observations, the median relative differences are 4.9 and 3.2% for GOME-2A and B, respectively. For water vapour total columns below 10 kg m-2, large wet biases are observed, especially against GPS observations. Conversely, at values above 50 kg m-2, GOME-2 generally underestimates both ground-based observations.

Integration of Gas Enhanced Oil Recovery in Multiphase Fermentations for the Microbial Production of Fuels and Chemicals.

PubMed

Pedraza-de la Cuesta, Susana; Keijzers, Lore; van der Wielen, Luuk A M; Cuellar, Maria C

2018-04-01

In multiphase fermentations where the product forms a second liquid phase or where solvents are added for product extraction, turbulent conditions disperse the oil phase as droplets. Surface-active components (SACs) present in the fermentation broth can stabilize the product droplets thus forming an emulsion. Breaking this emulsion increases process complexity and consequently the production cost. In previous works, it has been proposed to promote demulsification of oil/supernatant emulsions in an off-line batch bubble column operating at low gas flow rate. The aim of this study is to test the performance of this recovery method integrated to a fermentation, allowing for continuous removal of the oil phase. A 500 mL bubble column is successfully integrated with a 2 L reactor during 24 h without affecting cell growth or cell viability. However, higher levels of surfactants and emulsion stability are measured in the integrated system compared to a base case, reducing its capacity for oil recovery. This is related to release of SACs due to cellular stress when circulating through the recovery column. Therefore, it is concluded that the gas bubble-induced oil recovery method allows for oil separation and cell recycling without compromising fermentation performance; however, tuning of the column parameters considering increased levels of SACs due to cellular stress is required for improving oil recovery. © 2018 The Authors. Biotechnology Journal Published by Wiley-VCHVerlag GmbH & Co. KGaA, Weinheim.

Reliability of macroscopic grading of intervertebral disk degeneration in dogs by use of the Thompson system and comparison with low-field magnetic resonance imaging findings.

PubMed

Bergknut, Niklas; Grinwis, Guy; Pickee, Emile; Auriemma, Edoardo; Lagerstedt, Anne-Sofie; Hagman, Ragnvi; Hazewinkel, Herman A W; Meij, Björn P

2011-07-01

To evaluate the reliability of the Thompson system for use in grading the gross pathological changes of intervertebral disk (IVD) degeneration in dogs and to investigate the agreement between gross pathological findings and low-field (0.2-T) magnetic resonance imaging (MRI) findings. Vertebral columns from cadavers of 19 dogs of various ages, breeds, and origins. 182 intervertebral segments were collected from 19 canine cadavers. Sagittal T2-weighted MRI of the T11 through S1 portion of the vertebral column was performed within 24 hours after the dogs were euthanized. The vertebral columns were subsequently divided in the midsagittal plane, and high-resolution photographs were obtained of each intervertebral segment (end plate-disk-end plate). The MRI images and photographs were graded separately in a blinded manner by 4 observers who used both Pfirrmann and Thompson grading criteria. The interobserver agreement for Thompson scores ranged from 0.76 to 0.88, and the intraobserver agreement ranged from 0.88 to 0.94 (Cohen weighted κ analysis). Agreement between scores for the Pfirrmann and Thompson grading criteria was κ = 0.70. Grading of IVD degeneration in dogs by use of the Thompson system resulted in high interobserver and intraobserver agreement, and scores for the Thompson system had substantial agreement with low-field MRI findings graded by use of the Pfirrmann system. This suggested that low-field MRI can be used to diagnose IVD degeneration in dogs.

Aqueous Reversed-Phase HPLC/FT-IR Using Diffuse Reflectance Detections

NASA Astrophysics Data System (ADS)

Kalasinsky, Victor F.; Pai, T. H.; Kenton, R. C.; Kalasinsky, Kathryn S.

1989-12-01

Solvent-elimination HPLC/FT-IR has become a viable combination of two important techniques, and we have been developing a system which is adaptable to both normal and reversed-phase liquid chromatography. The interface involves the deposition of HPLC eluites onto a KCI-laden train with subsequent analysis via diffuse reflectance spectroscopy, and with minor modifications, the system can be used with microbore and analytical columns. With aqueous solvents, the water is converted to methanol and acetone in a post-column reaction with 2,2-dimethoxypropane before the eluites are deposited. A number of different samples have been used to demonstrate the interface and its flexibility. Steroids, analgesics, and other pharmaceutical preparations have been separated with reverse-phase solvents and identified by their infrared spectra. For some of the compounds studied, different infrared spectra of a given compound have been found to exhibit intensity variations, which arise from different crystalline states. The differences can be concentration dependent and may be useful in obtaining semi-quantitative information from the infrared spectra. Applications involving both gradient elution and isocratic separations have been successful. The former provides the same advantages for HPLC/FT-IR as one finds in conventional HPLC. More recent work has been applied to the use of buffers such as those frequently used in bioanalytical separations. In trying to simplify the post-column reaction with water, we have immobilized dehydration reagents onto silica particles and packed these materials into a column which is inserted in-line after the analytical column. Of the reagents utilized to date, 3,3-dimethoxypropyltrimethoxysilane has been found to perform most efficiently. It has advantages over the simpler reagents because it can be regenerated in the reaction column. Results and the efficiency of the dehydration process and its relation to the type of reagent and its coverage will be discussed.

Development and application of a high-performance liquid chromatography method using monolithic columns for the analysis of ecstasy tablets.

PubMed

Mc Fadden, Kim; Gillespie, John; Carney, Brian; O'Driscoll, Daniel

2006-07-07

A rapid and selective HPLC method using monolithic columns was developed for the separation and quantification of the principal amphetamines in ecstasy tablets. Three monolithic (Chromolith RP18e) columns of different lengths (25, 50 and 100 mm) were assessed. Validation studies including linearity, selectivity, precision, accuracy and limit of detection and quantification were carried out using the Chromolith SpeedROD, RP-18e, 50 mm x 4.6 mm column. Column backpressure and van Deemter plots demonstrated that monolithic columns provide higher efficiency at higher flow rates when compared to particulate columns without the loss of peak resolution. Application of the monolithic column to a large number of ecstasy tablets seized in Ireland ensured its suitability for the routine analysis of ecstasy tablets.

The use of fortified soil-clay as on-site system for domestic wastewater purification.

PubMed

Oladoja, N A; Ademoroti, C M A

2006-02-01

The quest for simple, low-cost and high-performance decentralized wastewater treatment system for domestic application in developing nations necessitated this study. Clay samples collected from different deposits in Nigeria were characterized by studying the mineralogical and geochemical composition using X-ray diffraction (XRD) and atomic absorption spectroscopy (AAS), respectively. Three major clay minerals of kaolinite, illite and smectite were identified. The geochemical studies showed the abundance of SiO2, Al2O3 and H2O+ in each of the clay samples. Performance efficiency studies were conducted to determine the best combination ratio of pebbles/soil-clay. Soil-clay fortified by pebbles in combination ratios of 1:3 (i.e. pebbles:soil-clay = 1:3 (w/w) showed the optimum water purification, while the combination 3:1 gave the least. The flow rate studies showed that the wastewater had a longer residence time in non-fortified soil-clay than in fortified soil-clay. Two modes of treatment methods were employed-single and double column treatment methods (SCT and DCT). The two methods gave effluents of good quality characteristics, but those from the DCT were of better quality. The quality of effluents also varies from one clay type to another. The quality of effluents from media containing smectite clay mineral was better than those from other columns. Repeated usage of the fortified clay column showed a decrease of pH, TS and DO, and an increase of COD when monitored over a period of 10 days.

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. Copyright © 2011 Elsevier B.V. All rights reserved.

SIM_ADJUST -- A computer code that adjusts simulated equivalents for observations or predictions

USGS Publications Warehouse

Poeter, Eileen P.; Hill, Mary C.

2008-01-01

This report documents the SIM_ADJUST computer code. SIM_ADJUST surmounts an obstacle that is sometimes encountered when using universal model analysis computer codes such as UCODE_2005 (Poeter and others, 2005), PEST (Doherty, 2004), and OSTRICH (Matott, 2005; Fredrick and others (2007). These codes often read simulated equivalents from a list in a file produced by a process model such as MODFLOW that represents a system of interest. At times values needed by the universal code are missing or assigned default values because the process model could not produce a useful solution. SIM_ADJUST can be used to (1) read a file that lists expected observation or prediction names and possible alternatives for the simulated values; (2) read a file produced by a process model that contains space or tab delimited columns, including a column of simulated values and a column of related observation or prediction names; (3) identify observations or predictions that have been omitted or assigned a default value by the process model; and (4) produce an adjusted file that contains a column of simulated values and a column of associated observation or prediction names. The user may provide alternatives that are constant values or that are alternative simulated values. The user may also provide a sequence of alternatives. For example, the heads from a series of cells may be specified to ensure that a meaningful value is available to compare with an observation located in a cell that may become dry. SIM_ADJUST is constructed using modules from the JUPITER API, and is intended for use on any computer operating system. SIM_ADJUST consists of algorithms programmed in Fortran90, which efficiently performs numerical calculations.

HPLC separation post-column reaction, UV-visible and fluorescence detection of trace UO/sub 2//sup 2 +//U/sup 4 +/ species in aqueous solutions

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

Karimi, A.R.

In this study a method for the measurement of uranium in natural waters at sub-ppB concentration levels by the separation and determination of U/sup 4 +/ and UO/sub 2//sup 2 +/ species is proposed. Reversed phase high performance liquid chromatography, followed by a post-column reaction and a sensitive UV-visible detection system was the method of choice to determine qualitatively and quantitatively the two uranium species. Also a cation-exchange and fluorescence detection system was studied for separation and determination of UO/sub 2//sup 2 +/ ions. Uranyl ion was selectively complexed with L-phenylalanine moetie in the sample solution containing U/sup 4 +/more » ions. Uranium (IV)/U(VI)-ligand was separated on a C/sub 18/ column with acetate buffer. Hexanesulfonate was found to be the choice for ion-pair reagent. The separation was best done with the acetate buffer at .01 M concentration and pH of 3.5. Absorption of the two species were measured after a post-column reaction with Arsenazo-III. Chromatographic parameters were calculated and a calibration curves were constructed. The detection limit for the procedure was 0.7 ..mu..g/mo and 1.2..mu..g/ml for U(IV) and U(VI) respectively. When U(VI) was separated on the cation-exchange column the limit of detection was calculated to be 1 ..mu..g/ml. The direct fluorometric method for U(VI) measurement results in a detection limit of 2 ppB and upper concentration limit of 2 ppM. The effect of interfering ions in the direct method of determination could be eliminated by dilution of sample solution.« less

Experimental study on control performance of tuned liquid column dampers considering different excitation directions

NASA Astrophysics Data System (ADS)

Altunişik, Ahmet Can; Yetişken, Ali; Kahya, Volkan

2018-03-01

This paper gives experimental tests' results for the control performance of Tuned Liquid Column Dampers (TLCDs) installed on a prototype structure exposed to ground motions with different directions. The prototype structure designed in the laboratory consists of top and bottom plates with four columns. Finite element analyses and ambient vibration tests are first performed to extract the natural frequencies and mode shapes of the structure. Then, the damping ratio of the structure as well as the resonant frequency, head-loss coefficient, damping ratio, and water height-frequency diagram of the designed TLCD are obtained experimentally by the shaking table tests. To investigate the effect of TLCDs on the structural response, the prototype structure-TLCD coupled system is considered later, and its natural frequencies and related mode shapes are obtained numerically. The acceleration and displacement time-histories are obtained by the shaking table tests to evaluate its damping ratio. To consider different excitation directions, the measurements are repeated for the directions between 0° and 90° with 15° increment. It can be concluded from the study that TLCD causes to decrease the resonant frequency of the structure with increasing of the total mass. Damping ratio considerably increases with installing TLCD on the structure. This is more pronounced for the angles of 0°, 15°, 30° and 45°.

Application of colloidal gas aphron suspensions produced from Sapindus mukorossi for arsenic removal from contaminated soil.

PubMed

Mukhopadhyay, Soumyadeep; Mukherjee, Sumona; Hashim, Mohd Ali; Sen Gupta, Bhaskar

2015-01-01

Colloidal gas aphron dispersions (CGAs) can be described as a system of microbubbles suspended homogenously in a liquid matrix. This work examines the performance of CGAs in comparison to surfactant solutions for washing low levels of arsenic from an iron rich soil. Sodium Dodecyl Sulfate (SDS) and saponin, a biodegradable surfactant, obtained from Sapindus mukorossi or soapnut fruit were used for generating CGAs and solutions for soil washing. Column washing experiments were performed in down-flow and up flow modes at a soil pH of 5 and 6 using varying concentration of SDS and soapnut solutions as well as CGAs. Soapnut CGAs removed more than 70% arsenic while SDS CGAs removed up to 55% arsenic from the soil columns in the soil pH range of 5-6. CGAs and solutions showed comparable performances in all the cases. CGAs were more economical since it contains 35% of air by volume, thereby requiring less surfactant. Micellar solubilization and low pH of soapnut facilitated arsenic desorption from soil column. FT-IR analysis of effluent suggested that soapnut solution did not interact chemically with arsenic thereby facilitating the recovery of soapnut solution by precipitating the arsenic. Damage to soil was minimal arsenic confirmed by metal dissolution from soil surface and SEM micrograph. Copyright © 2014 Elsevier Ltd. All rights reserved.

Approaches to characterise chromatographic column performance based on global parameters accounting for peak broadening and skewness.

PubMed

Baeza-Baeza, J J; Pous-Torres, S; Torres-Lapasió, J R; García-Alvarez-Coque, M C

2010-04-02

Peak broadening and skewness are fundamental parameters in chromatography, since they affect the resolution capability of a chromatographic column. A common practice to characterise chromatographic columns is to estimate the efficiency and asymmetry factor for the peaks of one or more solutes eluted at selected experimental conditions. This has the drawback that the extra-column contributions to the peak variance and skewness make the peak shape parameters depend on the retention time. We propose and discuss here the use of several approaches that allow the estimation of global parameters (non-dependent on the retention time) to describe the column performance. The global parameters arise from different linear relationships that can be established between the peak variance, standard deviation, or half-widths with the retention time. Some of them describe exclusively the column contribution to the peak broadening, whereas others consider the extra-column effects also. The estimation of peak skewness was also possible for the approaches based on the half-widths. The proposed approaches were applied to the characterisation of different columns (Spherisorb, Zorbax SB, Zorbax Eclipse, Kromasil, Chromolith, X-Terra and Inertsil), using the chromatographic data obtained for several diuretics and basic drugs (beta-blockers). Copyright (c) 2010 Elsevier B.V. All rights reserved.

Site-directed immobilization of a genetically engineered anti-methotrexate antibody via an enzymatically introduced biotin label significantly increases the binding capacity of immunoaffinity columns.

PubMed

Davenport, Kaitlynn R; Smith, Christopher A; Hofstetter, Heike; Horn, James R; Hofstetter, Oliver

2016-05-15

In this study, the effect of random vs. site-directed immobilization techniques on the performance of antibody-based HPLC columns was investigated using a single-domain camelid antibody (VHH) directed against methotrexate (MTX) as a model system. First, the high flow-through support material POROS-OH was activated with disuccinimidyl carbonate (DSC), and the VHH was bound in a random manner via amines located on the protein's surface. The resulting column was characterized by Frontal Affinity Chromatography (FAC). Then, two site-directed techniques were explored to increase column efficiency by immobilizing the antibody via its C-terminus, i.e., away from the antigen-binding site. In one approach, a tetra-lysine tail was added, and the antibody was immobilized onto DSC-activated POROS. In the second site-directed approach, the VHH was modified with the AviTag peptide, and a biotin-residue was enzymatically incorporated at the C-terminus using the biotin ligase BirA. The biotinylated antibody was subsequently immobilized onto NeutrAvidin-derivatized POROS. A comparison of the FAC analyses, which for all three columns showed excellent linearity (R(2)>0.999), revealed that both site-directed approaches yield better results than the random immobilization; the by far highest efficiency, however, was determined for the immunoaffinity column based on AviTag-biotinylated antibody. As proof of concept, all three columns were evaluated for quantification of MTX dissolved in phosphate buffered saline (PBS). Validation using UV-detection showed excellent linearity in the range of 0.04-12μM (R(2)>0.993). The lower limit of detection (LOD) and lower limit of quantification (LLOQ) were found to be independent of the immobilization strategy and were 40nM and 132nM, respectively. The intra- and inter-day precision was below 11.6%, and accuracy was between 90.7% and 112%. To the best of our knowledge, this is the first report of the AviTag-system in chromatography, and the first application of immunoaffinity chromatography for the analysis of MTX. Copyright © 2016 Elsevier B.V. All rights reserved.

Analysis and simulation of industrial distillation processes using a graphical system design model

NASA Astrophysics Data System (ADS)

Boca, Maria Loredana; Dobra, Remus; Dragos, Pasculescu; Ahmad, Mohammad Ayaz

2016-12-01

The separation column used for experimentations one model can be configured in two ways: one - two columns of different diameters placed one within the other extension, and second way, one column with set diameter [1], [2]. The column separates the carbon isotopes based on the cryogenic distillation of pure carbon monoxide, which is fed at a constant flow rate as a gas through the feeding system [1],[2]. Based on numerical control systems used in virtual instrumentation was done some simulations of the distillation process in order to obtain of the isotope 13C at high concentrations. The experimental installation for cryogenic separation can be configured from the point of view of the separation column in two ways: Cascade - two columns of different diameters and placed one in the extension of the other column, and second one column with a set diameter. It is proposed that this installation is controlled to achieve data using a data acquisition tool and professional software that will process information from the isotopic column based on a logical dedicated algorithm. Classical isotopic column will be controlled automatically, and information about the main parameters will be monitored and properly display using one program. Take in consideration the very-low operating temperature, an efficient thermal isolation vacuum jacket is necessary. Since the "elementary separation ratio" [2] is very close to unity in order to raise the (13C) isotope concentration up to a desired level, a permanent counter current of the liquid-gaseous phases of the carbon monoxide is created by the main elements of the equipment: the boiler in the bottom-side of the column and the condenser in the top-side.

Dynamic tables: an architecture for managing evolving, heterogeneous biomedical data in relational database management systems.

PubMed

Corwin, John; Silberschatz, Avi; Miller, Perry L; Marenco, Luis

2007-01-01

Data sparsity and schema evolution issues affecting clinical informatics and bioinformatics communities have led to the adoption of vertical or object-attribute-value-based database schemas to overcome limitations posed when using conventional relational database technology. This paper explores these issues and discusses why biomedical data are difficult to model using conventional relational techniques. The authors propose a solution to these obstacles based on a relational database engine using a sparse, column-store architecture. The authors provide benchmarks comparing the performance of queries and schema-modification operations using three different strategies: (1) the standard conventional relational design; (2) past approaches used by biomedical informatics researchers; and (3) their sparse, column-store architecture. The performance results show that their architecture is a promising technique for storing and processing many types of data that are not handled well by the other two semantic data models.

Screening and identification of radical scavengers from Neo-Taraxacum siphonanthum by online rapid screening method and nuclear magnetic resonance experiments.

PubMed

Shi, Shu Yun; Zhang, Yu Ping; Zhou, Hong Hao; Huang, Ke Long; Jiang, Xin Yu

2010-01-01

An online rapid screening method, the high-performance liquid chromatography (HPLC)-diode array detector (DAD)-radical scavenging detection (RSD)-electrospray ionization (ESI)-mass spectroscopy (MS)/MS system, was developed for the screening and identification of radical scavengers from Neo-Taraxacum siphonanthum, a new species found in China in 1989. For further characterization, the target compounds were isolated by silica column chromatography, preparative high-performance liquid chromatography (HPLC), HSCCC, and Sephadex LH-20 column chromatography and elucidated on the basis of ultraviolet (UV), ESI-MS/MS, and nuclear magnetic resonance (NMR) spectroscopy, as well as the chemical analysis. Eighteen antioxidative polyphenols (5 caffeic acid derivatives and 13 flavonoid derivatives) were characterized from Neo-T. siphonanthum. The distribution of all compounds was discussed in a chemosystematic context, which suggested that the genera Neo-Taraxacum and Taraxacum might relate chemosystematically.

Chromatographic behavior of small organic compounds in low-temperature high-performance liquid chromatography using liquid carbon dioxide as the mobile phase.

PubMed

Motono, Tomohiro; Nagai, Takashi; Kitagawa, Shinya; Ohtani, Hajime

2015-07-01

Low-temperature high-performance liquid chromatography, in which a loop injector, column, and detection cell were refrigerated at -35ºC, using liquid carbon dioxide as the mobile phase was developed. Small organic compounds (polyaromatic hydrocarbons, alkylbenzenes, and quinones) were separated by low-temperature high-performance liquid chromatography at temperatures from -35 to -5ºC. The combination of liquid carbon dioxide mobile phase with an octadecyl-silica (C18 ) column provided reversed phase mode separation, and a bare silica-gel column resulted in normal phase mode separation. In both the cases, nonlinear behavior at approximately -15ºC was found in the relationship between the temperature and the retention factors of the analytes (van't Hoff plots). In contrast to general trends in high-performance liquid chromatography, the decrease in temperature enhanced the separation efficiency of both the columns. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Supermacroporous cryogel matrix for integrated protein isolation. Immobilized metal affinity chromatographic purification of urokinase from cell culture broth of a human kidney cell line.

PubMed

Kumar, Ashok; Bansal, Vibha; Andersson, Jonatan; Roychoudhury, Pradip K; Mattiasson, Bo

2006-01-20

A new type of supermacroporous, monolithic, cryogel affinity adsorbent was developed, allowing the specific capture of urokinase from conditioned media of human fibrosarcoma cell line HT1080. The affinity adsorbent was designed with the objective of using it as a capture column in an integrated perfusion/protein separation bioreactor setup. A comparative study between the utility of this novel cryogel based matrix and the conventional Sepharose based affinity matrix for the continuous capture of urokinase in an integrated bioreactor system was performed. Cu(II)-ion was coupled to epoxy activated polyacrylamide cryogel and Sepharose using iminodiacetic acid (IDA) as the chelating ligand. About 27-fold purification of urokinase from the conditioned culture media was achieved with Cu(II)-IDA-polyacrylamide cryogel column giving specific activity of about 814 Plough units (PU)/mg protein and enzyme yields of about 80%. High yields (95%) were obtained with Cu(II)-IDA-Sepharose column by virtue of its high binding capacity. However, the adsorbent showed lower selectivity as compared to cryogel matrix giving specific activity of 161 PU/mg protein and purification factor of 5.3. The high porosity, selectivity and reasonably good binding capacity of Cu(II)-IDA-polyacrylamide cryogel column make it a promising option for use as a protein capture column in integrated perfusion/separation processes. The urokinase peak pool from Cu(II)-IDA-polyacrylamide cryogel column could be further resolved into separate fractions for high and low molecular weight forms of urokinase by gel filtration chromatography on Sephacryl S-200. The selectivity of the cryogel based IMAC matrix for urokinase was found to be higher as compared to that of Cu(II)-IDA-Sepharose column.

Comparison of ultra high performance supercritical fluid chromatography, ultra high performance liquid chromatography, and gas chromatography for the separation of synthetic cathinones.

PubMed

Carnes, Stephanie; O'Brien, Stacey; Szewczak, Angelica; Tremeau-Cayel, Lauriane; Rowe, Walter F; McCord, Bruce; Lurie, Ira S

2017-09-01

A comparison of ultra high performance supercritical fluid chromatography, ultra high performance liquid chromatography, and gas chromatography for the separation of synthetic cathinones has been conducted. Nine different mixtures of bath salts were analyzed in this study. The three different chromatographic techniques were examined using a general set of controlled synthetic cathinones as well as a variety of other synthetic cathinones that exist as positional isomers. Overall 35 different synthetic cathinones were analyzed. A variety of column types and chromatographic modes were examined for developing each separation. For the ultra high performance supercritical fluid chromatography separations, analyses were performed using a series of Torus and Trefoil columns with either ammonium formate or ammonium hydroxide as additives, and methanol, ethanol or isopropanol organic solvents as modifiers. Ultra high performance liquid chromatographic separations were performed in both reversed phase and hydrophilic interaction chromatographic modes using SPP C18 and SPP HILIC columns. Gas chromatography separations were performed using an Elite-5MS capillary column. The orthogonality of ultra high performance supercritical fluid chromatography, ultra high performance liquid chromatography, and gas chromatography was examined using principal component analysis. For the best overall separation of synthetic cathinones, the use of ultra high performance supercritical fluid chromatography in combination with gas chromatography is recommended. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Investigation into Generation of Micro Features by Localised Electrochemical Deposition

NASA Astrophysics Data System (ADS)

Debnath, Subhrajit; Laskar, Hanimur Rahaman; Bhattacharyya, B.

2017-11-01

With the fast advancement of technology, localised electrochemical deposition (LECD) is becoming very advantageous in generating high aspect ratio micro features to meet the steep demand in modern precision industries of the present world. Except many other advantages, this technology is highly uncomplicated and economical for fabricating metal micro-parts with in micron ranges. In the present study, copper micro-columns have been fabricated utilizing LECD process. Different process parameters such as voltage, frequency, duty ratio and electrolyte concentration, which affect the deposition performance have been identified and their effects on deposition performances such as deposition rate, height and diameter of the micro-columns have been experimentally investigated. Taguchi's methodology has been used to study the effects as well as to obtain the optimum values of process parameters so that localised deposition with best performance can be achieved. Moreover, the generated micro-columns were carefully observed under optical and scanning electron microscope from where the surface quality of the deposited micro-columns has been studied qualitatively. Also, an array of copper micro-columns has been fabricated on stainless steel (SS-304) substrate for further exploration of LECD process capability.

Stability Analysis of Flow Induced by the Traveling Magnetic Field

NASA Technical Reports Server (NTRS)

Mazuruk, Konstantin

2003-01-01

Re-circulating flow in molten metal columns can be conveniently induced by the axisymmetric traveling magnetic field. A number of applications can benefit from this technique, such as mixing under microgravity environment, or.crysta1 growth from metallic melts. For small magnetic field excitations, the flow is laminar and stationary. As the imposed field increases, a more complex flow will set up in the cylindrical column. Conditions for stable laminar flow are of importance for practical applications. In this work, a linear stability analysis is performed in order to determine the onset of the bifurcation in the system. Here the analysis is restricted to the axisymmetric modes and the low-frequency regime.

Stability Analysis of Flow Induced by the Traveling Magnetic Field

NASA Technical Reports Server (NTRS)

Mazuruk, Konstantin

2003-01-01

Re-circulating flow in molten metal columns can be conveniently induced by the axisymmetric traveling magnetic field. A number of applications can benefit from this technique, such as mixing under microgravity environment, or crysta1 growth from metallic melts. For small magnetic field excitations, the flow is laminar and stationary. As the imposed field increases, a more complex flow will set up in the cylindrical column. Conditions for stable laminar flow are of importance for practical applications. In this work, a linear stability analysis is performed in order to determine the onset of the bifurcation in the system. Here the analysis is restricted to the axisymmetric modes and the low-frequency regime.

Fabrication and investigation of electrochromatographic columns with a simplex configuration.

PubMed

Liu, Qing; Yang, Lijun; Wang, Qiuquan; Zhang, Bo

2014-07-04

Duplex capillary columns with a packed and an open section are widely used in electrochromatography (CEC). The duplex column configuration leads to non-uniform voltage drop, electrical field distribution and separation performance. It also adds to the complexity in understanding and optimizing electrochromatographic process. In this study, we introduced a simplex column configuration based on single particle fritting technology. The new column configuration has an essentially uniform packed bed through the entire column length, with only 1mm length left unpacked serving as the optical detection window. The study shows that a simplex column has higher separation efficiency than a duplex column, especially at the high voltage range, due to the consistent distribution of electrical field over the column length. In comparison to the duplex column, the simplex column presented a lower flow rate at the same applied voltage, suggesting that an open section may support a higher speed than a packed section. In practice, the long and short ends of the simplex column could be used as independent CEC columns respectively. This "two-in-one" bi-functional column configuration provided extra flexibilities in selecting and optimizing electrochromatographic conditions. Copyright © 2014 Elsevier B.V. All rights reserved.

A silica monolithic column prepared by the sol-gel process for enantiomeric separation by capillary electrochromatography.

PubMed

Kang, Jingwu; Wistuba, Dorothee; Schurig, Volker

2002-04-01

A method for the preparation of a silica monolithic capillary electrochromatography (CEC) column for the separation of enantiomers has been developed. The porous silica monolith was fabricated inside a fused-silica capillary column by using the sol-gel process. After gelation for 24 h, hydrothermal treatment at 100 degrees C for 24 h was performed to prevent the sol-gel matrix from cracking. The prepared monolith was then coated with Chirasil-beta-Dex which represents a chiral polymer prepared by grafting permethyl-beta-cyclodextrin to polymethylsiloxane with an octamethylene spacer. Immobilization of Chirasil-beta-Dex was performed by heat treatment at 120 degrees C for 48 h to give a nonextractable coating. The column performance was evaluated by using racemic hexobarbital as a model compound. The efficiency of 9.2 x 10(4) theoretical plates/m for the first eluted enantiomer of hexobarbital was obtained at an optimal flow rate of the mobile phase. The effect of mobile phase composition on enantiomeric separation of hexobarbital was also investigated. The column proved to be stable for more than one hundreds of runs during a two-months period. The enantiomers of several neutral and negatively charged chiral compounds were baseline separated on this column.

[Simultaneous analysis of trehalose, glucose and maltose in biotransformation samples by high performance anion exchange chromatography with pulsed ampere detection].

PubMed

Xu, Ying; Zang, Ying; Jiang, Ting; Zheng, Zhaojuan; Quyang, Jia

2014-12-01

An analytical method for the determination of trehalose, maltose, and glucose in biotransformation samples was developed by using high performance anion exchange chromatography coupled with pulsed ampere detection (HPAEC-PAD). The analysis was performed on a CarboPac™ 10 column (250 mm x 2 mm) with the gradient elution of NaOH-NaAc as the mobile phase. The column temperature was set at 30 °C, the flow rate was 0. 30 mL/min. The results showed that trehalose, maltose, and glucose in biotransformation system were completely separated and determined in 15 min. The linear ranges and the working curves were determined by using standard samples. The correlation coefficients of three kinds of carbohydrates were over 0. 9998 . The detection limits (LODs) were 0. 010 - 0. 100 mg/L. Under the optimized separation conditions, the recoveries of saccharides in the transformation system at three different spiked levels ranged from 89. 4% to 103. 2%. In biotransformation system, 50 IU trehalose synthase were added into 200 g/L maltose for reaction of 8 h at 37 °C, pH 8. 0. Under the above conditions, the concentration of trehalose in biotransformation sample was 101. 084 g/L, and the conversion rate of trehalose reached 50. 5%. The method can be applied to determine the composition in the transformation system with the advantages of simplicity and convenience.

Monolithic columns with organic sorbent based on poly-1-vinylimidazole for high performance liquid chromatography

NASA Astrophysics Data System (ADS)

Patrushev, Y. V.; Sidelnikov, V. N.; Yudina, Y. S.

2017-03-01

Monolithic chromatographic columns for HPLC with sorbent based on 1-vinylimidazole are prepared. It is shown that changing the 1-vinylimidazole content in the initial solution allows us to change the polarity of columns. An example of aromatic hydrocarbons separation is presented.

Use of emulsified vegetable oil to support bioremediation of TCE DNAPL in soil columns.

PubMed

Harkness, Mark; Fisher, Angela

2013-08-01

The interaction between emulsified vegetable oil (EVO) and trichloroethylene (TCE) dense non-aqueous phase liquid (DNAPL) was observed using two soil columns and subsequent reductive dechlorination of TCE was monitored over a three year period. Dyed TCE DNAPL (~75 g) was emplaced in one column (DNAPL column), while the second was DNAPL-free (plume column). EVO was added to both columns and partitioning of the EVO into the TCE DNAPL was measured and quantified. TCE (1.9 mM) was added to the influent of the plume column to simulate conditions down gradient of a DNAPL source area and the columns were operated independently for more than one year, after which they were connected in series. Initially limited dechlorination of TCE to cDCE was observed in the DNAPL column, while the plume column supported complete reductive dechlorination of TCE to ethene. Upon connection and reamendment of the plume column with EVO, near saturation levels of TCE from the effluent of the DNAPL column were rapidly dechlorinated to c-DCE and VC in the plume column; however, this high rate dechlorination produced hydrochloric acid which overwhelmed the buffering capacity of the system and caused the pH to drop below 6.0. Dechlorination efficiency in the columns subsequently deteriorated, as measured by the chloride production and Dehalococcoides counts, but was restored by adding sodium bicarbonate buffer to the influent groundwater. Robust dechlorination was eventually observed in the DNAPL column, such that the TCE DNAPL was largely removed by the end of the study. Partitioning of the EVO into the DNAPL provided significant operational benefits to the remediation system both in terms of electron donor placement and longevity. Copyright © 2013 Elsevier B.V. All rights reserved.

Device to improve detection in electro-chromatography

DOEpatents

Garguilo, Michael G.; Paul, Phillip H.; Rakestraw, David J.

2000-01-01

Apparatus and method for improving the resolution of non-pressure driven capillary chromatographic systems, and particularly for capillary electrochromatography (CEC) systems. By reducing the cross-sectional area of a packed capillary column by means of a second open capillary contiguous with the outlet end of a packed capillary column, where the packed capillary column has a cross sectional area of between about 2 and 5 times that of the open capillary column, the phenomenon of band broadening in the transition region between the open capillary and the packed capillary column, where the individual components of the mixture are analyzed, can be eliminated, thereby providing for a significant improvement in resolution and more accurate detection and analysis.

Device to improve detection in electro-chromatography

DOEpatents

Garguilo, Michael G.; Paul, Phillip H.; Rakestraw, David J.

2002-01-01

Apparatus and method for improving the resolution of non-pressure driven capillary chromatographic systems, and particularly for capillary electrochromatography (CEC) systems. By reducing the cross-sectional area of a packed capillary column by means of a second open capillary contiguous with the outlet end of a packed capillary column, where the packed capillary column has a cross sectional area of between about 2 and 5 times that of the open capillary column, the phenomenon of band broadening in the transition region between the open capillary and the packed capillary column, where the individual components of the mixture are analyzed, can be eliminated, thereby providing for a significant improvement in resolution and more accurate detection and analysis.

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.

[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.

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.

Annotation of the human serum metabolome by coupling three liquid chromatography methods to high-resolution mass spectrometry.

PubMed

Boudah, Samia; Olivier, Marie-Françoise; Aros-Calt, Sandrine; Oliveira, Lydie; Fenaille, François; Tabet, Jean-Claude; Junot, Christophe

2014-09-01

This work aims at evaluating the relevance and versatility of liquid chromatography coupled to high resolution mass spectrometry (LC/HRMS) for performing a qualitative and comprehensive study of the human serum metabolome. To this end, three different chromatographic systems based on a reversed phase (RP), hydrophilic interaction chromatography (HILIC) and a pentafluorophenylpropyl (PFPP) stationary phase were used, with detection in both positive and negative electrospray modes. LC/HRMS platforms were first assessed for their ability to detect, retain and separate 657 metabolite standards representative of the chemical families occurring in biological fluids. More than 75% were efficiently retained in either one LC-condition and less than 5% were exclusively retained by the RP column. These three LC/HRMS systems were then evaluated for their coverage of serum metabolome. The combination of RP, HILIC and PFPP based LC/HRMS methods resulted in the annotation of about 1328 features in the negative ionization mode, and 1358 in the positive ionization mode on the basis of their accurate mass and precise retention time in at least one chromatographic condition. Less than 12% of these annotations were shared by the three LC systems, which highlights their complementarity. HILIC column ensured the greatest metabolome coverage in the negative ionization mode, whereas PFPP column was the most effective in the positive ionization mode. Altogether, 192 annotations were confirmed using our spectral database and 74 others by performing MS/MS experiments. This resulted in the formal or putative identification of 266 metabolites, among which 59 are reported for the first time in human serum. Copyright © 2014 Elsevier B.V. All rights reserved.

A microfluidic chip with a staircase pH gradient generator, a packed column and a fraction collector for chromatofocusing of proteins.

PubMed

Rho, Hoon Suk; Hanke, Alexander Thomas; Ottens, Marcel; Gardeniers, Han J G E

2018-04-01

A microfluidic device for pH gradient chromatofocusing is presented, which performs creation of a micro-column, pH gradient generation, and fraction collection in a single device. Using a sieve micro-valve, anion exchange particles were packed into a microchannel in order to realize a solid-phase absorption column. To fractionate proteins according to their isoelectric points, elution buffer solutions with a stepwise pH gradient were prepared in 16 parallel mixing reactors and flowed through the micro-column, wherein a protein mixture was previously loaded. The volume of the column is only 20 nL, hence it allows extremely low sample consumption and fast analysis compared with a conventional system. We demonstrated separation of two proteins, albumin-fluorescein isothiocyanate conjugate (FITC-BSA) and R-Phycoerythrin (R-PE), by using a microcolumn of commercial charged polymeric particles (Source 15Q). The microfluidic device can be used as a rapid diagnostic tool to analyse crude mixtures of proteins or nucleic acids and determine adsorption/desorption characteristics of various biochemical products, which can be helpful for scientific fundamental understanding as well as instrumental in various industrial applications, especially in early stage screening and process development. © 2018 The Authors Electrophoresis Published by WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

Brown, Garrett N.; Russell, Renee L.; Peterson, Reid A.

This report summarizes the work performed to evaluate multiple, cesium loading, and elution cycles for small columns containing SRF resin using a simple, high-level waste (HLW) simulant. Cesium ion exchange loading and elution curves were generated for a nominal 5 M Na, 2.4E-05 M Cs, 0.115 M Al loading solution traced with 134Cs followed by elution with variable HNO3 (0.02, 0.07, 0.15, 0.23, and 0.28 M) containing variable CsNO3 (5.0E-09, 5.0E-08, and 5.0E-07 M) and traced with 137Cs. The ion exchange system consisted of a pump, tubing, process solutions, and a single, small ({approx}15.7 mL) bed of SRF resin withmore » a water-jacketed column for temperature-control. The columns were loaded with approximately 250 bed volumes (BVs) of feed solution at 45 C and at 1.5 to 12 BV per hour (0.15 to 1.2 cm/min). The columns were then eluted with 29+ BVs of HNO3 processed at 25 C and at 1.4 BV/h. The two independent tracers allowed analysis of the on-column cesium interaction between the loading and elution solutions. The objective of these tests was to improve the correlation between the spent resin cesium content and cesium leached out of the resin in subsequent loading cycles (cesium leakage) to help establish acid strength and purity requirements.« less

Estimating surface NO2 and SO2 mixing ratios from fast-response total column observations and potential application to geostationary missions.

PubMed

Knepp, T; Pippin, M; Crawford, J; Chen, G; Szykman, J; Long, R; Cowen, L; Cede, A; Abuhassan, N; Herman, J; Delgado, R; Compton, J; Berkoff, T; Fishman, J; Martins, D; Stauffer, R; Thompson, A M; Weinheimer, A; Knapp, D; Montzka, D; Lenschow, D; Neil, D

Total-column nitrogen dioxide (NO 2 ) data collected by a ground-based sun-tracking spectrometer system (Pandora) and an photolytic-converter-based in-situ instrument collocated at NASA's Langley Research Center in Hampton, Virginia were analyzed to study the relationship between total-column and surface NO 2 measurements. The measurements span more than a year and cover all seasons. Surface mixing ratios are estimated via application of a planetary boundary-layer (PBL) height correction factor. This PBL correction factor effectively corrects for boundary-layer variability throughout the day, and accounts for up to ≈75 % of the variability between the NO 2 data sets. Previous studies have made monthly and seasonal comparisons of column/surface data, which has shown generally good agreement over these long average times. In the current analysis comparisons of column densities averaged over 90 s and 1 h are made. Applicability of this technique to sulfur dioxide (SO 2 ) is briefly explored. The SO 2 correlation is improved by excluding conditions where surface levels are considered background. The analysis is extended to data from the July 2011 DISCOVER-AQ mission over the greater Baltimore, MD area to examine the method's performance in more-polluted urban conditions where NO 2 concentrations are typically much higher.

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.

An Examination of the Effect of Boundary Layer Ingestion on Turboelectric Distributed Propulsion Systems

NASA Technical Reports Server (NTRS)

Felder, James L.; Kim, Huyn Dae; Brown, Gerald V.; Chu, Julio

2011-01-01

A Turboelectric Distributed Propulsion (TeDP) system differs from other propulsion systems by the use of electrical power to transmit power from the turbine to the fan. Electrical power can be efficiently transmitted over longer distances and with complex topologies. Also the use of power inverters allows the generator and motors speeds to be independent of one another. This decoupling allows the aircraft designer to place the core engines and the fans in locations most advantageous for each. The result can be very different installation environments for the different devices. Thus the installation effects on this system can be quite different than conventional turbofans where the fan and core both see the same installed environments. This paper examines a propulsion system consisting of two superconducting generators, each driven by a turboshaft engine located so that their inlets ingest freestream air, superconducting electrical transmission lines, and an array of superconducting motor driven fan positioned across the upper/rear fuselage area of a hybrid wing body aircraft in a continuous nacelle that ingests all of the upper fuselage boundary layer. The effect of ingesting the boundary layer on the design of the system with a range of design pressure ratios is examined. Also the impact of ingesting the boundary layer on off-design performance is examined. The results show that when examining different design fan pressure ratios it is important to recalculate of the boundary layer mass-average Pt and MN up the height for each inlet height during convergence of the design point for each fan design pressure ratio examined. Correct estimation of off-design performance is dependent on the height of the column of air measured from the aircraft surface immediately prior to any external diffusion that will flow through the fan propulsors. The mass-averaged Pt and MN calculated for this column of air determine the Pt and MN seen by the propulsor inlet. Since the height of this column will change as the amount of air passing through the fans change as the propulsion system is throttled, and since the mass-average Pt and MN varies by height, this capture height must be recalculated as the airflow through the propulsor is varied as the off-design performance point is converged.

Randomized subspace-based robust principal component analysis for hyperspectral anomaly detection

NASA Astrophysics Data System (ADS)

Sun, Weiwei; Yang, Gang; Li, Jialin; Zhang, Dianfa

2018-01-01

A randomized subspace-based robust principal component analysis (RSRPCA) method for anomaly detection in hyperspectral imagery (HSI) is proposed. The RSRPCA combines advantages of randomized column subspace and robust principal component analysis (RPCA). It assumes that the background has low-rank properties, and the anomalies are sparse and do not lie in the column subspace of the background. First, RSRPCA implements random sampling to sketch the original HSI dataset from columns and to construct a randomized column subspace of the background. Structured random projections are also adopted to sketch the HSI dataset from rows. Sketching from columns and rows could greatly reduce the computational requirements of RSRPCA. Second, the RSRPCA adopts the columnwise RPCA (CWRPCA) to eliminate negative effects of sampled anomaly pixels and that purifies the previous randomized column subspace by removing sampled anomaly columns. The CWRPCA decomposes the submatrix of the HSI data into a low-rank matrix (i.e., background component), a noisy matrix (i.e., noise component), and a sparse anomaly matrix (i.e., anomaly component) with only a small proportion of nonzero columns. The algorithm of inexact augmented Lagrange multiplier is utilized to optimize the CWRPCA problem and estimate the sparse matrix. Nonzero columns of the sparse anomaly matrix point to sampled anomaly columns in the submatrix. Third, all the pixels are projected onto the complemental subspace of the purified randomized column subspace of the background and the anomaly pixels in the original HSI data are finally exactly located. Several experiments on three real hyperspectral images are carefully designed to investigate the detection performance of RSRPCA, and the results are compared with four state-of-the-art methods. Experimental results show that the proposed RSRPCA outperforms four comparison methods both in detection performance and in computational time.

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-VCH Verlag GmbH & Co. KGaA, Weinheim.

Development of a split-flow system for high precision variable sample introduction in supercritical fluid chromatography.

PubMed

Sakai, Miho; Hayakawa, Yoshihiro; Funada, Yasuhiro; Ando, Takashi; Fukusaki, Eiichiro; Bamba, Takeshi

2017-09-15

In this study, we propose a novel variable sample injection system based on full-loop injection, named the split-flow sample introduction system, for application in supercritical fluid chromatography (SFC). In this system, the mobile phase is split by the differential pressure between two back pressure regulators (BPRs) after full-loop injection suitable for SFC, and this differential pressure determines the introduction rate. Nine compounds with a wide range of characteristics were introduced with high reproducibility and universality, confirming that a robust variable sample injection system was achieved. We also investigated the control factors of our proposed system. Sample introduction was controlled by the ratio between the column-side pressure drops in splitless and split flow, ΔP columnsideinsplitless and ΔP columnsideinsplit , respectively, where ΔP columnsideinsplitless is related to the mobile phase flow rate and composition and the column resistance. When all other conditions are kept constant, increasing the make-up flow induces an additional pressure drop on the column side of the system, which leads to a reduced column-side flow rate, and hence decreased the amount of sample injected, even when the net pressure drop on the column side remains the same. Thus, sample introduction could be highly controlled at low sample introduction rate, regardless of the introduction conditions. This feature is advantageous because, as a control factor, the solvent in the make-up pump is independent of the column-side pressure drop. Copyright © 2017. Published by Elsevier B.V.

Effect of Coriolis force on counter-current chromatographic separation by centrifugal partition chromatography.

PubMed

Ikehata, Jun-Ichi; Shinomiya, Kazufusa; Kobayashi, Koji; Ohshima, Hisashi; Kitanaka, Susumu; Ito, Yoichiro

2004-02-06

The effect of Coriolis force on the counter-current chromatographic separation was studied using centrifugal partition chromatography (CPC) with four different two-phase solvent systems including n-hexane-acetonitrile (ACN); tert-butyl methyl ether (MtBE)-aqueous 0.1% trifluoroacetic acid (TFA) (1:1); MtBE-ACN-aqueous 0.1% TFA (2:2:3); and 12.5% (w/w) polyethylene glycol (PEG) 1000-12.5% (w/w) dibasic potassium phosphate. Each separation was performed by eluting either the upper phase in the ascending mode or the lower phase in the descending mode, each in clockwise (CW) and counterclockwise column rotation. Better partition efficiencies were attained by the CW rotation in both mobile phases in all the two-phase solvent systems examined. The mathematical analysis also revealed the Coriolis force works favorably under the CW column rotation for both mobile phases. The overall results demonstrated that the Coriolis force produces substantial effects on CPC separation in both organic-aqueous and aqueous-aqueous two-phase systems.

Effect of the thermal environment on the efficiency of packed columns in supercritical fluid chromatography.

PubMed

Zauner, Jordan; Lusk, Ryan; Koski, Steven; Poe, Donald P

2012-11-30

When a packed column is operated at temperatures and pressures near the critical point in supercritical fluid chromatography, the thermal environment in which it is placed has a significant impact on retention and efficiency. We measured the retention factors, plate heights, and related parameters for elution of a test mixture of alkylbenzenes with 5% methanol/95% carbon dioxide mobile phase on a 250 mm × 4.6 mm i.d. column packed with 5-micron Luna-C18 particles. Separations were performed at outlet pressures from 100 to 150 bar and a column oven temperature of 323K. For a bare column thermostated with convective air, significant efficiency losses were observed for outlet pressures equal to or less than 120 bar. These large efficiency losses are attributed to radial temperature gradients. Addition of foam insulation resulted in significant improvements in efficiency. Operating the column in still air using a commercially available column heater provided the best overall performance, with no measurable efficiency loss over the entire range of pressures studied. A reduced plate height of 1.88 was obtained at an optimum flow rate of 3.0 mL/min at 100 bar outlet pressure and with the temperature of the incoming mobile phase set approximately 2.3K above the temperature of the column oven. Retention time repeatability for all three thermal conditions was equal to or less than 0.5% RSD. These results demonstrate that it is possible to perform fast, efficient separations with excellent repeatability using SFC under near-critical conditions if the thermal environment is optimized to minimize the generation of radial temperature gradients. Copyright © 2012 Elsevier B.V. All rights reserved.

A Simplified Method for Sampling and Analysis of High Volume Surface Water for Organic Contaminants Using XAD-2

USGS Publications Warehouse

Datta, S.; Do, L.V.; Young, T.M.

2004-01-01

A simple compressed-gas driven system for field processing and extracting water for subsequent analyses of hydrophobic organic compounds is presented. The pumping device is a pneumatically driven pump and filtration system that can easily clarify at 4L/min. The extraction device uses compressed gas to drive filtered water through two parallel XAD-2 resin columns, at about 200 mL/min. No batteries or inverters are required for water collection or processing. Solvent extractions were performed directly in the XAD-2 glass columns. Final extracts are cleaned-up on Florisil cartridges without fractionation and contaminants analyzed by GC-MS. Method detection limits (MDLs) and recoveries for dissolved organic contaminants, polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs) and pesticides are reported along with results of surface water analysis for the San Francisco Bay, CA.

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

Sesigur, Haluk; Cili, Feridun

Seismic isolation is an effective design strategy to mitigate the seismic hazard wherein the structure and its contents are protected from the damaging effects of an earthquake. This paper presents the Hangar Project in Sabiha Goekcen Airport which is located in Istanbul, Turkey. Seismic isolation system where the isolation layer arranged at the top of the columns is selected. The seismic hazard analysis, superstructure design, isolator design and testing were based on the Uniform Building Code (1997) and met all requirements of the Turkish Earthquake Code (2007). The substructure which has the steel vertical trusses on facades and RC Hmore » shaped columns in the middle axis of the building was designed with an R factor limited to 2.0 in accordance with Turkish Earthquake Code. In order to verify the effectiveness of the isolation system, nonlinear static and dynamic analyses are performed. The analysis revealed that isolated building has lower base shear (approximately 1/4) against the non-isolated structure.« less

Design of a novel coil satellite centrifuge and its performance on counter-current chromatographic separation of 4-methylumbelliferyl sugar derivatives with organic-aqueous two-phase solvent systems

PubMed Central

Shinomiya, Kazufusa; Tokura, Koji; Kimura, Emiru; Takai, Midori; Harikai, Naoki; Yoshida, Kazunori; Yanagidaira, Kazuhiro; Ito, Yoichiro

2015-01-01

A new high-speed counter-current chromatograph, named coil satellite centrifuge (CSC), was designed and fabricated in our laboratory. The CSC apparatus produces the satellite motion such that the coiled column simultaneously rotates around the sun axis (the angular velocity, ω1), the planet axis (ω2) and the satellite axis (the central axis of the column) (ω3). In order to achieve this triplicate rotary motion without twisting of the flow tube, the rotation of each axis was determined by the following formula: ω1 = ω2 + ω3. This relation enabled to lay out the flow tube by two different ways, the SS type and the JS type. In the SS type, the flow tube was introduced from the upper side of the apparatus into the sun axis of the first rotary frame and connected to the planet axis of the second rotary frame like a double letter SS. In the JS type, the flow tube was introduced from the bottom of the apparatus into the sun axis reaching the upper side of the planet axis an inversed letter J, followed by distribution as in the SS type. The performance of the apparatus was examined on separation of 4-methylumbelliferyl (MU) sugar derivatives as test samples with organic-aqueous two-phase solvent systems composed of ethyl acetate/1-butanol/water (3 : 2 : 5, v/v) for lower phase mobile and (1 : 4 : 5, v/v) for upper phase mobile. With lower phase mobile, five 4-MU sugar derivatives including β-D-cellobioside (Cel), β-D-glucopyranoside, α-D-mannopyranoside, β-D-fucopyranoside and α-L-fucopyranoside (α-L-Fuc) were separated with the combined rotation around each axis at counterclockwise (CCW) (ω1) – CCW (ω2) – CCW (ω3) by the JS type flow tube distribution. With upper phase mobile, three 4-MU sugar derivatives including α-L-Fuc, β-D-galactopyranoside and Cel were separated with the combined rotation around each axis at clockwise (CW) (ω1) – CW (ω2) – CW (ω3) by the JS type flow tube distribution. A series of experiments on peak resolution and stationary phase retention revealed that better partition efficiencies were obtained at the flow rate of 0.5 mL/min (column 1) and 0.8 mL/min (column 2) for lower phase mobile and 0.2 mL/min (column 1) and 0.4 mL/min (column 2) for upper phase mobile when using the left-handed multilayer coil (total capacity: 57.0 mL for column 1 and 75.0 mL for column 2) under the rotation speeds of approximately ω1 = 300 rpm, ω2 = 150 rpm and ω3 = 150 rpm. PMID:25805719

Comparison of Eight Years Total Column Ozone Retrievals form Brewer and Dobson Spectrophotometers in South Pole

NASA Astrophysics Data System (ADS)

Feng, K. H.; Moeini, O.; McElroy, C. T.; Evans, R. D.; Petropavlovskikh, I. V.

2015-12-01

Total column ozone measured by a Brewer Mark III spectrophotometer (#85) from 2008 to 2015 is compared to the data obtained from three different Dobson spectrophotometers (#80, #82 and #42) that have been operating in parallel with the Brewer at the Amundsen-Scott Station near the South Pole. Measurements are made using either direct sunlight or light from the moon (up to 2 weeks per month). The result of the comparison was used to assess the performance of the two instrument types and determine the stability of the measurement systems. Both instruments suffer from non-linearity due to the presence of instrumental stray light caused by the out-off-band radiations scattered from the optics within the instrument. Stray light results in an underestimated ozone column at large ozone path lengths. Since measurements made at the location of the station (Latitude 89.99o, Longitude -24.80o) have solar zenith angles of 66.5 degrees or greater, the issue of stray light is a particular concern.

Multivariable model predictive control design of reactive distillation column for Dimethyl Ether production

NASA Astrophysics Data System (ADS)

Wahid, A.; Putra, I. G. E. P.

2018-03-01

Dimethyl ether (DME) as an alternative clean energy has attracted a growing attention in the recent years. DME production via reactive distillation has potential for capital cost and energy requirement savings. However, combination of reaction and distillation on a single column makes reactive distillation process a very complex multivariable system with high non-linearity of process and strong interaction between process variables. This study investigates a multivariable model predictive control (MPC) based on two-point temperature control strategy for the DME reactive distillation column to maintain the purities of both product streams. The process model is estimated by a first order plus dead time model. The DME and water purity is maintained by controlling a stage temperature in rectifying and stripping section, respectively. The result shows that the model predictive controller performed faster responses compared to conventional PI controller that are showed by the smaller ISE values. In addition, the MPC controller is able to handle the loop interactions well.

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

Nash, C.; Williams, M.; Restivo, M.

All prior testing with SuperLig® 639 has been done with the aqueous concentration of LAW at ~5 M [Na+], where the resin sinks, and can be used in a conventional down-flow column orientation. However, the aqueous LAW stream from the Waste Treatment Plant is expected to be ~8 M [Na+]. The resin would float in this higher density liquid, potentially disrupting the ability to achieve a good decontamination due to poor packing of the resin that leads to channeling. Testing was completed with a higher salt concentration in the feed simulant (7.8 M [Na+]) in an engineering-scale apparatus with twomore » columns, each containing ~0.9 L of resin. Testing of this system used a simulant of the LAW solution, and substituted ReO4 - as a surrogate for TcO4 -. Results were then compared using computer modeling. Bench-scale testing was also performed, and examined an unconstrained resin bed, while engineering-scale tests used both constrained and unconstrained beds in a two-column, lead and lag sequential arrangement.« less

Column compression strength of tubular packaging forms made from paper

Treesearch

Thomas J. Urbanik; Sung K. Lee; Charles G. Johnson

2006-01-01

Tubular packaging forms fabricated and shaped from rolled paper are used as reinforcing corner posts for major appliances packaged in corrugated containers. Tests of column compression strength simulate the expected performance loads from appliances stacked in warehouses. Column strength depends on tube geometry, paper properties, basis weight, and number of...

10 CFR Appendix J to Part 110 - Illustrative List of Uranium Conversion Plant Equipment and Plutonium Conversion Plant Equipment...

Code of Federal Regulations, 2010 CFR

2010-01-01

... reactors, flame tower reactors, liquid centrifuges, distillation columns and liquid-liquid extraction... to UF6 is performed by exothermic reaction with fluorine in a tower reactor. UF6 is condensed from..., flame tower reactors, liquid centrifuges, distillation columns and liquid-liquid extraction columns. Hot...

High performance liquid chromatographic determination of caffeine in decaffeinated coffee, tea, and beverage products.

PubMed

Ashoor, S H; Seperich, G J; Monte, W C; Welty, J

1983-05-01

A method was developed for determining caffeine in decaffeinated coffee, tea, and beverage products by high performance liquid chromatography (HPLC). The HPLC system consisted of a Bio-Sil ODS-5S C18 column, methanol-water (25 + 75) mobile phase at 1 mL/min, and a UV detector. The method is simple and specific. Caffeine recoveries were 93.8-98.3% and coefficients of variation were 0.90-2.25%.

Using contemporary liquid chromatography theory and technology to improve capillary gradient ion-exchange separations.

PubMed

Wouters, Bert; Broeckhoven, Ken; Wouters, Sam; Bruggink, Cees; Agroskin, Yury; Pohl, Christopher A; Eeltink, Sebastiaan

2014-11-28

The gradient-performance limits of capillary ion chromatography have been assessed at maximum system pressure (34.5 MPa) using capillary columns packed with 4.1 μm macroporous anion-exchange particles coated with 65 nm positively-charged nanobeads. In analogy to the van-Deemter curve, the gradient performance was assessed applying different flow rates, while decreasing the gradient time inversely proportional to the increase in flow rate in order to maintain the same retention properties. The gradient kinetic-performance limits were determined at maximum system pressure, applying tG/t0=5, 10, and 20. In addition, the effect of retention on peak width was assessed in gradient mode for mono-, di-, and trivalent inorganic anions. The peak width of late-eluting ions can be significantly reduced by using concave gradient, resulting in better detection sensitivity. A signal enhancement factor of 8 was measured for a late-eluting ion when applying a concave instead of a linear gradient. For the analysis of a complex anion mixture, a coupled column with a total length of 1.05 m was operated at the kinetic-performance limit applying a linear 250 min gradient (tG/t0=10). The peak capacity varied between 200 and 380 depending on analyte retention, and hence on charge and size of the ion. Copyright © 2014 Elsevier B.V. All rights reserved.

Comparison of three different C18 HPLC columns with different particle sizes for the optimization of aflatoxins analysis.

PubMed

Medina, A; Magan, N

2012-03-15

In this work we compared the performance of chromatography columns with particles of 5 and 3 μm with the new 2.7 μm solid core particles for the analysis of aflatoxins B1, G1, B2, and G2 using trifluoroacetic acid pre-column derivatization. Three different columns have been used and chromatographic parameters as retention time, resolution, limit of detection (LOD), limit of quantification (LOQ) were obtained from all of them and compared. The results show that comparing with the traditional columns, shorter columns (100 mm × 4.6 mm) with the new solid core particles are suitable for the analysis of these mycotoxins and allowed the reduction of the analysis time by 45.5% and 33.3% with respect to columns with particle size 5 μm (150 mm × 4.6 mm) and 3 μm (150 mm × 4.6 mm) respectively, without any detrimental effect on performance. This leads to the reduction of the analysis costs by saving on organic solvents and increasing the total number of analyses per day. The capability of these columns for analyzing samples, in different culture media, was assessed by analyzing different samples from: yeasts extract sucrose medium, corn meal agar medium and fresh hazelnut media. Copyright © 2012 Elsevier B.V. All rights reserved.

Modelling dynamic transport and adsorption of arsenic in soil-bed filters for long-term performance evaluation

NASA Astrophysics Data System (ADS)

Mondal, Sourav; Mondal, Raka; de, Sirshendu; Griffiths, Ian

2017-11-01

Purification of contaminated water following the safe water guidelines while generating sufficiently large throughput is a crucial requirement for the steady supply of safe water to large populations. Adsorption-based filtration processes using a multilayer soil bed has been posed as a viable method to achieve this goal. This work describes the theory of operation and prediction of the long-term behaviour of such a system. The fixed-bed column has a single input of contaminated water from the top and an output from the bottom. As the contaminant passes through the column, it is adsorbed by the medium. Like any other adsorption medium, the filter has a certain lifespan, beyond which the filtrate does not meet the safe limit of drinking water, which is defined as `breakthrough'. A mathematical model is developed that couples the fluid flow through the porous medium to the convective, diffusive and adsorptive transport of the contaminant. The results are validated with experimental observations and the model is then used to predict the breakthrough and lifetime of the filter. The key advantage of this model is that it can predict the long-term behaviour of any adsorption column system for any set of physical characteristics of the system. This worked was supported by the EPSRC Global Challenge Research Fund Institutional Sponsorship 2016.

Critical assessment of three high performance liquid chromatography analytical methods for food carotenoid quantification.

PubMed

Dias, M Graça; Oliveira, Luísa; Camões, M Filomena G F C; Nunes, Baltazar; Versloot, Pieter; Hulshof, Paul J M

2010-05-21

Three sets of extraction/saponification/HPLC conditions for food carotenoid quantification were technically and economically compared. Samples were analysed for carotenoids alpha-carotene, beta-carotene, beta-cryptoxanthin, lutein, lycopene, and zeaxanthin. All methods demonstrated good performance in the analysis of a composite food standard reference material for the analytes they are applicable to. Methods using two serial connected C(18) columns and a mobile phase based on acetonitrile, achieved a better carotenoid separation than the method using a mobile phase based on methanol and one C(18)-column. Carotenoids from leafy green vegetable matrices appeared to be better extracted with a mixture of methanol and tetrahydrofuran than with tetrahydrofuran alone. Costs of carotenoid determination in foods were lower for the method with mobile phase based on methanol. However for some food matrices and in the case of E-Z isomer separations, this was not technically satisfactory. Food extraction with methanol and tetrahydrofuran with direct evaporation of these solvents, and saponification (when needed) using pyrogallol as antioxidant, combined with a HPLC system using a slight gradient mobile phase based on acetonitrile and a stationary phase composed by two serial connected C(18) columns was the most technically and economically favourable method. 2010. Published by Elsevier B.V.

Two-dimensional chromatographic analysis using three second-dimension columns for continuous comprehensive analysis of intact proteins.

PubMed

Zhu, Zaifang; Chen, Huang; Ren, Jiangtao; Lu, Juan J; Gu, Congying; Lynch, Kyle B; Wu, Si; Wang, Zhe; Cao, Chengxi; Liu, Shaorong

2018-03-01

We develop a new two-dimensional (2D) high performance liquid chromatography (HPLC) approach for intact protein analysis. Development of 2D HPLC has a bottleneck problem - limited second-dimension (second-D) separation speed. We solve this problem by incorporating multiple second-D columns to allow several second-D separations to be proceeded in parallel. To demonstrate the feasibility of using this approach for comprehensive protein analysis, we select ion-exchange chromatography as the first-dimension and reverse-phase chromatography as the second-D. We incorporate three second-D columns in an innovative way so that three reverse-phase separations can be performed simultaneously. We test this system for separating both standard proteins and E. coli lysates and achieve baseline resolutions for eleven standard proteins and obtain more than 500 peaks for E. coli lysates. This is an indication that the sample complexities are greatly reduced. We see less than 10 bands when each fraction of the second-D effluents are analyzed by sodium dodecyl sulfate - polyacrylamide gel electrophoresis (SDS-PAGE), compared to hundreds of SDS-PAGE bands as the original sample is analyzed. This approach could potentially be an excellent and general tool for protein analysis. Copyright © 2017 Elsevier B.V. All rights reserved.

Cross flow cyclonic flotation column for coal and minerals beneficiation

DOEpatents

Lai, Ralph W.; Patton, Robert A.

2000-01-01

An apparatus and process for the separation of coal from pyritic impurities using a modified froth flotation system. The froth flotation column incorporates a helical track about the inner wall of the column in a region intermediate between the top and base of the column. A standard impeller located about the central axis of the column is used to generate a centrifugal force thereby increasing the separation efficiency of coal from the pyritic particles and hydrophillic tailings.

Electrophoretic fractional elution apparatus employing a rotational seal fraction collector

NASA Technical Reports Server (NTRS)

Bier, M. (Inventor)

1977-01-01

Electrophoretic fractional elution apparatus which has a column with a rotating seal joint is described. A thin jet of eluting buffer is directed across the lumen of the electrophoretic column in a direction perpendicular to that of electrophoretic migration. Either the content of the column is rotated with respect to the stationary jet, or the jet is rotated with respect to the column. The system may employ electrophoresis either in free solution or in packed columns.

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.

Limestone and Zeolite as Alternative Media in Horizontal Subsurface Flow Constructed Wetlands: Laboratory-Scale Studies

NASA Astrophysics Data System (ADS)

Lizama, K.; Jaque, I.; Ayala, J.

2016-12-01

Arsenic is well known for its chronic toxicity. Millions of people around the world are currently at risk, drinking water with As concentrations above 10 ppb, the WHO drinking water guideline. Although different treatment options exist, they are often limited by elevated costs and maintenance requirements. Constructed wetlands are a natural water treatment system, capable to remove metals and metalloids -including As- via different physical, chemical and biological processes. The use of alternative supporting media to enhance As removal in subsurface flow wetlands has been recommended, but not sufficiently studied. Limestone and zeolite have been identified as effective supporting media in subsurface flow wetlands aiming As removal. However, there are still key aspects to be addressed, such as the implications of using these media, the speciation in the solid phase, the role of vegetation, etc. This study investigated the performance of limestone and zeolite in three types of experiments: batch, column and as main supporting media in a bench scale horizontal subsurface flow wetland system. Synthetic water resembling a contaminated river in Chile (As concentration=3 mg/L, Fe concentration= 100 mg/L, pH=2) was used in all experiments. In the batch experiments, the As concentration, the mass of media and the contact time were varied. The column system consisted of three limestone columns and three zeolite columns, operated under a hydraulic loading of 20 mm/d. The wetland system consisted of twelve PVC cells: six filled with zeolite and six with limestone. Phragmites australis were planted in three cells of each media type, as control cells. From the batch experiments, maximum As sorption capacities as indicated by Langmuir model were 1.3 mg/g for limestone and 0.17 mg/g for zeolite, at 18 h contact time and 6.3 g/L medium concentration. EDS and XPS analyses revealed that As and Fe were retained in zeolite at the end of the batch experiments. Zeolite and limestone columns presented As removal >99.5% on average. In the wetland system, As removal percentages were also similar between media types, regardless of the presence of vegetation: For limestone, removal percentages were 99.7% and 99.6%, for vegetated and non-vegetated cells respectively; whereas for zeolite, removal percentages were 99.8% and 99.7% respectively.

Determination of citrus limonoid glucosides by high performance liquid chromatography coupled to post-column reaction with Ehrlich’s Reagent

USDA-ARS?s Scientific Manuscript database

A method for the identification and quantification of citrus limonoid glucosides in juices based upon high performance liquid chromatography (HPLC) separation coupled to post-column reaction with Ehrlichs’s reagent has been developed. This method utilizes a phenyl stationary phase and an isocratic ...

One-pot preparation of a sulfamethoxazole functionalized affinity monolithic column for selective isolation and purification of trypsin.

PubMed

Xiao, Yuan; Guo, Jialiang; Ran, Danni; Duan, Qianqian; Crommen, Jacques; Jiang, Zhengjin

2015-06-26

A facile and efficient "one-pot" copolymerization strategy was used for the preparation of sulfonamide drug (SA) functionalized monolithic columns. Two novel SA-immobilized methacrylate monolithic columns, i.e. poly(GMA-SMX-co-EDMA) and poly(GMA-SAA-co-EDMA) were prepared by one-pot in situ copolymerization of the drug ligand (sulfamethoxazole (SMX) or sulfanilamide (SAA)), the monomer (glycidyl methacrylate, GMA) and the cross-linker (ethylene dimethacrylate, EDMA) within 100 μm i.d. capillaries under optimized polymerization conditions. The physicochemical properties and column performance of the fabricated monolithic columns were characterized by elemental analysis, scanning electron microscopy and micro-HPLC. Satisfactory column permeability, efficiency and separation performance were obtained on the optimized poly(GMA-SMX-co-EDMA) monolithic column for small molecules, such as a standard test mixture and eight aromatic ketones. Notably, it was found that the poly(GMA-SMX-co-EDMA) monolith showed a selective affinity to trypsin, while the poly(GMA-SAA-co-EDMA) monolith containing sulfanilamide did not exhibit such affinity at all. This research not only provides a novel monolith for the selective isolation and purification of trypsin, but it also offers the possibility to easily prepare novel drug functionalized methacrylate monoliths through a one-pot copolymerization strategy. Copyright © 2015 Elsevier B.V. All rights reserved.

10 CFR Appendix J to Part 110 - Illustrative List of Uranium Conversion Plant Equipment and Plutonium Conversion Plant Equipment...

Code of Federal Regulations, 2011 CFR

2011-01-01

... reactors, flame tower reactors, liquid centrifuges, distillation columns and liquid-liquid extraction... UF4 to UF6 is performed by exothermic reaction with fluorine in a tower reactor. UF6 is condensed from..., flame tower reactors, liquid centrifuges, distillation columns and liquid-liquid extraction columns. Hot...

Investigation of Gas Holdup in a Vibrating Bubble Column

NASA Astrophysics Data System (ADS)

Mohagheghian, Shahrouz; Elbing, Brian

2015-11-01

Synthetic fuels are part of the solution to the world's energy crisis and climate change. Liquefaction of coal during the Fischer-Tropsch process in a bubble column reactor (BCR) is a key step in production of synthetic fuel. It is known from the 1960's that vibration improves mass transfer in bubble column. The current study experimentally investigates the effect that vibration frequency and amplitude has on gas holdup and bubble size distribution within a bubble column. Air (disperse phase) was injected into water (continuous phase) through a needle shape injector near the bottom of the column, which was open to atmospheric pressure. The air volumetric flow rate was measured with a variable area flow meter. Vibrations were generated with a custom-made shaker table, which oscillated the entire column with independently specified amplitude and frequency (0-30 Hz). Geometric dependencies can be investigated with four cast acrylic columns with aspect ratios ranging from 4.36 to 24, and injector needle internal diameters between 0.32 and 1.59 mm. The gas holdup within the column was measured with a flow visualization system, and a PIV system was used to measure phase velocities. Preliminary results for the non-vibrating and vibrating cases will be presented.

Modeling of intensity-modulated continuous-wave laser absorption spectrometer systems for atmospheric CO(2) column measurements.

PubMed

Lin, Bing; Ismail, Syed; Wallace Harrison, F; Browell, Edward V; Nehrir, Amin R; Dobler, Jeremy; Moore, Berrien; Refaat, Tamer; Kooi, Susan A

2013-10-10

The focus of this study is to model and validate the performance of intensity-modulated continuous-wave (IM-CW) CO(2) laser absorption spectrometer (LAS) systems and their CO(2) column measurements from airborne and satellite platforms. The model accounts for all fundamental physics of the instruments and their related CO(2) measurement environments, and the modeling results are presented statistically from simulation ensembles that include noise sources and uncertainties related to the LAS instruments and the measurement environments. The characteristics of simulated LAS systems are based on existing technologies and their implementation in existing systems. The modeled instruments are specifically assumed to be IM-CW LAS systems such as the Exelis' airborne multifunctional fiber laser lidar (MFLL) operating in the 1.57 μm CO(2) absorption band. Atmospheric effects due to variations in CO(2), solar radiation, and thin clouds, are also included in the model. Model results are shown to agree well with LAS atmospheric CO(2) measurement performance. For example, the relative bias errors of both MFLL simulated and measured CO(2) differential optical depths were found to agree to within a few tenths of a percent when compared to the in situ observations from the flight of 3 August 2011 over Railroad Valley (RRV), Nevada, during the summer 2011 flight campaign. In addition, the horizontal variations in the model CO(2) differential optical depths were also found to be consistent with those from MFLL measurements. In general, the modeled and measured signal-to-noise ratios (SNRs) of the CO(2) column differential optical depths (τd) agreed to within about 30%. Model simulations of a spaceborne IM-CW LAS system in a 390 km dawn/dusk orbit for CO(2) column measurements showed that with a total of 42 W of transmitted power for one offline and two different sideline channels (placed at different locations on the side of the CO(2) absorption line), the accuracy of the τd measurements for surfaces similar to the playa of RRV, Nevada, will be better than 0.1% for 10 s averages. For other types of surfaces such as low-reflectivity snow and ice surfaces, the precision and bias errors will be within 0.23% and 0.1%, respectively. Including thin clouds with optical depths up to 1, the SNR of the τd measurements with 0.1 s integration period for surfaces similar to the playa of RRV, Nevada, will be greater than 94 and 65 for sideline positions placed +3 and +10  pm, respectively, from the CO(2) line center at 1571.112 nm. The CO(2) column bias errors introduced by the thin clouds are ≤0.1% for cloud optical depth ≤0.4, but they could reach ∼0.5% for more optically thick clouds with optical depths up to 1. When the cloud and surface altitudes and scattering amplitudes are obtained from matched filter analysis, the cloud bias errors can be further reduced. These results indicate that the IM-CW LAS instrument approach when implemented in a dawn/dusk orbit can make accurate CO(2) column measurements from space with preferential weighting across the mid to lower troposphere in support of a future ASCENDS mission.

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.

Comparison of UHPLC and HPLC in benzodiazepines analysis of postmortem samples: a case-control study.

PubMed

Behnoush, Behnam; Sheikhazadi, Ardeshir; Bazmi, Elham; Fattahi, Akbar; Sheikhazadi, Elham; Saberi Anary, Seyed Hossein

2015-04-01

The aim of this study was to compare system efficiency and analysis duration regarding the solvent consumption and system maintenance in high-pressure liquid chromatography (HPLC) and ultra high-pressure liquid chromatography (UHPLC). In a case-control study, standard solutions of 7 benzodiazepines (BZs) and 73 biological samples such as urine, tissue, stomach content, and bile that screened positive for BZs were analyzed by HPLC and UHPLC in laboratory of forensic toxicology during 2012 to 2013. HPLC analysis was performed using a Knauer by 100-5 C-18 column (250 mm × 4.6 mm) and Knauer photodiode array detector (PAD). UHPLC analysis was performed using Knauer PAD detector with cooling autosampler and Eurospher II 100-3 C-18 column (100 mm × 3 mm) and also 2 pumps. The mean retention time, standard deviation, flow rate, and repeatability of analytical results were compared by using 2 methods. Routine runtimes in HPLC and UHPLC took 40 and 15 minutes, respectively. Changes in mobile phase composition of the 2 methods were not required. Flow rate and solvent consumption in UHPLC decreased. Diazepam and flurazepam were detected more frequently in biological samples. In UHPLC, small particle size and short length of column cause effective separation of BZs in a very short time. Reduced flow rate, solvent consumption, and injection volume cause more efficiency and less analysis costs. Thus, in the detection of BZs, UHPLC is an accurate, sensitive, and fast method with less cost of analysis.

Thought-based row-column scanning communication board for individuals with cerebral palsy.

PubMed

Scherer, Reinhold; Billinger, Martin; Wagner, Johanna; Schwarz, Andreas; Hettich, Dirk Tassilo; Bolinger, Elaina; Lloria Garcia, Mariano; Navarro, Juan; Müller-Putz, Gernot

2015-02-01

Impairment of an individual's ability to communicate is a major hurdle for active participation in education and social life. A lot of individuals with cerebral palsy (CP) have normal intelligence, however, due to their inability to communicate, they fall behind. Non-invasive electroencephalogram (EEG) based brain-computer interfaces (BCIs) have been proposed as potential assistive devices for individuals with CP. BCIs translate brain signals directly into action. Motor activity is no longer required. However, translation of EEG signals may be unreliable and requires months of training. Moreover, individuals with CP may exhibit high levels of spontaneous and uncontrolled movement, which has a large impact on EEG signal quality and results in incorrect translations. We introduce a novel thought-based row-column scanning communication board that was developed following user-centered design principles. Key features include an automatic online artifact reduction method and an evidence accumulation procedure for decision making. The latter allows robust decision making with unreliable BCI input. Fourteen users with CP participated in a supporting online study and helped to evaluate the performance of the developed system. Users were asked to select target items with the row-column scanning communication board. The results suggest that seven among eleven remaining users performed better than chance and were consequently able to communicate by using the developed system. Three users were excluded because of insufficient EEG signal quality. These results are very encouraging and represent a good foundation for the development of real-world BCI-based communication devices for users with CP. Copyright © 2015 Elsevier Masson SAS. All rights reserved.

Comparison of UHPLC and HPLC in Benzodiazepines Analysis of Postmortem Samples

PubMed Central

Behnoush, Behnam; Sheikhazadi, Ardeshir; Bazmi, Elham; Fattahi, Akbar; Sheikhazadi, Elham; Saberi Anary, Seyed Hossein

2015-01-01

Abstract The aim of this study was to compare system efficiency and analysis duration regarding the solvent consumption and system maintenance in high-pressure liquid chromatography (HPLC) and ultra high-pressure liquid chromatography (UHPLC). In a case–control study, standard solutions of 7 benzodiazepines (BZs) and 73 biological samples such as urine, tissue, stomach content, and bile that screened positive for BZs were analyzed by HPLC and UHPLC in laboratory of forensic toxicology during 2012 to 2013. HPLC analysis was performed using a Knauer by 100-5 C-18 column (250 mm × 4.6 mm) and Knauer photodiode array detector (PAD). UHPLC analysis was performed using Knauer PAD detector with cooling autosampler and Eurospher II 100-3 C-18 column (100 mm × 3 mm) and also 2 pumps. The mean retention time, standard deviation, flow rate, and repeatability of analytical results were compared by using 2 methods. Routine runtimes in HPLC and UHPLC took 40 and 15 minutes, respectively. Changes in mobile phase composition of the 2 methods were not required. Flow rate and solvent consumption in UHPLC decreased. Diazepam and flurazepam were detected more frequently in biological samples. In UHPLC, small particle size and short length of column cause effective separation of BZs in a very short time. Reduced flow rate, solvent consumption, and injection volume cause more efficiency and less analysis costs. Thus, in the detection of BZs, UHPLC is an accurate, sensitive, and fast method with less cost of analysis. PMID:25860209

GC-MS quantification of suspected volatile allergens in fragrances. 2. Data treatment strategies and method performances.

PubMed

Bassereau, Maud; Chaintreau, Alain; Duperrex, Stéphanie; Joulain, Daniel; Leijs, Hans; Loesing, Gerd; Owen, Neil; Sherlock, Alan; Schippa, Christine; Thorel, Pierre-Jean; Vey, Matthias

2007-01-10

The performances of the GC-MS determination of suspected allergens in fragrance concentrates have been investigated. The limit of quantification was experimentally determined (10 mg/L), and the variability was investigated for three different data treatment strategies: (1) two columns and three quantification ions; (2) two columns and one quantification ion; and (3) one column and three quantification ions. The first strategy best minimizes the risk of determination bias due to coelutions. This risk was evaluated by calculating the probability of coeluting a suspected allergen with perfume constituents exhibiting ions in common. For hydroxycitronellal, when using a two-column strategy, this may statistically occur more than once every 36 analyses for one ion or once every 144 analyses for three ions in common.

Silver-modified mobile phase for normal-phase liquid chromatographic determination of prostaglandins and their 5,6-trans isomers in prostaglandin bulk drugs and triacetin solutions.

PubMed

Kissinger, L D; Robins, R H

1985-03-15

A silver-modified, normal-phase, high-performance liquid chromatographic system has been developed for prostaglanding bulk drugs and triacetin solutions. Silver nitrate present in the mobile phase results in high selectivity for cis/trans isomers with conventional silica columns. Prostaglandins were esterified with alpha-bromo-2'-acetonaphthone prior to chromatography to provide high detectability at 254 nm. For dilute triacetin solutions, a sample preparation scheme based on gravity-flow chromatography with silica columns was developed to isolate the prostaglandin from triacetin prior to derivatization. The analytical technique was applied to triacetin solutions containing as little as 10 micrograms/ml arbaprostil [15-(R)-methyl-PGE2].

New Insights in Tropospheric Ozone and its Variability

NASA Technical Reports Server (NTRS)

Oman, Luke D.; Douglass, Anne R.; Ziemke, Jerry R.; Rodriquez, Jose M.

2011-01-01

We have produced time-slice simulations using the Goddard Earth Observing System Version 5 (GEOS-5) coupled to a comprehensive stratospheric and tropospheric chemical mechanism. These simulations are forced with observed sea surface temperatures over the past 25 years and use constant specified surface emissions, thereby providing a measure of the dynamically controlled ozone response. We examine the model performance in simulating tropospheric ozone and its variability. Here we show targeted comparisons results from our simulations with a multi-decadal tropical tropospheric column ozone dataset obtained from satellite observations of total column ozone. We use SHADOZ ozonesondes to gain insight into the observed vertical response and compare with the simulated vertical structure. This work includes but is not limited to ENSO related variability.

SEMG-controlled telephone interface for people with disabilities.

PubMed

Chen, Yu-Luen; Lai, Jin-Shin; Luh, Jer-Junn; Kuo, Te-Son

2002-01-01

This paper proposes the development of a surface electromyographic (SEMG)-controlled telephone interface for the disabled. The system is composed of three major components: (1) a SEMG receiving/signal-processing module; (2) a row-column scanning interface for the telephone dialling pad; and (3) a main controller, the Intel-8951 microprocessor. The design concept was based on the idea of using a SEMG generated by the disabled and converting it into a trigger pulse. This could allow convenient control of the dialing motion in the row-column scanning keys of a telephone dialling pad. People with disabilities are competent for certain kinds of work such as being a telephone operator. The increase of opportunities to perform a job for the disabled would help them live independently.

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.

Application of a Fast Separation Method for Anti-diabetics in Pharmaceuticals Using Monolithic Column: Comparative Study With Silica Based C-18 Particle Packed Column.

PubMed

Hemdan, A; Abdel-Aziz, Omar

2018-04-01

Run time is a predominant factor in HPLC for quality control laboratories especially if there is large number of samples have to be analyzed. Working at high flow rates cannot be attained with silica based particle packed column due to elevated backpressure issues. The use of monolithic column as an alternative to traditional C-18 column was tested for fast separation of pharmaceuticals, where the results were very competitive. The performance comparison of both columns was tested for separation of anti-diabetic combination containing Metformin, Pioglitazone and Glimepiride using Gliclazide as an internal standard. Working at high flow rates with less significant backpressure was obtained with the monolithic column where the run time was reduced from 6 min in traditional column to only 1 min in monolithic column with accepted resolution. The structure of the monolith contains many pores which can adapt the high flow rate of the mobile phase. Moreover, peak symmetry and equilibration time were more efficient with monolithic column.

Design of two-column batch-to-batch recirculation to enhance performance in ion-exchange chromatography.

PubMed

Persson, Oliver; Andersson, Niklas; Nilsson, Bernt

2018-01-05

Preparative liquid chromatography is a separation technique widely used in the manufacturing of fine chemicals and pharmaceuticals. A major drawback of traditional single-column batch chromatography step is the trade-off between product purity and process performance. Recirculation of impure product can be utilized to make the trade-off more favorable. The aim of the present study was to investigate the usage of a two-column batch-to-batch recirculation process step to increase the performance compared to single-column batch chromatography at a high purity requirement. The separation of a ternary protein mixture on ion-exchange chromatography columns was used to evaluate the proposed process. The investigation used modelling and simulation of the process step, experimental validation and optimization of the simulated process. In the presented case the yield increases from 45.4% to 93.6% and the productivity increases 3.4 times compared to the performance of a batch run for a nominal case. A rapid concentration build-up product can be seen during the first cycles, before the process reaches a cyclic steady-state with reoccurring concentration profiles. The optimization of the simulation model predicts that the recirculated salt can be used as a flying start of the elution, which would enhance the process performance. The proposed process is more complex than a batch process, but may improve the separation performance, especially while operating at cyclic steady-state. The recirculation of impure fractions reduces the product losses and ensures separation of product to a high degree of purity. Copyright © 2017 Elsevier B.V. All rights reserved.

Looking East at Motor Control System, Clarity Columns and Blend ...

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

Looking East at Motor Control System, Clarity Columns and Blend Tank Along East Side of Recycle Recovery Building - Hematite Fuel Fabrication Facility, Recycle Recovery Building, 3300 State Road P, Festus, Jefferson County, MO

Fault-tolerant Control of a Cyber-physical System

NASA Astrophysics Data System (ADS)

Roxana, Rusu-Both; Eva-Henrietta, Dulf

2017-10-01

Cyber-physical systems represent a new emerging field in automatic control. The fault system is a key component, because modern, large scale processes must meet high standards of performance, reliability and safety. Fault propagation in large scale chemical processes can lead to loss of production, energy, raw materials and even environmental hazard. The present paper develops a multi-agent fault-tolerant control architecture using robust fractional order controllers for a (13C) cryogenic separation column cascade. The JADE (Java Agent DEvelopment Framework) platform was used to implement the multi-agent fault tolerant control system while the operational model of the process was implemented in Matlab/SIMULINK environment. MACSimJX (Multiagent Control Using Simulink with Jade Extension) toolbox was used to link the control system and the process model. In order to verify the performance and to prove the feasibility of the proposed control architecture several fault simulation scenarios were performed.

Pesticide dissipation and microbial community changes in a biopurification system: influence of the rhizosphere.

PubMed

Diez, M C; Elgueta, S; Rubilar, O; Tortella, G R; Schalchli, H; Bornhardt, C; Gallardo, F

2017-12-01

The dissipation of atrazine, chlorpyrifos and iprodione in a biopurification system and changes in the microbial and some biological parameters influenced by the rhizosphere of Lolium perenne were studied in a column system packed with an organic biomixture. Three column depths were analyzed for residual pesticides, peroxidase, fluorescein diacetate activity and microbial communities. Fungal colonization was analyzed by confocal laser scanning microscopy to assess the extent of its proliferation in wheat straw. The L. perenne rhizosphere enhanced pesticide dissipation and negligible pesticide residues were detected at 20-30 cm column depth. Atrazine, chlorpyrifos and iprodione removal was 82, 89 and 74% respectively in the first 10 cm depth for columns with vegetal cover. The presence of L. perenne in contaminated columns stimulated peroxidase activity in all three column depth sections. Fluorescein diacetate activity decreased over time in all column sections with the highest values in biomixtures with vegetal cover. Microbial communities, analyzed by PCR-DGGE, were not affected by the pesticide mixture application, presenting high values of similarity (>65%) with and without vegetal cover. Microbial abundance of Actinobacteria varied according to treatment and no clear link was observed. However, bacterial abundance increased over time and was similar with and without vegetal cover. On the other hand, fungal abundance decreased in all sections of columns after 40 days, but an increase was observed in response to pesticide application. Fungal colonization and straw degradation during pesticide dissipation were verified by monitoring the lignin autofluorescence loss.

High sensitivity detection of bisphenol A using liposome chromatography.

PubMed

Liu, Xue-Ying; Nakamura, Chikashi; Tanimoto, Itsuro; Miyake, Shiro; Nakamura, Noriyuki; Hirano, Takashi; Miyake, Jun

2006-09-18

An antibody column in tandem with a fluorescent dye entrapped liposome column was developed for highly sensitive detection of an endocrine disruptor, bisphenol A (BPA). Anti-BPA antibody was immobilized in a protein G column with orientation control. A derivative of BPA was conjugated to phospholipase A2 (PLA2). BPA sample solutions mixed with the BPA-PLA2 conjugates were injected on to the anti-BPA antibody column and competitive binding occurred in the antibody column. The amount of the free conjugate was proportional to the concentration of the BPA sample. The eluted conjugates were injected on to the second column gel on which calcein-entrapped liposomes were immobilized and the PLA2-catalyzed hydrolysis of liposomal phospholipids causing fluorescent dye leakage as a signal amplification. In this system, the mixture of BPA and BPA-PLA2 conjugate were incubated for 60 min in the anti-BPA column, and then the collected solution was applied to the liposome column. The BPA detection range of 0.02-140 ng mL(-1) was wider than 0.03-6.6 ng mL(-1) obtained by the method of competitive ELISA using the same antibody. Moreover, this system could be adapted to an HPLC system resulting in almost the same detection limit in online detection. The method could be applied to environmental samples, river water and soil extracts. The BPA concentration of 0.1 ng mL(-1) and 10 ng g(-1) was detectable in water and soil extract, respectively.

9. Detail view of columns on first floor. This row ...

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

9. Detail view of columns on first floor. This row of columns indicates the former location of the exterior mill wall before World War II era expansion. The unusual column and beam connection was a key part of the mill structural system patented by Providence, Rhode Island engineers Charles Praray and Charles Makepeace in 1894. Each column was originally located in the apex of triangular window bay, but not connected to the exterior wall. Modifications on the right side of each column support the beams of the addition. - Dixie Cotton Mill, 710 Greenville Street, La Grange, Troup County, GA

The Impact of IBM Cell Technology on the Programming Paradigm in the Context of Computer Systems for Climate and Weather Models

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

Zhou, Shujia; Duffy, Daniel; Clune, Thomas

The call for ever-increasing model resolutions and physical processes in climate and weather models demands a continual increase in computing power. The IBM Cell processor's order-of-magnitude peak performance increase over conventional processors makes it very attractive to fulfill this requirement. However, the Cell's characteristics, 256KB local memory per SPE and the new low-level communication mechanism, make it very challenging to port an application. As a trial, we selected the solar radiation component of the NASA GEOS-5 climate model, which: (1) is representative of column physics components (half the total computational time), (2) has an extremely high computational intensity: the ratiomore » of computational load to main memory transfers, and (3) exhibits embarrassingly parallel column computations. In this paper, we converted the baseline code (single-precision Fortran) to C and ported it to an IBM BladeCenter QS20. For performance, we manually SIMDize four independent columns and include several unrolling optimizations. Our results show that when compared with the baseline implementation running on one core of Intel's Xeon Woodcrest, Dempsey, and Itanium2, the Cell is approximately 8.8x, 11.6x, and 12.8x faster, respectively. Our preliminary analysis shows that the Cell can also accelerate the dynamics component (~;;25percent total computational time). We believe these dramatic performance improvements make the Cell processor very competitive as an accelerator.« less

Mini-column assay for rapid detection of malachite green in fish.

PubMed

Shalaby, Ali R; Emam, Wafaa H; Anwar, Mervat M

2017-07-01

A simple, rapid and economical mini-column method for detecting malachite green (MG) residue in fish was developed. The method used a column with 2mm ID that was tightly packed with silica gel followed by alumina. Detection of MG was performed by viewing the developed mini-column at visible light by naked eye; where MG was seen as compact green band at the confluence of the silica gel layer with alumina layer. The limit of detection of the assay was 2ng which conform the minimum required performance limit (MRPL). Evaluation utility of the method indicated that all blank and spiked samples at levels below MRPL were assessed as accepted. The intensity of the green band increased whenever MG level in the extract increased; indicated that suggested mini-column technique could be used for semi-quantitative determination of MG in fish samples. The method can be used to select the questionable samples. Copyright © 2017 Elsevier Ltd. All rights reserved.

Comprehensive two-dimensional chromatography with coupling of reversed phase high performance liquid chromatography and supercritical fluid chromatography.

PubMed

Stevenson, Paul G; Tarafder, Abhijit; Guiochon, Georges

2012-01-13

A 2D comprehensive chromatographic separation of blackberry sage fragrant oil was performed by using HPLC in the first dimension and SFC in the second. A C(18)-bonded silica column eluted with an ACN gradient was used in the HPLC dimension and an amino-bonded silica column eluted with ACN as a modifier in the SFC dimension. This 2D separation was completed in the off-line mode, the fractions from the HPLC column being collected and injected in the SFC column. The retention factors on the two columns have a -0.757 correlation coefficient. The method provides a practical peak capacity of 2400 in 280 min. The first eluted peaks in HPLC are the last ones eluted in SFC and vice versa. The results demonstrate that the coupling of an HPLC and an SFC separation have a great potential for 2D chromatographic separations. Copyright © 2011 Elsevier B.V. All rights reserved.

Highly sensitive assay for tyrosine hydroxylase activity by high-performance liquid chromatography.

PubMed

Nagatsu, T; Oka, K; Kato, T

1979-07-21

A highly sensitive assay for tyrosine hydroxylase (TH) activity by high-performance liquid chromatography (HPLC) with amperometric detection was devised based on the rapid isolation of enzymatically formed DOPA by a double-column procedure, the columns fitted together sequentially (the top column of Amberlite CG-50 and the bottom column of aluminium oxide). DOPA was adsorbed on the second aluminium oxide column, then eluted with 0.5 M hydrochloric acid, and assayed by HPLC with amperometric detection. D-Tyrosine was used for the control. alpha-Methyldopa was added to the incubation mixture as an internal standard after incubation. This assay was more sensitive than radioassays and 5 pmol of DOPA formed enzymatically could be measured in the presence of saturating concentrations of tyrosine and 6-methyltetrahydropterin. The TH activity in 2 mg of human putamen could be easily measured, and this method was found to be particularly suitable for the assay of TH activity in a small number of nuclei from animal and human brain.

Investigation of the column performance of cadmium(II) biosorption by Cladophora crispata flocs in a packed bed

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

Aksu, Z.; Kutsal, T.; Caglar, A.

1998-03-01

In this study the biosorption of cadmium(II) ions to dried flocs of Cladophora crispata, a kind of green algae, was investigated in a packed bed column. The cadmium(II) removal performance of the column was investigated as a function of the cadmium(II)-bearing solution flow rate and the inlet cadmium(II) concentration. Removal and total removal percentages of cadmium(II) related to flow volume were determined by evaluating the breakthrough curves obtained at three different flow rates for two different constant inlet concentrations. At the lowest flow rate the effect of inlet cadmium(II) concentration on the column capacity was also investigated. Data confirmed thatmore » early saturation and lower cadmium(II) removals were observed at higher flow rates and at higher cadmium(II) concentrations. Column experiments also showed that maximum specific cadmium(II) uptake values of C. crispata flocs were as high as those of other biomass sorbents.« less

Status of the NOAO evaluation of the Hughes 20x64 Si:As impurity band conduction array. [for ground and space-based astronomy

NASA Technical Reports Server (NTRS)

Fowler, A. M.; Joyce, R. R.

1990-01-01

The Hughes 20 x 64 Si:As impurity band conduction arrays designed for ground-based and spaceborne astronomy observations is described together with experiments performed at NOAO to test these arrays. Special attention is given to the design and the characteristics of the test system and to the test methods. The initial tests on two columns of one array indicate that the array is easy to operate and performed satisfactorily.

Impacts of the IBM Cell Processor to Support Climate Models

NASA Technical Reports Server (NTRS)

Zhou, Shujia; Duffy, Daniel; Clune, Tom; Suarez, Max; Williams, Samuel; Halem, Milt

2008-01-01

NASA is interested in the performance and cost benefits for adapting its applications to the IBM Cell processor. However, its 256KB local memory per SPE and the new communication mechanism, make it very challenging to port an application. We selected the solar radiation component of the NASA GEOS-5 climate model, which: (1) is representative of column physics (approximately 50% computational time), (2) has a high computational load relative to transferring data from and to main memory, (3) performs independent calculations across multiple columns. We converted the baseline code (single-precision, Fortran) to C and ported it with manually SIMDizing 4 independent columns and found that a Cell with 8 SPEs can process 2274 columns per second. Compared with the baseline results, the Cell is approximately 5.2X, approximately 8.2X, approximately 15.1X faster than a core on Intel Woodcrest, Dempsey, and Itanium2, respectively. We believe this dramatic performance improvement makes a hybrid cluster with Cell and traditional nodes competitive.

Removal of Cr(VI) from groundwater by Fe(0)

NASA Astrophysics Data System (ADS)

Gao, Yanjiao; Liu, Rui

2017-11-01

This research was conducted to investigate the treatment of hexavalent chromium (Cr(VI)) by iron powder (Fe(0)) columns of simulated permeable reactive barriers with and without calcium carbonate (CaCO3). Two columns filled with Fe(0) were used as Cr(VI) removal equipment running at a flow velocity of 10 ml/min at room temperature. After 200 days running of the two columns, the results showed that Fe(0) was an effective material for Cr(VI) reduction with an average removal rate of above 84.6%. The performance of Column 2 with CaCO3 was better than Column 1 without CaCO3 in terms of average Cr(VI) removal rate. The presence of CaCO3 buffered the increasing pH caused by Fe(0) corrosion in Column 2 and enhanced the removal rate of Column 2. Scanning Electron Microscopy (SEM) images of Fe(0) in the three stages of running of the two columns illustrated that the coat layer of Column 1 was a little thicker than that of Column 2. Energy-dispersive spectrometry (EDS) results showed that the surface of Fe(0) of Column 2 contained more chromium elements. Raman spectroscopy found that all iron oxide was generated on the Fe(0) surface of Column 1 and Column 2 and chromium class objects were only detected on Fe(0) surface in Column 2.

Engineering solutions to improve the removal of fecal indicator bacteria by bioinfiltration systems during intermittent flow of stormwater.

PubMed

Mohanty, Sanjay K; Torkelson, Andrew A; Dodd, Hanna; Nelson, Kara L; Boehm, Alexandria B

2013-10-01

Bioinfiltration systems facilitate the infiltration of urban stormwater into soil and reduce high flow events and flooding. Stormwater carries a myriad of pollutants including fecal indicator bacteria (FIB). Significant knowledge gaps exist about the ability of bioinfiltration systems to remove and retain FIB. The present study investigates the ability of model, simplified bioinfiltration systems containing quartz sand and iron oxide-coated quartz sand (IOCS) to remove two FIB (Enterococcus faecalis and Escherichia coli) suspended in synthetic stormwater with and without natural organic matter (NOM) as well as the potential for accumulated FIB to be remobilized during intermittent flow. The experiments were conducted in two phases: (1) the saturated columns packed with either sand or IOCS were contaminated by injecting stormwater with bacteria followed by injection of sterile stormwater and (2) the contaminated columns were subjected to intermittent infiltration of sterile stormwater preceded by a pause during which columns were either kept saturated or drained by gravity. During intermittent flow, fewer bacteria were released from the saturated column compared to the column drained by gravity: 12% of attached E. coli and 3% of attached Ent. faecalis were mobilized from the drained sand column compared to 3% of attached E. coli and 2% attached Ent. faecalis mobilized from the saturated sand column. Dry and wet cycles introduce moving air-water interfaces that can scour bacteria from grain surfaces. During intermittent flows, less than 0.2% of attached bacteria were mobilized from IOCS, which bound both bacteria irreversibly in the absence of NOM. Addition of NOM, however, increased bacterial mobilization from IOCS: 50% of attached E. coli and 8% of attached Ent. faecalis were released from IOCS columns during draining and rewetting. Results indicate that using geomedia such as IOCS that promote irreversible attachment of bacteria, and maintaining saturated condition, could minimize the mobilization of previous attached bacteria from bioinfiltration systems, although NOM may significantly decrease these benefits.

High-speed and high-resolution UPLC separation at zero degrees Celsius

PubMed Central

Wales, Thomas E.; Fadgen, Keith E.; Gerhardt, Geoff C.; Engen, John R.

2008-01-01

The conformational properties of proteins can be probed with hydrogen/deuterium exchange mass spectrometry (HXMS). In order to maintain the deuterium label during LC/MS analyses, chromatographic separation must be done rapidly (usually in under 8–10 minutes) and at zero degrees Celsius. Traditional RP-HPLC with ~3 micron particles has shown generally poor chromatographic performance under these conditions and thereby has been prohibitive for HXMS analyses of larger proteins and many protein complexes. Ultra performance liquid chromatography (UPLC) employs particles smaller than 2 microns in diameter to achieve superior resolution, speed, and sensitivity as compared to HPLC. UPLC has previously been shown to be compatible with the fast separation and low temperature requirements of HXMS. Here we present construction and validation of a custom UPLC system for HXMS. The system is based on the Waters nanoACQUITY platform and contains a Peltier-cooled module that houses the injection and switching valves, online pepsin digestion column, and C-18 analytical separation column. Single proteins in excess of 95 kDa and a four-protein mixture in excess of 250 kDa have been used to validate the performance of this new system. Near baseline resolution was achieved in 6 minute separations at 0 °C and displayed a median chromatographic peak width of ~2.7 sec at half height. Deuterium recovery was similar to that obtained using a conventional HPLC and icebath. This new system represents a significant advancement in HXMS technology that is expected to make the technique more accessible and mainstream in the near future. PMID:18672890

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.

Separation of carbon nanotubes into chirally enriched fractions

DOEpatents

Doorn, Stephen K [Los Alamos, NM; Niyogi, Sandip [Los Alamos, NM

2012-04-10

A mixture of single-walled carbon nanotubes ("SWNTs") is separated into fractions of enriched chirality by preparing an aqueous suspension of a mixture of SWNTs and a surfactant, injecting a portion of the suspension on a column of separation medium having a density gradient, and centrifuging the column. In some embodiments, salt is added prior to centrifugation. In other embodiments, the centrifugation is performed at a temperature below room temperature. Fractions separate as colored bands in the column. The diameter of the separated SWNTs decreases with increasing density along the gradient of the column. The colored bands can be withdrawn separately from the column.

Core-Shell in Liquid Chromatography: Application for Determining Sulphonamides in Feed and Meat Using Conventional Chromatographic Systems

PubMed Central

Armentano, Antonio; Summa, Simona; Magro, Sonia Lo; D’Antini, Pasquale; Palermo, Carmen; Muscarella, Marilena

2016-01-01

A C18 column packed with core-shell particles was used for the chromatographic separation of sulphonamides in feed and meat by a conventional high performance liquid chromatography system coupled with a diode array detector. Two analytical methods, already used in our laboratory, have been modified without any changes in the extraction and clean-up steps and in the liquid chromatography instrumentation. Chromatographic conditions applied on a traditional 5-µm column have been optimized on a column packed with 2.6 µm core-shell particles. A binary mobile phase [acetate buffer solution at pH 4.50 and a mixture of methanol acetonitrile 50: 50 (v/v)] was employed in gradient mode at the flow rate of 1.2 mL with an injection volume of 6 µL. These chromatographic conditions allow the separation of 13 sulphonamides with an entire run of 13 minutes. Preliminary studies have been carried out comparing blanks and spiked samples of feed and meat. A good resolution and the absence of interferences were achieved in chromatograms for both matrices. Since no change was made to the sample preparation, the optimized method does not require a complete revalidation and can be used to make routine analysis faster. PMID:28217560

40 CFR Appendix E to Part 63 - Monitoring Procedure for Nonthoroughly Mixed Open Biological Treatment Systems at Kraft Pulp...

Code of Federal Regulations, 2014 CFR

2014-07-01

... for each data set that is collected during the initial performance test. A single composite value of... Multiple Zone Concentrations Calculations Procedure based on inlet and outlet concentrations (Column A of... composite value of Ks discussed in section III.C of this appendix. This value of Ks is calculated during the...

Experiments on water detritiation and cryogenic distillation at TLK; Impact on ITER fuel cycle subsystems interfaces

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

Cristescu, I.; Cristescu, I. R.; Doerr, L.

2008-07-15

The ITER Isotope Separation System (ISS) and Water Detritiation System (WDS) should be integrated in order to reduce potential chronic tritium emissions from the ISS. This is achieved by routing the top (protium) product from the ISS to a feed point near the bottom end of the WDS Liquid Phase Catalytic Exchange (LPCE) column. This provides an additional barrier against ISS emissions and should mitigate the memory effects due to process parameter fluctuations in the ISS. To support the research activities needed to characterize the performances of various components for WDS and ISS processes under various working conditions and configurationsmore » as needed for ITER design, an experimental facility called TRENTA representative of the ITER WDS and ISS protium separation column, has been commissioned and is in operation at TLK The experimental program on TRENTA facility is conducted to provide the necessary design data related to the relevant ITER operating modes. The operation availability and performances of ISS-WDS have impact on ITER fuel cycle subsystems with consequences on the design integration. The preliminary experimental data on TRENTA facility are presented. (authors)« less

49 CFR 393.209 - Steering wheel systems.

Code of Federal Regulations, 2011 CFR

2011-10-01

... Transportation Other Regulations Relating to Transportation (Continued) FEDERAL MOTOR CARRIER SAFETY ADMINISTRATION, DEPARTMENT OF TRANSPORTATION FEDERAL MOTOR CARRIER SAFETY REGULATIONS PARTS AND ACCESSORIES...) Steering column. The steering column must be securely fastened. (d) Steering system. Universal joints and...

49 CFR 393.209 - Steering wheel systems.

Code of Federal Regulations, 2013 CFR

2013-10-01

... Transportation Other Regulations Relating to Transportation (Continued) FEDERAL MOTOR CARRIER SAFETY ADMINISTRATION, DEPARTMENT OF TRANSPORTATION FEDERAL MOTOR CARRIER SAFETY REGULATIONS PARTS AND ACCESSORIES...) Steering column. The steering column must be securely fastened. (d) Steering system. Universal joints and...

49 CFR 393.209 - Steering wheel systems.

Code of Federal Regulations, 2014 CFR

2014-10-01

... Transportation Other Regulations Relating to Transportation (Continued) FEDERAL MOTOR CARRIER SAFETY ADMINISTRATION, DEPARTMENT OF TRANSPORTATION FEDERAL MOTOR CARRIER SAFETY REGULATIONS PARTS AND ACCESSORIES...) Steering column. The steering column must be securely fastened. (d) Steering system. Universal joints and...

49 CFR 393.209 - Steering wheel systems.

Code of Federal Regulations, 2010 CFR

2010-10-01

... Transportation Other Regulations Relating to Transportation (Continued) FEDERAL MOTOR CARRIER SAFETY ADMINISTRATION, DEPARTMENT OF TRANSPORTATION FEDERAL MOTOR CARRIER SAFETY REGULATIONS PARTS AND ACCESSORIES...) Steering column. The steering column must be securely fastened. (d) Steering system. Universal joints and...

49 CFR 393.209 - Steering wheel systems.

Code of Federal Regulations, 2012 CFR

2012-10-01

... Transportation Other Regulations Relating to Transportation (Continued) FEDERAL MOTOR CARRIER SAFETY ADMINISTRATION, DEPARTMENT OF TRANSPORTATION FEDERAL MOTOR CARRIER SAFETY REGULATIONS PARTS AND ACCESSORIES...) Steering column. The steering column must be securely fastened. (d) Steering system. Universal joints and...

Experiment and modeling for the separation of guaifenesin enantiomers using simulated moving bed and Varicol units.

PubMed

Gong, Rujin; Lin, Xiaojian; Li, Ping; Yu, Jianguo; Rodrigues, Alirio E

2014-10-10

The separation of guaifenesin enantiomers by both simulated moving bed (SMB) process and Varicol process was investigated experimentally and theoretically, where the columns were packed with cellulose tris 3,5-dimethylphenylcarbamate (Chiralcel OD) stationary phase and a mixture of n-hexane and ethanol was used as mobile phase. The operation conditions were designed based on the separation region with the consideration of mass transfer resistance and axial dispersion, and the experiments to separate guaifenesin enantiomers were carried out on VARICOL-Micro unit using SMB process with the column configuration of 1/2/2/1 and Varicol process with the column configuration of 1/1.5/1.5/1, respectively. Single enantiomer with more than 99.0% purity was obtained in both processes with the productivity of 0.42 genantiomer/dcm(3) CSP for SMB process and 054 genantiomer/dcm(3) CSP for Varicol process. These experimental results obtained from SMB and Varicol processes were compared with those reported from literatures. In addition, according to the numerical simulation, the effects of solid-film mass transfer resistance and axial dispersion on the internal profiles were discussed, and the effect of column configuration on the separation performance of SMB and Varicol processes was analyzed for a few columns system. The feasibility and efficiency for the separation of guaifenesin enantiomers by SMB and Varicol processes were evaluated. Copyright © 2014 Elsevier B.V. All rights reserved.

Unraveling the Fate and Transport of SrEDTA-2 and Sr+2 in Hanford Sediments

NASA Astrophysics Data System (ADS)

Pace, M. N.; Mayes, M. A.; Jardine, P. M.; Mehlhorn, T. L.; Liu, Q. G.; Yin, X. L.

2004-12-01

Accelerated migration of strontium-90 has been observed in the vadose zone beneath the Hanford tank farm. The goal of this paper is to provide an improved understanding of the hydrogeochemical processes that contribute to strontium transport in the far-field Hanford vadose zone. Laboratory scale batch, saturated packed column experiments, and an unsaturated transport experiment in an undisturbed core were conducted to quantify geochemical and hydrological processes controlling Sr+2 and SrEDTA-2 sorption to Hanford flood deposits. After experimentation, the undisturbed core was disassembled and samples were collected from different bedding units as a function of depth. Sequential extractions were then performed on the samples. It has been suggested that organic chelates such as EDTA may be responsible for the accelerated transport of strontium due to the formation of stable anionic complexes. Duplicate batch and column experiments performed with Sr+2 and SrEDTA-2 suggested that the SrEDTA-2 complex was not stable in the presence of soil and rapid dissociation allowed strontium to be transported as a divalent cation. Batch experiments indicated a decrease in sorption with increasing rock:water ratios, whereas saturated packed column experiments indicated equal retardation in columns of different lengths. This difference between the batch and column experiments is primarily due to the difference between equilibrium conditions where dissolution of cations may compete for sorption sites versus flowing conditions where any dissolved cations are flushed through the system minimizing competition for sorption sites. Unsaturated transport in the undisturbed core resulted in significant Sr+2 retardation despite the presence of physical nonequilibrium. Core disassembly and sequential extractions revealed the mass wetness distribution and reactive mineral phases associated with strontium in the core. Overall, results indicated that strontium will most likely be transported through the Hanford far-field vadose zone as a divalent cation.

Three-column classification and Schatzker classification: a three- and two-dimensional computed tomography characterisation and analysis of tibial plateau fractures.

PubMed

Patange Subba Rao, Sheethal Prasad; Lewis, James; Haddad, Ziad; Paringe, Vishal; Mohanty, Khitish

2014-10-01

The aim of the study was to evaluate inter-observer reliability and intra-observer reproducibility between the three-column classification and Schatzker classification systems using 2D and 3D CT models. Fifty-two consecutive patients with tibial plateau fractures were evaluated by five orthopaedic surgeons. All patients were classified into Schatzker and three-column classification systems using x-rays and 2D and 3D CT images. The inter-observer reliability was evaluated in the first round and the intra-observer reliability was determined during the second round 2 weeks later. The average intra-observer reproducibility for the three-column classification was from substantial to excellent in all sub classifications, as compared with Schatzker classification. The inter-observer kappa values increased from substantial to excellent in three-column classification and to moderate in Schatzker classification The average values for three-column classification for all the categories are as follows: (I-III) k2D = 0.718, 95% CI 0.554-0.864, p < 0.0001 and average 3D = 0.874, 95% CI 0.754-0.890, p < 0.0001. For Schatzker classification system, the average values for all six categories are as follows: (I-VI) k2D = 0.536, 95% CI 0.365-0.685, p < 0.0001 and average k3D = 0.552 95% CI 0.405-0.700, p < 0.0001. The values are statistically significant. Statistically significant inter-observer values in both rounds were noted with the three-column classification, making it statistically an excellent agreement. The intra-observer reproducibility for the three-column classification improved as compared with the Schatzker classification. The three-column classification seems to be an effective way to characterise and classify fractures of tibial plateau.

IN-SITU REMEDIATION OF ARSENIC IN SIMULATED GROUNDWATER USING ZEROVALENT IRON: LABORATORY COLUMN TESTS ON COMBINED EFFECTS OF PHOSPHATE AND SILICATE

EPA Science Inventory

We performed three column tests to study the behavior of permeable reactive barrier (PRB) materials to remove arsenic under dynamic flow conditions in the absence, as well as in the presence, of added phosphate and silicate. The column consisted of a 10.3-cm depth of 50 : 50 (w :...

49 CFR 173.240 - Bulk packaging for certain low hazard solid materials.

Code of Federal Regulations, 2014 CFR

2014-10-01

... this subchapter and the special provisions specified in column 7 of the § 172.101 table. (a) Rail cars... the IBC packaging code specified for the specific hazardous material in Column (7) of the § 172.101... subchapter at the Packing Group performance level as specified in Column (5) of the § 172.101 Table of this...

49 CFR 173.240 - Bulk packaging for certain low hazard solid materials.

Code of Federal Regulations, 2012 CFR

2012-10-01

... this subchapter and the special provisions specified in column 7 of the § 172.101 table. (a) Rail cars... the IBC packaging code specified for the specific hazardous material in Column (7) of the § 172.101... subchapter at the Packing Group performance level as specified in Column (5) of the § 172.101 Table of this...

49 CFR 173.240 - Bulk packaging for certain low hazard solid materials.

Code of Federal Regulations, 2011 CFR

2011-10-01

... this subchapter and the special provisions specified in column 7 of the § 172.101 table. (a) Rail cars... the IBC packaging code specified for the specific hazardous material in Column (7) of the § 172.101... subchapter at the Packing Group performance level as specified in Column (5) of the § 172.101 Table of this...

49 CFR 173.240 - Bulk packaging for certain low hazard solid materials.

Code of Federal Regulations, 2013 CFR

2013-10-01

... this subchapter and the special provisions specified in column 7 of the § 172.101 table. (a) Rail cars... the IBC packaging code specified for the specific hazardous material in Column (7) of the § 172.101... subchapter at the Packing Group performance level as specified in Column (5) of the § 172.101 Table of this...

49 CFR 173.240 - Bulk packaging for certain low hazard solid materials.

Code of Federal Regulations, 2010 CFR

2010-10-01

... this subchapter and the special provisions specified in column 7 of the § 172.101 table. (a) Rail cars... the IBC packaging code specified for the specific hazardous material in Column (7) of the § 172.101... subchapter at the Packing Group performance level as specified in Column (5) of the § 172.101 Table of this...

Determination of nitrite, nitrate, bromide, and iodide in seawater by ion chromatography with UV detection using dilauryldimethylammonium-coated monolithic ODS columns and sodium chloride as an eluent.

PubMed

Ito, Kazuaki; Nomura, Ryosuke; Fujii, Takuya; Tanaka, Masahito; Tsumura, Tomoaki; Shibata, Hiroyuki; Hirokawa, Takeshi

2012-11-01

A method was developed for determination of inorganic anions, including nitrite (NO(2)(-)), nitrate (NO(3)(-)), bromide (Br(-)), and iodide (I(-)), in seawater by ion chromatography (IC). The IC system used two dilauryldimethylammonium bromide (DDAB)-coated monolithic ODS columns (50 × 4.6 mm i.d. and 100 × 4.6 mm i.d.) connected in series for separation of the ions. Aqueous NaCl (0.5 mol/L; flow rate, 3 mL/min) containing 5 mmol/L phosphate buffer (pH 5) was used as the eluent, and detection was with a UV detector at 225 nm. The monolithic ODS columns were coated and equilibrated with a 1-mmol/L DDAB solution (in H(2)O/methanol, 90:10 v/v). The hydrophilic ions (NO(2)(-), NO(3)(-), and Br(-)) were separated within 3 min and the retention time of I(-) was 16 min. No interferences from matrix ions, such as chloride and sulfate ions, were observed in 35 ‰ artificial seawater. The detection limits were 0.6 μg/L for NO(2)(-), 1.1 μg/L for NO(3)(-), 70 μg/L for Br(-), and 1.6 μg/L for I(-) with a 200-μL sample injection. The performance of the coated columns was maintained without addition of DDAB in the eluent. The IC system was successfully applied to real seawater samples with recovery rates of 94-108 % for all ions.

Radionuclide Sensors and Systems for Monitoring Technetium-99 and Strontium-90 in Groundwater at the Hanford Site

NASA Astrophysics Data System (ADS)

Grate, J. W.; O'Hara, M. J.; Egorov, O. B.; Burge, S. R.

2009-12-01

We have developed automated sensor and analyzer devices for detection and monitoring of trace radionuclides in water, using preconcentrating columns and radiometric detection. The preconcentrating minicolumn sensor concept combines selective capture and detection in a single functional unit, where the column contains tens to hundreds of milligrams of selectively sorbent material, and the entire column content is monitored with a radiometric detector. Compared to thin film sensors with a few microgram of sorbent, this approach achieves tremendous preconcentration with efficient mass transport via pumping. Furthermore, in an equilibration-based mode of operation, the preconcentration by the sensor is maximized while eliminating the need for consumable reagents to regenerate the column; it can simply be re-equilibrated. We have demonstrated quantification of radionuclides such as technetium-99 to levels below drinking water standards in an equilibration-based process that produces steady state signals, signal proportional to concentration, and easy re-equilibration to new concentration levels. Alternatively, analyzers can be developed with separate separation and detection units that are fluidically linked. We have demonstrated detection of strontium-90 to levels below drinking water standards by this approach. We are developing autonomous systems for at-site monitoring on the Hanford Site in Washington State, using the fluidic sensor and analyzer methods, with the aim of monitoring natural and accelerated attenuation processes, remediation and barrier performance, and contaminant fluxes in the environment. Figure 1. The strontium-90 monitoring method deployed as part of the Burge Environmental Universal Sensor Platform, shown on the shores of the Columbia River on the Hanford site in Washington State.

40 CFR Appendix A to Subpart C of... - Alternative Testing Methods Approved for Analyses Under the Safe Drinking Water Act

Code of Federal Regulations, 2013 CFR

2013-07-01

... Chromatography/Mass Spectrometry (GC/MS) 525.3 24 Carbofuran High-performance liquid chromatography (HPLC) with... (HPLC) with Post-Column Derivatization and Fluorescence Detection 6651 B 6651 B 6651 B-00. Heptachlor... Spectrometry (GC/MS) 525.3 24 Oxamyl High-performance liquid chromatography (HPLC) with post-column...

(99)Tc(VII) Retardation, Reduction, and Redox Rate Scaling in Naturally Reduced Sediments.

PubMed

Liu, Yuanyuan; Liu, Chongxuan; Kukkadapu, Ravi K; McKinley, James P; Zachara, John; Plymale, Andrew E; Miller, Micah D; Varga, Tamas; Resch, Charles T

2015-11-17

An experimental and modeling study was conducted to investigate pertechnetate (Tc(VII)O4(-)) retardation, reduction, and rate scaling in three sediments from Ringold formation at U.S. Department of Energy's Hanford site, where (99)Tc is a major contaminant in groundwater. Tc(VII) was reduced in all the sediments in both batch reactors and diffusion columns, with a faster rate in a sediment containing a higher concentration of HCl-extractable Fe(II). Tc(VII) migration in the diffusion columns was reductively retarded with retardation degrees correlated with Tc(VII) reduction rates. The reduction rates were faster in the diffusion columns than those in the batch reactors, apparently influenced by the spatial distribution of redox-reactive minerals along transport paths that supplied Tc(VII). X-ray computed tomography and autoradiography were performed to identify the spatial locations of Tc(VII) reduction and transport paths in the sediments, and results generally confirmed the newly found behavior of reaction rate changes from batch to column. The results from this study implied that Tc(VII) migration can be reductively retarded at Hanford site with a retardation degree dependent on reactive Fe(II) content and its distribution in sediments. This study also demonstrated that an effective reaction rate may be faster in transport systems than that in well-mixed reactors.

Removal of diclofenac and sulfamethoxazole from synthetic municipal waste water in microcosm downflow constructed wetlands: Start-up results.

PubMed

Nowrotek, Monika; Sochacki, Adam; Felis, Ewa; Miksch, Korneliusz

2016-01-01

The objectives of this study were to investigate the start-up removal of pharmaceutical compounds diclofenac and sulfamethoxazole in microcosm downflow constructed wetlands and their effect on the performance of the studied constructed wetlands, and also to assess the effect of plants on the removal of these compounds. The experimental system that was used in this 86-day experiment consisted of 24 columns filled up to 70 cm with predominantly sandy material. Four types of columns were used (six replicates) depending on the presence of plants (Phalaris arundinacea L. var. picta L.) and the presence of pharmaceutical compounds in the influent. The influent was synthetic municipal waste water to which a mixture of 5 mg/L of diclofenac and 5 mg/L of sulfamethoxazole was added. The observed removal of diclofenac was moderate (approx. 50%) and the removal of sulfamethoxazole was relatively low (24-30%). It was found that the removal of diclofenac and sulfamethoxazole was not affected by the vegetation. The presence of diclofenac and sulfamethoxazole in the influent had significant effect on the effluent concentration of N-NO3 and the water loss in the columns, which in both cases were lower than in the control columns. The scope for further research was discussed.

Titanium-scaffolded organic-monolithic stationary phases for ultra-high-pressure liquid chromatography.

PubMed

Vonk, Rudy J; Vaast, Axel; Eeltink, Sebastiaan; Schoenmakers, Peter J

2014-09-12

Organic-polymer monoliths with overall dimensions larger than one millimetre are prone to rupture - either within the monolith itself or between the monoliths and the containing wall - due to the inevitable shrinkage accompanying the formation of a cross-linked polymeric network. This problem has been addressed by creating titanium-scaffolded poly(styrene-co-divinylbenzene) (S-co-DVB) monoliths. Titanium-scaffolded monoliths were successfully used in liquid chromatography at very high pressures (up to 80MPa) and using gradients spanning the full range of water-acetonitrile compositions (0 to 100%). The kinetic-performance of (50-mm long) titanium-scaffolded monoliths was compared to that of similar monolith created in 1-mm i.d. glass-lined tubing at pressures up to 50MPa. The peak capacities obtained with the titanium-scaffolded column was about 30% lower. An increased Eddy-diffusion, due to the pillar-structure, and a decreased permeability are thought to be the main reasons for this reduced kinetic-performance. No decrease in performance was observed when the titanium-scaffolded columns were operated at pressures of 80MPa for up to 12h. The column-to-column repeatability (n=5) was acceptable in terms of observed peak widths at half heights (RSD ca. 10%) The run-to-run repeatability (n=135) in terms of retention times and peak widths at half height were found to be good. Titanium-scaffolded columns coupled in series up to a combined length of (200mm) were used for the analyses of a complex Escherichia coli protein sample. Our experiments demonstrate that columns based on titanium-scaffolded organic-polymer monolith can be operated under strenuous conditions without loss in performance. The titanium-scaffolded approach makes it feasible to create organic-polymer monoliths in wide-bore columns with accurate temperature control. Copyright © 2014 Elsevier B.V. All rights reserved.

The effect of column purification on cDNA indirect labelling for microarrays

PubMed Central

Molas, M Lia; Kiss, John Z

2007-01-01

Background The success of the microarray reproducibility is dependent upon the performance of standardized procedures. Since the introduction of microarray technology for the analysis of global gene expression, reproducibility of results among different laboratories has been a major problem. Two of the main contributors to this variability are the use of different microarray platforms and different laboratory practices. In this paper, we address the latter question in terms of how variation in one of the steps of a labelling procedure affects the cDNA product prior to microarray hybridization. Results We used a standard procedure to label cDNA for microarray hybridization and employed different types of column chromatography for cDNA purification. After purifying labelled cDNA, we used the Agilent 2100 Bioanalyzer and agarose gel electrophoresis to assess the quality of the labelled cDNA before its hybridization onto a microarray platform. There were major differences in the cDNA profile (i.e. cDNA fragment lengths and abundance) as a result of using four different columns for purification. In addition, different columns have different efficiencies to remove rRNA contamination. This study indicates that the appropriate column to use in this type of protocol has to be experimentally determined. Finally, we present new evidence establishing the importance of testing the method of purification used during an indirect labelling procedure. Our results confirm the importance of assessing the quality of the sample in the labelling procedure prior to hybridization onto a microarray platform. Conclusion Standardization of column purification systems to be used in labelling procedures will improve the reproducibility of microarray results among different laboratories. In addition, implementation of a quality control check point of the labelled samples prior to microarray hybridization will prevent hybridizing a poor quality sample to expensive micorarrays. PMID:17597522

The effect of column purification on cDNA indirect labelling for microarrays.

PubMed

Molas, M Lia; Kiss, John Z

2007-06-27

The success of the microarray reproducibility is dependent upon the performance of standardized procedures. Since the introduction of microarray technology for the analysis of global gene expression, reproducibility of results among different laboratories has been a major problem. Two of the main contributors to this variability are the use of different microarray platforms and different laboratory practices. In this paper, we address the latter question in terms of how variation in one of the steps of a labelling procedure affects the cDNA product prior to microarray hybridization. We used a standard procedure to label cDNA for microarray hybridization and employed different types of column chromatography for cDNA purification. After purifying labelled cDNA, we used the Agilent 2100 Bioanalyzer and agarose gel electrophoresis to assess the quality of the labelled cDNA before its hybridization onto a microarray platform. There were major differences in the cDNA profile (i.e. cDNA fragment lengths and abundance) as a result of using four different columns for purification. In addition, different columns have different efficiencies to remove rRNA contamination. This study indicates that the appropriate column to use in this type of protocol has to be experimentally determined. Finally, we present new evidence establishing the importance of testing the method of purification used during an indirect labelling procedure. Our results confirm the importance of assessing the quality of the sample in the labelling procedure prior to hybridization onto a microarray platform. Standardization of column purification systems to be used in labelling procedures will improve the reproducibility of microarray results among different laboratories. In addition, implementation of a quality control check point of the labelled samples prior to microarray hybridization will prevent hybridizing a poor quality sample to expensive micorarrays.

Generating multiple independent retention index data in dual-secondary column comprehensive two-dimensional gas chromatography.

PubMed

Bieri, Stefan; Marriott, Philip J

2006-12-01

A method producing simultaneously three retention indexes for compounds has been developed for comprehensive two-dimensional gas chromatography by using a dual secondary column approach (GC x 2GC). For this purpose, the primary flow of the first dimension column was equally diverted into two secondary microbore columns of identical geometry by means of a three-way flow splitter positioned after the longitudinally modulated cryogenic system. This configuration produced a pair of comprehensive two-dimensional chromatograms and generated retention data on three different stationary phases in a single run. First dimension retention indexes were determined on a polar SolGel-Wax column under linear programmed-temperature conditions according to the van den Dool approach using primary alcohol homologues as the reference scale. Calculation of pseudoisothermal retention indexes in both second dimensions was performed on low-polarity 5% phenyl equivalent polysilphenylene/siloxane (BPX5) and 14% cyanopropylphenyl/86% dimethylpolysiloxane (BP10) columns. To construct a retention correlation map in the second dimension separation space upon which KovAts indexes can be derived, two methods exploiting "isovolatility" relationships of alkanes were developed. The first involved 15 sequential headspace samplings of selected n-alkanes by solid-phase microextraction (SPME), with each sampling followed by their injection into the GC at predetermined times during the chromatographic run. The second method extended the second dimension retention map and consisted of repetitive introduction of SPME-sampled alkane mixtures at various isothermal conditions incremented over the temperature program range. Calculated second dimension retention indexes were compared with experimental values obtained in conventional one-dimensional GC. A case study mixture including 24 suspected allergens (i.e., fragrance ingredients) was used to demonstrate the feasibility and potential of retention index information in comprehensive 2D-GC.

Remote calorimetric detection of urea via flow injection analysis

PubMed Central

Gaddes, David E.; Demirel, Melik C.; Reeves, W. Brian; Tadigadapa, Srinivas

2017-01-01

The design and development of a calorimetric biosensing system enabling relatively high throughput sample analysis are reported. The calorimetric biosensor system consists of a thin (~20 μm) micromachined Y-cut quartz crystal resonator (QCR) as a temperature sensor placed in close proximity to a fluidic chamber packed with an immobilized enzyme. Layer by layer enzyme immobilization of urease is demonstrated and its activity as a function of the number of layers, pH, and time has been evaluated. This configuration enables a sensing system where a transducer element is physically separated from the analyte solution of interest and is thereby free from fouling effects typically associated with biochemical reactions occuring on the sensor surface. The performance of this biosensing system is demonstrated by detection of 1–200 mM urea in phosphate buffer via a flow injection analysis (FIA) technique. Miniaturized fluidic systems were used to provide continuous flow through a reaction column. Under this configuration the biosensor has an ultimate resolution of less than 1 mM urea and showed a linear response between 0–50 mM. This work demonstrates a sensing modality in which the sensor itself is not fouled or contaminated by the solution of interest and the enzyme immobilized Kapton® fluidic reaction column can be used as a disposable cartridge. Such a system enables reuse and reliability for long term sampling measurements. Based on this concept a biosensing system is envisioned which can perform rapid measurements to detect biomarkers such as glucose, creatinine, cholesterol, urea and lactate in urine and blood continuously over extended periods of time. PMID:26479269

Remote calorimetric detection of urea via flow injection analysis.

PubMed

Gaddes, David E; Demirel, Melik C; Reeves, W Brian; Tadigadapa, Srinivas

2015-12-07

The design and development of a calorimetric biosensing system enabling relatively high throughput sample analysis are reported. The calorimetric biosensor system consists of a thin (∼20 μm) micromachined Y-cut quartz crystal resonator (QCR) as a temperature sensor placed in close proximity to a fluidic chamber packed with an immobilized enzyme. Layer by layer enzyme immobilization of urease is demonstrated and its activity as a function of the number of layers, pH, and time has been evaluated. This configuration enables a sensing system where a transducer element is physically separated from the analyte solution of interest and is thereby free from fouling effects typically associated with biochemical reactions occuring on the sensor surface. The performance of this biosensing system is demonstrated by detection of 1-200 mM urea in phosphate buffer via a flow injection analysis (FIA) technique. Miniaturized fluidic systems were used to provide continuous flow through a reaction column. Under this configuration the biosensor has an ultimate resolution of less than 1 mM urea and showed a linear response between 0-50 mM. This work demonstrates a sensing modality in which the sensor itself is not fouled or contaminated by the solution of interest and the enzyme immobilized Kapton® fluidic reaction column can be used as a disposable cartridge. Such a system enables reuse and reliability for long term sampling measurements. Based on this concept a biosensing system is envisioned which can perform rapid measurements to detect biomarkers such as glucose, creatinine, cholesterol, urea and lactate in urine and blood continuously over extended periods of time.

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

Seco, J; Giantsoudi, D; Eaton, BR

Purpose: To investigate the trade-off between vertebral column sparing and thecal-sac target coverage in craniospinal irradiation (CSI) of pediatric patients treated with passive-scattering (PS) and intensity modulated (IMPT) proton therapy. Methods: We selected 2 pediatric patients treated with PS CSI for medulloblastoma. Spinal irradiation was re-planned with IMPT. For all cases, we assumed prescription dose of 23.4 Gy(RBE), with the spinal canal receiving at least 95% of 23.4 Gy(RBE). PS planning was performed using the commercial system XiO. IMPT planning was done using the Astroid planning system. Beam arrangements consisted of (a) PS posterior-anterior (PA) field, PS-PA, (b) IMPT PAmore » field, IMPT-PA, and (c) two posterior oblique IMPT fields, IMPT2 (-35°, 35°). Dose distributions were re-calculated using TOPAS Monte Carlo, along with LET distributions, to investigate LET variations within the target and vertebra anatomy. Variable RBE-weighed dose distributions were also calculated based on a dose and LET-dependent biophysical model. Dosimetric data were compared among the plans for the target volume, spinal cord and adjacent critical organs (thecal-sac and cauda equina). Results: IMPT2 resulted in better sparing of the posterior vertebral column (entrance region posterior to thecal-sac), where planned dose was approximately 6–8Gy(RBE). For IMPT-PA and PS-PA the MC-calculated dose to the posterior vertebral column was, on average, 20Gy and 18Gy respectively. For IMPT2 higher mean-LET (5keV/µm/(g/cm3)) values were observed in anterior vertebral column (beyond the thecal-sac) relative to IMPT-PA and PS-PA, where mean-LET was 3.5keV/µm/(g/cm3) and 2.5keV/µm/(g/cm3) respectively. The higher LET region observed for both IMPT plans was in the distal end of treatment fields, where dose delivered was less 5Gy(RBE). Conclusion: The two-oblique proton beams IMPT2 best spared the spinal column, while reducing the dose to the posterior spinal column from 18–20 to 6–8 Gy(RBE). The best LET distribution was obtained with the PS-PA fields.« less

Design and Operation of Cryogenic Distillation Research Column for Ultra-Low Background Experiments

NASA Astrophysics Data System (ADS)

Chiller, Christopher; Alanson Chiller, Angela; Jasinski, Benjamin; Snyder, Nathan; Mei, Dongming

2013-04-01

Motivated by isotopically enriched germanium (76Ge and 73Ge) for monocrystalline crystal growth for neutrinoless double-beta decay and dark matter experiments, a cryogenic distillation research column was developed. Without market availability of distillation columns in the temperature range of interest with capabilities necessary for our purposes, we designed, fabricated, tested, refined and operated a two-meter research column for purifying and separating gases in the temperature range from 100-200K. Due to interest in defining stratification, purity and throughput optimization, capillary lines were integrated at four equidistant points along the length of the column such that real-time residual gas analysis could guide the investigation. Interior gas column temperatures were monitored and controlled within 0.1oK accuracy at the top and bottom. Pressures were monitored at the top of the column to four significant figures. Subsequent impurities were measured at partial pressures below 2E-8torr. We report the performance of the column in this paper.

Isotopic generator for bismuth-212 and lead-212 based on radium

DOEpatents

Hines, J.J.; Atcher, R.W.; Friedman, A.M.

1985-01-30

Disclosed are method and apparatus for providing radionuclides of bismuth-212 and lead-212. Thorium-228 and carrier solution starting material is input to a radiologically contained portion of an isotopic generator system, and radium-224 is separated from thorium-228 which is retained by a strongly basic anion exchange column. The separated radium-224 is transferred to an accessible, strongly acidic cationic exchange column. The cationic column retains the radium-224, and natural radioactive decay generates bismuth-212 and lead-212. The cationic exchange column can also be separated from the contained portion of the system and utilized without the extraordinary safety measures necessary in the contained portion. Furthermore, the cationic exchange column provides over a relatively long time period the short lived lead-212 and bismuth-212 radionuclides which are useful for a variety of medical therapies.

Isotopic generator for bismuth-212 and lead-212 from radium

DOEpatents

Atcher, Robert W.; Friedman, Arnold M.; Hines, John

1987-01-01

A method and apparatus for providing radionuclides of bismuth-212 and lead-212. Thorium-228 and carrier solution starting material is input to a radiologically contained portion of an isotopic generator system, and radium-224 is separated from thorium-228 which is retained by a strongly basic anion exchange column. The separated radium-224 is transferred to an accessible, strongly acidic cationic exchange column. The cationic column retains the radium-224, and natural radioactive decay generates bismuth-212 and lead-212. The cationic exchange column can also be separated from the contained portion of the system and utilized without the extraordinary safety measures necessary in the contained portion. Furthermore, the cationic exchange column provides over a relatively long time period the short lived lead-212 and bismuth-212 radionuclides which are useful for a variety of medical therapies.

Determination of strontium-90 in milk samples using a controlled precipitation clean-up step prior to ion-chromatography.

PubMed

Cobb, J; Warwick, P; Carpenter, R C; Morrison, R T

1995-12-01

Strontium-90 may be determined by beta-counting its yttrium-90 daughter following separation by ion-chromatography, using a three column system comprising a chelating concentrator column, a cation-exchange column and an anion-exchange separator column. The column system has previously been applied to the determination of strontium-90 in water and urine samples. The applicability of the system to the analysis of milk is hampered by the large concentrations of calcium present, which significantly reduces the extraction of yttrium-90 by the concentrator column. A maximum of approximately 200 mg of calcium can be present for the successful extraction of yttrium-90, which greatly limits the quantity of milk that can be analysed. The quantity of milk analysed can be increased by the inclusion of a controlled precipitation step prior to the ion-chromatographic separation. The precipitation is carried out on acid digested milk samples by the addition of ammonia solution until the addition of one drop causes a reduction in pH resulting in the precipitation of calcium hydrogenphosphate. Under these conditions, approximately 20% of the calcium present in the original milk sample is precipitated, yttrium-90 is precipitated whereas strontium-90 is not precipitated. Dissolution of the precipitate, followed by separation of yttrium-90 using the ion-chromatography system facilitates the analysis of a litre of milk with recoveries of greater than 80%.

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.

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 the current study, four full-scale corner beam-column joint subassemblies, with slab included, were designed, built, instrumented, tested, and analyzed. The specimens were tested under unidirectional and bidirectional displacement-controlled quasi-static loading that incorporated varying axial loads that simulated overturning seismic moment effects. The axial loads varied between tension and high compression loads reaching about 50% of the column axial capacity. The test parameters were axial load level, loading history, joint aspect ratio, and beam reinforcement ratio. The test results proved that high axial load increases joint shear strength and decreases the deformability of joints failing in pure shear failure mode without beam yielding. On the contrary, high axial load did not affect the strength of joints failing in shear after significant beam yielding; however, it substantially increased their displacement ductility. Joint aspect ratio proved to be instrumental in deciding joint shear strength; that is the deeper the joint the lower the shear strength. Bidirectional loading reduced the apparent strength of the joint in the uniaxial principal axes. However, circular shear strength interaction is an appropriate approximation to predict the biaxial strength. The developed shear strength models predicted successfully the strength of test specimens. Based on the literature database investigation, the shear and axial capacity models developed and the test results of the current study, an analytical finite element component model based on a proposed joint shear stress-rotation backbone constitutive curve was developed to represent the behavior of unconfined beam-column joints in computer numerical simulations of concrete frame buildings. The proposed finite element model included the effect of axial load, mode of joint failure, joint aspect ratio and axial capacity of joint. The proposed backbone curve along with the developed joint element exhibited high accuracy in simulating the test response of the current test specimens as well as previous test joints. Finally, a parametric study was conducted to assess the axial failure vulnerability of unconfined beam-column joints based on the developed shear and axial capacity models. This parametric study compared the axial failure potential of unconfined beam-column joint with that of shear critical columns to provide a preliminary insight into the axial collapse vulnerability of older-type buildings during intense ground shaking.

Fabry-Perot Interferometer for Column CO2

NASA Technical Reports Server (NTRS)

Heaps, William S.; Kawa, Randolph; Bhartia, P. K. (Technical Monitor)

2002-01-01

Global atmospheric CO2 measurements are essential to resolving significant discrepancies in our understanding of the global carbon budget and, hence, humankind's role in global climate change. The science measurement requirements for CO2 are extremely demanding (precision approx. 0.3%). No atmospheric chemical species has ever been measured from space with this precision. We are developing a novel application of a Fabry-Perot interferometer to detect spectral absorption of reflected sunlight by CO2 and O2 in the atmosphere. Preliminary design studies indicate that the method will be able to achieve the sensitivity and signal-to-noise detection required to measure column CO2 at the target specification. The objective of this program is to construct a prototype instrument for deployment on an aircraft to test the instrument performance and our ability to retrieve the data in the real atmosphere. To date we have assembled a laboratory bench system to begin testing the optical and electronic components. We are also measuring signal and noise levels in actual sunlight to evaluate component performance.

Assay of common sunscreen agents in suncare products by high-performance liquid chromatography on a cyanopropyl-bonded silica column.

PubMed

Simeoni, Silvia; Tursilli, Rosanna; Bianchi, Anna; Scalia, Santo

2005-06-15

A rapid high-performance liquid chromatographic method was developed for the simultaneous assay of eight of the most common sunscreen agents (octyl-methoxycinnamate, oxybenzone, butyl-methoxydibenzoylmethane, octyl-salicilate, methylbenzylidene camphor, octyl-dimethylamminobenzoate, phenylbenzimidazole sulphonic acid and octocrylene) in sun protection products. Evaluation of the influence of different stationary phases and eluents on the separation selectivity showed that optimal resolution was obtained on a cyanopropyl-silica column eluted with methanol-acetonitrile-tetrahydrofuran-aqueous acetic acid. A small adjustment of the proposed chromatographic system (reduction in the aqueous content of the mobile phase) permitted also the determination of the extremely hydrophobic UV filter, methylene bis-benzotriazolyl tetramethylbutylphenol along with three other sunscreen agents, octyl-methoxycinnamate, oxybenzone, butyl-methoxydibenzoylmethane. Recoveries of the UV filters from the spiked formulation were between 95.7 and 103.7% and the precision of the method was better than 6.1% relative standard deviation. The developed HPLC procedure is suitable for quality control and photostability analyses of commercial suncare products.

A combined A431 cell membrane chromatography and online high performance liquid chromatography/mass spectrometry method for screening compounds from total alkaloid of Radix Caulophylli acting on the human EGFR.

PubMed

Sun, Meng; Ren, Jing; Du, Hui; Zhang, Yanmin; Zhang, Jie; Wang, Sicen; He, Langchong

2010-10-15

We have developed an online analytical method that combines A431 cell membrane chromatography (A431/CMC) with high performance liquid chromatography and mass spectrometry (LC/MS) for identifying active components from Radix Caulophylli acting on human EGFR. Retention fractions on A431/CMC model were captured onto an enrichment column and the components were directly analyzed by combining a 10-port column switcher with an LC/MS system for separation and preliminary identification. Using Sorafenib tosylate as a positive control, taspine and caulophine from Radix Caulophylli were identified as the active molecules which could act on the EGFR. This A431/CMC-online-LC/MS method can be applied for screening active components acting on EGFR from traditional Chinese medicines exemplified by Radix Caulophylli and will be of great utility in drug discovery using natural medicinal herbs as a source of novel compounds. Copyright © 2010 Elsevier B.V. All rights reserved.

Automated two-dimensional interface for capillary gas chromatography

DOEpatents

Strunk, M.R.; Bechtold, W.E.

1996-02-20

A multidimensional gas chromatograph (GC) system is disclosed which has wide bore capillary and narrow bore capillary GC columns in series and has a novel system interface. Heart cuts from a high flow rate sample, separated by a wide bore GC column, are collected and directed to a narrow bore GC column with carrier gas injected at a lower flow compatible with a mass spectrometer. A bimodal six-way valve is connected with the wide bore GC column outlet and a bimodal four-way valve is connected with the narrow bore GC column inlet. A trapping and retaining circuit with a cold trap is connected with the six-way valve and a transfer circuit interconnects the two valves. The six-way valve is manipulated between first and second mode positions to collect analyte, and the four-way valve is manipulated between third and fourth mode positions to allow carrier gas to sweep analyte from a deactivated cold trap, through the transfer circuit, and then to the narrow bore GC capillary column for separation and subsequent analysis by a mass spectrometer. Rotary valves have substantially the same bore width as their associated columns to minimize flow irregularities and resulting sample peak deterioration. The rotary valves are heated separately from the GC columns to avoid temperature lag and resulting sample deterioration. 3 figs.

Automated two-dimensional interface for capillary gas chromatography

DOEpatents

Strunk, Michael R.; Bechtold, William E.

1996-02-20

A multidimensional gas chromatograph (GC) system having wide bore capillary and narrow bore capillary GC columns in series and having a novel system interface. Heart cuts from a high flow rate sample, separated by a wide bore GC column, are collected and directed to a narrow bore GC column with carrier gas injected at a lower flow compatible with a mass spectrometer. A bimodal six-way valve is connected with the wide bore GC column outlet and a bimodal four-way valve is connected with the narrow bore GC column inlet. A trapping and retaining circuit with a cold trap is connected with the six-way valve and a transfer circuit interconnects the two valves. The six-way valve is manipulated between first and second mode positions to collect analyte, and the four-way valve is manipulated between third and fourth mode positions to allow carrier gas to sweep analyte from a deactivated cold trap, through the transfer circuit, and then to the narrow bore GC capillary column for separation and subsequent analysis by a mass spectrometer. Rotary valves have substantially the same bore width as their associated columns to minimize flow irregularities and resulting sample peak deterioration. The rotary valves are heated separately from the GC columns to avoid temperature lag and resulting sample deterioration.

Putting it altogether: improving performance in heart failure outcomes, part 2.

PubMed

Clancy, Thomas R

2009-09-01

As systems evolve over time, their natural tendency is to become increasingly more complex. Studies in the field of complex systems have generated new perspectives on management in social organizations such as hospitals. Much of this research appears as a natural extension of the cross-disciplinary field of systems theory. This is the 10th in a series of articles applying complex systems science to the traditional management concepts of planning, organizing, directing, coordinating, and controlling. As follow-up to the case study in this column's June 2009 article, this article highlights the interventions and outcomes of the study.

Silver ion bactericide system. [for Space Shuttle Orbiter potable water

NASA Technical Reports Server (NTRS)

Jasionowski, W. J.; Allen, E. T.

1974-01-01

Description of a preliminary flight prototype system which uses silver ions as the bactericide to preserve sterility of the water used for human consumption and hygiene in the Space Shuttle Orbiter. The performance of silver halide columns for passively dosing fuel cell water with silver ions is evaluated. Tests under simulated Orbiter mission conditions show that silver ion doses of 0.05 ppm are bactericidal for Pseudomonas aeruginosa and Type IIIa, the two bacteria found in Apollo potable water systems. The design of the Advance Prototype Silver Ion Water Bactericide System now under development is discussed.

Branched-chain dicationic ionic liquids for fatty acid methyl ester assessment by gas chromatography.

PubMed

Talebi, Mohsen; Patil, Rahul A; Sidisky, Leonard M; Berthod, Alain; Armstrong, Daniel W

2017-12-06

Twelve bis- or dicationic ionic liquids (ILs) including eight based on imidazolium, a single one based on phosphonium, and three based on pyrrolidinium cationic units were prepared with the bis(trifluoromethyl sulfonyl) imide anion. The two identical cationic moieties were attached by different alkyl spacers having three or five carbons and differing alkyl substituents attached to the spacer. The SLB-IL111 column, as the most polar commercial stationary phase known, was included in the study for comparison. Isothermal separations of a rapeseed oil fatty acid methyl ester (FAME) sample were used to study and compare the 12 IL-based column performances and selectivities. The retention times of the most retained methyl esters of lignoceric (C24:0) and erucic (C22:1) acids were used to estimate the IL polarity. The phosphonium dicationic IL column was, by far, the least polar. Imidazolium-based dicationic IL columns were the most polar. Polarity and selectivity for the FAME separation were somewhat related. The separation of a 37-FAME standard mixture allowed the investigation of selectivity variations observed on the 12 IL-based columns under temperature gradients up to 230 °C. The remarkable selectivity of the IL-based columns is demonstrated by the detailed analysis of the cis/trans C18:1 isomers of a partially hydrogenated vegetable oil sample on 30-m columns, separations competing with that done following an "official method" performed on a 100-m column. Graphical abstract Separation of fatty acid methyl esters on a 30-m 3m 2 C 5 (mpy) 2 . 2NTf 2 branched-chain dicationic IL-based column. Branched chain dicationic ILs show great selectivity for separation of cis/trans, ω-3/ω-6, and detailed analysis of cis/trans fats.

Adsorptive removal of heavy metals from water using sodium titanate nanofibres loaded onto GAC in fixed-bed columns.

PubMed

Sounthararajah, D P; Loganathan, P; Kandasamy, J; Vigneswaran, S

2015-04-28

Heavy metals are serious pollutants in aquatic environments. A study was undertaken to remove Cu, Cd, Ni, Pb and Zn individually (single metal system) and together (mixed metals system) from water by adsorption onto a sodium titanate nanofibrous material. Langmuir adsorption capacities (mg/g) at 10(-3)M NaNO3 ionic strength in the single metal system were 60, 83, 115 and 149 for Ni, Zn, Cu, and Cd, respectively, at pH 6.5 and 250 for Pb at pH 4.0. In the mixed metals system they decreased at high metals concentrations. In column experiments with 4% titanate material and 96% granular activated carbon (w/w) mixture at pH 5.0, the metals breakthrough times and adsorption capacities (for both single and mixed metals systems) decreased in the order Pb>Cd, Cu>Zn>Ni within 266 bed volumes. The amounts adsorbed were up to 82 times higher depending on the metal in the granular activated carbon+titanate column than in the granular activated carbon column. The study showed that the titanate material has high potential for removing heavy metals from polluted water when used with granular activated carbon at a very low proportion in fixed-bed columns. Copyright © 2015 Elsevier B.V. All rights reserved.

49 CFR 173.241 - Bulk packagings for certain low hazard liquid and solid materials.

Code of Federal Regulations, 2013 CFR

2013-10-01

... B of part 173 of this subchapter and the special provisions specified in column 7 of the § 172.101... for the specific hazardous material in Column (7) of the § 172.101 Table of this subchapter and the... performance level as specified in Column (5) of the § 172.101 Table for the material being transported. (1...

49 CFR 173.241 - Bulk packagings for certain low hazard liquid and solid materials.

Code of Federal Regulations, 2011 CFR

2011-10-01

... B of part 173 of this subchapter and the special provisions specified in column 7 of the § 172.101... for the specific hazardous material in Column (7) of the § 172.101 Table of this subchapter and the... performance level as specified in Column (5) of the § 172.101 Table for the material being transported. (1...

49 CFR 173.241 - Bulk packagings for certain low hazard liquid and solid materials.

Code of Federal Regulations, 2010 CFR

2010-10-01

... B of part 173 of this subchapter and the special provisions specified in column 7 of the § 172.101... for the specific hazardous material in Column (7) of the § 172.101 Table of this subchapter and the... performance level as specified in Column (5) of the § 172.101 Table for the material being transported. (1...

49 CFR 173.241 - Bulk packagings for certain low hazard liquid and solid materials.

Code of Federal Regulations, 2012 CFR

2012-10-01

... B of part 173 of this subchapter and the special provisions specified in column 7 of the § 172.101... for the specific hazardous material in Column (7) of the § 172.101 Table of this subchapter and the... performance level as specified in Column (5) of the § 172.101 Table for the material being transported. (1...

49 CFR 173.241 - Bulk packagings for certain low hazard liquid and solid materials.

Code of Federal Regulations, 2014 CFR

2014-10-01

... B of part 173 of this subchapter and the special provisions specified in column 7 of the § 172.101... for the specific hazardous material in Column (7) of the § 172.101 Table of this subchapter and the... performance level as specified in Column (5) of the § 172.101 Table for the material being transported. (1...

Separation of Nitration By-Products in Commercial-Grade Trinitro-Toluene by High Performance Liquid Chromatography.

DTIC Science & Technology

1982-06-01

Columns Columns used were:- Alltech 10 micron Silica 250 mm x 4.6 - I.D. Alltech 10 micron C18 Reverse-Phase 250 a x 4.6 mm I.D. Excalibar 10 micron...column with dichloromethane/n-heptane eluent. Ethyl acetate/n-heptane eluent has the advantage that it does not require flushing out at the end of each

Water column imaging on hydrothermal vent in Central Indian Ridge

NASA Astrophysics Data System (ADS)

Koh, J.; Park, Y.

2017-12-01

Water column imaging with Multibeam echosounder systems (MBES) is recently becoming of increasing interest for oceanographic studies. Especially gas bubbles and hot water exposed from hydrothermal vents make acoustic impedance anomalies in cold seawater, water column imaging is very useful for the researchers who want to detect some kinds of hydrothermal activity. We conducted a hydrothermal exploration program, called "INVENT17", using the MBES system, KONGBERG EM122 (12kHz, 1°×1°), mounted on R/V ISABU and we deployed other equipments including video guided hydraulic grab, tow-yo CTD and general CTD with MAPR (Miniature Autonomous Plume Recorder) in 2017. First, to evaluate its capabilities of detection of hydrothermal vent, the surveys using the MBES were conducted at the Solitaire Field, previously identified hydrothermal area of the Central Indian Ridge. The bathymetric data obtained from MBES provided information about detailed morphology of seafloor, but we were not able to achieve the information from the water column imaging data. But the clue of existence of active hydrothermal vent was detected through the values of ΔNTU, dEh/dt, and OPR gained from MAPR, the data means that the hydrothermal activity affects 100m from the seafloor. It could be the reason that we can't find the hydrothermal activity because the range resolution of water column imaging is pretty rough so that the size of 100m-scaled activity has low possibility to distinguish from seafloor. The other reason is there are no sufficient objects to cause strong scattering like as CO2 bubbles or droplets unlike in the mid-Okinawa Trough. And this suggests that can be a important standard to identify properties of hydrothermal vent sites depending on the presence of scattering objects in water mass. To justify this, we should perform more chemical analysis of hot water emanating from hydrothermal vent and collected several bottles of water sample to do that.

Assessment of removal efficiency of perfluorocompounds (PFCs) in a semiconductor fabrication plant by gas chromatography.

PubMed

Ou Yang, Chang-Feng; Kam, Seak-Hong; Liu, Chia-Hung; Tzou, Jiren; Wang, Jia-Lin

2009-08-01

This study investigated a gas chromatographic (GC) method to assess the destruction or removal efficiency (DRE) of local scrubbers on five perfluorocompounds (PFCs), i.e., SF(6), NF(3), CF(4), C(2)F(6), and C(3)F(8), which are very potent greenhouse gases used in a semiconductor fabrication plant. Air samples taken at inlets and outlets of local scrubbers were analyzed by a self-constructed multi-column GC system equipped with thermal conductivity detection. Three packed columns were integrated into the heart-cut GC system to allow simultaneous analysis of the five target PFCs. The Porapak Q pre-column performs rough separation and cuts eluent groups to two analytical columns for optimal separation. The Molecular Sieve - 5A column separated NF(3), CF(4), and C(3)F(8) and the second Porapak Q separated SF(6) and C(2)F(6). Linearity was greater than 0.995 (R(2)) for the five PFCs, and the reproducibility was about 4% (relative standard deviation) for NF(3), and better than 0.5% for the other four PFCs. DRE for the combustion (CB) and electric-thermal types of local scrubbers was evaluated by taking into account the in-line dilution from air and fuel gases. Both flow and tracer methods were employed to deduce the dilution factors (DFs). For the tracer method, helium was employed as the tracer and injected upstream of the scrubbers and thus mixed with the exhaust gas. With this method, the DFs were determined to be in the range from 4.8 to 5.9 for the CB unit, significantly higher than the value of 3.3 based on the flow method. The DREs for the CB unit for C(3)F(8) were greater than 90% and between 40% and 50% for CF(4).

Spaceflight and Neurosurgery: A Comprehensive Review of the Relevant Literature.

PubMed

Swinney, Christian C; Allison, Zain

2018-01-01

Spaceflight and the associated gravitational fluctuations may impact various components of the central nervous system. These include changes in intracranial pressure, the spine, and neurocognitive performance. The implications of altered astronaut performance on critical spaceflight missions are potentially significant. The current body of research on this important topic is extremely limited, and a comprehensive review has not been published. Herein, the authors address this notable gap, as well as the role of the neurosurgeon in optimizing potential diagnostic and therapeutic modalities. A literature search was conducted using the PubMed, EMBASE, and Google Scholar databases, with no time constraints. Significant manuscripts on physiologic changes associated with spaceflight and microgravity were identified and reviewed. Manifestations were separated into 1 of 3 general categories, including changes in intracranial pressure, the spine, and neurocognitive performance. A comprehensive literature review yielded 27 studies with direct relevance to the impact of microgravity and spaceflight on nervous system physiology. This included 7 studies related to intracranial pressure fluctuations, 17 related to changes in the spinal column, and 3 related to neurocognitive change. The microgravity environment encountered during spaceflight impacts intracranial physiology. This includes changes in intracranial pressure, the spinal column, and neurocognitive performance. Herein, we present a systematic review of the published literature on this issue. Neurosurgeons should have a key role in the continued study of this important topic, contributing to both diagnostic and therapeutic understanding. Copyright © 2017 Elsevier Inc. All rights reserved.

Item Order, Response Format, and Examinee Sex and Handedness and Performance on a Multiple-Choice Test.

ERIC Educational Resources Information Center

Kleinke, David J.

Four forms of a 36-item adaptation of the Stanford Achievement Test were administered to 484 fourth graders. External factors potentially influencing test performance were examined, namely: (1) item order (easy-to-difficult vs. uniform); (2) response location (left column vs. right column); (3) handedness which may interact with response location;…

40 CFR Appendix A to Subpart C of... - Alternative Testing Methods Approved for Analyses Under the Safe Drinking Water Act

Code of Federal Regulations, 2014 CFR

2014-07-01

... Spectrometry (GC/MS) 525.3 24 Carbofuran High-performance liquid chromatography (HPLC) with post-column... (HPLC) with Post-Column Derivatization and Fluorescence Detection 6651 B 6651 B 6651 B-00, B-05... Chromatography/Mass Spectrometry (GC/MS) 525.3 24 Oxamyl High-performance liquid chromatography (HPLC) with post...

21 CFR 862.2250 - Gas liquid chromatography system for clinical use.

Code of Federal Regulations, 2012 CFR

2012-04-01

... 21 Food and Drugs 8 2012-04-01 2012-04-01 false Gas liquid chromatography system for clinical use... Instruments § 862.2250 Gas liquid chromatography system for clinical use. (a) Identification. A gas liquid... pressure. The device may include accessories such as columns, gases, column supports, and liquid coating...

21 CFR 862.2250 - Gas liquid chromatography system for clinical use.

Code of Federal Regulations, 2014 CFR

2014-04-01

... 21 Food and Drugs 8 2014-04-01 2014-04-01 false Gas liquid chromatography system for clinical use... Instruments § 862.2250 Gas liquid chromatography system for clinical use. (a) Identification. A gas liquid... pressure. The device may include accessories such as columns, gases, column supports, and liquid coating...

21 CFR 862.2250 - Gas liquid chromatography system for clinical use.

Code of Federal Regulations, 2013 CFR

2013-04-01

... 21 Food and Drugs 8 2013-04-01 2013-04-01 false Gas liquid chromatography system for clinical use... Instruments § 862.2250 Gas liquid chromatography system for clinical use. (a) Identification. A gas liquid... pressure. The device may include accessories such as columns, gases, column supports, and liquid coating...

21 CFR 862.2250 - Gas liquid chromatography system for clinical use.

Code of Federal Regulations, 2010 CFR

2010-04-01

... 21 Food and Drugs 8 2010-04-01 2010-04-01 false Gas liquid chromatography system for clinical use... Instruments § 862.2250 Gas liquid chromatography system for clinical use. (a) Identification. A gas liquid... pressure. The device may include accessories such as columns, gases, column supports, and liquid coating...

21 CFR 862.2250 - Gas liquid chromatography system for clinical use.

Code of Federal Regulations, 2011 CFR

2011-04-01

... 21 Food and Drugs 8 2011-04-01 2011-04-01 false Gas liquid chromatography system for clinical use... Instruments § 862.2250 Gas liquid chromatography system for clinical use. (a) Identification. A gas liquid... pressure. The device may include accessories such as columns, gases, column supports, and liquid coating...

Characterization of a compost biofiltration system degrading dichloromethane

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

Ergas, S.J.; Kinney, K.; Fuller, M.E.

1994-11-05

The effects of acclimatization of microbial populations, compound concentration, and media pH on the biodegradation of low concentration dichloromethane emissions in biofiltration systems was evaluated. Greater than 98% removal efficiency was achieved for dichloromethane at superficial velocities from 1 to 15 m[sup 3]/m[sup 2][center dot]min and inlet concentrations of 3 and 50 ppm[sub v]. Although acclimatization of microbial populations to toluene occurred within 2 weeks of operation start-up, initial dichloromethane acclimatization took place over a period of 10 weeks. This period was shortened to 10 days when a laboratory grown consortium of dichloromethane degrading organisms, isolated from a previously acclimatizedmore » column, was introduced into fresh biofilter media. The mixed culture consisted of 12 members, which together were able to degrade dichloromethane at concentrations up to 500 mg/L. Only one member of the consortium was able to degrade dichloromethane in pure culture, and the presence of the other members did not affect the rate of biodegradation in solution culture. Although high removal efficiencies for dichloromethane were sustained for more than 4 months in a biofilter column receiving an inlet gas stream with 3 ppm[sub v] of dichloromethane, acidification of the column and resulting decline in performance occurred when a 50-ppm[sub v] inlet concentration was used. A biofilm model incorporating first order biodegradation kinetics provided a good fit to observed concentration profiles, and may prove to be a useful tool for designing biofiltration systems for low concentration VOC emissions.« less

Evaluation of the suitability of chromatographic systems to predict human skin permeation of neutral compounds.

PubMed

Hidalgo-Rodríguez, Marta; Soriano-Meseguer, Sara; Fuguet, Elisabet; Ràfols, Clara; Rosés, Martí

2013-12-18

Several chromatographic systems (three systems of high-performance liquid chromatography and two micellar electrokinetic chromatography systems) besides the reference octanol-water partition system are evaluated by a systematic procedure previously proposed in order to know their ability to model human skin permeation. The precision achieved when skin-water permeability coefficients are correlated against chromatographic retention factors is predicted within the framework of the solvation parameter model. It consists in estimating the contribution of error due to the biological and chromatographic data, as well as the error coming from the dissimilarity between the human skin permeation and the chromatographic systems. Both predictions and experimental tests show that all correlations are greatly affected by the considerable uncertainty of the skin permeability data and the error associated to the dissimilarity between the systems. Correlations with much better predictive abilities are achieved when the volume of the solute is used as additional variable, which illustrates the main roles of both lipophilicity and size of the solute to penetrate through the skin. In this way, the considered systems are able to give precise estimations of human skin permeability coefficients. In particular, the HPLC systems with common C18 columns provide the best performances in emulating the permeation of neutral compounds from aqueous solution through the human skin. As a result, a methodology based on easy, fast, and economical HPLC measurements in a common C18 column has been developed. After a validation based on training and test sets, the method has been applied with good results to the estimation of skin permeation of several hormones and pesticides. Copyright © 2013 Elsevier B.V. All rights reserved.

Laser Eye Protection Groupware Application Information System

DTIC Science & Technology

1998-11-01

Q^ Concenlralion ^ Data & Program Res ■>i Excfted Stele Cross-Section ’^> EKtrnction Coefficient ^s Ground Stale Cross-Section ?> Reference...2nd Level (2nd column) 4 Chemical Compound Bio material name 3nd Level (3rd column) 4th Level (4th column) Figure 14A. Reference Date View

29 CFR 1926.751 - Definitions.

Code of Federal Regulations, 2014 CFR

2014-07-01

... brakes, rolls, or other methods to shape steel into desired cross sections at room temperature. Column means a load-carrying vertical member that is part of the primary skeletal framing system. Columns do..., such as a wall or column and work with both hands free while leaning. Post means a structural member...

29 CFR 1926.751 - Definitions.

Code of Federal Regulations, 2013 CFR

2013-07-01

... brakes, rolls, or other methods to shape steel into desired cross sections at room temperature. Column means a load-carrying vertical member that is part of the primary skeletal framing system. Columns do..., such as a wall or column and work with both hands free while leaning. Post means a structural member...

29 CFR 1926.751 - Definitions.

Code of Federal Regulations, 2012 CFR

2012-07-01

... brakes, rolls, or other methods to shape steel into desired cross sections at room temperature. Column means a load-carrying vertical member that is part of the primary skeletal framing system. Columns do..., such as a wall or column and work with both hands free while leaning. Post means a structural member...

Dscam2 mediates axonal tiling in the Drosophila visual system

PubMed Central

Millard, S. Sean; Flanagan, John J.; Pappu, Kartik S.; Wu, Wei; Zipursky, S. Lawrence

2009-01-01

Sensory processing centres in both the vertebrate and the invertebrate brain are often organized into reiterated columns, thus facilitating an internal topographic representation of the external world. Cells within each column are arranged in a stereotyped fashion and form precise patterns of synaptic connections within discrete layers. These connections are largely confined to a single column, thereby preserving the spatial information from the periphery. Other neurons integrate this information by connecting to multiple columns. Restricting axons to columns is conceptually similar to tiling. Axons and dendrites of neighbouring neurons of the same class use tiling to form complete, yet non-overlapping, receptive fields1-3. It is thought that, at the molecular level, cell-surface proteins mediate tiling through contact-dependent repulsive interactions1,2,4,5, but proteins serving this function have not yet been identified. Here we show that the immunoglobulin superfamily member Dscam2 restricts the connections formed by L1 lamina neurons to columns in the Drosophila visual system. Our data support a model in which Dscam2 homophilic interactions mediate repulsion between neurites of L1 cells in neighbouring columns. We propose that Dscam2 is a tiling receptor for L1 neurons. PMID:17554308

Effects of model error on control of large flexible space antenna with comparisons of decoupled and linear quadratic regulator control procedures

NASA Technical Reports Server (NTRS)

Hamer, H. A.; Johnson, K. G.

1986-01-01

An analysis was performed to determine the effects of model error on the control of a large flexible space antenna. Control was achieved by employing two three-axis control-moment gyros (CMG's) located on the antenna column. State variables were estimated by including an observer in the control loop that used attitude and attitude-rate sensors on the column. Errors were assumed to exist in the individual model parameters: modal frequency, modal damping, mode slope (control-influence coefficients), and moment of inertia. Their effects on control-system performance were analyzed either for (1) nulling initial disturbances in the rigid-body modes, or (2) nulling initial disturbances in the first three flexible modes. The study includes the effects on stability, time to null, and control requirements (defined as maximum torque and total momentum), as well as on the accuracy of obtaining initial estimates of the disturbances. The effects on the transients of the undisturbed modes are also included. The results, which are compared for decoupled and linear quadratic regulator (LQR) control procedures, are shown in tabular form, parametric plots, and as sample time histories of modal-amplitude and control responses. Results of the analysis showed that the effects of model errors on the control-system performance were generally comparable for both control procedures. The effect of mode-slope error was the most serious of all model errors.

Integrated on-line system for DNA sequencing by capillary electrophoresis: From template to called bases

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

Ton, H.; Yeung, E.S.

1997-02-15

An integrated on-line prototype for coupling a microreactor to capillary electrophoresis for DNA sequencing has been demonstrated. A dye-labeled terminator cycle-sequencing reaction is performed in a fused-silica capillary. Subsequently, the sequencing ladder is directly injected into a size-exclusion chromatographic column operated at nearly 95{degree}C for purification. On-line injection to a capillary for electrophoresis is accomplished at a junction set at nearly 70{degree}C. High temperature at the purification column and injection junction prevents the renaturation of DNA fragments during on-line transfer without affecting the separation. The high solubility of DNA in and the relatively low ionic strength of 1 x TEmore » buffer permit both effective purification and electrokinetic injection of the DNA sample. The system is compatible with highly efficient separations by a replaceable poly(ethylene oxide) polymer solution in uncoated capillary tubes. Future automation and adaptation to a multiple-capillary array system should allow high-speed, high-throughput DNA sequencing from templates to called bases in one step. 32 refs., 5 figs.« less

The control algorithm of the system ‘frequency converter - asynchronous motor’ of the batcher

NASA Astrophysics Data System (ADS)

Lyapushkin, S. V.; Martyushev, N. V.; Shiryaev, S. Y.

2017-01-01

The paper is devoted to the solution of the problem of optimum batching of bulk mixtures according to the criterion of accuracy and maximally possible performance. This problem is solved for applied utilization when running the system ‘frequency converter - asynchronous motor’ having pulse-width modulation of a screw batcher of agricultural equipment. The developed control algorithm allows batching small components of a bulk mixture with the prescribed accuracy due to the weight consideration of the falling column of the material being in the air after the screw stoppage. The paper also shows that in order to reduce the influence of the mass of the ‘falling column’ on the accuracy of batching, it is necessary to specify the sequence of batching of components inside of the recipe beginning from the largest component ending with the least one. To exclude the variable error of batching, which arises owing to the mass of the material column, falling into the batcher-bunker, the algorithm of dynamic correction of the task is used in the control system.

Hand-portable liquid chromatographic instrumentation.

PubMed

Sharma, Sonika; Tolley, Luke T; Tolley, H Dennis; Plistil, Alex; Stearns, Stanley D; Lee, Milton L

2015-11-20

Over the last four decades, liquid chromatography (LC) has experienced an evolution to smaller columns and particles, new stationary phases and low flow rate instrumentation. However, the development of person-portable LC has not followed, mainly due to difficulties encountered in miniaturizing pumps and detectors, and in reducing solvent consumption. The recent introduction of small, non-splitting pumping systems and UV-absorption detectors for use with capillary columns has finally provided miniaturized instrumentation suitable for high-performance hand-portable LC. Fully integrated microfabricated LC still remains a significant challenge. Ion chromatography (IC) has been successfully miniaturized and applied for field analysis; however, applications are mostly limited to inorganic and small organic ions. This review covers advancements that make possible more rapid expansion of portable forms of LC and IC. Copyright © 2015 Elsevier B.V. All rights reserved.

Investigation of transient cavitating flow in viscoelastic pipes

NASA Astrophysics Data System (ADS)

Keramat, A.; Tijsseling, A. S.; Ahmadi, A.

2010-08-01

A study on water hammer in viscoelastic pipes when the fluid pressure drops to liquid vapour pressure is performed. Two important concepts including column separation and the effects of retarded strains in the pipe wall on the fluid response have been investigated separately in recent works, but there is some curiosity as to how the results for pressure and discharge are when column separation occurs in a viscoelastic pipe. For pipes made of plastic such as polyethylene (PE) and polyvinyl chloride (PVC), viscoelasticity is a crucial mechanical property which changes the hydraulic and structural transient responses. Based on previous developments in the analysis of water hammer, a model which is capable of analysing column separation in viscoelastic pipes is presented and used for solving the selected case studies. For the column-separation modelling the Discrete Vapour Cavity Model (DVCM) is utilised and the viscoelasticity property of the pipe wall is modelled by Kelvin-Voigt elements. The effects of viscoelasticity play an important role in the column separation phenomenon because it changes the water hammer fundamental frequency and so affects the time of opening or collapse of the cavities. Verification of the implemented computer code is performed for the effects of viscoelasticity and column separation - separately and simultaneously - using experimental results from the literature. In the provided examples the focus is placed on the simultaneous effect of viscoelasticity and column separation on the hydraulic transient response. The final conclusions drawn are that if rectangular grids are utilised the DVCM gives acceptable predictions of the phenomenon and that the pipe wall material's retarded behaviour strongly dampens the pressure spikes caused by column separation.

Microchip electrospray: improvements in spray and signal stability during gradient elution by an inverted postcolumn makeup flow.

PubMed

Jung, Stephanie; Effelsberg, Uwe; Tallarek, Ulrich

2011-12-01

Dynamic changes in mobile phase composition during high-performance liquid chromatography (HPLC) gradient elution coupled to mass spectrometry (MS) sensitively affect electrospray modes. We investigate the impact of the eluent composition on spray stability and MS response by infusion and injection experiments with a small tetrapeptide in water-acetonitrile mixtures. The employed HPLC/electrospray (ESI)-MS configuration uses a microchip equipped with an enrichment column, a separation column, and a makeup flow (MUF) channel. One nano pump is connected to the separation column, while a second one delivers solvent of exactly inverted composition to the MUF channel. Both solvent streams are united behind the separation column, before the ESI tip, such that the resulting electrosprayed solution always has identical composition during a gradient elution. Analyte peak parameters without and with MUF compensation are determined and discussed with respect to the electrospray mode and eluent composition. The postcolumn MUF significantly improves spray and signal stability over the entire solvent gradient, without compromising the performance of the HPLC separation column. It can also be conveniently implemented on microchip platforms.

Separation of Ellagitannin-Rich Phenolics from U.S. Pecans and Chinese Hickory Nuts Using Fused-Core HPLC Columns and Their Characterization.

PubMed

Gong, Yi; Pegg, Ronald B

2017-07-19

U.S. pecans and Chinese hickory nuts possess a wide array of phenolic constituents with potential health benefits including phenolic acids and proanthocyanidins. Only limited information is available, however, on their compositions. The present study optimized the separation performance and characterized the low-molecular-weight phenolic fractions of these nuts with C18 and pentafluorophenyl (PFP) fused-core LC columns by employing a kinetic approach. Although both types of reversed-phase columns demonstrated similar performance in general, the PFP column furnished greater plate numbers and superior peak shapes for the low-molecular-weight fractions as well as overall separations of ellagic acid derivatives. The high-molecular-weight fraction of pecans, analyzed by a 3-μm HILIC column, possessed more proanthocyanidins than the Chinese hickory nuts with dimers and trimers (31.4 and 18.34 mg/g crude extract, respectively) being present at the greatest levels. Chinese hickory nuts had lower proanthocyanidin content but possessed tetramers and pentamers at 4.46 and 4.01 mg/g crude extract, respectively.

Direct enantioseparation of nitrogen-heterocyclic pesticides on cellulose-based chiral column by high-performance liquid chromatography.

PubMed

Chai, Tingting; Yang, Wenwen; Qiu, Jing; Hou, Shicong

2015-01-01

The enantiomeric separation of eight pesticides including bitertanol (), diclobutrazol (), fenbuconazole (), triticonazole (), imazalil (), triapenthenol (), ancymidol (), and carfentrazone-ethyl () was achieved, using normal-phase high-performance liquid chromatography on two cellulosed-based chiral columns. The effects of isopropanol composition from 2% to 30% in the mobile phase and column temperature from 5 to 40 °C were investigated. Satisfactory resolutions were obtained for bitertanol (), triticonazole (), imazalil () with the (+)-enantiomer eluted first and fenbuconazole () with the (-)-enantiomer eluted first on Lux Cellulose-2 and Lux Cellulose-3. (+)-Enantiomers of diclobutrazol () and triapenthenol () were first eluted on Lux Cellulose-2. (-)-Carfentrazone-ethyl () were eluted first on Lux Cellulose-2 and Lux Cellulose-3 with incomplete separation. Reversed elution orders were obtained for ancymidol (7). (+)-Ancymidol was first eluted on Lux Cellulose-2 while on Lux Cellulose-3 (-)-ancymidol was first eluted. The results of the elution order at different column temperatures suggested that column temperature did not affect the optical signals of the enantiomers. These results will be helpful to prepare and analyze individual enantiomers of chiral pesticides. © 2014 Wiley Periodicals, Inc.

On-line sample cleanup and enrichment chromatographic technique for the determination of ambroxol in human serum.

PubMed

Emara, Samy; Kamal, Maha; Abdel Kawi, Mohamed

2012-02-01

A sensitive and efficient on-line clean up and pre-concentration method has been developed using column-switching technique and protein-coated µ-Bondapak CN silica pre-column for quantification of ambroxol (AM) in human serum. The method is performed by direct injection of serum sample onto a protein-coated µ-Bondapak CN silica pre-column, where AM is pre-concentrated and retained, while proteins and very polar constituents are washed to waste using a phosphate buffer saline (pH 7.4). The retained analyte on the pre-column is directed onto a C(18) analytical column for separation, with a mobile phase consisting of a mixture of methanol and distilled deionized water (containing 1% triethylamine adjusted to pH 3.5 with ortho-phosphoric acid) in the ratio of 50:50 (v/v). Detection is performed at 254 nm. The calibration curve is linear over the concentration range of 12-120 ng/mL (r(2) = 0.9995). The recovery, selectivity, linearity, precision, and accuracy of the method are convenient for pharmacokinetic studies or routine assays.

Blind column selection protocol for two-dimensional high performance liquid chromatography.

PubMed

Burns, Niki K; Andrighetto, Luke M; Conlan, Xavier A; Purcell, Stuart D; Barnett, Neil W; Denning, Jacquie; Francis, Paul S; Stevenson, Paul G

2016-07-01

The selection of two orthogonal columns for two-dimensional high performance liquid chromatography (LC×LC) separation of natural product extracts can be a labour intensive and time consuming process and in many cases is an entirely trial-and-error approach. This paper introduces a blind optimisation method for column selection of a black box of constituent components. A data processing pipeline, created in the open source application OpenMS®, was developed to map the components within the mixture of equal mass across a library of HPLC columns; LC×LC separation space utilisation was compared by measuring the fractional surface coverage, fcoverage. It was found that for a test mixture from an opium poppy (Papaver somniferum) extract, the combination of diphenyl and C18 stationary phases provided a predicted fcoverage of 0.48 and was matched with an actual usage of 0.43. OpenMS®, in conjunction with algorithms designed in house, have allowed for a significantly quicker selection of two orthogonal columns, which have been optimised for a LC×LC separation of crude extractions of plant material. Copyright © 2016 Elsevier B.V. All rights reserved.

Development Of ABEC Column For Separation Of Tc-99 From Northstar Dissolved Target Solution

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

Stepinski, Dominique C.; Bennett, Megan E.; Naik, Seema R.

Batch and column breakthrough experiments were performed to determine isotherms and mass-transfer parameters for adsorption of Tc on aqueous biphasic extraction chromatographic (ABEC) sorbent in two solutions: 200 g/L Mo, 5.1 M K +, 1 M OH -, and 0.1 M NO 3 - (Solution A) and 200 g/L Mo, 9.3 M K +, 5 M OH -, and 0.1 M NO 3 - (Solution B). Good agreement was found between the isotherm values obtained by batch and column breakthrough studies for both Solutions A and B. Potassium-pertechnetate intra-particle diffusivity on ABEC resin was estimated by VERSE simulations, and goodmore » agreement was found among a series of column-breakthrough experiments at varying flow velocities, column sizes, and technetium concentrations. However, testing of 10 cc cartridges provided by NorthStar with Solutions A and B did not give satisfactory results, as significant Tc breakthrough was observed and ABEC cartridge performance varied widely among experiments. These different experimental results are believed to be due to inconsistent preparation of the ABEC resin prior to packing and/or inconsistent packing.« less

The Star Schema Benchmark and Augmented Fact Table Indexing

NASA Astrophysics Data System (ADS)

O'Neil, Patrick; O'Neil, Elizabeth; Chen, Xuedong; Revilak, Stephen

We provide a benchmark measuring star schema queries retrieving data from a fact table with Where clause column restrictions on dimension tables. Clustering is crucial to performance with modern disk technology, since retrievals with filter factors down to 0.0005 are now performed most efficiently by sequential table search rather than by indexed access. DB2’s Multi-Dimensional Clustering (MDC) provides methods to "dice" the fact table along a number of orthogonal "dimensions", but only when these dimensions are columns in the fact table. The diced cells cluster fact rows on several of these "dimensions" at once so queries restricting several such columns can access crucially localized data, with much faster query response. Unfortunately, columns of dimension tables of a star schema are not usually represented in the fact table. In this paper, we show a simple way to adjoin physical copies of dimension columns to the fact table, dicing data to effectively cluster query retrieval, and explain how such dicing can be achieved on database products other than DB2. We provide benchmark measurements to show successful use of this methodology on three commercial database products.

Application of high-performance liquid chromatography to the determination of glyoxylate synthesis in chick embryo liver.

PubMed

Qureshi, A A; Elson, C E; Lebeck, L A

1982-11-19

The isolation and identification of three major alpha-keto end products (glyoxylate, pyruvate, alpha-ketoglutarate) of the isocitrate lyase reaction in 18-day chick embryo liver have been described. This was accomplished by the separation of these alpha-keto acids as their 2,4-dinitrophenylhydrazones (DNPHs) by high-performance liquid chromatography (HPLC). The DNPHs of alpha-keto acids were eluted with an isocratic solvent system of methanol-water-acetic acid (60:38.5:1.5) containing 5 mM tetrabutylammonium phosphate from a reversed-phase ultrasphere C18 (IP) and from a radial compression C18 column. The separation can be completed on the radial compression column within 15-20 min as compared to 30-40 min with a conventional reversed-phase column. Retention times and peak areas were integrated for both the assay samples and reference compounds. A relative measure of alpha-keto acid in the peak was calculated by comparison with the standard. The identification of each peak was done on the basis of retention time matching, co-chromatography with authentic compounds, and stopped flow UV-VIS scanning between 240 and 440 nm. Glyoxylate represented 5% of the total product of the isocitrate lyase reaction. Day 18 parallels the peak period of embryonic hepatic glycogenesis which occurs at a time when the original egg glucose reserve has been depleted.

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.

Seismic Performance of Self-Consolidating Concrete Bridge Columns

DOT National Transportation Integrated Search

2017-09-01

The high amount of confining lateral steel required by seismic design provisions for rectangular bridge columns can cause steel congestion. The high amount of confining steel may hinder the placement of conventional concrete (CC). Self-consolidating ...

Low pressure ion chromatography with a low cost paired emitter-detector diode based detector for the determination of alkaline earth metals in water samples.

PubMed

Barron, Leon; Nesterenko, Pavel N; Diamond, Dermot; O'Toole, Martina; Lau, King Tong; Paull, Brett

2006-09-01

The use of a low pressure ion chromatograph based upon short (25 mm x 4.6 mm) surfactant coated monolithic columns and a low cost paired emitter-detector diode (PEDD) based detector, for the determination of alkaline earth metals in aqueous matrices is presented. The system was applied to the separation of magnesium, calcium, strontium and barium in less than 7min using a 0.15M KCl mobile phase at pH 3, with post-column reaction detection at 570 nm using o-cresolphthalein complexone. A comparison of the performance of the PEDD detector with a standard laboratory absorbance detector is shown, with limits of detection for magnesium and calcium using the low cost PEDD detector equal to 0.16 and 0.23 mg L(-1), respectively. Finally, the developed system was used for the determination of calcium and magnesium in a commercial spring water sample.

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.

Effect of load eccentricity on the buckling of thin-walled laminated C-columns

NASA Astrophysics Data System (ADS)

Wysmulski, Pawel; Teter, Andrzej; Debski, Hubert

2018-01-01

The study investigates the behaviour of short, thin-walled laminated C-columns under eccentric compression. The tested columns are simple-supported. The effect of load inaccuracy on the critical and post-critical (local buckling) states is examined. A numerical analysis by the finite element method and experimental tests on a test stand are performed. The samples were produced from a carbon-epoxy prepreg by the autoclave technique. The experimental tests rest on the assumption that compressive loads are 1.5 higher than the theoretical critical force. Numerical modelling is performed using the commercial software package ABAQUS®. The critical load is determined by solving an eigen problem using the Subspace algorithm. The experimental critical loads are determined based on post-buckling paths. The numerical and experimental results show high agreement, thus demonstrating a significant effect of load inaccuracy on the critical load corresponding to the column's local buckling.

Determination of active components of Ginkgo biloba in human urine by capillary high-performance liquid chromatography/mass spectrometry with on-line column-switching purification.

PubMed

Ding, Shujing; Dudley, Ed; Chen, Lijuan; Plummer, Sue; Tang, Jiandong; Newton, Russell P; Brenton, A Gareth

2006-01-01

Ginkgo biloba is one of the most popular herbal nutritional supplements, with terpene lactones and flavonoids being the two major active components. An on-line purification high-performance liquid chromatography/mass spectrometry (HPLC/MS) method was successfully developed for the quantitative determination of flavonoids and terpene lactones excreted in human urine after ingesting the herbal supplement. Satisfactory separation was obtained using a C18 capillary column made in-house with sample clean-up and pre-concentration achieved using a C18 pre-column with column switching. High selectivity and limits of detection of 1-18 ng/mL were achieved using a selected ion monitoring (SIM) scan in negative ion mode; the on-line solid-phase extraction (SPE) recovery of the active components in Ginkgo biloba determined in this study was greater than 75%. Copyright 2006 John Wiley & Sons, Ltd.

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.

Evaluation of the removal of Strontium-90 from groundwater using a zeolite rich-rock permeable treatment wall

NASA Astrophysics Data System (ADS)

Seneca, S. M.; Rabideau, A. J.; Bandilla, K.

2010-12-01

Experimental and modeling studies are in progress to evaluate the long-term performance of a permeable treatment wall comprised of zeolite-rich rock for the removal of strontium-90 from groundwater. Multiple column tests were performed at the University at Buffalo and on-site West Valley Environmental Services; columns were supplied with synthetic groundwater referenced to anticipate field conditions and radioactive groundwater on-site WVES. The primary focus in this work is on quantifying the competitive ion exchange among five cations (Na+, K+, Ca2+, Mg2+, and Sr2+); the data obtained from the column studies is used to support the robust estimation of zeolite cation exchange parameters. This research will produce a five-solute cation exchange model describing the removal efficiency of the zeolite, using the various column tests to calibrate and validate the geochemical transport model. The field-scale transport model provides flexibility to explore design parameters and potential variations in groundwater geochemistry to investigate the long-term performance of a full scale treatment wall at the Western New York nuclear facility.

Natural zeolite permeable treatment wall for removing Sr-90 from groundwater.

PubMed

Seneca, Shannon M; Rabideau, Alan J

2013-02-05

Experimental and modeling studies were completed to investigate the potential performance of a sorbing permeable treatment wall (PTW) comprised of natural zeolite for removal of strontium-90 (Sr-90) from groundwater at the West Valley Demonstration Project (WVDP) near Buffalo, NY. Multiple column tests were performed at the University at Buffalo (UB) and WVDP for periods ranging from 6 months to 2 years; UB columns were supplied with synthetic groundwater referenced to anticipated field conditions, while radioactive groundwater obtained on site was used for the WVDP columns. The primary focus was on quantifying the competitive cation reactions among five cations (Na(+), K(+), Ca(2+), Mg(2+), Sr(2+)) and Sr-90 with data obtained from the column studies used to estimate Gaines-Thomas (GT) selectivity coefficients. The resulting six-solute transport model provided flexibility to explore the influence of PTW parameters on long-term PTW performance, including variations in Sr-90 concentrations and groundwater geochemistry. The natural zeolite PTW is a viable method for in situ removal of Sr-90 from groundwater and potentially applicable to other sites contaminated by Sr-90.

Guar gum coupled microscale ZVI for in situ treatment of CAHs: continuous-flow column study.

PubMed

Velimirovic, Milica; Simons, Queenie; Bastiaens, Leen

2014-01-30

A column study was performed under in situ conditions to evaluate to which extend the inactivation of the microscale zerovalent iron (mZVI) by guar gum occurs under continuous flow conditions. Five aquifer containing columns were set up under different conditions. Efficient removal of trichloroethene was observed for the column amended by mZVI. Stabilization of the mZVI with guar gum led to slightly reduced activity. More reduced reactivity was observed in the poisoned column containing guar gum stabilized mZVI. This confirms that soil microorganisms can degrade guar gum and that subsequent removal of the oligosaccharides by the groundwater flow (flushing effect) can reactivate the mZVI. After more than six months of continuous operation the columns were dismantled. DNA-based qPCR analysis revealed that mZVI does not significantly affect the bacterial community, while guar gum stabilized mZVI particles can even induce bacterial growth. Overall, this study suggests that the temporarily decreased mZVI reactivity due to guar gum, has a rather limited impact on the performance of in situ reactive zones. The presence of guar gum slightly reduced the reactivity of iron, but also slowed down the iron corrosion rate which prolongs the life time of reactive zone. Copyright © 2013 Elsevier B.V. All rights reserved.

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.

Research on miniature gas analysis systems

NASA Technical Reports Server (NTRS)

Angell, J. B.

1974-01-01

Technology for fabricating very small valves, whose function will be to introduce a small sample of the gas to be analyzed into the main carrier gas stream flowing through the chromatograph column is described. In addition, some analyses were made of the factors governing the resolution of gas chromatographs, particularly those with miniature columns. These analyses show how important the column lining thickness is in governing the ability of a miniature column to separate components of an unknown gas. A brief description of column lining factors is included. Preliminary work on a super small thermistor detector is included.

Automated high performance liquid chromatography with on-line reduction of disulfides and chemiluminescence detection for determination of thiols and disulfides in biological fluids.

PubMed

Bai, Shouli; Chen, Qingshuo; Lu, Chao; Lin, Jin-Ming

2013-03-20

In general, the reduction of disulfide bonds with tris(2-carboxyethyl)phosphine (TCEP) is performed using off-line operation, which is not only time-consuming but also vulnerable to the spontaneous re-oxidation of thiols during sample preparation and subsequent analysis procedures. To the best of our knowledge, there has been not any case on the on-line reduction for biological disulfides coupled with high performance liquid chromatography (HPLC). In this study, these obstacles are overcome by packing Zn(II)-TCEP complexes into a home-made column. The as-synthesized Zn(II)-TCEP complexes enable efficient reduction of disulfide bonds at pH 3.0. This acidic pH value was compatible with that of the mobile phase for HPLC separation of thiols and disulfides. Therefore, using fluorosurfactant-prepared triangular gold nanoparticles as HPLC postcolumn specific chemiluminescence (CL) reagents for thiols, the feasibility of the established on-line reduction column has been confirmed for the direct identification of both thiols and disulfides by incorporating this reduction column into a single chromatographic separation. Detection limits for these analytes range from 8.3 to 25.4 nM and the linear range in a log-log plot can comprise three orders of magnitude. Finally, the utility of this automated on-line reduction of disulfides-HPLC-CL system has been demonstrated for the reliable determination of thiols and disulfides in human urine and plasma samples. Copyright © 2013 Elsevier B.V. All rights reserved.

Evolution in miniaturized column liquid chromatography instrumentation and applications: An overview.

PubMed

Nazario, Carlos E D; Silva, Meire R; Franco, Maraíssa S; Lanças, Fernando M

2015-11-20

The purpose of this article is to underline the miniaturized LC instrumental system and describe the evolution of commercially available systems by discussing their advantages and drawbacks. Nowadays, there are already many miniaturized LC systems available with a great variety of pump design, interface and detectors as well as efficient columns technologies and reduced connections devices. The solvent delivery systems are able to drive the mobile phase without flow splitters and promote gradient elution using either dual piston reciprocating or syringe-type pumps. The mass spectrometry as detection system is the most widely used detection system; among many alternative ionization sources direct-EI LC-MS is a promising alternative to APCI. In addition, capillary columns are now available showing many possibilities of stationary phases, inner diameters and hardware materials. This review provides a discussion about miniaturized LC demonstrating fundamentals and instrumentals' aspects of the commercially available miniaturized LC instrumental system mainly nano and micro LC formats. This review also covers the recent developments and trends in instrumentation, capillary and nano columns, and several applications of this very important and promising field. Copyright © 2015 Elsevier B.V. All rights reserved.

Adaptive P300 based control system

PubMed Central

Jin, Jing; Allison, Brendan Z.; Sellers, Eric W.; Brunner, Clemens; Horki, Petar; Wang, Xingyu; Neuper, Christa

2015-01-01

An adaptive P300 brain-computer interface (BCI) using a 12 × 7 matrix explored new paradigms to improve bit rate and accuracy. During online use, the system adaptively selects the number of flashes to average. Five different flash patterns were tested. The 19-flash paradigm represents the typical row/column presentation (i.e., 12 columns and 7 rows). The 9- and 14-flash A & B paradigms present all items of the 12 × 7 matrix three times using either nine or 14 flashes (instead of 19), decreasing the amount of time to present stimuli. Compared to 9-flash A, 9-flash B decreased the likelihood that neighboring items would flash when the target was not flashing, thereby reducing interference from items adjacent to targets. 14-flash A also reduced adjacent item interference and 14-flash B additionally eliminated successive (double) flashes of the same item. Results showed that accuracy and bit rate of the adaptive system were higher than the non-adaptive system. In addition, 9- and 14-flash B produced significantly higher performance than their respective A conditions. The results also show the trend that the 14-flash B paradigm was better than the 19-flash pattern for naïve users. PMID:21474877

Rational design of the column of a heavy multipurpose machining center

NASA Astrophysics Data System (ADS)

Atapin, V. V.; Kurlaev, N. V.

2016-04-01

The main purpose in the design of supporting constructions of heavy multipurpose machining center is the reduction of mass at the given precision and productivity of machining. Accomplish these ends the technology of rational design of supporting constructions is offered. This technology is based on the decomposition method and the finite elements method in the combination with optimization methods. The technology has four stages: 1) calculation of external forces and loads, 2) as a result the boundary conditions (force, kinematics) for individual supporting constructions are formed, 3) a problem about final optimal distribution of a material by the individual supporting constructions with the real cross-section is solved; 4) dynamic analysis. By the example of design of the column of a heavy multipurpose machining center the main stages of rational design of the individual supporting constructions are shown. At a design stage of the carrying system consisting of load-bearing structures with simplified geometry, optimum overall dimensions of the column are identified. For the admitted system of preferences, it is necessary to accept the fact that the carrying system with the column with the sizes of cross section of 1.8 m (along x axis) and 2.6 m (along y axis) is the best. The analysis of the work of the column under the torsion condition with the use of method of mechanics shows that the column with square cross sections = 2.46·2.46 m which rigidity on torsion is 26 % higher in comparison with a production version is the best. The results of calculation show that a production-release design of the column with longitudinal and transverse edges of rigidity is 24 % heavier than the column with the edges located on a diagonally at equal rigidity.

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.

A Theory of How Columns in the Neocortex Enable Learning the Structure of the World

PubMed Central

Hawkins, Jeff; Ahmad, Subutai; Cui, Yuwei

2017-01-01

Neocortical regions are organized into columns and layers. Connections between layers run mostly perpendicular to the surface suggesting a columnar functional organization. Some layers have long-range excitatory lateral connections suggesting interactions between columns. Similar patterns of connectivity exist in all regions but their exact role remain a mystery. In this paper, we propose a network model composed of columns and layers that performs robust object learning and recognition. Each column integrates its changing input over time to learn complete predictive models of observed objects. Excitatory lateral connections across columns allow the network to more rapidly infer objects based on the partial knowledge of adjacent columns. Because columns integrate input over time and space, the network learns models of complex objects that extend well beyond the receptive field of individual cells. Our network model introduces a new feature to cortical columns. We propose that a representation of location relative to the object being sensed is calculated within the sub-granular layers of each column. The location signal is provided as an input to the network, where it is combined with sensory data. Our model contains two layers and one or more columns. Simulations show that using Hebbian-like learning rules small single-column networks can learn to recognize hundreds of objects, with each object containing tens of features. Multi-column networks recognize objects with significantly fewer movements of the sensory receptors. Given the ubiquity of columnar and laminar connectivity patterns throughout the neocortex, we propose that columns and regions have more powerful recognition and modeling capabilities than previously assumed. PMID:29118696

Local connections between the columns of the periaqueductal gray matter: a case for intrinsic neuromodulation.

PubMed

Jansen, A S; Farkas, E; Mac Sams, J; Loewy, A D

1998-02-16

Chemical stimulation of the lateral or ventrolateral columns of the midbrain periaqueductal gray matter (PAG) in conscious animals produces opposite responses (viz., defensive behavior and pressor responses from the lateral column vs. quiescence and depressor responses from the ventrolateral column), raising the possibility that the two columns are interconnected. To test this hypothesis, two types of anatomical experiments were performed in rats. First, the anterograde axonal marker Phaseolus vulgaris leuco-agglutinin (PHA-L) was injected into individual PAG columns or adjoining regions which included the Edinger-Westphal, dorsal raphe, and precommissural nuclei. The results shows that each column projects bilaterally to all of the other PAG columns, and also provides local connections within its own column. Furthermore, the Edinger-Westphal and precommissural nuclei project to all four PAG columns, while the dorsal raphe nucleus projects only to the ventrolateral and lateral columns. In a second experiment, we found that cardiovascular-related PAG projection neurons of both the lateral and ventrolateral columns receive an input from the reciprocal PAG column. This was demonstrated by a double tracer neuroanatomical study in which PHA-L was first iontophoretically ejected into either the lateral or ventrolateral PAG columns and then, several days later the retrograde transneuronal viral tracer, pseudorabies virus, was injected into the stellate sympathetic ganglion. Intra-PAG circuits were visualized by a dual immunohistochemical procedure. These results suggest that during the fight-or-flight response when the 'fight' program is activated, inhibition of the 'flight' PAG network may occur and the converse situation may occur during the flight response. Copyright 1997 Elsevier Science B.V.

Development of and fabrication of high resolution gas chromatographic capillary columns

NASA Technical Reports Server (NTRS)

Zlatkis, A.

1982-01-01

Gas chromatographic columns which are used in the trace gas analyzer (TGA) for the space shuttle are coated with a polyoxyethylene lauryl ether. This stationary phase is of medium polarity and has a temperature limit of 160 C. A polymer for this application which has an improved thermal stability is investigated. The use of fused silica capillary columns with specially bonded phases as well as an introduction system (on column) was also studied.

Experimental Evaluation of the Failure of a Seismic Design Category - B Precast Concrete Beam-Column Connection System

DTIC Science & Technology

2014-12-01

27  Figure 37. Posttest view of SDC-B experimental specimen...center vertical displacement (y2) vs. time (x). .............................................. 28  Figure 40. Posttest front view of the SDC B top...center column. .......................................................... 30  Figure 41. Posttest front view of end columns

Mixed retention mechanism of proteins in weak anion-exchange chromatography.

PubMed

Liu, Peng; Yang, Haiya; Geng, Xindu

2009-10-30

Using four commercial weak anion-exchange chromatography (WAX) columns and 11 kinds of different proteins, we experimentally examined the involvement of hydrophobic interaction chromatography (HIC) mechanism in protein retention on the WAX columns. The HIC mechanism was found to operate in all four WAX columns, and each of these columns had a better resolution in the HIC mode than in the corresponding WAX mode. Detailed analysis of the molecular interactions in a chromatographic system indicated that it is impossible to completely eliminate hydrophobic interactions from a WAX column. Based on these results, it may be possible to employ a single WAX column for protein separation by exploiting mixed modes (WAX and HIC) of retention. The stoichiometric displacement theory and two linear plots were used to show that mechanism of the mixed modes of retention in the system was a combination of two kinds of interactions, i.e., nonselective interactions in the HIC mode and selective interactions in the IEC mode. The obtained U-shaped elution curve of proteins could be distinguished into four different ranges of salt concentration, which also represent four retention regions.

Numerical and experimental analyses of lighting columns in terms of passive safety

NASA Astrophysics Data System (ADS)

Jedliński, Tomasz Ireneusz; Buśkiewicz, Jacek

2018-01-01

Modern lighting columns have a very beneficial influence on road safety. Currently, the columns are being designed to keep the driver safe in the event of a car collision. The following work compares experimental results of vehicle impact on a lighting column with FEM simulations performed using the Ansys LS-DYNA program. Due to high costs of experiments and time-consuming research process, the computer software seems to be very useful utility in the development of pole structures, which are to absorb kinetic energy of the vehicle in a precisely prescribed way.

Optimized anion exchange column isolation of zirconium-89 ( 89 Zr) from yttrium cyclotron target: Method development and implementation on an automated fluidic platform

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

O’Hara, Matthew J.; Murray, Nathaniel J.; Carter, Jennifer C.

Zirconium-89 (89Zr), produced by the (p,n) reaction from naturally monoisotopic yttrium (natY), is a promising positron emitting isotope for immunoPET imaging. Its long half-life of 78.4 h is sufficient for evaluating slow physiological processes. A prototype automated fluidic system, coupled to on-line and in-line detectors, has been constructed to facilitate development of new 89Zr purification methodologies. The highly reproducible reagent delivery platform and near-real time monitoring of column effluents allows for efficient method optimization. The separation of Zr from dissolved Y metal targets was evaluated using several anion exchange resins. Each resin was evaluated against its ability to quantitatively capturemore » Zr from a load solution that is high in dissolved Y. The most appropriate anion exchange resin for this application was identified, and the separation method was optimized. The method is capable of a high Y decontamination factor (>105) and has been shown to separate Fe, an abundant contaminant in Y foils, from the 89Zr elution fraction. Finally, the performance of the method was evaluated using cyclotron bombarded Y foil targets. The separation method was shown to achieve >95% recovery of the 89Zr present in the foils. The 89Zr eluent, however, was in a chemical matrix not immediately conducive to labeling onto proteins. The main intent of this study was to develop a tandem column 89Zr purification process, wherein the anion exchange column method described here is the first separation in a dual-column purification process.« less

Transport and Transformation of Selenium and Other Constituents of Flue-Gas Desulfurization Wastewater in Water-Saturated Soil Materials.

PubMed

Galkaduwa, Madhubhashini B; Hettiarachchi, Ganga M; Kluitenberg, Gerard J; Hutchinson, Stacy L; Davis, Lawrence; Erickson, Larry E

2017-03-01

Constructed wetland treatment systems are used to remove selenium (Se) from flue-gas desulfurization (FGD) wastewater (WW). However, direct confirmation of the mechanism responsible for FGD WW Se retention in soil is lacking. A laboratory-based soil column study was performed to develop an evidence-based mechanism of Se retention and to study the behavior and the retention capacity of FGD WW constituents in water-saturated soil. A deoxygenated 1:1 mixture of FGD WW and raw water was delivered to the columns bottom-up at a flux of 1.68 cm d for 100 d. Some of the columns were flushed with the raw water at the same rate for an additional 100 d. Column effluent was analyzed for constituents of concern. Results showed a complete retention of FGD WW Se in the soil materials. Boron and fluorine were partially retained; however, sulfur, sodium, and chlorine retention was poor, agreeing with field observations. The FGD WW Se was retained in soil near the inlet end of the columns, indicating its limited mobility under reduced conditions. Sequential extraction procedure revealed that retained Se was mainly sequestered as stable/residual forms. Bulk- and micro-X-ray absorption near-edge structure spectroscopy confirmed that Se was mainly retained as reduced/stable species [Se(IV), organic Se, and Se(0)]. This study provides direct evidence for FGD WW Se retention in water-saturated soil via the transformation of oxidized Se into reduced/stable forms. Copyright © by the American Society of Agronomy, Crop Science Society of America, and Soil Science Society of America, Inc.

Determination of model parameters for zinc (II) ion biosorption onto powdered waste sludge (PWS) in a fed-batch system.

PubMed

Kargi, Fikret; Cikla, Sinem

2007-12-01

Biosorption of zinc (II) ions onto pre-treated powdered waste sludge (PWS) was investigated using a completely mixed tank operating in fed-batch mode instead of an adsorption column. Experiments with variable feed flow rate (0.05-0.5 L h(-1)), feed Zn(II) ion concentrations (37.5-275 mg L(-1)) and amount of adsorbent (1-6 g PWS) were performed using fed-batch operation at pH 5 and room temperature (20-25 degrees C). Break-through curves describing variations of aqueous (effluent) zinc ion concentrations with time were determined for different operating conditions. Percent zinc removal from the aqueous phase decreased, but the biosorbed (solid phase) zinc ion concentration increased with increasing feed flow rate and zinc concentration. A modified Bohart-Adams equation was used to determine the biosorption capacity of PWS (q'(s)) and the rate constant (K) for zinc ion biosorption. Biosorption capacity (q'(s)=57.7 g Zn kg(-1) PWS) of PWS in fed-batch operation was found to be comparable with powdered activated carbon (PAC) in column operations. However, the adsorption rate constant (K=9.17 m(3) kg(-1) h(-1)) in fed-batch operation was an order of magnitude larger than those obtained in adsorption columns because of elimination of mass transfer limitations encountered in the column operations. Therefore, a completely mixed tank operated in fed-batch mode was proven to be more advantageous as compared to adsorption columns due to better contact between the phases yielding faster adsorption rates.

Mechanism of nucleation and growth of catalyst-free self-organized GaN columns by MOVPE

NASA Astrophysics Data System (ADS)

Wang, Xue; Li, Shunfeng; Fündling, Sönke; Wehmann, Hergo-H.; Strassburg, Martin; Lugauer, Hans-Jürgen; Steegmüller, Ulrich; Waag, Andreas

2013-05-01

The growth mechanism of catalyst-free self-organized GaN nuclei and three-dimensional columns on sapphire by metal organic vapour phase epitaxy (MOVPE) is investigated. Temperature- and time-dependent growth is performed. The growth behaviour can be characterized by two different kinetic regimes: mass-transport-limited growth and thermodynamically limited growth. The sum of activation energies for thermodynamic barrier of nucleation and for surface diffusion/mass-transport limitation, i.e. Whet +Ed, is 0.57 eV in the ‘low’-temperature region and 2.43 eV in the ‘high’-temperature region. GaN columns grown under the same conditions have very comparable height, which is not dependent on their diameter or the distance to other columns. Therefore, the growth rate is presumably limited by the incorporation rate on the top surface of columns. The height and diameter at the top of the GaN columns increase linearly with time and no height limit is observed. The GaN columns can reach more than 40 µm in height. Moreover, the investigated GaN columns are Ga-polar.

Stability and Structure of Star-Shape Granules

NASA Astrophysics Data System (ADS)

Zhao, Yuchen; Bares, Jonathan; Zheng, Matthew; Dierichs, Karola; Menges, Achim; Behringer, Robert

2015-11-01

Columns are made of convex non-cohesive grains like sand collapse after being released from initial positions. On the other hand, various architectures built by concave grains can maintain stability. We explore why these structures are stable, and how stable they can be. We performed experiments by randomly pouring identical star-shape particles into hollow cylinders left on glass and a rough base, and observed stable granular columns after lifting the cylinders. Particles have six 9 mm arms, which extend symmetrically in the xyz directions. Both the probability of creating a stable column and mechanical stability aspects have been investigated. We define r as the weight fraction of particles that fall out of the column after removing confinement. r gradually increases as the column height increases, or the column diameter decreases. We also explored different experiment conditions such as vibration of columns with confinement, or large basal friction. We also consider different stability measures such as the maximum inclination angle or maximum weight a column can support. In order to understand structure leading to stability, 3D CT scan reconstructions of columns have been done and coordination number and packing density will be discussed. We acknowledge supports from W.M.Keck Foundation and Research Triangle MRSEC.

Seismic retrofit of spliced sleeve connections for precast bridge piers : research brief.

DOT National Transportation Integrated Search

2017-03-01

The rehabilitation method described in this paper concerns connections between precast columns and footings, and precast columns and pier caps. This research uses high-performance materials, including headed reinforcing bar, epoxy, nonshrink or expan...

Cu2+-imprinted cross-linked chitosan resin as micro-column packing materials for online chemiluminescence determination of trace copper.

PubMed

Nie, Feng; Hao, Liang; Gao, Mei; Wu, Yingchun; Li, Xinsheng; Yu, Sha

2011-01-01

The Cu(2+)-imprinted cross-linked chitosan resin was synthesized and the binding characteristic of the resin to Cu(2+) was evaluated. The prepared resin was packed into a micro-glass column and used as micro-separating column. The micro-separating column was connected into the chemiluminescence flow system and placed in front of the window of the photomultiplier tube. Based on the luminol-hydrogen peroxide chemiluminescence system, a flow injection online chemiluminescence method for determination of trace copper was developed and trace Cu(2+) in complex samples was successfully determined. The proposed method improved the shortcomings of chemiluminescence method's poor selectivity. Copyright © 2010 John Wiley & Sons, Ltd.

Nondestructive evaluation of the preservation state of stone columns in the Hospital Real of Granada

NASA Astrophysics Data System (ADS)

Moreno de Jong van Coevorden, C.; Cobos Sánchez, C.; Rubio Bretones, A.; Fernández Pantoja, M.; García, Salvador G.; Gómez Martín, R.

2012-12-01

This paper describes the results of the employment of two nondestructive evaluation methods for the diagnostic of the preservation state of stone elements. The first method is based on ultrasonic (US) pulses while the second method uses short electromagnetic pulses. Specifically, these methods were applied to some columns, some of them previously restored. These columns are part of the architectonic heritage of the University of Granada, in particular they are located at the patio de la capilla del Hospital Real of Granada. The objective of this work was the application of systems based on US pulses (in transmission mode) and the ground-penetrating radar systems (electromagnetic tomography) in the diagnosis and detection of possible faults in the interior of columns.

Capillary Columns with a Sorbent Based on Functionalized Poly(1-Trimethylsilyl-1-Propyne) for the Elution Analysis of Natural Gas

NASA Astrophysics Data System (ADS)

Yakovleva, E. Yu.; Patrushev, Yu. V.; Pai, Z. P.

2018-05-01

The chromatographic properties of capillary columns prepared using functionalized poly(1- trimethylsilyl-1-propyne) (PTMSP) are evaluated and compared with the performance of a commercial column with divinylbenzene polymer sorbent. The loading capacity of a PTMSP column with dimensions of 30 m × 0.53 mm × 0.8 μm is shown to be about 2.5 times higher than that of a divinylbenzene polymer column with a diameter of 0.32 mm and a film thickness of 10 μm. The increased value of the background current for PTMSP columns at 220°C is explained by the presence of non-polar bulky substituents in the polymer chain. Differences in the order of elution are found for the following pairs of compounds: acetylene-ethylene; ethane-water; butene-1-isobutane; and sulfur dioxide-carbonyl sulfide. On a column with the functionalized PTMC, analysis of a mixture composition close to natural gas is found to be complete within 27 min.

Development of a highly sensitive methodology for quantitative determination of fexofenadine in a microdose study by multiple injection method using ultra-high performance liquid chromatography with tandem mass spectrometry.

PubMed

Tanaka, Yukari; Yoshikawa, Yutaka; Yasui, Hiroyuki

2012-01-01

An ultra high-sensitivity method for quantifying fexofenadine concentration in rat plasma samples by multiple injection method (MIM) was developed for a microdose study. In this study, MIM involved continuous injections of multiple samples containing the single compound into a column of the ultra-HPLC (UHPLC) system, and then, temporary trapping of the analyte at the column head. This was followed by elution of the compound from the column and detection by mass spectrometer. Fexofenadine, used as a model compound in this study, was extracted from the plasma samples by a protein precipitation method. Chromatographic separation was achieved on a reversed-phase C18 column by using a gradient method with 0.1% formic acid and 0.1% formic acid in acetonitrile as the mobile phase. The analyte was quantified in the positive-ion electrospray ionization mode using selected reaction monitoring. In this study, the analytical time per fexofenadine sample was approximately 2 min according to the UHPLC system. The method exhibited the linear dynamic ranges of 5-5000 pg/mL for fexofenadine in rat plasma. The intra-day precisions were from 3.2 to 8.7% and the accuracy range was 95.2-99.3%. The inter-day precisions and accuracies ranged from 3.5 to 8.4% and from 98.6 to 102.6%, respectively. The validated MIM was successfully applied to a microdose study in the rats that received oral administration of 100 µg/kg fexofenadine. We suggest that this method might be beneficial for the quantification of fexofenadine concentrations in a microdose clinical study.

Evaluation of the Cytosorb™ Hemoadsorptive Column in a Pig Model of Severe Smoke and Burn Injury.

PubMed

Linden, Katharina; Scaravilli, Vittorio; Kreyer, Stefan F X; Belenkiy, Slava M; Stewart, Ian J; Chung, Kevin K; Cancio, Leopoldo C; Batchinsky, Andriy I

2015-11-01

Host inflammatory response to any form of tissue injury, including burn, trauma, or shock, has been well documented. After significant burns, cytokines can increase substantially within the first 24 h after injury and may contribute to subsequent organ failure. Hemoadsorption by cytokine-adsorbing columns may attenuate this maladaptive response, thereby improving outcomes. The aim of this study was to investigate the feasibility, technical safety, and efficacy of cytokine and myoglobin removal by early use of a cytokine absorbing column (CytoSorb) in a porcine model of smoke inhalation and burn injury. Anesthetized female Yorkshire pigs (n = 15) were injured by wood bark smoke inhalation and a 40% total body surface area deep burn and observed for 72 h or death. The animals were randomized to hemoadsorption treatment (n = 9) or a sham group (n = 6) before injury. A 6-h hemoadsorption or sham session was performed on days one, two, and three. Serum cytokines (IL-1b, IL-6, IL-8, IL-10, TNF-alpha) and myoglobin were measured systemically, locally in bronchoalveolar lavage fluid and also in circulating blood before and after the adsorbing column to evaluate single pass clearance by the device. Hemoadsorption caused significant removal of IL-1b, IL-6, IL-10, and myoglobin across the device mainly during the first run, ranging from 22% for IL-6 to 29% for IL-1b and 41% removal rates for myoglobin after 15  min of treatment. Systemic cytokine or myoglobin serum concentrations did not change. In a porcine model of smoke and burn injury, hemoadsorption using the CytoSorb cartridge did not result in significant systemic or pulmonary reductions in the measured cytokines or myoglobin despite efficient transmembrane reductions. Further investigations are needed to optimize the efficiency of mediator clearance to affect both circulating levels and clinically relevant outcomes.

New Standards in Liquid Waste Treatment at Fukushima Dai-ichi - 13134

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

Sylvester, Paul; Milner, Tim; Ruffing, Jennifer

The earthquake and tsunami on March 11, 2011 severely damaged the Fukushima Dai-ichi nuclear plant leading to the most severe nuclear incident since Chernobyl. Ongoing operations to cool the damaged reactors at the site have led to the generation of highly radioactive coolant water. This is currently mainly treated to remove Cs-137 and Cs-134 and passed through a reverse osmosis (RO) unit to reduce the salinity before being cycled back to the reactors. Because only the Cs isotopes are removed, the RO reject water still contains many radioactive isotopes and this has led to the accumulation of over 200,000 cubicmore » meters (52 million gallons) of extremely contaminated water which is currently stored on site in tanks. EnergySolutions, in partnership with Toshiba, were contracted to develop a system to reduce 62 isotopes in this waste down to allowable levels. This was a significant technical challenge given the high background salt content of the wastewater, the variation in aqueous chemistry of the radioactive isotopes and the presence of non-active competing ions (e.g. Ca and Mg) which inhibit the removal of isotopes such as Sr-89 and Sr-90. Extensive testing was performed to design a suitable system that could meet the required decontamination goals. These tests were performed over a 6 month period at facilities available in the nearby Fukushima Dai-ni laboratory using actual waste samples. This data was then utilized to design a Multi Radioactive Nuclides Removal System (MRRS) for Fukushima which is a modified version of EnergySolutions' proprietary Advanced Liquid Processing System (ALPS)'. The stored tank waste is fed into a preliminary precipitation system where iron flocculation is performed to remove a number of isotopes, including Sb-125, Ru-106, Mn-54 and Co-60. The supernatant is then fed into a second precipitation tank where the pH is adjusted and the bulk of the Mg, Ca and Sr precipitated out as carbonates and hydroxides. After passing through a cross-flow ultrafiltration membrane, the permeate then goes through a total of 14 fixed ion exchange and adsorbent columns followed by a disposable polishing column to polish the residual isotopes down to allowable levels. At the end of the system, the effluent is filtered for a final time to removal any particulates that may have been picked up from the media columns and then stored prior to analysis. (authors)« less

Mathematical solution of the stone column effect on the load bearing capacity and settlement using numerical analysis

NASA Astrophysics Data System (ADS)

Madun, A.; Meghzili, S. A.; Tajudin, SAA; Yusof, M. F.; Zainalabidin, M. H.; Al-Gheethi, A. A.; Dan, M. F. Md; Ismail, M. A. M.

2018-04-01

The most important application of various geotechnical construction techniques is for ground improvement. Many soil improvement project had been developed due to the ongoing increase in urban and industrial growth and the need for greater access to lands. Stone columns are one of the best effective and feasible techniques for soft clay soil improvement. Stone columns increase the bearing capacity and reduce the settlement of soil. Finite element analyses were performed using the program PLAXIS 2D. An elastic-perfectly plastic constitutive relation, based on the Mohr–Coulomb criterion, governs the soft clay and stone column behaviour. This paper presents on how the response surface methodology (RSM) software is used to optimize the effect of the diameters and lengths of column on the load bearing capacity and settlement of soft clay. Load tests through the numerical modelling using Plaxis 2D were carried out on the loading plate at 66 mm. Stone column load bearing capacity increases with the increasing diameter of the column and settlement decreases with the increasing length of the column. Results revealed that the bigger column diameter, the higher load bearing capacity of soil while the longer column length, the lower settlement of soil. However, the optimum design of stone column was varied with each factor (diameter and length) separately for improvement.

Small Column Ion Exchange Testing of Superlig 644 for Removal of 137Cs from Hanford Tank Waste Envelope A (Tank 241-AW-101)

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

DE Kurath; DL Blanchard; JR Bontha

The current BNFL Inc. flow sheet for the pretreatment of the Hanford High-Level tank wastes includes the use of Superlig{reg_sign} materials for the removal of {sup 137}Cs from the aqueous fraction of the waste. The Superlig materials applicable to cesium removal include the cesium selective Superlig 632 and Superlig 644. These materials have been developed and supplied by IBC Advanced Technologies, Inc., American Fork, UT. The work contained in this report involves testing the Superlig 644 ion exchange material in a small dual column system (15 mL each; L/D = 5.7). The sample processed was approximately 2.5 L of dilutedmore » waste [Na{sup +}] = 4.6M from Tank 241-AW-101 (Envelope A). This waste had been previously clarified in a single tube cross-flow filtration unit. All ion exchange process steps were tested including resin bed preparation, loading, feed displacement water rinse, elution and resin regeneration. During the initial run, the lag column did not perform as expected so that the {sup 137}Cs concentration in the effluent composite was above the LAW treatment limits. This required a second column run with the partially decontaminated feed that was conducted at a higher flow rate. A summary of performance measures for both runs is shown in Table S1. The Cs {lambda} values represent a measure of the effective capacity of the SL-644 resin. The Cs {lambda} of 143 for the lead column in run 1 is very similar to the value obtained by the Savannah River Technology Center during Phase 1A testing. The larger Cs {lambda} value for run 2 reflects a general trend for the effective capacity of the SL-644 material to increase as the cesium concentration decreases. The low value for the lag column during the first run indicates that it did not perform as expected. This may have been due to insufficient conditioning of the bed prior to the start of the loading step or to air in the bed that caused channeling. Equilibrium data obtained with batch contacts using the AW-101 Cs IX feed indicates a range for the Cs {lambda} of 80--97. The maximum decontamination factor (DF) for {sup 137}CS is based on analysis of the first samples collected from each column and the concentration in the feed for each run. While the DF's are lower for the second run, this is attributed to the lower {sup 137}Cs concentration in the feed and the increased flowrate. The overall composite DF for run 2 was quite good since both columns functioned well. The overall DF for both runs was 3,000, which provided an effluent with a {sup 137}Cs concentration of 5.89E-02 Ci/m{sup 3} (C/C{sub 0} = 3.3 IE-04). The {sup 137}Cs concentration in the effluent composite was 7.3% of the contract limit for {sup 137}Cs and also below the basis of design limit.« less

Latching mechanism for deployable/re-stowable columns useful in satellite construction

NASA Technical Reports Server (NTRS)

Ahl, E. L., Jr. (Inventor)

1986-01-01

A column longeron latch assembly provides the securing mechanism for the deployable, telescoping column of a hoop/column antenna. The column is an open lattice structure with three longerons disposed 120 deg apart as the principle load bearing member. The column is deployed from a pair of eleven nested bays disposed on opposite sides of a center section under the influence of a motor-cable-pulley system. The longeron latch is a four bar linkage mechanism using the over-center principle for automatically locking the longeron sections into position during deployment. The latch is unlocked when the antenna is to be restowed. A spring pack disposed in the end of each longeron serves to absorb stress forces on the deployed column through the cam head piston and abutting latch from an adjacent longeron.