Liquid chromatographic extraction medium

DOEpatents

Horwitz, E.P.; Dietz, M.L.

1994-09-13

A method and apparatus are disclosed for extracting strontium and technetium values from biological, industrial and environmental sample solutions using a chromatographic column. An extractant medium for the column is prepared by generating a solution of a diluent containing a Crown ether and dispersing the solution on a resin substrate material. The sample solution is highly acidic and is introduced directed to the chromatographic column and strontium or technetium is eluted using deionized water. 1 fig.

Theoretical study of the accuracy of the elution by characteristic points method for bi-langmuir isotherms.

PubMed

Ravald, L; Fornstedt, T

2001-01-26

The bi-Langmuir equation has recently been proven essential to describe chiral chromatographic surfaces and we therefore investigated the accuracy of the elution by characteristic points method (ECP) for estimation of bi-Langmuir isotherm parameters. The ECP calculations was done on elution profiles generated by the equilibrium-dispersive model of chromatography for five different sets of bi-Langmuir parameters. The ECP method generates two different errors; (i) the error of the ECP calculated isotherm and (ii) the model error of the fitting to the ECP isotherm. Both errors decreased with increasing column efficiency. Moreover, the model error was strongly affected by the weight of the bi-Langmuir function fitted. For some bi-Langmuir compositions the error of the ECP calculated isotherm is too large even at high column efficiencies. Guidelines will be given on surface types to be avoided and on column efficiencies and loading factors required for adequate parameter estimations with ECP.

High throughput screening of active pharmaceutical ingredients by UPLC.

PubMed

Al-Sayah, Mohammad A; Rizos, Panagiota; Antonucci, Vincent; Wu, Naijun

2008-07-01

Ultra performance LC (UPLC) was evaluated as an efficient screening approach to facilitate method development for drug candidates. Three stationary phases were screened: C-18, phenyl, and Shield RP 18 with column dimensions of 150 mm x 2.1 mm, 1.7 microm, which should theoretically generate 35,000 plates or 175% of the typical column plate count of a conventional 250 mm x 4.6 mm, 5 microm particle column. Thirteen different active pharmaceutical ingredients (APIs) were screened using this column set with a standardized mobile-phase gradient. The UPLC method selectivity results were compared to those obtained for these compounds via methods developed through laborious trial and error screening experiments using numerous conventional HPLC mobile and stationary phases. Peak capacity was compared for columns packed with 5 microm particles and columns packed with 1.7 microm particles. The impurities screened by UPLC were confirmed by LC/MS. The results demonstrate that simple, high efficiency UPLC gradients are a feasible and productive alternative to more conventional multiparametric chromatographic screening approaches for many compounds in the early stages of drug development.

Apparatus and process for the separation of hydrophobic and hydrophilic particles using microbubble column flotation together with a process and apparatus for generation of microbubbles

DOEpatents

Yoon, Roe-Hoan; Adel, Gregory T.; Luttrell, Gerald H.

1992-01-01

A method and apparatus are disclosed for the microbubble flotation separation of very fine and coarse particles, especially coal and minerals, so as to produce high purity and high recovery efficiency. This is accomplished through the use of a flotation column, microbubbles, recycling of the flotation pulp, and countercurrent wash water to gently wash the froth. Also disclosed are unique processes and apparatus for generating microbubbles for flotation in a highly efficient and inexpensive manner using either a porous tube or in-line static generators.

Apparatus and process for the separation of hydrophobic and hydrophilic particles using microbubble column flotation together with a process and apparatus for generation of microbubbles

DOEpatents

Yoon, Roe-Hoan; Adel, Gregory T.; Luttrell, Gerald H.

1998-01-01

A method and apparatus are disclosed for the microbubble flotation separation of very fine and coarse particles, especially coal and minerals, so as to produce high purity and high recovery efficiency. This is accomplished through the use of a flotation column, microbubbles, recycling of the flotation pulp, and countercurrent wash water to gently wash the froth. Also disclosed are unique processes and apparatus for generating microbubbles for flotation in a highly efficient and inexpensive manner using either a porous tube or in-line static generators.

40 CFR 799.6786 - TSCA water solubility: Generator column method.

Code of Federal Regulations, 2010 CFR

2010-07-01

... quantitative) analysis of solvent extract in paragraph (c)(3)(iv) of this section. The design of the generator... partition coefficients of hydrophobic substances. Journal of Research, National Bureau of Standards, 86:361...

Use of the Oak Ridge National Laboratory tungsten-188/rhenium-188 generator for preparation of the rhenium-188 HDD/lipiodol complex for trans-arterial liver cancer therapy

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

Jeong, J M; Knapp Jr, Russ F

2008-01-01

This work describes the installation, use, and quality control (QC) of the alumina-based tungsten-188 ({sup 188}W)/rhenium-188 ({sup 188}Re) generators provided by the Oak Ridge National Laboratory (ORNL). In addition, methods used for concentration of the {sup 188}Re-perrhenate bolus and preparation of {sup 188}Re-labeled HDD (4-hexadecyl-2,2,9,9-tetramethyl-4,7-diaza-1,10-decanethiol) for trans-arterial administration for therapy of nonresectable liver cancer also are described. The {sup 188}W/{sup 188}Re generator has a long useful shelf-life of several months and is a convenient on-site {sup 188}Re production system. {sup 188}Re has excellent therapeutic and imaging properties (T{sub 1/2} 16.9 hours; E{sub {beta}max} 2.12 MeV; 155-keV gamma ray, 15%) andmore » is cost effectively obtained on demand by saline elution of the generator. The clinical efficacy of a variety of {sup 188}Re-labeled agents has been demonstrated for several therapeutic applications. Because of the favorable physical properties of {sup 188}Re, several {sup 188}Re-labeled agents are being developed and evaluated for the treatment of nonresectable/refractory liver cancer. {sup 188}Re-labeled HDD has been the most widely studied of these agents for this application and has been introduced into clinical trials at a number of institutions. The trans-arterial administration of {sup 188}Re-labeled agents for treatment of inoperable liver cancer requires use of high-level (1-2 Ci) {sup 188}W/{sup 188}Re generators. The handling of such high levels of {sup 188}Re imposes radiological precautions normally not encountered in a radiopharmacy and adequate care and ALARA (i.e., 'As Low As Reasonably Achievable') principles must be followed. The ORNL generator provides consistently high {sup 188}Re yields (>75%) and low {sup 188}W parent breakthrough (<10{sup -3}%) over an extended shelf-life of several months. However, the high elution volumes (20-40 mL for 1-2 Ci generators) can require concentration of the {sup 188}Re bolus by postelution passage through silver cation chloride trapping columns used in the cost-effective tandem cation/anion column system. The silver column removes the high levels of chloride anion as insoluble AgCl, thus allowing subsequent specific trapping of the perrhenate anion on the small (QMA SeaPak) anion column. This method permits subsequent elution of {sup 188}Re-perrhenate with a small volume of saline, providing a very high activity-concentration solution. Because the {sup 188}Re-specific volume-activity concentration continually decreases with time, the tandem system is especially effective method for extending the useful generator shelf-life. Low elution flow rates (<1 mL/min) minimize any high back pressure which may be encountered during generator/tandem column elution when using tightly packed, small-particle-size commercial columns. In-house preparation of silver cation columns is recommended since the chloride trapping capacity is essentially unlimited, it is inexpensive and not limited in availability to any one supplier, and back pressure can be eliminated by the use of larger particles. Methods for the preparation of {sup 188}Re-HDD have been optimized and this agent can be obtained in high yield (80%).« less

Use of the ORNL Tungsten-188/Rhenium-188 Generator for Preparation of the Rhenium-188 HDD/Lipiodol Complex for Transarterial Liver Cancer Therapy

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

Knapp Jr, Russ F; Jeong, J M

2008-01-01

This work describes the installation, use, and quality control (QC) of the alumina-based tungsten-188 ({sup 188}W)/rhenium-188 ({sup 188}Re) generators provided by the Oak Ridge National Laboratory (ORNL). In addition, methods used for concentration of the {sup 188}Re-perrhenate bolus and preparation of {sup 188}Re-labeled HDD (4-hexadecyl-2,2,9,9-tetramethyl-4,7-diaza-1,10-decanethiol) for trans-arterial administration for therapy of nonresectable liver cancer also are described. The {sup 188}W/{sup 188}Re generator has a long useful shelf-life of several months and is a convenient on-site {sup 188}Re production system. {sup 188}Re has excellent therapeutic and imaging properties (T{sub 1/2} 16.9 hours; E{beta}{sub max} 2.12 MeV; 155-keV gamma ray, 15%) andmore » is cost effectively obtained on demand by saline elution of the generator. The clinical efficacy of a variety of {sup 188}Re-labeled agents has been demonstrated for several therapeutic applications. Because of the favorable physical properties of {sup 188}Re, several {sup 188}Re-labeled agents are being developed and evaluated for the treatment of nonresectable/refractory liver cancer. {sup 188}Re-labeled HDD has been the most widely studied of these agents for this application and has been introduced into clinical trials at a number of institutions. The trans-arterial administration of {sup 188}Re-labeled agents for treatment of inoperable liver cancer requires use of high-level (1-2 Ci) {sup 188}W/{sup 188}Re generators. The handling of such high levels of {sup 188}Re imposes radiological precautions normally not encountered in a radiopharmacy and adequate care and ALARA (ie, 'As Low As Reasonably Achievable') principles must be followed. The ORNL generator provides consistently high {sup 188}Re yields (>75%) and low {sup 188}W parent breakthrough (<10{sup -3}%) over an extended shelf-life of several months. However, the high elution volumes (20-40 mL for 1-2 Ci generators) can require concentration of the {sup 188}Re bolus by postelution passage through silver cation chloride trapping columns used in the cost-effective tandem cation/anion column system. The silver column removes the high levels of chloride anion as insoluble AgCl, thus allowing subsequent specific trapping of the perrhenate anion on the small (QMA SeaPak) anion column. This method permits subsequent elution of {sup 188}Re-perrhenate with a small volume of saline, providing a very high activity-concentration solution. Because the {sup 188}Re-specific volume-activity concentration continually decreases with time, the tandem system is especially effective method for extending the useful generator shelf-life. Low elution flow rates (<1 mL/min) minimize any high back pressure which may be encountered during generator/tandem column elution when using tightly packed, small-particle-size commercial columns. In-house preparation of silver cation columns is recommended since the chloride trapping capacity is essentially unlimited, it is inexpensive and not limited in availability to any one supplier, and back pressure can be eliminated by the use of larger particles. Methods for the preparation of {sup 188}Re-HDD have been optimized and this agent can be obtained in high yield (80%).« less

QSAR models for predicting octanol/water and organic carbon/water partition coefficients of polychlorinated biphenyls.

PubMed

Yu, S; Gao, S; Gan, Y; Zhang, Y; Ruan, X; Wang, Y; Yang, L; Shi, J

2016-04-01

Quantitative structure-property relationship modelling can be a valuable alternative method to replace or reduce experimental testing. In particular, some endpoints such as octanol-water (KOW) and organic carbon-water (KOC) partition coefficients of polychlorinated biphenyls (PCBs) are easier to predict and various models have been already developed. In this paper, two different methods, which are multiple linear regression based on the descriptors generated using Dragon software and hologram quantitative structure-activity relationships, were employed to predict suspended particulate matter (SPM) derived log KOC and generator column, shake flask and slow stirring method derived log KOW values of 209 PCBs. The predictive ability of the derived models was validated using a test set. The performances of all these models were compared with EPI Suite™ software. The results indicated that the proposed models were robust and satisfactory, and could provide feasible and promising tools for the rapid assessment of the SPM derived log KOC and generator column, shake flask and slow stirring method derived log KOW values of PCBs.

Apparatus and process for the separation of hydrophobic and hydrophilic particles using microbubble column flotation together with a process and apparatus for generation of microbubbles

DOEpatents

Yoon, R.H.; Adel, G.T.; Luttrell, G.H.

1992-12-01

A method and apparatus are disclosed for the microbubble flotation separation of very fine and coarse particles, especially coal and minerals, so as to produce high purity and high recovery efficiency. This is accomplished through the use of a flotation column, microbubbles, recycling of the flotation pulp, and countercurrent wash water to gently wash the froth. Also disclosed are unique processes and apparatus for generating microbubbles for flotation in a highly efficient and inexpensive manner using either a porous tube or in-line static generators. 14 figs.

Apparatus and process for the separation of hydrophobic and hydrophilic particles using microbubble column flotation together with a process and apparatus for generation of microbubbles

DOEpatents

Yoon, R.H.; Adel, G.T.; Luttrell, G.H.

1998-09-29

A method and apparatus are disclosed for the microbubble flotation separation of very fine and coarse particles, especially coal and minerals, so as to produce high purity and high recovery efficiency. This is accomplished through the use of a flotation column, microbubbles, recycling of the flotation pulp, and countercurrent wash water to gently wash the froth. Also disclosed are unique processes and apparatus for generating microbubbles for flotation in a highly efficient and inexpensive manner using either a porous tube or in-line static generators. 14 figs.

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.

Method for the chemical separation of GE-68 from its daughter Ga-68

DOEpatents

Fitzsimmons, Jonathan M.; Atcher, Robert W.

2010-06-01

The present invention is directed to a generator apparatus for separating a daughter gallium-68 radioisotope substantially free of impurities from a parent gernanium-68 radioisotope, including a first resin-containing column containing parent gernanium-68 radioisotope and daughter gallium-68 radioisotope, a source of first eluent connected to said first resin-containing column for separating daughter gallium-68 radioisotope from the first resin-containing column, said first eluent including citrate whereby the separated gallium is in the form of gallium citrate, a mixing space connected to said first resin-containing column for admixing a source of hydrochloric acid with said separated gallium citrate whereby gallium citrate is converted to gallium tetrachloride, a second resin-containing column for retention of gallium-68 tetrachloride, and, a source of second eluent connected to said second resin-containing column for eluting the daughter gallium-68 radioisotope from said second resin-containing column.

Neutron measurement at the thermal column of the Malaysian Triga Mark II reactor using gold foil activation method and TLD

NASA Astrophysics Data System (ADS)

Shalbi, Safwan; Salleh, Wan Norhayati Wan; Mohamad Idris, Faridah; Aliff Ashraff Rosdi, Muhammad; Syahir Sarkawi, Muhammad; Liyana Jamsari, Nur; Nasir, Nur Aishah Mohd

2018-01-01

In order to design facilities for boron neutron capture therapy (BNCT), the neutron measurement must be considered to obtain the optimal design of BNCT facility such as collimator and shielding. The previous feasibility study showed that the thermal column could generate higher thermal neutrons yield for BNCT application at the TRIGA MARK II reactor. Currently, the facility for BNCT are planned to be developed at thermal column. Thus, the main objective was focused on the thermal neutron and epithermal neutron flux measurement at the thermal column. In this measurement, pure gold and cadmium were used as a filter to obtain the thermal and epithermal neutron fluxes from inside and outside of the thermal column door of the 200kW reactor power using a gold foil activation method. The results were compared with neutron fluxes using TLD 600 and TLD 700. The outcome of this work will become the benchmark for the design of BNCT collimator and the shielding

Simultaneous beam sampling and aperture shape optimization for SPORT

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

Zarepisheh, Masoud; Li, Ruijiang; Xing, Lei, E-mail: Lei@stanford.edu

Purpose: Station parameter optimized radiation therapy (SPORT) was recently proposed to fully utilize the technical capability of emerging digital linear accelerators, in which the station parameters of a delivery system, such as aperture shape and weight, couch position/angle, gantry/collimator angle, can be optimized simultaneously. SPORT promises to deliver remarkable radiation dose distributions in an efficient manner, yet there exists no optimization algorithm for its implementation. The purpose of this work is to develop an algorithm to simultaneously optimize the beam sampling and aperture shapes. Methods: The authors build a mathematical model with the fundamental station point parameters as the decisionmore » variables. To solve the resulting large-scale optimization problem, the authors devise an effective algorithm by integrating three advanced optimization techniques: column generation, subgradient method, and pattern search. Column generation adds the most beneficial stations sequentially until the plan quality improvement saturates and provides a good starting point for the subsequent optimization. It also adds the new stations during the algorithm if beneficial. For each update resulted from column generation, the subgradient method improves the selected stations locally by reshaping the apertures and updating the beam angles toward a descent subgradient direction. The algorithm continues to improve the selected stations locally and globally by a pattern search algorithm to explore the part of search space not reachable by the subgradient method. By combining these three techniques together, all plausible combinations of station parameters are searched efficiently to yield the optimal solution. Results: A SPORT optimization framework with seamlessly integration of three complementary algorithms, column generation, subgradient method, and pattern search, was established. The proposed technique was applied to two previously treated clinical cases: a head and neck and a prostate case. It significantly improved the target conformality and at the same time critical structure sparing compared with conventional intensity modulated radiation therapy (IMRT). In the head and neck case, for example, the average PTV coverage D99% for two PTVs, cord and brainstem max doses, and right parotid gland mean dose were improved, respectively, by about 7%, 37%, 12%, and 16%. Conclusions: The proposed method automatically determines the number of the stations required to generate a satisfactory plan and optimizes simultaneously the involved station parameters, leading to improved quality of the resultant treatment plans as compared with the conventional IMRT plans.« less

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.

Optimal graph based segmentation using flow lines with application to airway wall segmentation.

PubMed

Petersen, Jens; Nielsen, Mads; Lo, Pechin; Saghir, Zaigham; Dirksen, Asger; de Bruijne, Marleen

2011-01-01

This paper introduces a novel optimal graph construction method that is applicable to multi-dimensional, multi-surface segmentation problems. Such problems are often solved by refining an initial coarse surface within the space given by graph columns. Conventional columns are not well suited for surfaces with high curvature or complex shapes but the proposed columns, based on properly generated flow lines, which are non-intersecting, guarantee solutions that do not self-intersect and are better able to handle such surfaces. The method is applied to segment human airway walls in computed tomography images. Comparison with manual annotations on 649 cross-sectional images from 15 different subjects shows significantly smaller contour distances and larger area of overlap than are obtained with recently published graph based methods. Airway abnormality measurements obtained with the method on 480 scan pairs from a lung cancer screening trial are reproducible and correlate significantly with lung function.

Model Predictive Control-based Power take-off Control of an Oscillating Water Column Wave Energy Conversion System

NASA Astrophysics Data System (ADS)

Rajapakse, G.; Jayasinghe, S. G.; Fleming, A.; Shahnia, F.

2017-07-01

Australia’s extended coastline asserts abundance of wave and tidal power. The predictability of these energy sources and their proximity to cities and towns make them more desirable. Several tidal current turbine and ocean wave energy conversion projects have already been planned in the coastline of southern Australia. Some of these projects use air turbine technology with air driven turbines to harvest the energy from an oscillating water column. This study focuses on the power take-off control of a single stage unidirectional oscillating water column air turbine generator system, and proposes a model predictive control-based speed controller for the generator-turbine assembly. The proposed method is verified with simulation results that show the efficacy of the controller in extracting power from the turbine while maintaining the speed at the desired level.

Simultaneous beam sampling and aperture shape optimization for SPORT.

PubMed

Zarepisheh, Masoud; Li, Ruijiang; Ye, Yinyu; Xing, Lei

2015-02-01

Station parameter optimized radiation therapy (SPORT) was recently proposed to fully utilize the technical capability of emerging digital linear accelerators, in which the station parameters of a delivery system, such as aperture shape and weight, couch position/angle, gantry/collimator angle, can be optimized simultaneously. SPORT promises to deliver remarkable radiation dose distributions in an efficient manner, yet there exists no optimization algorithm for its implementation. The purpose of this work is to develop an algorithm to simultaneously optimize the beam sampling and aperture shapes. The authors build a mathematical model with the fundamental station point parameters as the decision variables. To solve the resulting large-scale optimization problem, the authors devise an effective algorithm by integrating three advanced optimization techniques: column generation, subgradient method, and pattern search. Column generation adds the most beneficial stations sequentially until the plan quality improvement saturates and provides a good starting point for the subsequent optimization. It also adds the new stations during the algorithm if beneficial. For each update resulted from column generation, the subgradient method improves the selected stations locally by reshaping the apertures and updating the beam angles toward a descent subgradient direction. The algorithm continues to improve the selected stations locally and globally by a pattern search algorithm to explore the part of search space not reachable by the subgradient method. By combining these three techniques together, all plausible combinations of station parameters are searched efficiently to yield the optimal solution. A SPORT optimization framework with seamlessly integration of three complementary algorithms, column generation, subgradient method, and pattern search, was established. The proposed technique was applied to two previously treated clinical cases: a head and neck and a prostate case. It significantly improved the target conformality and at the same time critical structure sparing compared with conventional intensity modulated radiation therapy (IMRT). In the head and neck case, for example, the average PTV coverage D99% for two PTVs, cord and brainstem max doses, and right parotid gland mean dose were improved, respectively, by about 7%, 37%, 12%, and 16%. The proposed method automatically determines the number of the stations required to generate a satisfactory plan and optimizes simultaneously the involved station parameters, leading to improved quality of the resultant treatment plans as compared with the conventional IMRT plans.

Strain, curvature, and twist measurements in digital holographic interferometry using pseudo-Wigner-Ville distribution based method

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

Rajshekhar, G.; Gorthi, Sai Siva; Rastogi, Pramod

2009-09-15

Measurement of strain, curvature, and twist of a deformed object play an important role in deformation analysis. Strain depends on the first order displacement derivative, whereas curvature and twist are determined by second order displacement derivatives. This paper proposes a pseudo-Wigner-Ville distribution based method for measurement of strain, curvature, and twist in digital holographic interferometry where the object deformation or displacement is encoded as interference phase. In the proposed method, the phase derivative is estimated by peak detection of pseudo-Wigner-Ville distribution evaluated along each row/column of the reconstructed interference field. A complex exponential signal with unit amplitude and the phasemore » derivative estimate as the argument is then generated and the pseudo-Wigner-Ville distribution along each row/column of this signal is evaluated. The curvature is estimated by using peak tracking strategy for the new distribution. For estimation of twist, the pseudo-Wigner-Ville distribution is evaluated along each column/row (i.e., in alternate direction with respect to the previous one) for the generated complex exponential signal and the corresponding peak detection gives the twist estimate.« less

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.

Two novel approaches to study arthropod anatomy by using dualbeam FIB/SEM.

PubMed

Di Giulio, Andrea; Muzzi, Maurizio

2018-03-01

Transmission Electron Microscopy (TEM) has always been the conventional method to study arthropod ultrastructure, while the use of Scanning Electron Microscopy (SEM) was mainly devoted to the examination of the external cuticular structures by secondary electrons. The new generation field emission SEMs are capable to generate images at sub-cellular level, comparable to TEM images employing backscattered electrons. The potential of this kind of acquisition becomes very powerful in the dual beam FIB/SEM where the SEM column is combined with a Focused Ion Beam (FIB) column. FIB uses ions as a nano-scalpel to slice samples fixed and embedded in resin, replacing traditional ultramicrotomy. We here present two novel methods, which optimize the use of FIB/SEM for studying arthropod anatomy. Copyright © 2017 Elsevier Ltd. All rights reserved.

Repeatability of gradient ultrahigh pressure liquid chromatography-tandem mass spectrometry methods in instrument-controlled thermal environments.

PubMed

Grinias, James P; Wong, Jenny-Marie T; Kennedy, Robert T

2016-08-26

The impact of viscous friction on eluent temperature and column efficiency in liquid chromatography is of renewed interest as the need for pressures exceeding 1000bar to use with columns packed with sub-2μm particles has grown. One way the development of axial and radial temperature gradients that arise due to viscous friction can be affected is by the thermal environment the column is placed in. In this study, a new column oven integrated into an ultrahigh pressure liquid chromatograph that enables both still-air and forced-air operating modes is investigated to find the magnitude of the effect of the axial thermal gradient that forms in 2.1×100mm columns packed with sub-2μm particles in these modes. Temperature increases of nearly 30K were observed when the generated power of the column exceeded 25W/m. The impact of the heating due to viscous friction on the repeatability of peak capacity, elution time, and peak area ratio to an internal standard for a gradient UHPLC-MS/MS method to analyze neurotransmitters was found to be limited. This result indicates that high speed UHPLC-MS/MS gradient methods under conditions of high viscous friction may be possible without the negative effects typically observed with isocratic separations under similar conditions. Copyright © 2016 Elsevier B.V. All rights reserved.

40 CFR 799.6786 - TSCA water solubility: Generator column method.

Code of Federal Regulations, 2014 CFR

2014-07-01

... quantitative) analysis of solvent extract in paragraph (c)(3)(iv) of this section. The design of the generator.... Finally, the design of most chemical tests and many ecological and health tests requires precise knowledge..., molality, and mole fraction. For example, to convert from weight/volume to molarity molecular mass is...

40 CFR 799.6786 - TSCA water solubility: Generator column method.

Code of Federal Regulations, 2013 CFR

2013-07-01

... quantitative) analysis of solvent extract in paragraph (c)(3)(iv) of this section. The design of the generator.... Finally, the design of most chemical tests and many ecological and health tests requires precise knowledge..., molality, and mole fraction. For example, to convert from weight/volume to molarity molecular mass is...

40 CFR 799.6786 - TSCA water solubility: Generator column method.

Code of Federal Regulations, 2012 CFR

2012-07-01

... quantitative) analysis of solvent extract in paragraph (c)(3)(iv) of this section. The design of the generator.... Finally, the design of most chemical tests and many ecological and health tests requires precise knowledge..., molality, and mole fraction. For example, to convert from weight/volume to molarity molecular mass is...

Sugar, acid and furfural quantification in a sulphite pulp mill: Feedstock, product and hydrolysate analysis by HPLC/RID.

PubMed

Llano, Tamara; Quijorna, Natalia; Andrés, Ana; Coz, Alberto

2017-09-01

Waste from pulp and paper mills consist of sugar-rich fractions comprising hemicellulose derivatives and cellulose by-products. A complete characterisation of the waste streams is necessary to study the possibilities of an existing mill. In this work, four chromatographic methods have been developed to obtain the most suitable chromatographic method conditions for measuring woody feedstocks, lignocellulosic hydrolysates and cellulose pulp in sulphite pulping processes. The analysis of major and minor monosaccharides, aliphatic carboxylic acids and furfurals has been optimised. An important drawback of the spent liquors generated after sulphite pulping is their acidic nature, high viscosity and adhesive properties that interfere in the column lifetime. This work recommends both a CHO-782Pb column for the sugar analysis and an SH-1011 resin-based cross-linked gel column to separate low-molecular-weight chain acids, alcohols and furfurals. Such columns resulted in a good separation with long lifetime, wide pH operating range and low fouling issues.

[Spectral investigation of atmospheric pressure plasma column].

PubMed

Li, Xue-Chen; Chang, Yuan-Yuan; Xu, Long-Fei

2012-07-01

Atmospheric pressure plasma column has many important applications in plasma stealth for aircraft. In the present paper, a plasma column with a length of 65 cm was generated in argon at atmospheric pressure by using dielectric barrier discharge device with water electrodes in coaxial configurations. The discharge mechanism of the plasma column was studied by optical method and the result indicates that a moving layer of light emission propagates in the upstream region. The propagation velocity of the plasma bullet is about 0.6 x 10(5) m x s(-1) through optical measurement. Spectral intensity ratios as functions of the applied voltage and driving frequency were also investigated by spectroscopic method. The variation in spectral intensity ratio implies a change in the averaged electron energy. Results show that the averaged electron energy increases with the increase in the applied voltage and the driving frequency. These results have significant values for industrial applications of the atmospheric pressure discharge and have extensive application potentials in stealth for military aircraft.

Determination of vapor pressure of low-volatility compounds using a method to obtain saturated vapor with coated capillary columns.

PubMed

Rittfeldt, L

2001-06-01

The vapor pressures of O-ethyl S-2-diisopropylaminoethyl methylphosphonothiolate (VX), O-isobutyl S-2-diethylaminoethyl methylphosphonothiolate (RVX), and 2,4-dinitrotoluene (2,4-DNT) were determined with the gas saturation method in temperatures ranging from -12 to 103 degrees C. The saturated vapor was generated using a fused-silica column coated with the compound. This column was placed in a gas chromatograph, and the vapor pressure was determined directly from the detector signal or by sampling on Tenax tubes that were subsequently analyzed. From the linear relationships obtained by plotting log P vs 1/T, the enthalpies of vaporization (deltaHvap) and the vapor pressures at selected temperatures were determined. The vapor pressure of VX at 25 degrees C was 0.110 Pa and the deltaHvap 77.9 kJ x mol(-1). The corresponding results for RVX were 0.082 Pa and 76.6 kJ x mol(-1). The vapor pressure of 2,4-DNT at 72 degrees C (melting point) was determined to 6.0 Pa, and the enthalpies of the solid and the liquid state were 94.2 and 75.3 kJ x mol(-1), respectively. Using capillary columns to generate saturated vapors has three major advantages: short equilibrium time, low consumption of sample, and safe handling of toxic compounds.

77 FR 46289 - Technical Corrections to Organizational Names, Addresses, and OMB Control Numbers

Federal Register 2010, 2011, 2012, 2013, 2014

2012-08-03

...]795.232 Inhalation and dermal pharmacokinetics of commercial hexane. * * * * * (c) * * * (2) * * * (i... to read as follows: Sec. 799.6755 TSCA partition coefficient (n-octanol/water), shake flask method... read as follows: Sec. 799.6756 TSCA partition coefficient (n-octanol/water), generator column method...

Determination of organic peroxides by liquid chromatography with on-line post-column ultraviolet irradiation and peroxyoxalate chemiluminescence detection.

PubMed

Wada, Mitsuhiro; Inoue, Keiyu; Thara, Ayuko; Kishikawa, Naoya; Nakashima, Kenichiro; Kuroda, Naotaka

2003-02-14

A HPLC method was developed for the simultaneous determination of organic peroxides and hydrogen peroxide with peroxyoxalate chemiluminescence (PO-CL) detection following on-line UV irradiation. Organic peroxides [i.e., benzoyl peroxide (BP), tert.-butyl hydroperoxide (BHP), tert.-butyl perbenzoate (BPB), cumene hydroperoxide (CHP)] were UV irradiated (254 nm, 15 W) to generate hydrogen peroxide, which was determined by PO-CL detection. The conditions for UV irradiation and PO-CL detection were optimized by a flow injection analysis (FIA) system. Generation of hydrogen peroxide from peroxides with on-line UV irradiation also was confirmed by the FIA system by incorporating an enzyme column reactor immobilized with catalase. The separation of four organic peroxides and hydrogen peroxide by HPLC was accomplished isocratically on an ODS column within 30 min. The detection limits (signal-to-noise ratio=3) were 1.1 microM for hydrogen peroxide, 6.8 microM for BP, 31.3 microM for BHP, 7.5 microM for BPB and 1.3 microM for CHP. The proposed method was applied to the determination of BP in wheat flour.

Huffman and linear scanning methods with statistical language models.

PubMed

Roark, Brian; Fried-Oken, Melanie; Gibbons, Chris

2015-03-01

Current scanning access methods for text generation in AAC devices are limited to relatively few options, most notably row/column variations within a matrix. We present Huffman scanning, a new method for applying statistical language models to binary-switch, static-grid typing AAC interfaces, and compare it to other scanning options under a variety of conditions. We present results for 16 adults without disabilities and one 36-year-old man with locked-in syndrome who presents with complex communication needs and uses AAC scanning devices for writing. Huffman scanning with a statistical language model yielded significant typing speedups for the 16 participants without disabilities versus any of the other methods tested, including two row/column scanning methods. A similar pattern of results was found with the individual with locked-in syndrome. Interestingly, faster typing speeds were obtained with Huffman scanning using a more leisurely scan rate than relatively fast individually calibrated scan rates. Overall, the results reported here demonstrate great promise for the usability of Huffman scanning as a faster alternative to row/column scanning.

Method of recovering adsorbed liquid compounds from molecular sieve columns

DOEpatents

Burkholder, H.R.; Fanslow, G.E.

1983-12-20

Molecularly adsorbed volatile liquid compounds are recovered from molecular sieve adsorbent columns by directionally applying microwave energy to the bed of the adsorbent to produce a mixed liquid-gas effluent. The gas portion of the effluent generates pressure within the bed to promote the discharge of the effluent from the column bottoms. Preferably the discharged liquid-gas effluent is collected in two to three separate fractions, the second or intermediate fraction having a substantially higher concentration of the desorbed compound than the first or third fractions. The desorption does not need to be assisted by passing a carrier gas through the bed or by applying reduced pressure to the outlet from the bed. 8 figs.

Method of recovering adsorbed liquid compounds from molecular sieve columns

DOEpatents

Burkholder, Harvey R.; Fanslow, Glenn E.

1983-01-01

Molecularly adsorbed volatile liquid compounds are recovered from molecular sieve adsorbent columns by directionally applying microwave energy to the bed of the adsorbent to produce a mixed liquid-gas effluent. The gas portion of the effluent generates pressure within the bed to promote the discharge of the effluent from the column bottoms. Preferably the discharged liquid-gas effluent is collected in two to three separate fractions, the second or intermediate fraction having a substantially higher concentration of the desorbed compound than the first or third fractions. The desorption does not need to be assisted by passing a carrier gas through the bed or by applying reduced pressure to the outlet from the bed.

On-line preconcentration and speciation of arsenic by flow injection hydride generation atomic absorption spectrophotometry.

PubMed

Narcise, Cristine Ingrid S; Coo, Lilibeth Dlc; Del Mundo, Florian R

2005-12-15

A flow injection-column preconcentration-hydride generation atomic absorption spectrophotometric (FI-column-HGAAS) method was developed for determining mug/l levels of As(III) and As(V) in water samples, with simultaneous preconcentration and speciation. The speciation scheme involved determining As(V) at neutral pH and As(III+V) at pH 12, with As(III) obtained by difference. The enrichment factor (EF) increased with increase in sample loading volume from 2.5 to 10ml, and for preconcentration using the chloride-form anion exchange column, EFs ranged from 5 to 48 for As(V) and 4 to 24 for As(III+V), with corresponding detection limits of 0.03-0.3 and 0.07-0.3mug/l. Linear concentration range (LCR) also varied with sample loading volume, and for a 5-ml sample was 0.3-5 and 0.2-8mug/l for As(V) and As(III+V), respectively. Sample throughput, which decreased with increase in sample volume, was 8-17 samples/h. For the hydroxide-form column, the EFS for 2.5-10ml samples were 3-23 for As(V) and 2-15 for As(III+V), with corresponding detection limits of 0.07-0.4 and 0.1-0.5mug/l. The LCR for a 5-ml sample was 0.3-10mug/l for As(V) and 0.2-20mug/l for As(III+V). Sample throughput was 10-20 samples/h. The developed method has been effectively applied to tap water and mineral water samples, with recoveries ranging from 90 to 102% for 5-ml samples passed through the two columns.

Measurement of the eddy diffusion term in chromatographic columns. I. Application to the first generation of 4.6mm I.D. monolithic columns.

PubMed

Gritti, Fabrice; Guiochon, Georges

2011-08-05

The corrected heights equivalent to a theoretical plate (HETP) of three 4.6mm I.D. monolithic Onyx-C(18) columns (Onyx, Phenomenex, Torrance, CA) of different lengths (2.5, 5, and 10 cm) are reported for retained (toluene, naphthalene) and non-retained (uracil, caffeine) small molecules. The moments of the peak profiles were measured according to the accurate numerical integration method. Correction for the extra-column contributions was systematically applied. The peak parking method was used in order to measure the bulk diffusion coefficients of the sample molecules, their longitudinal diffusion terms, and the eddy diffusion term of the three monolithic columns. The experimental results demonstrate that the maximum efficiency was 60,000 plates/m for retained compounds. The column length has a large impact on the plate height of non-retained species. These observations were unambiguously explained by a large trans-column eddy diffusion term in the van Deemter HETP equation. This large trans-rod eddy diffusion term is due to the combination of a large trans-rod velocity bias (≃3%), a small radial dispersion coefficient in silica monolithic columns, and a poorly designed distribution and collection of the sample streamlets at the inlet and outlet of the monolithic rod. Improving the performance of large I.D. monolithic columns will require (1) a detailed knowledge of the actual flow distribution across and along these monolithic rod and (2) the design of appropriate inlet and outlet distributors designed to minimize the nefarious impact of the radial flow heterogeneity on band broadening. Copyright © 2011 Elsevier B.V. All rights reserved.

Column Chromatography To Obtain Organic Cation Sorption Isotherms.

PubMed

Jolin, William C; Sullivan, James; Vasudevan, Dharni; MacKay, Allison A

2016-08-02

Column chromatography was evaluated as a method to obtain organic cation sorption isotherms for environmental solids while using the peak skewness to identify the linear range of the sorption isotherm. Custom packed HPLC columns and standard batch sorption techniques were used to intercompare sorption isotherms and solid-water sorption coefficients (Kd) for four organic cations (benzylamine, 2,4-dichlorobenzylamine, phenyltrimethylammonium, oxytetracycline) with two aluminosilicate clay minerals and one soil. A comparison of Freundlich isotherm parameters revealed isotherm linearity or nonlinearity was not significantly different between column chromatography and traditional batch experiments. Importantly, skewness (a metric of eluting peak symmetry) analysis of eluting peaks can establish isotherm linearity, thereby enabling a less labor intensive means to generate the extensive data sets of linear Kd values required for the development of predictive sorption models. Our findings clearly show that column chromatography can reproduce sorption measures from conventional batch experiments with the benefit of lower labor-intensity, faster analysis times, and allow for consistent sorption measures across laboratories with distinct chromatography instrumentation.

[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.

Simple new method for effective concentration of 188Re solutions from alumina-based 188W-188Re generator.

PubMed

Guhlke, S; Beets, A L; Oetjen, K; Mirzadeh, S; Biersack, H J; Knapp, F F

2000-07-01

(188)Re is a useful generator-produced radioisotope currently under evaluation for a variety of therapeutic applications, including bone pain palliation and intravascular radiation therapy. Because the (188)W parent is available only in a relatively low specific activity (<0.15-0.19 GBq/mg) from reactor irradiation of enriched (186)W, relatively large volumes of 0.9% saline (>15 mL) are required for elution of the (188)Re daughter from traditional alumina-based (188)W-(188)Re generators. Because these large bolus volumes result in solutions with a relatively low specific volume activity of (188)Re (<1 GBq/mL for the 18.5-GBq generator), the availability of effective methods for eluent concentration is important. Our new approach is based on the use of 0.3 mol/L ammonium acetate as a representative salt of a weak acid instead of saline for generator elution. After generator elution, the ammonium acetate generator eluent (15-20 mL) is passed through a tandem IC-H Plus cation (Dowex-H)-anion (QMA Light) column system. Exchange of ammonium cations with hydrogen ions on the cation column forms an acetic acid solution containing perrhenate anions from which the macroscopic levels of the acetate anion of the eluent have been effectively removed. Because perrhenic acid is fully dissociated at this pH, the QMA Light column specifically traps the (188)Re-perrhenate, which is subsequently eluted with a low volume (<1 mL) of saline. Concentration ratios greater than 20:1 are readily achieved with this method. A typical clinical-scale generator loaded with 19.2 GBq (188)W was used to validate the approach. Saline elution provided (188)Re in a 75%-80% yield. Although elution with 0.15 mol/L NH4OAc gave lower yields (55%-60%), use of 0.3 mol/L NH4OAc provided yields comparable with those of saline (70%-75%). (188)W parent breakthrough was not detected after passage of the bolus through the tandem concentration system. Bolus volumes of 15-20 mL, which initially contained as much as 11.1-14.8 GBq (188)Re, were readily concentrated to less than 1 mL saline using QMA Light cartridges. The generator was evaluated for more than 3 mo with no decrease in performance. This approach represents a simple, rapid, and effective method using inexpensive disposable components of concentrating solutions of (188)Re for preparation of therapeutic agents.

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

PubMed

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

2018-01-16

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

SU-E-T-295: Simultaneous Beam Sampling and Aperture Shape Optimization for Station Parameter Optimized Radiation Therapy (SPORT)

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

Zarepisheh, M; Li, R; Xing, L

Purpose: Station Parameter Optimized Radiation Therapy (SPORT) was recently proposed to fully utilize the technical capability of emerging digital LINACs, in which the station parameters of a delivery system, (such as aperture shape and weight, couch position/angle, gantry/collimator angle) are optimized altogether. SPORT promises to deliver unprecedented radiation dose distributions efficiently, yet there does not exist any optimization algorithm to implement it. The purpose of this work is to propose an optimization algorithm to simultaneously optimize the beam sampling and aperture shapes. Methods: We build a mathematical model whose variables are beam angles (including non-coplanar and/or even nonisocentric beams) andmore » aperture shapes. To solve the resulting large scale optimization problem, we devise an exact, convergent and fast optimization algorithm by integrating three advanced optimization techniques named column generation, gradient method, and pattern search. Column generation is used to find a good set of aperture shapes as an initial solution by adding apertures sequentially. Then we apply the gradient method to iteratively improve the current solution by reshaping the aperture shapes and updating the beam angles toward the gradient. Algorithm continues by pattern search method to explore the part of the search space that cannot be reached by the gradient method. Results: The proposed technique is applied to a series of patient cases and significantly improves the plan quality. In a head-and-neck case, for example, the left parotid gland mean-dose, brainstem max-dose, spinal cord max-dose, and mandible mean-dose are reduced by 10%, 7%, 24% and 12% respectively, compared to the conventional VMAT plan while maintaining the same PTV coverage. Conclusion: Combined use of column generation, gradient search and pattern search algorithms provide an effective way to optimize simultaneously the large collection of station parameters and significantly improves quality of resultant treatment plans as compared with conventional VMAT or IMRT treatments.« less

Unintentional contaminant transfer from groundwater to the vadose zone during source zone remediation of volatile organic compounds.

PubMed

Chong, Andrea D; Mayer, K Ulrich

2017-09-01

Historical heavy use of chlorinated solvents in conjunction with improper disposal practices and accidental releases has resulted in widespread contamination of soils and groundwater in North America and worldwide. As a result, remediation of chlorinated solvents is required at many sites. For source zone treatment, common remediation strategies include in-situ chemical oxidation (ISCO) using potassium or sodium permanganate, and the enhancement of biodegradation by primary substrate addition. It is well known that these remediation methods tend to generate gas (carbon dioxide (CO 2 ) in the case of ISCO using permanganate, CO 2 and methane (CH 4 ) in the case of bioremediation). Vigorous gas generation in the presence of chlorinated solvents, which are categorized as volatile organic contaminants (VOCs), may cause gas exsolution, ebullition and stripping of the contaminants from the treatment zone. This process may lead to unintentional 'compartment transfer', whereby VOCs are transported away from the contaminated zone into overlying clean sediments and into the vadose zone. To this extent, benchtop column experiments were conducted to quantify the effect of gas generation during remediation of the common chlorinated solvent trichloroethylene (TCE/C 2 Cl 3 H). Both ISCO and enhanced bioremediation were considered as treatment methods. Results show that gas exsolution and ebullition occurs for both remediation technologies. Facilitated by ebullition, TCE was transported from the source zone into overlying clean groundwater and was subsequently released into the column headspace. For the case of enhanced bioremediation, the intermediate degradation product vinyl chloride (VC) was also stripped from the treatment zone. The concentrations measured in the headspace of the columns (TCE ∼300ppm in the ISCO column, TCE ∼500ppm and VC ∼1380ppm in the bioremediation column) indicate that substantial transfer of VOCs to the vadose zone is possible. These findings provide direct evidence for the unintended spreading of contaminants as a result of remediation efforts, which can, under some circumstances, result in enhanced risks for soil vapour intrusion. Copyright © 2017 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.

Mobility of as, Cu, Cr, and Zn from tailings covered with sealing materials using alkaline industrial residues: a comparison between two leaching methods.

PubMed

Jia, Yu; Maurice, Christian; Öhlander, Björn

2016-01-01

Different alkaline residue materials (fly ash, green liquor dregs, and lime mud) generated from the pulp and paper industry as sealing materials were evaluated to cover aged mine waste tailings (<1% sulfur content, primarily pyrite). The mobility of four selected trace elements (Cr, Cu, Zn, and As) was compared based on batch and column leaching studies to assess the effectiveness of these alkaline materials as sealing agents. Based on the leaching results, Cr, Cu, and Zn were immobilized by the alkaline amendments. In the amended tailings in the batch system only As dramatically exceeded the limit values at L/S 10 L/kg. The leaching results showed similar patterns to the batch results, though leached Cr, Cu, and Zn showed higher levels in the column tests than in the batch tests. However, when the columns were compared with the batches, the trend for Cu was opposite for the unamended tailings. By contrast, both batch and column results showed that the amendment caused mobilization of As compared with the unamended tailings in the ash-amended tailings. The amount of As released was greatest in the ash column and decreased from the dregs to the lime columns. The leaching of As at high levels can be a potential problem whenever alkaline materials (especially for fly ash) are used as sealing materials over tailings. The column test was considered by the authors to be a more informative method in remediation of the aged tailings with low sulfur content, since it mimics better actual situation in a field.

Glycan profiling of monoclonal antibodies using zwitterionic-type hydrophilic interaction chromatography coupled with electrospray ionization mass spectrometry detection.

PubMed

Mauko, Lea; Nordborg, Anna; Hutchinson, Joseph P; Lacher, Nathan A; Hilder, Emily F; Haddad, Paul R

2011-01-15

We present a new method for the analysis of glycans enzymatically released from monoclonal antibodies (MAbs) employing a zwitterionic-type hydrophilic interaction chromatography (ZIC-HILIC) column coupled with electrospray ionization mass spectrometry (ESI-MS). Both native and reduced glycans were analyzed, and the developed procedure was compared with a standard HILIC procedure used in the pharmaceutical industry whereby fluorescent-labeled glycans are analyzed using a TSK Amide-80 column coupled with fluorescence detection. The separation of isobaric alditol oligosaccharides present in monoclonal antibodies and ribonuclease B is demonstrated, and ZIC-HILIC is shown to have good capability for structural recognition. Glycan profiles obtained with the ZIC-HILIC column and ESI-MS provided detailed information on MAb glycosylation, including identification of some less abundant glycan species, and are consistent with the profiles generated with the standard procedure. This new ZIC-HILIC method offers a simpler and faster approach for glycosylation analysis of therapeutic antibodies. Copyright © 2010 Elsevier Inc. All rights reserved.

Removal of furan and phenolic compounds from simulated biomass hydrolysates by batch adsorption and continuous fixed-bed column adsorption methods.

PubMed

Lee, Sang Cheol; Park, Sunkyu

2016-09-01

It has been proposed to remove all potential inhibitors and sulfuric acid in biomass hydrolysates generated from dilute-acid pretreatment of biomass, based on three steps of sugar purification process. This study focused on its first step in which furan and phenolic compounds were selectively removed from the simulated hydrolysates using activated charcoal. Batch adsorption experiments demonstrated that the affinity of activated charcoal for each component was highest in the order of vanillic acid, 4-hydroxybenzoic acid, furfural, acetic acid, sulfuric acid, and xylose. The affinity of activated charcoal for furan and phenolic compounds proved to be significantly higher than that of the other three components. Four separation strategies were conducted with a combination of batch adsorption and continuous fixed-bed column adsorption methods. It was observed that xylose loss was negligible with near complete removal of furan and phenolic compounds, when at least one fixed-bed column adsorption was implemented in the strategy. Copyright © 2016 Elsevier Ltd. All rights reserved.

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.

A Fast Gradient Method for Nonnegative Sparse Regression With Self-Dictionary

NASA Astrophysics Data System (ADS)

Gillis, Nicolas; Luce, Robert

2018-01-01

A nonnegative matrix factorization (NMF) can be computed efficiently under the separability assumption, which asserts that all the columns of the given input data matrix belong to the cone generated by a (small) subset of them. The provably most robust methods to identify these conic basis columns are based on nonnegative sparse regression and self dictionaries, and require the solution of large-scale convex optimization problems. In this paper we study a particular nonnegative sparse regression model with self dictionary. As opposed to previously proposed models, this model yields a smooth optimization problem where the sparsity is enforced through linear constraints. We show that the Euclidean projection on the polyhedron defined by these constraints can be computed efficiently, and propose a fast gradient method to solve our model. We compare our algorithm with several state-of-the-art methods on synthetic data sets and real-world hyperspectral images.

Quality by design (QbD) based development and validation of an HPLC method for amiodarone hydrochloride and its impurities in the drug substance.

PubMed

Karmarkar, S; Yang, X; Garber, R; Szajkovics, A; Koberda, M

2014-11-01

The USP monograph describes an HPLC method for seven impurities in the amiodarone drug substance using a L1 column, 4.6mm×150mm, 5μm packing (PF listed ODS2 GL-Science, Inertsil column) at 30°C with detection at 240nm. The standard contains 0.01mg/mL of amiodarone, and USP specified impurities D and E with a resolution requirement of NLT 3.5 between peaks D and E. Impurities in a 5mg/mL sample are quantitated against the standard. Impurity A peak elutes just before peak D. We observed two problems with the method; the column lot-to-lot variability resulted in unresolved A, D, and E peaks, and peak D in the sample preparation eluted much later than that in the standard solution. Therefore, optimization experiments were conducted on the USP method following the QbD approach with Fusion AE™ software (S-Matrix Corporation). The resulting optimized conditions were within the allowable changes per USP 〈621〉. Lot-to-lot variability was negligible with the Atlantis T3 (Waters Corporation) L1 column. Peak D retention time remained constant from standard to sample. The optimized method was validated in terms of accuracy, precision, linearity, range, LOQ/LOD, specificity, robustness, equivalency to the USP method, and solution stability. The QbD based development helped in generating a design space and operating space with knowledge of all method performance characteristics and limitations and successful method robustness within the operating space. Copyright © 2014 Elsevier B.V. All rights reserved.

Development of pseudo-linear gradient elution for high-throughput resin selectivity screening in RoboColumn® Format.

PubMed

Kiesewetter, André; Menstell, Peter; Peeck, Lars H; Stein, Andreas

2016-11-01

Rapid development of chromatographic processes relies on effective high-throughput screening (HTS) methods. This article describes the development of pseudo-linear gradient elution for resin selectivity screening using RoboColumns ® . It gives guidelines for the implementation of this HTS method on a Tecan Freedom EVO ® robotic platform, addressing fundamental aspects of scale down and liquid handling. The creation of a flexible script for buffer preparation and column operation plus efficient data processing provided the basis for this work. Based on the concept of discretization, linear gradient elution was transformed into multistep gradients. The impact of column size, flow rate, multistep gradient design, and fractionation scheme on separation efficiency was systematically investigated, using a ternary model protein mixture. We identified key parameters and defined optimal settings for effective column performance. For proof of concept, we examined the selectivity of several cation exchange resins using various buffer conditions. The final protocol enabled a clear differentiation of resin selectivity on miniature chromatography column (MCC) scale. Distinct differences in separation behavior of individual resins and the influence of buffer conditions could be demonstrated. Results obtained with the robotic platform were representative and consistent with data generated on a conventional chromatography system. A study on antibody monomer/high molecular weight separation comparing MCC and lab scale under higher loading conditions provided evidence of the applicability of the miniaturized approach to practically relevant feedstocks with challenging separation tasks as well as of the predictive quality for larger scale. A comparison of varying degrees of robotic method complexity with corresponding effort (analysis time and labware consumption) and output quality highlights tradeoffs to select a method appropriate for a given separation challenge or analytical constraints. © 2016 American Institute of Chemical Engineers Biotechnol. Prog., 32:1503-1519, 2016. © 2016 American Institute of Chemical Engineers.

Quality by design: a systematic and rapid liquid chromatography and mass spectrometry method for eprosartan mesylate and its related impurities using a superficially porous particle column.

PubMed

Kalariya, Pradipbhai D; Kumar Talluri, Murali V N; Gaitonde, Vinay D; Devrukhakar, Prashant S; Srinivas, Ragampeta

2014-08-01

The present work describes the systematic development of a robust, precise, and rapid reversed-phase liquid chromatography method for the simultaneous determination of eprosartan mesylate and its six impurities using quality-by-design principles. The method was developed in two phases, screening and optimization. During the screening phase, the most suitable stationary phase, organic modifier, and pH were identified. The optimization was performed for secondary influential parameters--column temperature, gradient time, and flow rate using eight experiments--to examine multifactorial effects of parameters on the critical resolution and generated design space representing the robust region. A verification experiment was performed within the working design space and the model was found to be accurate. This study also describes other operating features of the column packed with superficially porous particles that allow very fast separations at pressures available in most liquid chromatography instruments. Successful chromatographic separation was achieved in less than 7 min using a fused-core C18 (100 mm × 2.1 mm, 2.6 μm) column with linear gradient elution of 10 mM ammonium formate (pH 3.0) and acetonitrile as the mobile phase. The method was validated for specificity, linearity, accuracy, precision, and robustness in compliance with the International Conference on Harmonization Q2 (R1) guidelines. The impurities were identified by liquid chromatography with mass spectrometry. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

An applicable method for efficiency estimation of operating tray distillation columns and its comparison with the methods utilized in HYSYS and Aspen Plus

NASA Astrophysics Data System (ADS)

Sadeghifar, Hamidreza

2015-10-01

Developing general methods that rely on column data for the efficiency estimation of operating (existing) distillation columns has been overlooked in the literature. Most of the available methods are based on empirical mass transfer and hydraulic relations correlated to laboratory data. Therefore, these methods may not be sufficiently accurate when applied to industrial columns. In this paper, an applicable and accurate method was developed for the efficiency estimation of distillation columns filled with trays. This method can calculate efficiency as well as mass and heat transfer coefficients without using any empirical mass transfer or hydraulic correlations and without the need to estimate operational or hydraulic parameters of the column. E.g., the method does not need to estimate tray interfacial area, which can be its most important advantage over all the available methods. The method can be used for the efficiency prediction of any trays in distillation columns. For the efficiency calculation, the method employs the column data and uses the true rates of the mass and heat transfers occurring inside the operating column. It is highly emphasized that estimating efficiency of an operating column has to be distinguished from that of a column being designed.

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

USGS Publications Warehouse

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

2018-01-01

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

Generator for ionic gallium-68 based on column chromatography

DOEpatents

Neirinckx, Rudi D.; Davis, Michael A.

1981-01-01

A physiologically acceptable solution of gallium-68 fluorides, having an activity of 0.1 to 50 millicuries per milliliter of solution is provided. The solution is obtained from a generator comprising germanium-68 hexafluoride bound to a column of an anion exchange resin which forms gallium-68 in situ by eluting the column with an acid solution to form a solution containing .sup.68 Ga-fluorides. The solution then is neutralized prior to administration.

SU-G-BRC-02: A Novel Multi-Criteria Optimization Approach to Generate Deliverable Intensity-Modulated Radiation Therapy (IMRT) Treatment Plans

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

Kirlik, G; D’Souza, W; Zhang, H

2016-06-15

Purpose: To present a novel multi-criteria optimization (MCO) solution approach that generates treatment plans with deliverable apertures using column generation. Methods: We demonstrate our method with 10 locally advanced head-and-neck cancer cases retrospectively. In our MCO formulation, we defined an objective function for each structure in the treatment volume. This resulted in 9 objective functions, including 3 distinct objectives for primary target volume, high-risk and low-risk target volumes, 5 objectives for each of the organs-at-risk (OARs) (two parotid glands, spinal cord, brain stem and oral cavity), and one for the non-target non-OAR normal tissue. Conditional value-at-risk (CVaR) constraints were utilizedmore » to ensure at least certain fraction of the target volumes receiving the prescription doses. To directly generate deliverable plans, column generation algorithm was embedded within our MCO approach for aperture shape generation. Final dose distributions for all plans were generated using a Monte Carlo kernel-superposition dose calculation. We compared the MCO plans with the clinical plans, which were created by clinicians. Results: At least 95% target coverage was achieved by both MCO plans and clinical plans. However, the average conformity indices of clinical plans and the MCO plans were 1.95 and 1.35, respectively (31% reduction, p<0.01). Compared to the conventional clinical plan, the proposed MCO method achieved average reductions in left parotid mean dose of 5% (p=0.06), right parotid mean dose of 18% (p<0.01), oral cavity mean dose of 21% (p=0.03), spinal cord maximum dose of 20% (p<0.01), brain stem maximum dose of 61% (p<0.01), and normal tissue maximum dose of 5% (p<0.01), respectively. Conclusion: We demonstrated that the proposed MCO method was able to obtain deliverable IMRT treatment plans while achieving significant improvements in dosimetric plan quality.« less

A microfluidic device for preparing next generation DNA sequencing libraries and for automating other laboratory protocols that require one or more column chromatography steps.

PubMed

Tan, Swee Jin; Phan, Huan; Gerry, Benjamin Michael; Kuhn, Alexandre; Hong, Lewis Zuocheng; Min Ong, Yao; Poon, Polly Suk Yean; Unger, Marc Alexander; Jones, Robert C; Quake, Stephen R; Burkholder, William F

2013-01-01

Library preparation for next-generation DNA sequencing (NGS) remains a key bottleneck in the sequencing process which can be relieved through improved automation and miniaturization. We describe a microfluidic device for automating laboratory protocols that require one or more column chromatography steps and demonstrate its utility for preparing Next Generation sequencing libraries for the Illumina and Ion Torrent platforms. Sixteen different libraries can be generated simultaneously with significantly reduced reagent cost and hands-on time compared to manual library preparation. Using an appropriate column matrix and buffers, size selection can be performed on-chip following end-repair, dA tailing, and linker ligation, so that the libraries eluted from the chip are ready for sequencing. The core architecture of the device ensures uniform, reproducible column packing without user supervision and accommodates multiple routine protocol steps in any sequence, such as reagent mixing and incubation; column packing, loading, washing, elution, and regeneration; capture of eluted material for use as a substrate in a later step of the protocol; and removal of one column matrix so that two or more column matrices with different functional properties can be used in the same protocol. The microfluidic device is mounted on a plastic carrier so that reagents and products can be aliquoted and recovered using standard pipettors and liquid handling robots. The carrier-mounted device is operated using a benchtop controller that seals and operates the device with programmable temperature control, eliminating any requirement for the user to manually attach tubing or connectors. In addition to NGS library preparation, the device and controller are suitable for automating other time-consuming and error-prone laboratory protocols requiring column chromatography steps, such as chromatin immunoprecipitation.

A Microfluidic Device for Preparing Next Generation DNA Sequencing Libraries and for Automating Other Laboratory Protocols That Require One or More Column Chromatography Steps

PubMed Central

Tan, Swee Jin; Phan, Huan; Gerry, Benjamin Michael; Kuhn, Alexandre; Hong, Lewis Zuocheng; Min Ong, Yao; Poon, Polly Suk Yean; Unger, Marc Alexander; Jones, Robert C.; Quake, Stephen R.; Burkholder, William F.

2013-01-01

Library preparation for next-generation DNA sequencing (NGS) remains a key bottleneck in the sequencing process which can be relieved through improved automation and miniaturization. We describe a microfluidic device for automating laboratory protocols that require one or more column chromatography steps and demonstrate its utility for preparing Next Generation sequencing libraries for the Illumina and Ion Torrent platforms. Sixteen different libraries can be generated simultaneously with significantly reduced reagent cost and hands-on time compared to manual library preparation. Using an appropriate column matrix and buffers, size selection can be performed on-chip following end-repair, dA tailing, and linker ligation, so that the libraries eluted from the chip are ready for sequencing. The core architecture of the device ensures uniform, reproducible column packing without user supervision and accommodates multiple routine protocol steps in any sequence, such as reagent mixing and incubation; column packing, loading, washing, elution, and regeneration; capture of eluted material for use as a substrate in a later step of the protocol; and removal of one column matrix so that two or more column matrices with different functional properties can be used in the same protocol. The microfluidic device is mounted on a plastic carrier so that reagents and products can be aliquoted and recovered using standard pipettors and liquid handling robots. The carrier-mounted device is operated using a benchtop controller that seals and operates the device with programmable temperature control, eliminating any requirement for the user to manually attach tubing or connectors. In addition to NGS library preparation, the device and controller are suitable for automating other time-consuming and error-prone laboratory protocols requiring column chromatography steps, such as chromatin immunoprecipitation. PMID:23894273

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

PubMed

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

2017-04-28

In the fields of essential oils and fragrances, samples often consist of mixtures of compounds with similar structural and physical characteristics (e.g. mono- and sesquiterpenoids), whose correct identification closely depends on the synergic combination of chromatographic and mass spectral data. This sample complexity means that new GC stationary phases with different selectivities are continually being investigated. Ionic liquids (ILs) are of great interest as GC stationary phases in this field because of their selectivity (significantly different than that of currently phases) and their high temperature stability. A first generation of IL GC columns was found to be competitive when applied to these field, in terms of selectivity and efficiency, compared to conventional columns (polydimethylsiloxane, (e.g. OV-1), methyl-polysiloxane 5%-phenyl (e.g. SE-52), 7%-cyanopropyl, 7%-phenyl polysiloxane (e.g. OV-1701), and polyethylen glycol (e.g. PEG-20M). However, these columns showed significant activity towards polar or active analytes, which primarily affected their quantitative performance. A new generation of highly-inactive columns coated with three of the most widely-used ionic liquid GC stationary phases has recently been introduced; these phases are SLB-IL60i (1,12-di(tripropylphosphonium) dodecane bis(trifluoromethylsulfonyl) imide [NTf 2 ], SLB-IL76i (tri-(tripropylphosphonium-hexanamido)-triethylamine [NTf 2 ]), and SLB-IL111i (1,5-di (2,3-dimethyllimidazolium) pentane [NTf 2 ]). This study carefully tested the new inert IL columns, in view of their routine application in the fragrance and essential oil fields. They were found to have unusually high selectivity, comparable to that of first-generation IL columns, while their inertness and efficiency were competitive with those of currently-used conventional columns. The IL column performance of first and second generations was compared, through the quali-quantitative analysis of components in a group of different complexity samples; these included the Grob test, a standard mixture of "suspected" skin allergens, and the essential oils of chamomile and sandalwood. Copyright © 2017 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.

Neutron camera employing row and column summations

DOEpatents

Clonts, Lloyd G.; Diawara, Yacouba; Donahue, Jr, Cornelius; Montcalm, Christopher A.; Riedel, Richard A.; Visscher, Theodore

2016-06-14

For each photomultiplier tube in an Anger camera, an R.times.S array of preamplifiers is provided to detect electrons generated within the photomultiplier tube. The outputs of the preamplifiers are digitized to measure the magnitude of the signals from each preamplifier. For each photomultiplier tube, a corresponding summation circuitry including R row summation circuits and S column summation circuits numerically add the magnitudes of the signals from preamplifiers for each row and for each column to generate histograms. For a P.times.Q array of photomultiplier tubes, P.times.Q summation circuitries generate P.times.Q row histograms including R entries and P.times.Q column histograms including S entries. The total set of histograms include P.times.Q.times.(R+S) entries, which can be analyzed by a position calculation circuit to determine the locations of events (detection of a neutron).

Method for enhancing selectivity and recovery in the fractional flotation of particles in a flotation column

DOEpatents

Klunder, Edgar B [Bethel Park, PA

2011-08-09

The method relates to particle separation from a feed stream. The feed stream is injected directly into the froth zone of a vertical flotation column in the presence of a counter-current reflux stream. A froth breaker generates a reflux stream and a concentrate stream, and the reflux stream is injected into the froth zone to mix with the interstitial liquid between bubbles in the froth zone. Counter-current flow between the plurality of bubbles and the interstitial liquid facilitates the attachment of higher hydrophobicity particles to bubble surfaces as lower hydrophobicity particles detach. The height of the feed stream injection and the reflux ratio may be varied in order to optimize the concentrate or tailing stream recoveries desired based on existing operating conditions.

New approaches with two cyano columns to the separation of acetaminophen, phenylephrine, chlorpheniramine and related compounds.

PubMed

Olmo, B; García, A; Marín, A; Barbas, C

2005-03-25

The development of new pharmaceutical forms with classical active compounds generates new analytical problems. That is the case of sugar-free sachets of cough-cold products containing acetaminophen, phenylephrine hydrochloride and chlorpheniramine maleate. Two cyanopropyl stationary phases have been employed to tackle the problem. The Discovery cyanopropyl (SUPELCO) column permitted the separation of the three actives, maleate and excipients (mainly saccharine and orange flavour) with a constant proportion of aqueous/ organic solvent (95:5, v/v) and a pH gradient from 7.5 to 2. The run lasted 14 min. This technique avoids many problems related to baseline shifts with classical organic solvent gradients and opens great possibilities to modify selectivity not generally used in reversed phase HPLC. On the other hand, the Agilent Zorbax SB-CN column with a different retention profile permitted us to separate not only the three actives and the excipients but also the three known related compounds: 4-aminophenol, 4-chloracetanilide and 4-nitrophenol in an isocratic method with a run time under 30 min. This method was validated following ICH guidelines and validation parameters showed that it could be employed as stability-indicating method for this pharmaceutical form.

Comparing mass balance and adjoint methods for inverse modeling of nitrogen dioxide columns for global nitrogen oxide emissions

NASA Astrophysics Data System (ADS)

Cooper, Matthew; Martin, Randall V.; Padmanabhan, Akhila; Henze, Daven K.

2017-04-01

Satellite observations offer information applicable to top-down constraints on emission inventories through inverse modeling. Here we compare two methods of inverse modeling for emissions of nitrogen oxides (NOx) from nitrogen dioxide (NO2) columns using the GEOS-Chem chemical transport model and its adjoint. We treat the adjoint-based 4D-Var modeling approach for estimating top-down emissions as a benchmark against which to evaluate variations on the mass balance method. We use synthetic NO2 columns generated from known NOx emissions to serve as "truth." We find that error in mass balance inversions can be reduced by up to a factor of 2 with an iterative process that uses finite difference calculations of the local sensitivity of NO2 columns to a change in emissions. In a simplified experiment to recover local emission perturbations, horizontal smearing effects due to NOx transport are better resolved by the adjoint approach than by mass balance. For more complex emission changes, or at finer resolution, the iterative finite difference mass balance and adjoint methods produce similar global top-down inventories when inverting hourly synthetic observations, both reducing the a priori error by factors of 3-4. Inversions of simulated satellite observations from low Earth and geostationary orbits also indicate that both the mass balance and adjoint inversions produce similar results, reducing a priori error by a factor of 3. As the iterative finite difference mass balance method provides similar accuracy as the adjoint method, it offers the prospect of accurately estimating top-down NOx emissions using models that do not have an adjoint.

Ultrafast treatment plan optimization for volumetric modulated arc therapy (VMAT)

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

Men Chunhua; Romeijn, H. Edwin; Jia Xun

2010-11-15

Purpose: To develop a novel aperture-based algorithm for volumetric modulated arc therapy (VMAT) treatment plan optimization with high quality and high efficiency. Methods: The VMAT optimization problem is formulated as a large-scale convex programming problem solved by a column generation approach. The authors consider a cost function consisting two terms, the first enforcing a desired dose distribution and the second guaranteeing a smooth dose rate variation between successive gantry angles. A gantry rotation is discretized into 180 beam angles and for each beam angle, only one MLC aperture is allowed. The apertures are generated one by one in a sequentialmore » way. At each iteration of the column generation method, a deliverable MLC aperture is generated for one of the unoccupied beam angles by solving a subproblem with the consideration of MLC mechanic constraints. A subsequent master problem is then solved to determine the dose rate at all currently generated apertures by minimizing the cost function. When all 180 beam angles are occupied, the optimization completes, yielding a set of deliverable apertures and associated dose rates that produce a high quality plan. Results: The algorithm was preliminarily tested on five prostate and five head-and-neck clinical cases, each with one full gantry rotation without any couch/collimator rotations. High quality VMAT plans have been generated for all ten cases with extremely high efficiency. It takes only 5-8 min on CPU (MATLAB code on an Intel Xeon 2.27 GHz CPU) and 18-31 s on GPU (CUDA code on an NVIDIA Tesla C1060 GPU card) to generate such plans. Conclusions: The authors have developed an aperture-based VMAT optimization algorithm which can generate clinically deliverable high quality treatment plans at very high efficiency.« less

Direct-injection screening for acidic drugs in plasma and neutral drugs in equine urine by differential-gradient LC-LC coupled MS/MS.

PubMed

Stanley, Shawn M R; Wee, Wei Khee; Lim, Boon Huat; Foo, Hsiao Ching

2007-04-01

Direct-injection LC-LC hybrid tandem MS methods have been developed for undertaking broad-based screening for acidic drugs in protein-precipitated plasma and neutral doping agents in equine urine. In both analyses, analytes present in the matrix were trapped using a HLB extraction column before being refocused and separated on a Chromolith RP-18e monolithic analytical column using a controlled differential gradient generated by proportional dilution of the first column's eluent with water. Each method has been optimised by the adoption of a mobile phase and gradient that was tailored to enhance ionisation in the MS source while maintaining good chromatographic behaviour for the majority of the target drugs. The analytical column eluent was fed into the heated nebulizer (HN) part of the Duospray interface attached to a 4000 QTRAP mass spectrometer. Information dependent acquisition (IDA) with dynamic background subtraction (DBS) was configured to trigger a sensitive enhanced product ion (EPI) scan when a multiple reaction monitoring (MRM) survey scan signal exceeded the defined criteria. Ninety-one percent of acidic drugs in protein-precipitated plasma and 80% of the neutral compounds in equine urine were detected when spiked at 10 ng/ml.

Soil Overconsolidation Changes Caused by Dynamic Replacement

NASA Astrophysics Data System (ADS)

Piotr, Kanty; Sławomir, Kwiecień; Jerzy, Sękowski

2017-10-01

In the dynamic replacement method (DR) the soil is improved by initially dropping a large weight (typically 8-20 t) pounder from a significant height up to 25 m. The created crater is filled with a stronger material (gravel, rubble, stone aggregate, debris), and the pounder is dropped once or multiple times again. The construction of dynamic replacement pillars influences the parameters of the adjacent soil. It results from the energy generated by dropping a pounder into the soil. In the current practice, these changes are not taken into the account during the design. This paper focuses on the changes of overconsolidation ratio (OCR) and in situ coefficient of lateral earth pressure (K) values estimated base on cone penetration test (CPTU) and Dilatometric test (DMT) performed at a test site. A single column was constructed and the ground around the column was examined using CPTU and DMT, performed at different distances from the column centre (2, 3, 4 and 6 m) and at different time intervals (during construction and 1, 8, 30 days later). The column was constructed in so-called transition soils (between cohesive and non-cohesive). While interpreting the results of the research, the authors addressed the matter of choosing the procedure of OCR and K indication for transition soils (in this case described as silts and/or sandy silts). Overconsolidation changes may differ depending on the chosen analysis procedure (for cohesive or non-cohesive soils). On the basis of the analysis presented in the paper and the observation of soil (acknowledged as cohesive according to macroscopic observations) during column excavation, it was decided that for more detailed analyses methods dedicated to cohesive soils should be applied. Generally, it can be stated that although the changes were complex, DR pillar formation process resulted in the increase of these parameters. The average increases of OCR and K values were 25% and 10% respectively. The post installation values are not significant from the engineering point of view, but they represent the influence of the formation process of only a single column. The described results indicate that Priebe’s column dimensioning method should be applied with caution, as it assumes the value K=1 which was not obtained in the described research. The results from the conducted tests indicate that different mechanisms occur during stone column formation with vibro-replacement and dynamic replacement. As the authors did not manage to find literature describing the results of K tests in the surrounding of a DR column, the presented results should be acknowledged as significant for designers who will apply the dynamic replacement method.

Calibration of a turbidity meter for making estimates of total suspended solids concentrations and beam attenuation coefficients in field experiments

NASA Technical Reports Server (NTRS)

Usry, J. W.; Whitlock, C. H.

1981-01-01

Management of water resources such as a reservoir requires using analytical models which describe such parameters as the suspended sediment field. To select or develop an appropriate model requires making many measurements to describe the distribution of this parameter in the water column. One potential method for making those measurements expeditiously is to measure light transmission or turbidity and relate that parameter to total suspended solids concentrations. An instrument which may be used for this purpose was calibrated by generating curves of transmission measurements plotted against measured values of total suspended solids concentrations and beam attenuation coefficients. Results of these experiments indicate that field measurements made with this instrument using curves generated in this study should correlate with total suspended solids concentrations and beam attenuation coefficients in the water column within 20 percent.

Hepatotoxic microcystin removal using pumice embedded monolithic composite cryogel as an alternative water treatment method.

PubMed

Gurbuz, Fatma; Ceylan, Şeyda; Odabaşı, Mehmet; Codd, Geoffrey A

2016-03-01

Microcystins are the most commonly encountered water-borne cyanotoxins which present short- and long-term risks to human health. Guidelines at international and national level, and legislation in some countries, have been introduced for the effective health risk management of these potent hepatotoxic, tumour-promoters. The stable cyclic structure of microcystins and their common production by cyanobacteria in waterbodies at times of high total dissolved organic carbon content presents challenges to drinking water treatment facilities, with conventional, advanced and novel strategies under evaluation. Here, we have studied the removal of microcystins using three different forms of pumice particles (PPs), which are embedded into macroporous cryogel columns. Macroporous composite cryogel columns (MCCs) are a new generation of separation media designed to face this challenging task. Three different MCCs were prepared by adding plain PPs, Cu(2+)-attached PPs and Fe(3+)-attached PPs to reaction media before the cryogelation step. Column studies showed that MCCs could be successfully used as an alternative water treatment method for successful microcystin removal. Copyright © 2016 Elsevier Ltd. All rights reserved.

Very high pressure liquid chromatography using fully porous particles: quantitative analysis of fast gradient separations without post-run times.

PubMed

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

2014-01-10

Using a column packed with fully porous particles, four methods for controlling the flow rates at which gradient elution runs are conducted in very high pressure liquid chromatography (VHPLC) were tested to determine whether reproducible thermal conditions could be achieved, such that subsequent analyses would proceed at nearly the same initial temperature. In VHPLC high flow rates are achieved, producing fast analyses but requiring high inlet pressures. The combination of high flow rates and high inlet pressures generates local heat, leading to temperature changes in the column. Usually in this case a post-run time is input into the analytical method to allow the return of the column temperature to its initial state. An alternative strategy involves operating the column without a post-run equilibration period and maintaining constant temperature variations for subsequent analysis after conducting one or a few separations to bring the column to a reproducible starting temperature. A liquid chromatography instrument equipped with a pressure controller was used to perform constant pressure and constant flow rate VHPLC separations. Six replicate gradient separations of a nine component mixture consisting of acetophenone, propiophenone, butyrophenone, valerophenone, hexanophenone, heptanophenone, octanophenone, benzophenone, and acetanilide dissolved in water/acetonitrile (65:35, v/v) were performed under various experimental conditions: constant flow rate, two sets of constant pressure, and constant pressure operation with a programmed flow rate. The relative standard deviations of the response factors for all the analytes are lower than 5% across the methods. Programming the flow rate to maintain a fairly constant pressure instead of using instrument controlled constant pressure improves the reproducibility of the retention times by a factor of 5, when plotting the chromatograms in time. Copyright © 2013 Elsevier B.V. All rights reserved.

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.

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.

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.

mirRICH, a simple method to enrich the small RNA fraction from over-dried RNA pellets.

PubMed

Choi, Cheolwon; Yoon, Seulgi; Moon, Hyesu; Bae, Yun-Ui; Kim, Chae-Bin; Diskul-Na-Ayudthaya, Penchatr; Ngu, Trinh Van; Munir, Javaria; Han, JaeWook; Park, Se Bin; Moon, Jong-Seok; Song, Sujung; Ryu, Seongho

2018-04-11

Techniques to isolate the small RNA fraction (<200nt) by column-based methods are commercially available. However, their use is limited because of the relatively high cost. We found that large RNA molecules, including mRNAs and rRNAs, are aggregated together in the presence of salts when RNA pellets are over-dried. Moreover, once RNA pellets are over-dried, large RNA molecules are barely soluble again during the elution process, whereas small RNA molecules (<100nt) can be eluted. We therefore modified the acid guanidinium thiocyanate-phenol-chloroform (AGPC)-based RNA extraction protocol by skipping the 70% ethanol washing step and over-drying the RNA pellet for 1 hour at room temperature. We named this novel small RNA isolation method "mirRICH." The quality of the small RNA sequences was validated by electrophoresis, next-generation sequencing, and quantitative PCR, and the findings support that our newly developed column-free method can successfully and efficiently isolate small RNAs from over-dried RNA pellets.

Elution of Re-188 from W-188/Re-188 generators with salts of weak acids permits efficient concentration to low volumes using a new tandem cation/anion exchange system

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

Guhlke, S.; Beets, A.L.; Knapp, F.F. Jr.

1997-05-01

Re-188, available from a W-188/Re-188 generator, is an important therapeutic radioisotope for bone pain palliation, cancer therapy and intravascular brachytherapy, etc. Because of the relatively low specific activity of reactor-produced W-188 (ORNL HFIR, 296-370 MBq mCi/mg W-186 for 2 cycles), methods of concentrating the Re-188 bolus (10-12 mL) from clinical scale (18.5-37 BGq W-188) generators (5-6 gm alumina) are thus very important. We demonstrate for the first time a new strategy of generator elution with salts of weak acids and specific perrhenate anion {open_quotes}trapping{close_quotes} with QMA anion columns. Re-188 perrhenate is efficiently eluted (65-75%) from the alumina-based generator with 0.15-0.3more » M ammonium acetate. An acetic acid solution of Re-188 perrhenic acid is obtained by subsequent on-line passage of the generator eluant through a DOWEX AG 50Wx8 (200-400 mesh, H{sup +} form) column. Since acetic acid is not ionized (< 0.001%) at this pH (< pK{sub a} = 4.76) the perrhenate anion is then specifically trapped on a QMA {open_quotes}Light{close_quotes} anion extraction column. QMA elution with 0.9% NaCl, provides Re-188 perrhenate solution in <1 mL. Concentration of 10-20 mL of Re-188 solution (> 15 BGq) in <1 mL has been demonstrated using this simple new approach, which is also effective for concentration of Tc-99m from low specific activity Mo-99 (n,y) generators. The cation/anion tandem system is inexpensive and disposable and use can be easily automated. The availability of this very simple, efficient system is important for broad use of rhenium-188.« less

Quality-by-design-based ultra high performance liquid chromatography related substances method development by establishing the proficient design space for sumatriptan and naproxen combination.

PubMed

Patel, Prinesh N; Karakam, Vijaya Saradhi; Samanthula, Gananadhamu; Ragampeta, Srinivas

2015-10-01

Quality-by-design-based methods hold greater level of confidence for variations and greater success in method transfer. A quality-by-design-based ultra high performance liquid chromatography method was developed for the simultaneous assay of sumatriptan and naproxen along with their related substances. The first screening was performed by fractional factorial design comprising 44 experiments for reversed-phase stationary phases, pH, and organic modifiers. The results of screening design experiments suggested phenyl hexyl column and acetonitrile were the best combination. The method was further optimized for flow rate, temperature, and gradient time by experimental design of 20 experiments and the knowledge space was generated for effect of variable on response (number of peaks ≥ 1.50 - resolution). Proficient design space was generated from knowledge space by applying Monte Carlo simulation to successfully integrate quantitative robustness metrics during optimization stage itself. The final method provided the robust performance which was verified and validated. Final conditions comprised Waters® Acquity phenyl hexyl column with gradient elution using ammonium acetate (pH 4.12, 0.02 M) buffer and acetonitrile at 0.355 mL/min flow rate and 30°C. The developed method separates all 13 analytes within a 15 min run time with fewer experiments compared to the traditional quality-by-testing approach. ©2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Process and apparatus for separating fine particles by microbubble flotation together with a process and apparatus for generation of microbubbles

DOEpatents

Yoon, R.H.; Adel, G.T.; Luttrell, G.H.

1991-01-01

A method and apparatus are disclosed for the microbubble flotation separation of very fine particles, especially coal, so as to produce a high purity and large recovery efficiently. This is accomplished through the use of a high aspect ratio flotation column, microbubbles, and a countercurrent use of wash water to gently wash the froth. Also, disclosed are unique processes and apparatus for generating microbubbles for flotation in a high efficient and inexpensive manner using either a porous tube or an in-line static generator. 23 figures.

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

PubMed

Wright, Bob W; Wright, Cherylyn W

2012-10-26

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

Computer-Aided Construction at Designing Reinforced Concrete Columns as Per Ec

NASA Astrophysics Data System (ADS)

Zielińska, M.; Grębowski, K.

2015-02-01

The article presents the authors' computer program for designing and dimensioning columns in reinforced concrete structures taking into account phenomena affecting their behaviour and information referring to design as per EC. The computer program was developed with the use of C++ programming language. The program guides the user through particular dimensioning stages: from introducing basic data such as dimensions, concrete class, reinforcing steel class and forces affecting the column, through calculating the creep coefficient taking into account the impact of imperfection depending on the support scheme and also the number of mating members at load shit, buckling length, to generating the interaction curve graph. The final result of calculations provides two dependence points calculated as per methods of nominal stiffness and nominal curvature. The location of those points relative to the limit curve determines whether the column load capacity is assured or has been exceeded. The content of the study describes in detail the operation of the computer program and the methodology and phenomena which are indispensable at designing axially and eccentrically the compressed members of reinforced concrete structures as per the European standards.

Unconstrained paving and plastering method for generating finite element meshes

DOEpatents

Staten, Matthew L.; Owen, Steven J.; Blacker, Teddy D.; Kerr, Robert

2010-03-02

Computer software for and a method of generating a conformal all quadrilateral or hexahedral mesh comprising selecting an object with unmeshed boundaries and performing the following while unmeshed voids are larger than twice a desired element size and unrecognizable as either a midpoint subdividable or pave-and-sweepable polyhedra: selecting a front to advance; based on sizes of fronts and angles with adjacent fronts, determining which adjacent fronts should be advanced with the selected front; advancing the fronts; detecting proximities with other nearby fronts; resolving any found proximities; forming quadrilaterals or unconstrained columns of hexahedra where two layers cross; and establishing hexahedral elements where three layers cross.

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.

A method for determining the column curve from tests of columns with equal restraints against rotation on the ends

NASA Technical Reports Server (NTRS)

Lundquist, Eugene E; Rossman, Carl A; Houbolt, John C

1943-01-01

The results are presented of a theoretical study for the determination of the column curve from tests of column specimens having ends equally restrained against rotation. The theory of this problem is studied and a curve is shown relating the fixity coefficient c to the critical load, the length of the column, and the magnitude of the elastic restraint. A method of using this curve for the determination of the column curve for columns with pin ends from tests of columns with elastically restrained ends is presented. The results of the method as applied to a series of tests on thin-strip columns of stainless steel are also given.

Simultaneous analysis of C1 and C4 oxidized oligosaccharides, the products of lytic polysaccharide monooxygenases acting on cellulose.

PubMed

Westereng, Bjørge; Arntzen, Magnus Ø; Aachmann, Finn L; Várnai, Anikó; Eijsink, Vincent G H; Agger, Jane Wittrup

2016-05-06

Lytic polysaccharide monooxygenases play a pivotal role in enzymatic deconstruction of plant cell wall material due to their ability to catalyze oxidative cleavage of glycosidic bonds. LPMOs may release different products, often in small amounts, with various oxidation patterns (C1 or C4) and with varying stabilities, making accurate analysis of product profiles a major challenge. So far, HPAEC has been the method of choice but it has limitations with respect to analysis of C4-oxidized products. Here, we compare various HPLC methods and present procedures that allow efficient separation of intact C1- and C4-oxidized products. We demonstrate that both PGC and HILIC (in WAX-mode) can separate C1- and C4-oxidized products and that PGC gives superior chromatographic performance. In contrast to HPAEC, these methods are directly compatible with mass spectroscopy and charged aerosol detection (CAD), which enables online peak validation and quantification with LOD levels in the low ng range. While the novel methods show lower resolution than HPAEC, this is compensated by easy peak identification, allowing, for example, discrimination between chromatographically highly similar native and C4-oxidized cello-oligomers. HPAEC-MS studies revealed chemical oxidation of C4-geminal diol products, which implies that peaks commonly believed to be C4-oxidized cello-oligomers, in fact are on-column generated derivatives. Non-destructive separation of C4-oxidized cello-oligosaccharides on the PGC column allowed us, for the first time, to isolate C4-oxidized standards. HPAEC fractionation of a purified C4-oxidized tetramer revealed that on-column decomposition leads to formation of the native trimer, which may explain why product mixtures generated by C4-oxidizing LPMOs seem to be rich in native oligosaccharides when analyzed by HPAEC. The findings and methods described here will aid in future studies in the emerging LPMO field. Copyright © 2016 Elsevier B.V. All rights reserved.

Systematic interpolation method predicts protein chromatographic elution with salt gradients, pH gradients and combined salt/pH gradients.

PubMed

Creasy, Arch; Barker, Gregory; Carta, Giorgio

2017-03-01

A methodology is presented to predict protein elution behavior from an ion exchange column using both individual or combined pH and salt gradients based on high-throughput batch isotherm data. The buffer compositions are first optimized to generate linear pH gradients from pH 5.5 to 7 with defined concentrations of sodium chloride. Next, high-throughput batch isotherm data are collected for a monoclonal antibody on the cation exchange resin POROS XS over a range of protein concentrations, salt concentrations, and solution pH. Finally, a previously developed empirical interpolation (EI) method is extended to describe protein binding as a function of the protein and salt concentration and solution pH without using an explicit isotherm model. The interpolated isotherm data are then used with a lumped kinetic model to predict the protein elution behavior. Experimental results obtained for laboratory scale columns show excellent agreement with the predicted elution curves for both individual or combined pH and salt gradients at protein loads up to 45 mg/mL of column. Numerical studies show that the model predictions are robust as long as the isotherm data cover the range of mobile phase compositions where the protein actually elutes from the column. Copyright © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

In-column bonded phase polymerization for improved packing uniformity

PubMed Central

Huckabee, Alexis G.; Yerneni, Charu; Jacobson, Rachel E.; Alzate, Edwin J.; Chen, Tse-Hong; Wirth, Mary J.

2017-01-01

It is difficult to pack chromatographic particles having polymeric-bonded phases because solvents used for making a stable slurry cause the polymer layer to swell. Growth of the polymer inside the column (in situ) after packing was investigated and compared with conventional, ex situ polymer growth. The method of activators generated by electron transfer, along with atom-transfer radical polymerization, enabled polymerization under ambient conditions. Nonporous, 0.62 µm silica particles with silane initiators were used. Polyacrylamide films with a hydrated thickness of 23 nm in 75:25 water/isopropanol grew in 55 min for both in situ and ex situ preparations, and the same carbon coverage was observed. Higher chromatographic resolution and better column-to-column reproducibility were observed for in situ polymer growth, as evaluated by hydrophilic interaction liquid chromatography for the model glycoprotein, ribonuclease B. In situ polymer growth was also found to give lower eddy diffusion, as shown by a narrower peak width for injected acetonitrile in 50:50 acetonitrile/water. When columns were packed more loosely, bed collapse occurred quickly for ex situ, but not for in situ, polymer growth. The higher resolution and stability for in situ polymer growth is explained by packing with hard, rather than soft, contacts between particles. PMID:28387037

Recent trends in ultra-fast HPLC: new generation superficially porous silica columns.

PubMed

Ali, Imran; Al-Othman, Zeid A; Nagae, Norikaju; Gaitonde, Vinay D; Dutta, Kamlesh K

2012-12-01

New generation columns, i.e. packed with superficially porous silica particles are available as trade names with following manufacturers: Halo, Ascentis Express, Proshell 120, Kinetex, Accucore, Sunshell, and Nucleoshell. These provide ultra-fast HPLC separations for a variety of compounds with moderate sample loading capacity and low back pressure. Chemistries of these columns are C(8), C(18), RP-Amide, hydrophilic interaction liquid chromatography, penta fluorophenyl (PFP), F5, and RP-aqua. Normally, the silica gel particles are of 2.7 and 1.7 μm as total and inner solid core diameters, respectively, with 0.5-μm-thick of outer porous layer having 90 Å pore sizes and 150 m(2)/g surface area. This article describes these new generation columns with special emphasis on their textures and chemistries, separations, optimization, and comparison (inter and intra stationary phases). Besides, future perspectives have also been discussed. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Electronic drive and acquisition system for mass spectrometry

NASA Technical Reports Server (NTRS)

Schaefer, Rembrandt Thomas (Inventor); Chutjian, Ara (Inventor); Tran, Tuan (Inventor); Madzunkov, Stojan M. (Inventor); Thomas, John L. (Inventor); Mojarradi, Mohammad (Inventor); MacAskill, John (Inventor); Blaes, Brent R. (Inventor); Darrach, Murray R. (Inventor); Burke, Gary R. (Inventor)

2010-01-01

The present invention discloses a mixed signal RF drive electronics board that offers small, low power, reliable, and customizable method for driving and generating mass spectra from a mass spectrometer, and for control of other functions such as electron ionizer, ion focusing, single-ion detection, multi-channel data accumulation and, if desired, front-end interfaces such as pumps, valves, heaters, and columns.

Determination of thimerosal in pharmaceutical industry effluents and river waters by HPLC coupled to atomic fluorescence spectrometry through post-column UV-assisted vapor generation.

PubMed

Acosta, Gimena; Spisso, Adrián; Fernández, Liliana P; Martinez, Luis D; Pacheco, Pablo H; Gil, Raúl A

2015-03-15

A high performance liquid chromatography coupled with atomic fluorescence spectrometry method for the determination of thimerosal (sodium ethylmercury thiosalicylate, C9H9HgNaO2S), ethylmercury, and inorganic mercury is proposed. Mercury vapor is generated by the post-column reduction of mercury species in formic acid media using UV-radiation. Thimerosal is quantitatively converted to Hg(II) followed by the reduction of Hg(II) to Hg(0). This method is applied to the determination of thimerosal (THM), ethylmercury (EtHg) and inorganic Hg in samples of a pharmaceutical industry effluent, and in waters of the San Luis River situated in the west side of San Luis city (Middle West, Argentine) where the effluents are dumped. The limit of detections, calculated on the basis of the 3σ criterion, where 0.09, 0.09 and 0.07 μg L(-1) for THM, EtHg(II) and for Hg(II), respectively. Linearity was attained from levels close to the detection limit up to at least 100 μg L(-1). Copyright © 2014 Elsevier B.V. All rights reserved.

High radioactive concentration of 99mTc from a zirconium [99Mo]molybdate gel generator using an acidic alumina column for purification and concentration.

PubMed

Sarkar, S K; Saraswathy, P; Arjun, G; Ramamoorthy, N

2004-06-01

Newer applications of radiopharmaceuticals in nuclear medicine require pertechnetate of moderate to high radioactive concentration. Hence there is a need to develop simple procedures for the concentration of pertechnetate, and such a procedure is given in this paper. Ten to 20 ml of sodium [Tc]pertechnetate eluted in de-ionized water from a zirconium [Mo]molybdate (ZrMo) gel column generator was passed through 2 g of an acidic alumina bed (35 x 8 mm) in order to remove the co-eluted traces of Mo and to retain the pertechnetate. The retained pertechnetate was then re-eluted, quantitatively, in 3 ml of normal saline, from the alumina column. About a 4-fold increase in radioactive concentration of Tc was obtained (cf. approximately 10-12 ml normal saline is required for the elution of Tc from the gel column). Generators containing up to 22.2 GBq (600 mCi) Mo in 6-7 g ZrMo gel column (35 x 13 mm) were prepared and a radioactive concentration of Tc up to 4 GBq x ml (110 mCi x ml) was obtained on the first day of use. The overall recovery of Tc was >90%, Mo breakthrough was 10 to 10% and the duration of concentration was 3-5 min. The chemical impurity in terms of Al, Mo and Zr was <10 ppm each. The same procedure for the concentration of pertechnetate was applied to generators with 12-15 g ZrMo gel beds to obtain a higher capacity Tc gel generator, with similar findings.

Ionic liquid phases with comprehensive two-dimensional gas chromatography of fatty acid methyl esters.

PubMed

Pojjanapornpun, Siriluck; Nolvachai, Yada; Aryusuk, Kornkanok; Kulsing, Chadin; Krisnangkura, Kanit; Marriott, Philip J

2018-02-17

New generation inert ionic liquid (iIL) GC columns IL60i, IL76i and IL111i, comprising phosphonium or imidazolium cationic species, were investigated for separation of fatty acid methyl esters (FAME). In general, the iIL phases provide comparable retention times to their corresponding conventional columns, with only minor selectivity differences. The average tailing factors and peak widths were noticeably improved (reduced) for IL60i and IL76i, while they were slightly improved for IL111i. Inert IL phase columns were coupled with conventional IL columns in comprehensive two-dimensional GC (GC × GC) with a solid-state modulator which offers variable modulation temperature (T M ), programmable T M during analysis and trapping stationary phase material during the trap/release (modulation) process, independent of oven T and column sets. Although IL phases are classified as polar, relative polarity of the two phases comprising individual GC × GC column sets permits combination of less-polar IL/polar IL and polar IL/less-polar IL column sets; it was observed that a polar/less-polar column set provided better separation of FAME. A higher first dimension ( 1 D) phase polarity combined with a lower 2 D phase polarity, for instance 1 D IL111i with 2 D IL59 gave the best result; the greater difference in 1 D/ 2 D phase polarity results in increasing occupancy of peak area in the 2D space. The IL111i/IL59 column set was selected for analysis of fatty acids in fat and oil products (butter, margarine, fish oil and canola oil). Compared with the conventional IL111, IL111i showed reduced column bleed which makes this more suited to GC × GC analysis of FAME. The proposed method offers a fast profiling approach with good repeatability of analysis of FAME.

Dogs lap using acceleration-driven open pumping

PubMed Central

Gart, Sean; Socha, John J.; Vlachos, Pavlos P.; Jung, Sunghwan

2015-01-01

Dogs lap because they have incomplete cheeks and cannot suck. When lapping, a dog’s tongue pulls a liquid column from the bath, suggesting that the hydrodynamics of column formation are critical to understanding how dogs drink. We measured lapping in 19 dogs and used the results to generate a physical model of the tongue’s interaction with the air–fluid interface. These experiments help to explain how dogs exploit the fluid dynamics of the generated column. The results demonstrate that effects of acceleration govern lapping frequency, which suggests that dogs curl the tongue to create a larger liquid column. Comparing lapping in dogs and cats reveals that, despite similar morphology, these carnivores lap in different physical regimes: an unsteady inertial regime for dogs and steady inertial regime for cats. PMID:26668382

Plasticity in skeletal characteristics of nursery-raised staghorn coral, Acropora cervicornis

USGS Publications Warehouse

Kuffner, Ilsa B.; Bartels, Erich; Stathakopoulos, Anastasios; Enochs, Ian C.; Kolodziej, Graham; Toth, Lauren; Manzello, Derek P.

2017-01-01

Staghorn coral, Acropora cervicornis, is a threatened species and the primary focus of western Atlantic reef restoration efforts to date. We compared linear extension, calcification rate, and skeletal density of nursery-raised A. cervicornis branches reared for 6 months either on blocks attached to substratum or hanging from PVC trees in the water column. We demonstrate that branches grown on the substratum had significantly higher skeletal density, measured using computerized tomography, and lower linear extension rates compared to water-column fragments. Calcification rates determined with buoyant weighing were not statistically different between the two grow-out methods, but did vary among coral genotypes. Whereas skeletal density and extension rates were plastic traits that depended on grow-out method, calcification rate was conserved. Our results show that the two rearing methods generate the same amount of calcium carbonate skeleton but produce colonies with different skeletal characteristics and suggest that there is genetically based variability in coral calcification performance.

Plasticity in skeletal characteristics of nursery-raised staghorn coral, Acropora cervicornis

NASA Astrophysics Data System (ADS)

Kuffner, Ilsa B.; Bartels, Erich; Stathakopoulos, Anastasios; Enochs, Ian C.; Kolodziej, G.; Toth, Lauren T.; Manzello, Derek P.

2017-09-01

Staghorn coral, Acropora cervicornis, is a threatened species and the primary focus of western Atlantic reef restoration efforts to date. We compared linear extension, calcification rate, and skeletal density of nursery-raised A. cervicornis branches reared for 6 months either on blocks attached to substratum or hanging from PVC trees in the water column. We demonstrate that branches grown on the substratum had significantly higher skeletal density, measured using computerized tomography, and lower linear extension rates compared to water-column fragments. Calcification rates determined with buoyant weighing were not statistically different between the two grow-out methods, but did vary among coral genotypes. Whereas skeletal density and extension rates were plastic traits that depended on grow-out method, calcification rate was conserved. Our results show that the two rearing methods generate the same amount of calcium carbonate skeleton but produce colonies with different skeletal characteristics and suggest that there is genetically based variability in coral calcification performance.

Seismic, satellite, and site observations of internal solitary waves in the NE South China Sea.

PubMed

Tang, Qunshu; Wang, Caixia; Wang, Dongxiao; Pawlowicz, Rich

2014-06-20

Internal solitary waves (ISWs) in the NE South China Sea (SCS) are tidally generated at the Luzon Strait. Their propagation, evolution, and dissipation processes involve numerous issues still poorly understood. Here, a novel method of seismic oceanography capable of capturing oceanic finescale structures is used to study ISWs in the slope region of the NE SCS. Near-simultaneous observations of two ISWs were acquired using seismic and satellite imaging, and water column measurements. The vertical and horizontal length scales of the seismic observed ISWs are around 50 m and 1-2 km, respectively. Wave phase speeds calculated from seismic observations, satellite images, and water column data are consistent with each other. Observed waveforms and vertical velocities also correspond well with those estimated using KdV theory. These results suggest that the seismic method, a new option to oceanographers, can be further applied to resolve other important issues related to ISWs.

Electro-osmotically driven liquid delivery method and apparatus

DOEpatents

Rakestraw, David J.; Anex, Deon S.; Yan, Chao; Dadoo, Rajeev; Zare, Richard N.

1999-01-01

Method and apparatus for controlling precisely the composition and delivery of liquid at sub-.mu.L/min flow rate. One embodiment of such a delivery system is an electro-osmotically driven gradient flow delivery system that generates dynamic gradient flows with sub-.mu.L/min flow rates by merging a plurality of electro-osmotic flows. These flows are delivered by a plurality of delivery arms attached to a mixing connector, where they mix and then flow into a receiving means, preferably a column. Each inlet of the plurality of delivery arms is placed in a corresponding solution reservoir. A plurality of independent programmable high-voltage power supplies is used to apply a voltage program to each of the plurality of solution reservoirs to regulate the electro-osmotic flow in each delivery arm. The electro-osmotic flow rates in the delivery arms are changed with time according to each voltage program to deliver the required gradient profile to the column.

Screening for basic drugs in equine urine using direct-injection differential-gradient LC-LC coupled to hybrid tandem MS/MS.

PubMed

Stanley, Shawn M R; Foo, Hsiao Ching

2006-05-19

A rapid, selective and robust direct-injection LC/hybrid tandem MS method has been developed for simultaneous screening of more than 250 basic drugs in the supernatant of enzyme hydrolysed equine urine. Analytes, trapped using a short HLB extraction column, are refocused and separated on a Sunfire C(18) analytical column using a controlled differential gradient generated by proportional dilution of the first column's eluent with water. Independent data acquisition (IDA) was configured to trigger a sensitive enhanced product ion (EPI) scan when a multiple reaction monitoring (MRM) survey scan signal exceeded the defined criteria. The decision on whether or not to report a sample as a positive result was based upon both the presence of a MRM response within the correct retention time range and a qualitative match between the EPI spectrum obtained and the corresponding reference standard. Ninety seven percent of the drugs targeted by this method met our detection criteria when spiked into urine at 100 ng/ml; 199 were found at 10 ng/ml, 83 at 1 ng/ml and 4 at 0.1 ng/ml.

Cellular Targets of Dietary Polyphenol Resveratrol

DTIC Science & Technology

2005-03-01

attempts to generate affinity columns tagged with other polyphenols, e.g., epigallocatechin gallate ( EGCG ). Conceivably such columns, if generated, would...Similar affinity chromatography with the related polyphenol Epigallocatechin gallate does not produce similar results.” Answer: We did not make...addition, the PI does not provid expression. If there is “increased ex many bind the resveratrol affinity co related polyphenol Epigallocatechin Response

Chemical stabilization of metals in mine wastes by transformed red mud and other iron compounds: laboratory tests.

PubMed

Ardau, C; Lattanzi, P; Peretti, R; Zucca, A

2014-01-01

A series of static and kinetic laboratory-scale tests were designed in order to evaluate the efficacy of transformed red mud (TRM) from bauxite refining residues, commercial zero-valent iron, and synthetic iron (III) hydroxides as sorbents/reagents to minimize the generation of acid drainage and the release of toxic elements from multi-contaminant-laden mine wastes. In particular, in some column experiments the percolation of meteoric water through a waste pile, alternated with periods of dryness, was simulated. Wastes were placed in columns together with sorbents/reagents in three different set-ups: as blended amendment (mixing method), as a bed at the bottom of the column (filtration method), or as a combination of the two previous methods. The filtration methods, which simulate the creation of a permeable reactive barrier downstream of a waste pile, are the most effective, while the use of sorbents/reagents as amendments leads to unsatisfactory results, because of the selective removal of only some contaminants. The efficacy of the filtration method is not significantly affected by the periods of dryness, except for a temporary rise of metal contents in the leachates due to dissolution of soluble salts formed upon evaporation in the dry periods. These results offer original information on advantages/limits in the use of TRM for the treatment of multi-contaminant-laden mine wastes, and represent the starting point for experimentation at larger scale.

Development of a high performance (188)W/(188)Re generator by using a synthetic alumina.

PubMed

Lee, Jun Sig; Lee, Jong-Soup; Park, Ul-Jae; Son, Kwang-Jae; Han, Hyon-Soo

2009-01-01

A synthetic alumina functionalized with a sulfate moiety has been developed as the column material of (99)Mo/(99m)Tc and (188)W/(188)Re generators. This material is synthesized by a sol-gel processing. In order to characterize the adsorbent for the (188)W/(188)Re separation, both batch and column contact experiments were conducted. As a result of the experiments, it is found that the maximum capacity of the adsorbent for tungsten is higher than 450mg/g. Hence it is possible to produce approximately 3Ci (188)W/(188)Re generator with only 1g of the adsorbent from (188)W solutions supplied from ORNL, USA or RIAR, Russia. A demonstration study was conducted to show the performance of an (188)W/(188)Re generator column. In this study, 1Ci of (188)W purchased from RIAR, Russia, is loaded on a 0.9cm ID column packed with 0.7g of the adsorbent. Elution of (188)Re is performed every 4-7 days by using the saline solution for more than three months. Nearly 100% of tungsten is loaded by passing 5ml of the (188)W solution (pH=8) through the dry packed column at a 1ml/min flow rate. Elution efficiency of (188)Re is 70-90% by using 5ml of the saline solution. The ratio of (188)W/(188)Re in the eluted solution is 0.002-0.003%. When a Sep-Pak containing 0.26g of acid alumina is installed as a tandem column, the ratio is decreased to less than 10(-3)%. Thin layer chromatography for the eluted (188)Re solution shows 100% radiochemical purity. Also, alumina content in the eluted solution shows less than 10ppm. Through this study, the performance of this adsorbent was successfully demonstrated. By using the developed adsorbent, minimization of the generator column and consequently the volume of eluant could be possible while maintaining the quality of (188)Re just as much as that available in the market.

Method to fabricate silicon chromatographic column comprising fluid ports

DOEpatents

Manginell, Ronald P.; Frye-Mason, Gregory C.; Heller, Edwin J.; Adkins, Douglas R.

2004-03-02

A new method for fabricating a silicon chromatographic column comprising through-substrate fluid ports has been developed. This new method enables the fabrication of multi-layer interconnected stacks of silicon chromatographic columns.

Prediction of axial limit capacity of stone columns using dimensional analysis

NASA Astrophysics Data System (ADS)

Nazaruddin A., T.; Mohamed, Zainab; Mohd Azizul, L.; Hafez M., A.

2017-08-01

Stone column is the most favorable method used by engineers in designing work for stabilization of soft ground for road embankment, and foundation for liquid structure. Easy installation and cheaper cost are among the factors that make stone column more preferable than other method. Furthermore, stone column also can acts as vertical drain to increase the rate of consolidation during preloading stage before construction work started. According to previous studied there are several parameters that influence the capacity of stone column. Among of them are angle friction of among the stones, arrangement of column (two pattern arrangement most applied triangular and square), spacing center to center between columns, shear strength of soil, and physical size of column (diameter and length). Dimensional analysis method (Buckingham-Pi Theorem) has used to carry out the new formula for prediction of load capacity stone columns. Experimental data from two previous studies was used for analysis of study.

Vessel structural support system

DOEpatents

Jenko, James X.; Ott, Howard L.; Wilson, Robert M.; Wepfer, Robert M.

1992-01-01

Vessel structural support system for laterally and vertically supporting a vessel, such as a nuclear steam generator having an exterior bottom surface and a side surface thereon. The system includes a bracket connected to the bottom surface. A support column is pivotally connected to the bracket for vertically supporting the steam generator. The system also includes a base pad assembly connected pivotally to the support column for supporting the support column and the steam generator. The base pad assembly, which is capable of being brought to a level position by turning leveling nuts, is anchored to a floor. The system further includes a male key member attached to the side surface of the steam generator and a female stop member attached to an adjacent wall. The male key member and the female stop member coact to laterally support the steam generator. Moreover, the system includes a snubber assembly connected to the side surface of the steam generator and also attached to the adjacent wall for dampening lateral movement of the steam generator. In addition, the system includes a restraining member of "flat" attached to the side surface of the steam generator and a bumper attached to the adjacent wall. The flat and the bumper coact to further laterally support the steam generator.

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.

Determination of carotenoids in Taraxacum formosanum by HPLC-DAD-APCI-MS and preparation by column chromatography.

PubMed

Kao, T H; Loh, C H; Inbaraj, B Stephen; Chen, B H

2012-07-01

The objectives of this study were to determine the variety and content of carotenoids in Taraxacum formosanum, a traditional Chinese herb possessing vital biological activities, by developing an HPLC-DAD-APCI-MS method and a preparative column chromatographic method for carotenoid isolation. A total of 25 carotenoids were resolved within 66 min by employing a YMC C30 column and a gradient mobile phase of methanol-acetonitrile-water (79:14:7, v/v/v) and methylene chloride (100%) with flow rate at 1.0 mL/min and detection at 450 nm. All-trans-canthaxanthin was shown to be an appropriate internal standard for quantitation, with all-trans-β-carotene and its cis isomers present in largest amount (413.6 μg/g), followed by all-trans-violoxanthin and its cis isomers (209.5 μg/g), all-trans-lutein and its cis isomers (212.4 μg/g), all-trans-neoxanthin and its cis isomers (134.6 μg/g), antheraxanthin (16.5 μg/g), all-trans-β-cryptoxanthin and its cis isomers (5.8 μg/g), all-trans-zeaxanthin (3.6 μg/g) and neochrome (0.1 μg/g). For preparative chromatography, with a glass column containing 52 g of magnesium oxide-diatomaceous earth (1:3, w/w) as adsorbent, the carotenoid fraction was eluted with 300 mL of ethyl acetate with flow rate at 10 mL/min. Some more epoxides and cis isomers of carotenoids were generated during preparative column chromatography. Nevertheless, the carotenoids isolated from T. formosanum may be used as raw material for possible production of health food in the future. Copyright © 2012 Elsevier B.V. All rights reserved.

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

NASA Technical Reports Server (NTRS)

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

1995-01-01

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

Feasibility study of tuned liquid column damper for ocean wave energy extraction

NASA Astrophysics Data System (ADS)

Wong, Yihong; King, Yeong-Jin; Lai, An-Chow; Chong, Kok-Keong; Lim, Boon-Han

2017-04-01

Intermittent nature and low efficiency are the major issues in renewable energy supply. To overcome these issues, one of the possible methods is through a hybrid system where multiple sources of renewable energy are combined to compensate each other's weaknesses. The hybrid of solar energy and wave energy becomes possible through the introduction of a stable floating platform which enables solar energy generation above it and wave energy harvesting underneath it. This paper is intended to study the feasibility of harnessing ocean wave energy using a tuned liquid column damper (TLCD), a type of passive damping device that is designed to suppress externally induced vibration force at a specific frequency range. The proposed TLCD is to be implemented within a floating offshore structure to serve as a vibration mitigating mechanism by reducing the dynamic response of the structure and simultaneously utilize the flowing motion of liquid within the TLCD for generating electricity. The constructed TLCD prototype is tuned according to theoretical study and tested using a shaking table with a predetermined frequency range. The oscillating motion of water within the TLCD and the potential of installation of hydro turbine generator in term of recoverable amount of energy are studied.

Adaptive low-rank subspace learning with online optimization for robust visual tracking.

PubMed

Liu, Risheng; Wang, Di; Han, Yuzhuo; Fan, Xin; Luo, Zhongxuan

2017-04-01

In recent years, sparse and low-rank models have been widely used to formulate appearance subspace for visual tracking. However, most existing methods only consider the sparsity or low-rankness of the coefficients, which is not sufficient enough for appearance subspace learning on complex video sequences. Moreover, as both the low-rank and the column sparse measures are tightly related to all the samples in the sequences, it is challenging to incrementally solve optimization problems with both nuclear norm and column sparse norm on sequentially obtained video data. To address above limitations, this paper develops a novel low-rank subspace learning with adaptive penalization (LSAP) framework for subspace based robust visual tracking. Different from previous work, which often simply decomposes observations as low-rank features and sparse errors, LSAP simultaneously learns the subspace basis, low-rank coefficients and column sparse errors to formulate appearance subspace. Within LSAP framework, we introduce a Hadamard production based regularization to incorporate rich generative/discriminative structure constraints to adaptively penalize the coefficients for subspace learning. It is shown that such adaptive penalization can significantly improve the robustness of LSAP on severely corrupted dataset. To utilize LSAP for online visual tracking, we also develop an efficient incremental optimization scheme for nuclear norm and column sparse norm minimizations. Experiments on 50 challenging video sequences demonstrate that our tracker outperforms other state-of-the-art methods. Copyright © 2017 Elsevier Ltd. All rights reserved.

Atom counting in HAADF STEM using a statistical model-based approach: methodology, possibilities, and inherent limitations.

PubMed

De Backer, A; Martinez, G T; Rosenauer, A; Van Aert, S

2013-11-01

In the present paper, a statistical model-based method to count the number of atoms of monotype crystalline nanostructures from high resolution high-angle annular dark-field (HAADF) scanning transmission electron microscopy (STEM) images is discussed in detail together with a thorough study on the possibilities and inherent limitations. In order to count the number of atoms, it is assumed that the total scattered intensity scales with the number of atoms per atom column. These intensities are quantitatively determined using model-based statistical parameter estimation theory. The distribution describing the probability that intensity values are generated by atomic columns containing a specific number of atoms is inferred on the basis of the experimental scattered intensities. Finally, the number of atoms per atom column is quantified using this estimated probability distribution. The number of atom columns available in the observed STEM image, the number of components in the estimated probability distribution, the width of the components of the probability distribution, and the typical shape of a criterion to assess the number of components in the probability distribution directly affect the accuracy and precision with which the number of atoms in a particular atom column can be estimated. It is shown that single atom sensitivity is feasible taking the latter aspects into consideration. © 2013 Elsevier B.V. All rights reserved.

Therapeutic drug monitoring of topiramate with a new HPLC method, SPE extraction and high sensitivity pre-column fluorescent derivatization.

PubMed

Bolner, Andreas; De Riva, Valentina; Galloni, Elisabetta; Perini, Francesco

2014-01-01

Topiramate is a 2nd generation antiepileptic drug (AED) recently approved by the FDA for migraine prophylaxis. Its pharmacological activity already appears significant at low doses. Unfortunately, the difficulty in determining the drug in serum at low concentrations hampers the completion of accurate pharmacokinetic studies in humans. Only chromatographic methods allow reaching the necessary sensitivities. Almost all of the HPLC methods proposed were based on the preliminary extraction of topiramate from the sample using organic solvents. In our study, the conditions for purifying topiramate through solid-liquid technique in disposable cartridges (SPE) packed with C18 reversed phase were examinated and optimised. After a pre-column derivatization step with 9-fluorenylmethyl chloroformate (FMOC-Cl) and internal standard addition, topiramate was analysed on a CN column with sodium phosphate buffer 50 mmol/L (pH 2.5) containing acetonitrile (60:40, v/v) as the mobile phase. The column effluent was monitored with a fluorescence detector (excitation and emission 1 260 and 315 nm, respectively). 122 samples from our routine laboratory work were analysed in order to confirm the existence of a relationship between topiramate dose and serum concentration and to evaluate the effect of concomitant therapies with enzyme-inducing AEDs. Sensitivity (2 ng/mL), precision (CV within assay of 3.8% and between assays of 6.6%), linearity and accuracy of the method were better than other analytical procedures previously reported. Serum topiramate levels in the group with enzyme-inducing AEDs showed a reduction with respect to the group with non-enzyme-inducing AEDs and the correlation between doses and mean serum concentration gives a linear trend (r2 = 0.916). The efficacy of SPE extraction together with the method's reliability proved very advantageous for pharmacokinetics studies and, in principle, for therapeutic drug monitoring and toxicological investigations.

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

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

PubMed

Laaniste, Asko; Kruve, Anneli; Leito, Ivo

2013-08-01

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

A simple and inexpensive on-column frit fabrication method for fused-silica capillaries for increased capacity and versatility in LC-MS/MS applications.

PubMed

Wang, Ling-Chi; Okitsu, Cindy Yen; Kochounian, Harold; Rodriguez, Anthony; Hsieh, Chih-Lin; Zandi, Ebrahim

2008-05-01

A modified sol-gel method for a one-step on-column frit preparation for fused-silica capillaries and its utility for peptide separation in LC-MS/MS is described. This method is inexpensive, reproducible, and does not require specialized equipments. Because the frit fabrication process does not damage polyimide coating, the frit-fabricated column can be tightly connected on-line for high pressure LC. These columns can replace any capillary liquid transfer tubing without any specialized connections up-stream of a spray tip column. Therefore multiple columns with different phases can be connected in series for one- or multiple-dimensional chromatography.

Automated Generation of 3D Volcanic Gas Plume Models for Geobrowsers

NASA Astrophysics Data System (ADS)

Wright, T. E.; Burton, M.; Pyle, D. M.

2007-12-01

A network of five UV spectrometers on Etna automatically gathers column amounts of SO2 during daylight hours. Near-simultaneous scans from adjacent spectrometers, comprising 210 column amounts in total, are then converted to 2D slices showing the spatial distribution of the gas by tomographic reconstruction. The trajectory of the plume is computed using an automatically-submitted query to NOAA's HYSPLIT Trajectory Model. This also provides local estimates of air temperature, which are used to determine the atmospheric stability and therefore the degree to which the plume is dispersed by turbulence. This information is sufficient to construct an animated sequence of models which show how the plume is advected and diffused over time. These models are automatically generated in the Collada Digital Asset Exchange format and combined into a single file which displays the evolution of the plume in Google Earth. These models are useful for visualising and predicting the shape and distribution of the plume for civil defence, to assist field campaigns and as a means of communicating some of the work of volcano observatories to the public. The Simultaneous Algebraic Reconstruction Technique is used to create the 2D slices. This is a well-known method, based on iteratively updating a forward model (from 2D distribution to column amounts). Because it is based on a forward model, it also provides a simple way to quantify errors.

Stability of column-supported embankments.

DOT National Transportation Integrated Search

2006-01-01

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

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

Mahmood, U; Dauer, L; Erdi, Y

Purpose: Our goal was to evaluate low contrast detectability (LCD) for abdominal CT protocols across two CT scanner manufacturers, while producing a similar noise texture and CTDIvol for acquired images. Methods: A CIRS tissue equivalent LCD phantom containing three columns of 7 spherical targets, ranging from 10 mm to 2.4 mm, that are 5, 10, and 20 HU below the background matrix (HUBB) was scanned using two a GE HD750 64 slice scanner and a Siemens Somatom Definition AS 64 slice scanner. Protocols were designed to deliver a CTDIvol of 12.26 mGy and images were reconstructed with FBP, ASIR andmore » Sapphire. Comparisons were made with those algorithms that had matching noise power spectrum peaks (NPS). NPS information was extracted from a previously published article that matched NPS peak frequencies across manufacturers by calculating the NPS from uniform phantom images reconstructed with several IR algorithms. Results: The minimum detectable lesion size in the 20 HUBB and 10 HUBB column was 6.3 mm, and 10 mm in the 5 HUBB column for the GE HD 750 scanner. The minimum detectable lesion size in the 20 HUBB column was 4.8 mm, in the 10 HUBB column, 9.5 mm, and the 5 HUBB column, 10 mm for the Siemens Somatom Definition AS. Conclusion: Reducing radiation dose while improving or maintaining LCD is possible with application of IR. However, there are several different IR algorithms, with each generating a different resolution and noise texture. In multi-manufacturer settings, matching only the CTDIvol between manufacturers may Result in a loss of clinically relevant information.« less

Study of axial mixing, holdup and slip velocity of dispersed phase in a pulsed sieve plate extraction column using radiotracer technique.

PubMed

Ghiyas Ud Din; Imran Rafiq Chughtai; Hameed Inayat, Mansoor; Hussain Khan, Iqbal

2009-01-01

Axial mixing, holdup and slip velocity of dispersed phase which are parameters of fundamental importance in the design and operation of liquid-liquid extraction pulsed sieve plate columns have been investigated. Experiments for residence time distribution (RTD) analysis have been carried out for a range of pulsation frequency and amplitude in a liquid-liquid extraction pulsed sieve plate column with water as dispersed and kerosene as continuous phase using radiotracer technique. The column was operated in emulsion region and (99m)Tc in the form of sodium pertechnetate eluted from a (99)Mo/(99m)Tc generator was used to trace the dispersed phase. Axial dispersed plug flow model with open-open boundary condition and two points measurement method was used to simulate the hydrodynamics of dispersed phase. It has been observed that the axial mixing and holdup of dispersed phase increases with increase in pulsation frequency and amplitude until a maximum value is achieved while slip velocity decreases with increase in pulsation frequency and amplitude until it approaches a minimum value. Short lived and low energy radiotracer (99m)Tc in the form of sodium pertechnetate was found to be a good water tracer to study the hydrodynamics of a liquid-liquid extraction pulsed sieve plate column operating with two immiscible liquids, water and kerosene. Axial dispersed plug flow model with open-open boundary condition was found to be a suitable model to describe the hydrodynamics of dispersed phase in the pulsed sieve plate extraction column.

Maximum Potential Hydrogen Gas Retention in the sRF Resin Ion Exchange Column for the LAWPS Process

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

Gauglitz, Phillip A.; Wells, Beric E.; Bottenus, Courtney LH

The Low-Activity Waste Pretreatment System (LAWPS) is being developed to provide treated supernatant liquid from the Hanford tank farms directly to the Low-Activity Waste (LAW) Vitrification Facility at the Hanford Tank Waste Treatment and Immobilization Plant. The design and development of the LAWPS is being conducted by Washington River Protection Solutions, LLC. A key process in LAWPS is the removal of radioactive Cs in ion exchange (IX) columns filled with spherical resorcinol-formaldehyde (sRF) resin. One accident scenario being evaluated is the loss of liquid flow through the sRF resin bed after it has been loaded with radioactive Cs and hydrogenmore » gas is being generated by radiolysis. In normal operations, the generated hydrogen is expected to remain dissolved in the liquid and be continuously removed by liquid flow. For an accident scenario with a loss of flow, hydrogen gas can be retained within the IX column both in the sRF resin and below the bottom screen that supports the resin within the column. The purpose of this report is to summarize calculations that estimate the upper-bound volume of hydrogen gas that can be retained in the column and potentially be released to the headspace of the IX column or to process equipment connected to the IX column and, thus, pose a flammability hazard.« less

Pumping bottom water to prevent Korean red tide damage caused by Cochlodinium polykrikoides Margalef.

PubMed

Cho, Eun Seob; Moon, Seong Yong; Shu, Young Sang; Hwang, Jae Dong; Youn, Seok Hyun

2015-09-01

Cochlodinium polykrikoides Margalef produces annual massive blooms in Korean coastal waters which cause great damage to aquaculture and fisheries. Although various methods have been developed to remove the red tide of C. polykrikoides, release of yellow loess has been regarded as the most desirable technique for mitigation for over 10 years. Each August, strong irradiation generates water column stratification separating warm surface from colder bottom waters. Water from a distance of 0 (St. 1), 5 (St. 2), 10 (St. 3), and 15 m (St. 4) was pumped by running a pump for 0, 10, 30 and 90 min and characterized water temperature, salinity collected, suspended solids, Chl-a, and phytoplankton including C. polykrikoides. After running for 30 min, was temperature and salinity in surface water was similar to those of bottom water, and water column stratification completely reversed after 90 min. Likewise, suspended solids, Chl-a, and total phytoplankton cell density decreased after 30 min, but C. polykrikoides did not show strong removal because of low cell density during sampling. However, the number of C. polykrikoides was significantly diluted (80%) after 90 min. These results suggested that pumping device was as an environmentally-friendly method convenient to be install in fish cages and effective to remove C. polykrikoides stratified water column conditions.

DEVELOPMENT AND APPLICATION OF IMMUNOAFFINITY COLUMN CHROMATOGRAPHY AS A CLEANUP METHOD FOR THE DETERMINATION OF ATRAZINE IN COMPLEX ENVIRONMENTAL SAMPLE MEDIA

EPA Science Inventory

A rabbit antibody immunoaffinity (IA) column procedure was evaluated as a cleanup method for the determination of atrazine in soil, sediment, and food. Four IA columns were prepared by immobilizing a polyclonal rabbit anti-atrazine antibody solution to HiTrap Sepharose columns. A...

Quasi-adiabatic vacuum-based column housing for very high-pressure liquid chromatography.

PubMed

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

2016-07-22

A prototype vacuum-based (10(-6)Torr) column housing was built to thermally isolate the chromatographic column from the external air environment. The heat transfer mechanism is solely controlled by surface radiation, which was minimized by wrapping the column with low-emissivity aluminum tape. The adiabaticity of the column housing was quantitatively assessed from the measurement of the operational pressure and fluid temperature at the outlet of a 2.1mm×100mm column (sub-2 μm particles). The pressure drop along the column was raised up to 1kbar. The enthalpy balance of the eluent (water, acetonitrile, and one water/acetonitrile mixture, 70/30, v/v) showed that less than 1% of the viscous heat generated by friction of the fluid against the packed bed was lost to the external air environment. Such a vacuum-based column oven minimizes the amplitude of the radial temperature gradients across the column diameter and maximizes its resolving power. Copyright © 2016 Elsevier B.V. All rights reserved.

Biomedical silver-109m isotope generator

DOEpatents

Wanek, Philip M.; Steinkruger, Frederick J.; Moody, David C.

1987-01-01

A method, composition of matter, and apparatus for producing substantially pure Ag-109m for use in biomedical imaging techniques. Cd-109, which decays with a half-life of 453 days to Ag-109m is loaded onto an ion exchange column consisting of particulate tin phosphate. After secular equilibrium is reached in about ten minutes, Ag-109m may be selectively eluted from the column by means of a physiologically acceptable aqueous buffered eluent solution of sodium thiosulfate, and either ascorbic acid or dextrose. The breakthrough of toxic Cd-109 is on the order of 1.times.10.sup.-7, which is sufficiently low to permit administration of the Ag-109m-containing eluate, with but a minor pH adjustment, directly to a human patient within a matter of seconds.

Biomedical silver-109m isotope generator

DOEpatents

Wanek, P.M.; Steinkruger, F.J.; Moody, D.C.

1985-03-05

A method, composition of matter, and apparatus for producing substantially pure Ag-109m for use in biomedical imaging techniques. Cd-109, which decays with a half-life of 453 days to Ag-109m, is loaded onto an ion exchange column consisting of particulate tin phosphate. After secular equilibrium is reached in about ten minutes, Ag-109m may be selectively eluted from the column by means of a physiologically acceptable aqueous buffered eluent solution of sodium thiosulfate, and either ascorbic acid or dextrose. The breakthrough of toxic Cd-109 is on the order of 1 x 10-7, which is sufficiently low to permit administration of the Ag-109m-containing eluate, with but a minor pH adjustment, directly to a human patient within a matter of seconds. 1 fig.

Reliability assessment of slender concrete columns at the stability failure

NASA Astrophysics Data System (ADS)

Valašík, Adrián; Benko, Vladimír; Strauss, Alfred; Täubling, Benjamin

2018-01-01

The European Standard for designing concrete columns within the use of non-linear methods shows deficiencies in terms of global reliability, in case that the concrete columns fail by the loss of stability. The buckling failure is a brittle failure which occurs without warning and the probability of its formation depends on the columns slenderness. Experiments with slender concrete columns were carried out in cooperation with STRABAG Bratislava LTD in Central Laboratory of Faculty of Civil Engineering SUT in Bratislava. The following article aims to compare the global reliability of slender concrete columns with slenderness of 90 and higher. The columns were designed according to methods offered by EN 1992-1-1 [1]. The mentioned experiments were used as basis for deterministic nonlinear modelling of the columns and subsequent the probabilistic evaluation of structural response variability. Final results may be utilized as thresholds for loading of produced structural elements and they aim to present probabilistic design as less conservative compared to classic partial safety factor based design and alternative ECOV method.

The formation of stable pH gradients with weak monovalent buffers for isoelectric focusing in free solution

NASA Technical Reports Server (NTRS)

Mosher, Richard A.; Thormann, Wolfgang; Graham, Aly; Bier, Milan

1985-01-01

Two methods which utilize simple buffers for the generation of stable pH gradients (useful for preparative isoelectric focusing) are compared and contrasted. The first employs preformed gradients comprised of two simple buffers in density-stabilized free solution. The second method utilizes neutral membranes to isolate electrolyte reservoirs of constant composition from the separation column. It is shown by computer simulation that steady-state gradients can be formed at any pH range with any number of components in such a system.

Generation of surface-wave microwave microplasmas in hollow-core photonic crystal fiber based on a split-ring resonator.

PubMed

Vial, Florian; Gadonna, Katell; Debord, Benoît; Delahaye, Frédéric; Amrani, Foued; Leroy, Olivier; Gérôme, Frédéric; Benabid, Fetah

2016-05-15

We report on a new and highly compact scheme for the generation and sustainment of microwave-driven plasmas inside the core of an inhibited coupling Kagome hollow-core photonic crystal fiber. The microwave plasma generator consists of a split-ring resonator that efficiently couples the microwave field into the gas-filled fiber. This coupling induces the concomitant generation of a microwave surface wave at the fiber core surround and a stable plasma column confined in the fiber core. The scheme allowed the generation of several centimeters long argon microplasma columns with a very low excitation power threshold. This result represents an important step toward highly compact plasma lasers or plasma-based photonic components.

Detecting gravesoil with headspace analysis with adsorption on short porous layer open tubular (PLOT) columns.

PubMed

Lovestead, Tara M; Bruno, Thomas J

2011-01-30

Victims of crimes are often buried in clandestine graves. There are several techniques for finding buried bodies or the scattered remains of a victim; however, none of these methods are very reliable or work in all scenarios. One way to detect gravesoil is to detect the biochemical changes of the surrounding soil due to cadaver decomposition, for example, the release of nitrogenous compounds. A simple and low-cost way to detect these compounds is based on the reaction of alpha amino groups with ninhydrin to form Ruhemann's purple. This test for ninhydrin-reactive nitrogen (NRN) has, to date, only been performed by direct solvent extraction of soil samples. Here, we present a method that detects trace quantities of NRN in the headspace air above gravesoil. Our method is based on an improved purge and trap method developed in our lab for sampling low volatility compounds, as well as volatile compounds at trace quantities, by applying low temperature collection on short alumina-coated porous layer open tubular (PLOT) columns. We modified this method to sample the headspace air above gravesoil with a motorized pipetter and a PLOT column at ambient temperatures. We generated gravesoil using rat cadavers and local soil. Trace quantities of NRN were successfully detected in the headspace air above gravesoil. We report the quantities of NRN recovered for buried rats, rats laid on top of soil, and blank graves (no rats) as a function of time (weeks to months). This work is the first (and thus far, only) example of a method for detecting NRN in the vapor phase, providing another tool for forensic investigators to aid in locating elusive clandestine graves. Published by Elsevier Ireland Ltd.

Volatile Transport by Volcanic Plumes on Earth, Venus and Mars

NASA Technical Reports Server (NTRS)

Glaze, Lori S.; Self, Stephen; Baloga, Steve; Stofan, Ellen R.

2012-01-01

Explosive volcanic eruptions can produce sustained, buoyant columns of ash and gas in the atmosphere (Fig. 1). Large flood basalt eruptions may also include significant explosive phases that generate eruption columns. Such eruptions can transport volcanic volatiles to great heights in the atmosphere. Volcanic eruption columns can also redistribute chemical species within the atmosphere by entraining ambient atmosphere at low altitudes and releasing those species at much higher altitudes.

Transferring research data to producers

USDA-ARS?s Scientific Manuscript database

A column will be written for Cow Country News, a monthly newspaper published by the Kentucky Cattlemen Association. The column will present research findings and technologies generated by collaborative research between the USDA-ARS Forage-Animal Production Research Unit and the University of Kentuc...

Apparatus for the separation of hydrophobic and hydrophilic particles using microbubble column flotation together with a process and apparatus for generation of microbubbles

DOEpatents

Yoon, Roe-Hoan; Adel, Gregory T.; Luttrell, Gerald H.

1995-01-01

An apparatus is disclosed for the microbubble flotation separation of very fine and coarse particles, especially coal, and minerals so as to produce high purity and high recovery efficiency. This is accomplished through the use of a flotation column, microbubbles, recycling of the flotation pulp, and countercurrent wash water to gently wash the froth. Also disclosed are unique processes and apparatus for generating microbubbles for flotation in a highly efficient and inexpensive manner using either a porous tube or in-line static generators.

Apparatus for the separation of hydrophobic and hydrophilic particles using microbubble column flotation together with a process and apparatus for generation of microbubbles

DOEpatents

Yoon, R.H.; Adel, G.T.; Luttrell, G.H.

1995-03-14

An apparatus is disclosed for the microbubble flotation separation of very fine and coarse particles, especially coal, and minerals so as to produce high purity and high recovery efficiency. This is accomplished through the use of a flotation column, microbubbles, recycling of the flotation pulp, and countercurrent wash water to gently wash the froth. Also disclosed are unique processes and apparatus for generating microbubbles for flotation in a highly efficient and inexpensive manner using either a porous tube or in-line static generators. 14 figs.

Single fiber lignin distributions based on the density gradient column method

Treesearch

Brian Boyer; Alan W. Rudie

2007-01-01

The density gradient column method was used to determine the effects of uniform and non-uniform pulping processes on variation in individual fiber lignin concentrations of the resulting pulps. A density gradient column uses solvents of different densities and a mixing process to produce a column of liquid with a smooth transition from higher density at the bottom to...

Ultrafast treatment plan optimization for volumetric modulated arc therapy (VMAT).

PubMed

Men, Chunhua; Romeijn, H Edwin; Jia, Xun; Jiang, Steve B

2010-11-01

To develop a novel aperture-based algorithm for volumetric modulated are therapy (VMAT) treatment plan optimization with high quality and high efficiency. The VMAT optimization problem is formulated as a large-scale convex programming problem solved by a column generation approach. The authors consider a cost function consisting two terms, the first enforcing a desired dose distribution and the second guaranteeing a smooth dose rate variation between successive gantry angles. A gantry rotation is discretized into 180 beam angles and for each beam angle, only one MLC aperture is allowed. The apertures are generated one by one in a sequential way. At each iteration of the column generation method, a deliverable MLC aperture is generated for one of the unoccupied beam angles by solving a subproblem with the consideration of MLC mechanic constraints. A subsequent master problem is then solved to determine the dose rate at all currently generated apertures by minimizing the cost function. When all 180 beam angles are occupied, the optimization completes, yielding a set of deliverable apertures and associated dose rates that produce a high quality plan. The algorithm was preliminarily tested on five prostate and five head-and-neck clinical cases, each with one full gantry rotation without any couch/collimator rotations. High quality VMAT plans have been generated for all ten cases with extremely high efficiency. It takes only 5-8 min on CPU (MATLAB code on an Intel Xeon 2.27 GHz CPU) and 18-31 s on GPU (CUDA code on an NVIDIA Tesla C1060 GPU card) to generate such plans. The authors have developed an aperture-based VMAT optimization algorithm which can generate clinically deliverable high quality treatment plans at very high efficiency.

Seismic, satellite, and site observations of internal solitary waves in the NE South China Sea

PubMed Central

Tang, Qunshu; Wang, Caixia; Wang, Dongxiao; Pawlowicz, Rich

2014-01-01

Internal solitary waves (ISWs) in the NE South China Sea (SCS) are tidally generated at the Luzon Strait. Their propagation, evolution, and dissipation processes involve numerous issues still poorly understood. Here, a novel method of seismic oceanography capable of capturing oceanic finescale structures is used to study ISWs in the slope region of the NE SCS. Near-simultaneous observations of two ISWs were acquired using seismic and satellite imaging, and water column measurements. The vertical and horizontal length scales of the seismic observed ISWs are around 50 m and 1–2 km, respectively. Wave phase speeds calculated from seismic observations, satellite images, and water column data are consistent with each other. Observed waveforms and vertical velocities also correspond well with those estimated using KdV theory. These results suggest that the seismic method, a new option to oceanographers, can be further applied to resolve other important issues related to ISWs. PMID:24948180

Silver Nanoscale Hexagonal Column Chips for Detecting Cell-free DNA and Circulating Nucleosomes in Cancer Patients.

PubMed

Ito, Hiroaki; Hasegawa, Katsuyuki; Hasegawa, Yuuki; Nishimaki, Tadashi; Hosomichi, Kazuyoshi; Kimura, Satoshi; Ohba, Motoi; Yao, Hiroshi; Onimaru, Manabu; Inoue, Ituro; Inoue, Haruhiro

2015-05-21

Blood tests, which are commonly used for cancer screening, generally have low sensitivity. Here, we developed a novel rapid and simple method to generate silver nanoscale hexagonal columns (NHCs) for use in surface-enhanced Raman scattering (SERS). We reported that the intensity of SERS spectra of clinical serum samples obtained from gastrointestinal cancer patients is was significantly higher than that of SERS spectra of clinical serum samples obtained from non-cancer patients. We estimated the combined constituents on silver NHCs by using a field emission-type scanning electron microscope, Raman microscopes, and a 3D laser scanning confocal microscope. We obtained the Raman scattering spectra of samples of physically fractured cells and clinical serum. No spectra were obtained for chemically lysed cultured cells and DNA, RNA, and protein extracted from cultured cells. We believe that our method, which uses SERS with silver NHCs to detect circulating nucleosomes bound by methylated cell-free DNA, may be successfully implemented in blood tests for cancer screening.

Electro-osmotically driven liquid delivery method and apparatus

DOEpatents

Rakestraw, D.J.; Anex, D.S.; Yan, C.; Dadoo, R.; Zare, R.N.

1999-08-24

Method and apparatus are disclosed for controlling precisely the composition and delivery of liquid at sub-{micro}L/min flow rate. One embodiment of such a delivery system is an electro-osmotically driven gradient flow delivery system that generates dynamic gradient flows with sub-{micro}L/min flow rates by merging a plurality of electro-osmotic flows. These flows are delivered by a plurality of delivery arms attached to a mixing connector, where they mix and then flow into a receiving means, preferably a column. Each inlet of the plurality of delivery arms is placed in a corresponding solution reservoir. A plurality of independent programmable high-voltage power supplies is used to apply a voltage program to each of the plurality of solution reservoirs to regulate the electro-osmotic flow in each delivery arm. The electro-osmotic flow rates in the delivery arms are changed with time according to each voltage program to deliver the required gradient profile to the column. 4 figs.

Characteristics of SnO2-based 68Ge/68Ga generator and aspects of radiolabelling DOTA-peptides.

PubMed

de Blois, Erik; Sze Chan, Ho; Naidoo, Clive; Prince, Deidre; Krenning, Eric P; Breeman, Wouter A P

2011-02-01

PET scintigraphy with (68)Ga-labelled analogs is of increasing interest in Nuclear Medicine and performed all over the world. Here we report the characteristics of the eluate of SnO(2)-based (68)Ge/(68)Ga generators prepared by iThemba LABS (Somerset West, South Africa). Three purification and concentration techniques of the eluate for labelling DOTA-TATE and concordant SPE purifications were investigated. Characteristics of 4 SnO(2)-based generators (range 0.4-1 GBq (68)Ga in the eluate) and several concentration techniques of the eluate (HCl) were evaluated. The elution profiles of SnO(2)-based (68)Ge/(68)Ga generators were monitored, while [HCl] of the eluens was varied from 0.3-1.0 M. Metal ions and sterility of the eluate were determined by ICP. Fractionated elution and concentration of the (68)Ga eluate were performed using anion and cation exchange. Concentrated (68)Ga eluate, using all three concentration techniques, was used for labelling of DOTA-TATE. (68)Ga-DOTA-TATE-containing solution was purified and RNP increased by SPE, therefore also 11 commercially available SPE columns were investigated. The amount of elutable (68)Ga activity varies when the concentration of the eluens, HCl, was varied, while (68)Ge activity remains virtually constant. SnO(2)-based (68)Ge/(68)Ga generator elutes at 0.6 M HCl >100% of the (68)Ga activity at calibration time and ±75% after 300 days. Eluate at discharge was sterile and Endotoxins were <0.5 EU/mL, RNP was always <0.01%. Metal ions in the eluate were <10 ppm (in total). Highest desorption for anion purification was obtained with the 30 mg Oasis WAX column (>80%). Highest desorption for cation purification was obtained using a solution containing 90% acetone at increasing molarity of HCl, resulted in a (68)Ga desorption of 68±8%. With all (68)Ge/(68)Ga generators and for all 3 purification methods a SA up to 50 MBq/nmol with >95% incorporation (ITLC) and RCP (radiochemical purity) by HPLC ±90% could be achieved. Purification and concentration of the eluate with anion exchange has the benefit of more elutable (68)Ga with 1 M HCl as eluens. The additional washing step of the anion column with NaCl and ethanol, resulted in a lower and less variable [H(+)] in the eluate, and, as a result the pH in the reaction vial is better controlled, more constant, and less addition of buffer is required and concordant smaller reaction volumes. Desorption of (68)Ga-DOTA-TATE of SPE columns varied, highest desorption was obtained with Baker C(18) 100 mg (84%). Purification of (68)Ga-DOTA-TATE by SPE resulted in an RNP of <10(-4)%. Eluate of SnO(2)-based (68)Ge/(68)Ga generator, either by fractionated elution as by ion exchange can be used for labelling DOTA-peptides with (68)Ga at a SA of 50 MBq/nmol at >95% incorporation and a RCP of ±90%. SPE columns are very effective to increase RNP. Copyright © 2010 Elsevier Ltd. All rights reserved.

Log-odds sequence logos

PubMed Central

Yu, Yi-Kuo; Capra, John A.; Stojmirović, Aleksandar; Landsman, David; Altschul, Stephen F.

2015-01-01

Motivation: DNA and protein patterns are usefully represented by sequence logos. However, the methods for logo generation in common use lack a proper statistical basis, and are non-optimal for recognizing functionally relevant alignment columns. Results: We redefine the information at a logo position as a per-observation multiple alignment log-odds score. Such scores are positive or negative, depending on whether a column’s observations are better explained as arising from relatedness or chance. Within this framework, we propose distinct normalized maximum likelihood and Bayesian measures of column information. We illustrate these measures on High Mobility Group B (HMGB) box proteins and a dataset of enzyme alignments. Particularly in the context of protein alignments, our measures improve the discrimination of biologically relevant positions. Availability and implementation: Our new measures are implemented in an open-source Web-based logo generation program, which is available at http://www.ncbi.nlm.nih.gov/CBBresearch/Yu/logoddslogo/index.html. A stand-alone version of the program is also available from this site. Contact: altschul@ncbi.nlm.nih.gov Supplementary information: Supplementary data are available at Bioinformatics online. PMID:25294922

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.

Semiconductor radiation detector

DOEpatents

Bell, Zane W.; Burger, Arnold

2010-03-30

A semiconductor detector for ionizing electromagnetic radiation, neutrons, and energetic charged particles. The detecting element is comprised of a compound having the composition I-III-VI.sub.2 or II-IV-V.sub.2 where the "I" component is from column 1A or 1B of the periodic table, the "II" component is from column 2B, the "III" component is from column 3A, the "IV" component is from column 4A, the "V" component is from column 5A, and the "VI" component is from column 6A. The detecting element detects ionizing radiation by generating a signal proportional to the energy deposited in the element, and detects neutrons by virtue of the ionizing radiation emitted by one or more of the constituent materials subsequent to capture. The detector may contain more than one neutron-sensitive component.

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

NASA Technical Reports Server (NTRS)

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

1971-01-01

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

High-efficiency liquid chromatography on conventional columns and instrumentation by using temperature as a variable I. Experiments with 25 cm x 4.6 mm I.D., 5 microm ODS columns.

PubMed

Lestremau, François; Cooper, Andrew; Szucs, Roman; David, Frank; Sandra, Pat

2006-03-24

High plate numbers were obtained in conventional LC by coupling columns and by using temperature to reduce the viscosity of the mobile phase. At 80 degrees C up to eight columns of 25 cm x 4.6 mm I.D. packed with 5 microm ODS particles could be coupled generating 180,000 effective plates while the pressure drop was only 350bar. For routine work, a set of four columns is preferred. The analysis times on one column operated at 30 degrees C and 1 mL/min flow rate and on four columns at 80 degrees C and 2 mL/min flow rate are the same in isoeluotropic conditions while the resolution is doubled. Multicolumn systems were successfully applied in isocratic and gradient mode for the analysis of pharmaceutical and environmental samples.

Magnetic isolation of Plasmodium falciparum schizonts iRBCs to generate a high parasitaemia and synchronized in vitro culture.

PubMed

Mata-Cantero, Lydia; Lafuente, Maria J; Sanz, Laura; Rodriguez, Manuel S

2014-03-21

The establishment of methods for an in vitro continuous culture of Plasmodium falciparum is essential for gaining knowledge into its biology and for the development of new treatments. Previously, several techniques have been used to synchronize, enrich and concentrate P. falciparum, although obtaining cultures with high parasitaemia continues being a challenging process. Current methods produce high parasitaemia levels of synchronized P. falciparum cultures by frequent changes of culture medium or reducing the haematocrit. However, these methods are time consuming and sometimes lead to the loss of synchrony. A procedure that combines Percoll and sorbitol treatments, the use of magnetic columns, and the optimization of the in vitro culture conditions to reach high parasitaemia levels for synchronized Plasmodium falciparum cultures is described. A new procedure has been established using P. falciparum 3D7, combining previous reported methodologies to achieve in vitro parasite cultures that reach parasitaemia up to 40% at any intra-erythrocytic stage. High parasitaemia levels are obtained only one day after magnetic column purification without compromising the parasite viability and synchrony. The described procedure allows obtaining a large scale synchronized parasite culture at a high parasitaemia with less manipulations than other methods previously described.

Multi-location peak parking method: an important new tool for the study of mass transfer kinetics in liquid chromatography.

PubMed

Gritti, Fabrice; Guiochon, Georges

2011-02-18

The peak parking (PP) method probes the longitudinal diffusion coefficient of a compound at a single location along the chromatographic column. We extended to a so-called multi-location peak parking (MLPP) method, in which a large number of axial locations along the column are selected in order to check the validity of the conventional PP method and to reveal possible defaults in the structure of the packed bed or pitfalls of the PP and the MLPP methods. MLPP was applied to a series of HILIC columns, including a 5.0 μm Venusil, a 3.0 μm Luna-diol, three 2.7 μm Halo, and a 1.7 μm Kinetex columns. The results demonstrate that the MLPP method may reveal local heterogeneities in the axial diffusion of small retained low molecular weight compounds along the column. Most importantly, experiments show that the sample zone should not be parked in the entrance of the column (i.e., at <1/10 th of the column length). The abrupt drop in the flow rate considerably affects the peak shape and prevents scientists from using the conventional PP method. Practical solutions to cope with that problem are proposed and their success/failure are discussed. Copyright © 2010 Elsevier B.V. All rights reserved.

TEFLON BELLOWS PULSE GENERATORS FOR SOLVENT EXTRACTION PULSE COLUMNS

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

McCarthy, P.B.

1954-01-01

A Teflon bellows-type pulse generator is described which consists of two 3-in. nominal diameter Teflon bellows mounted on either end of a flanged spool piece and rigidly connected internally by a push rod so that the two of bellows move in tandem. The ends of the two bellows are closed by means of blind flanges. Tne spool piece is designed for insertion in a 6-in. diameter nozzle on a solvent extraction pulse column. The double bellows arrangement constitutes a safety feature to prevent loss of the column contents in the event of failure of the inner bellows in contact withmore » column solution. Failure of the inner bellows may be detected by a conductivity probe mounted in the air space inside of the double bellows assembly. Reciprocating motion is imcrank arm rigidly connected through a cross head and push rod to the face of the external bellows flange. The push rod is guided by means of linear ball bushings. Frequency variation over a range of 30 to 100 cycles/ min.was obtained by use of a Thymotrol-controlled electric motor to drive the crank arm. Variable stroke adjustment (0 to 1-in. range) was possible by adjustment of linkages on the crank arm. A load compensating spring was founnd desirable to counteract the thrust on the push rod resulting tom the static pressure at the bottom of the solvent extraction column. Without the spring, accelerated wear of the bearing on the crank arm occured. The pulse generator operated uneventfully for 1776 hours (6.61x lO/sup 6/ cycles) at a frequency of 62 cycles/min. and a bellows travel of l-in. (equivalent to a displacement of 1.6 in. in a 3-in. diam. column). (auth)« less

Influence of the gas-flow Reynolds number on a plasma column in a glass tube

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

Jin, Dong Jun; Uhm, Han S.; Cho, Guangsup

2013-08-15

Atmospheric-plasma generation inside a glass tube is influenced by gas stream behavior as described by the Reynolds number (Rn). In experiments with He, Ne, and Ar, the plasma column length increases with an increase in the gas flow rate under laminar flow characterized by Rn < 2000. The length of the plasma column decreases as the flow rate increases in the transition region of 2000 < Rn < 4000. For a turbulent flow beyond Rn > 4000, the length of the plasma column is short in front of the electrode, eventually leading to a shutdown.

Dynamic Pressure Calibration Standard

NASA Technical Reports Server (NTRS)

Schutte, P. C.; Cate, K. H.; Young, S. D.

1986-01-01

Vibrating columns of fluid used to calibrate transducers. Dynamic pressure calibration standard developed for calibrating flush diaphragm-mounted pressure transducers. Pressures up to 20 kPa (3 psi) accurately generated over frequency range of 50 to 1,800 Hz. System includes two conically shaped aluminum columns one 5 cm (2 in.) high for low pressures and another 11 cm (4.3 in.) high for higher pressures, each filled with viscous fluid. Each column mounted on armature of vibration exciter, which imparts sinusoidally varying acceleration to fluid column. Signal noise low, and waveform highly dependent on quality of drive signal in vibration exciter.

SILLi 1.0: a 1-D numerical tool quantifying the thermal effects of sill intrusions

NASA Astrophysics Data System (ADS)

Iyer, Karthik; Svensen, Henrik; Schmid, Daniel W.

2018-01-01

Igneous intrusions in sedimentary basins may have a profound effect on the thermal structure and physical properties of the hosting sedimentary rocks. These include mechanical effects such as deformation and uplift of sedimentary layers, generation of overpressure, mineral reactions and porosity evolution, and fracturing and vent formation following devolatilization reactions and the generation of CO2 and CH4. The gas generation and subsequent migration and venting may have contributed to several of the past climatic changes such as the end-Permian event and the Paleocene-Eocene Thermal Maximum. Additionally, the generation and expulsion of hydrocarbons and cracking of pre-existing oil reservoirs around a hot magmatic intrusion are of significant interest to the energy industry. In this paper, we present a user-friendly 1-D finite element method (FEM)-based tool, SILLi, which calculates the thermal effects of sill intrusions on the enclosing sedimentary stratigraphy. The model is accompanied by three case studies of sills emplaced in two different sedimentary basins, the Karoo Basin in South Africa and the Vøring Basin off the shore of Norway. An additional example includes emplacement of a dyke in a cooling pluton which forgoes sedimentation within a basin. Input data for the model are the present-day well log or sedimentary column with an Excel input file and include rock parameters such as thermal conductivity, total organic carbon (TOC) content, porosity and latent heats. The model accounts for sedimentation and burial based on a rate calculated by the sedimentary layer thickness and age. Erosion of the sedimentary column is also included to account for realistic basin evolution. Multiple sills can be emplaced within the system with varying ages. The emplacement of a sill occurs instantaneously. The model can be applied to volcanic sedimentary basins occurring globally. The model output includes the thermal evolution of the sedimentary column through time and the changes that take place following sill emplacement such as TOC changes, thermal maturity and the amount of organic and carbonate-derived CO2. The TOC and vitrinite results can be readily benchmarked within the tool to present-day values measured within the sedimentary column. This allows the user to determine the conditions required to obtain results that match observables and leads to a better understanding of metamorphic processes in sedimentary basins.

Internal waves interacting with particles in suspension

NASA Astrophysics Data System (ADS)

Micard, Diane

2016-04-01

Internal waves are produced as a consequence of the dynamic balance between buoy- ancy and gravity forces when a particle of fluid is vertically displaced in a stable stratified environment. Geophysical systems such as ocean and atmosphere are naturally stratified and therefore suitable for internal waves to propagate. Furthermore, these two environ- ments stock a vast amount of particles in suspension, which present a large spectrum of physical properties (size, density, shape), and can be organic, mineral or pollutant agents. Therefore, it is reasonable to expect that internal waves will have an active effect over the dynamics of these particles. In order to study the interaction of internal waves and suspended particles, an ide- alized experimental setup has been implemented. A linear stratification is produced in a 80×40×17 cm3 tank, in which two dimensional plane waves are created thanks to the inno- vative wave generator GOAL. In addition, a particle injector has been developed to produce a vertical column of particles within the fluid, displaying the same two-dimensional sym- metry as the waves. The particle injector allows to control the volumic fraction of particles and the size of the column. The presence of internal waves passing through the column of particles allowed to observe two main effects: The column oscillates around an equilibrium position (which is observed in both, the contours an the interior of the column), and the column is displaced as a whole. The column is displaced depending on the characteristics of the column, the gradient of the density, and the intensity and frequency of the wave. When displaced, the particles within the column are sucked towards the source of waves. The direction of the displacement of the column is explained by computing the effect of the Lagrangian drift generated by the wave over the time the particles stay in the wave beam before settling.

Speciation of inorganic selenium and selenoamino acids by an HPLC-UV-HG-AFS system.

PubMed

Ipolyi, I; Corns, W; Stockwell, P; Fodor, P

2001-01-01

For the on-line speciation of selenocystine (SeCys), selenomethionine (SeMet), selenoethionine (SeEt), selenite (Se(IV)) and selenate (Se(VI)), a high-performance liquid chromatography-UV irradiation-hydride generation-atomic fluorescence spectro- metric method is described. Separation was carried out on a conventional reversed-phase C18 column modified with didodecyl- dimethylammonium bromide with gradient elution applying two concentrations of ammonium acetate as the mobile phase. UV irradiation and hydride generation parameters were optimized. The obtained detection limits for SeCys, SeMet, SeEt, Se(IV) and Se(VI) were 0.31, 0.43, 0.7, 0.44 and 0.32 ng ml(-1), respectively, using a 100-microl loop. The method was tested with spiked mineral water and two volunteers' urine samples.

Speciation of inorganic selenium and selenoamino acids by an HPLC-UV-HG-AFS system

PubMed Central

Ipolyi, I.; Corns, W.; Stockwell, P.; Fodor, P.

2001-01-01

For the on-line speciation of selenocystine (SeCys), selenomethionine (SeMet), selenoethionine (SeEt), selenite (Se(IV)) and selenate (Se(VI)), a high-performance liquid chromatography-UV irradiation-hydride generation-atomic fluorescence spectro- metric method is described. Separation was carried out on a conventional reversed-phase C18 column modified with didodecyl- dimethylammonium bromide with gradient elution applying two concentrations of ammonium acetate as the mobile phase. UV irradiation and hydride generation parameters were optimized. The obtained detection limits for SeCys, SeMet, SeEt, Se(IV) and Se(VI) were 0.31, 0.43, 0.7, 0.44 and 0.32 ng ml−1, respectively, using a 100-wl loop. The method was tested with spiked mineral water and two volunteers' urine samples. PMID:18924707

Planar cell polarity signaling coordinates oriented cell division and cell rearrangement in clonally expanding growth plate cartilage.

PubMed

Li, Yuwei; Li, Ang; Junge, Jason; Bronner, Marianne

2017-10-10

Both oriented cell divisions and cell rearrangements are critical for proper embryogenesis and organogenesis. However, little is known about how these two cellular events are integrated. Here we examine the linkage between these processes in chick limb cartilage. By combining retroviral-based multicolor clonal analysis with live imaging, the results show that single chondrocyte precursors can generate both single-column and multi-column clones through oriented division followed by cell rearrangements. Focusing on single column formation, we show that this stereotypical tissue architecture is established by a pivot-like process between sister cells. After mediolateral cell division, N-cadherin is enriched in the post-cleavage furrow; then one cell pivots around the other, resulting in stacking into a column. Perturbation analyses demonstrate that planar cell polarity signaling enables cells to pivot in the direction of limb elongation via this N-cadherin-mediated coupling. Our work provides new insights into the mechanisms generating appropriate tissue architecture of limb skeleton.

Planar cell polarity signaling coordinates oriented cell division and cell rearrangement in clonally expanding growth plate cartilage

PubMed Central

Li, Yuwei; Li, Ang; Junge, Jason

2017-01-01

Both oriented cell divisions and cell rearrangements are critical for proper embryogenesis and organogenesis. However, little is known about how these two cellular events are integrated. Here we examine the linkage between these processes in chick limb cartilage. By combining retroviral-based multicolor clonal analysis with live imaging, the results show that single chondrocyte precursors can generate both single-column and multi-column clones through oriented division followed by cell rearrangements. Focusing on single column formation, we show that this stereotypical tissue architecture is established by a pivot-like process between sister cells. After mediolateral cell division, N-cadherin is enriched in the post-cleavage furrow; then one cell pivots around the other, resulting in stacking into a column. Perturbation analyses demonstrate that planar cell polarity signaling enables cells to pivot in the direction of limb elongation via this N-cadherin-mediated coupling. Our work provides new insights into the mechanisms generating appropriate tissue architecture of limb skeleton. PMID:28994649

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.

Method for making a non-extractable stationary phase of polymer within a capillary column

DOEpatents

Springston, Stephen R.

1990-01-01

A method for coating interior capillary column surfaces, or packing material of a packed column, used for gas chromatography, with a stationary polymer phase that is cross-linked by exposing it to a low-temperature plasma that is uniformly distributed over the column or packing material for a predetermined period of time to effect the desired degree of cross-linking of the coating.

A standardized method for the calibration of thermodynamic data for the prediction of gas chromatographic retention times.

PubMed

McGinitie, Teague M; Ebrahimi-Najafabadi, Heshmatollah; Harynuk, James J

2014-02-21

A new method for calibrating thermodynamic data to be used in the prediction of analyte retention times is presented. The method allows thermodynamic data collected on one column to be used in making predictions across columns of the same stationary phase but with varying geometries. This calibration is essential as slight variances in the column inner diameter and stationary phase film thickness between columns or as a column ages will adversely affect the accuracy of predictions. The calibration technique uses a Grob standard mixture along with a Nelder-Mead simplex algorithm and a previously developed model of GC retention times based on a three-parameter thermodynamic model to estimate both inner diameter and stationary phase film thickness. The calibration method is highly successful with the predicted retention times for a set of alkanes, ketones and alcohols having an average error of 1.6s across three columns. Copyright © 2014 Elsevier B.V. All rights reserved.

An Excel macro for generating trilinear plots.

PubMed

Shikaze, Steven G; Crowe, Allan S

2007-01-01

This computer note describes a method for creating trilinear plots in Microsoft Excel. Macros have been created in MS Excel's internal language: Visual Basic for Applications (VBA). A simple form has been set up to allow the user to input data from an Excel worksheet. The VBA macro is used to convert the triangular data (which consist of three columns of percentage data) into X-Y data. The macro then generates the axes, labels, and grid for the trilinear plot. The X-Y data are plotted as scatter data in Excel. By providing this macro in Excel, users can create trilinear plots in a quick, inexpensive manner.

Two-dimensional ion chromatography for the separation of ionic organophosphates generated in thermally decomposed lithium hexafluorophosphate-based lithium ion battery electrolytes.

PubMed

Kraft, Vadim; Grützke, Martin; Weber, Waldemar; Menzel, Jennifer; Wiemers-Meyer, Simon; Winter, Martin; Nowak, Sascha

2015-08-28

A two-dimensional ion chromatography (IC/IC) technique with heart-cutting mode for the separation of ionic organophosphates was developed. These analytes are generated during thermal degradation of three different commercially available Selectilyte™ lithium ion battery electrolytes. The composition of the investigated electrolytes is based on 1M lithium hexafluorophosphate (LiPF6) dissolved in ethylene carbonate/dimethyl carbonate (50:50wt%, LP30), ethylene carbonate/diethyl carbonate (50:50wt%, LP40) and ethylene carbonate/ethyl methyl carbonate (50:50wt%, LP50). The organophosphates were pre-separated from PF6(-) anion on the low capacity A Supp 4 column, which was eluted with a gradient step containing acetonitrile. The fraction containing analytes was retarded on a pre-concentration column and after that transferred to the high capacity columns, where the separation was performed isocratically. Different stationary phases and eluents were applied on the 2nd dimension for the investigation of retention times, whereas the highly promising results were obtained with a high capacitive A Supp 10 column. The organophosphates generated in LP30 and LP40 electrolytes could be separated by application of an aqueous NaOH eluent providing fast analysis time within 35min. For the separation of the organophosphates of LP50 electrolyte due to its complexity a NaOH eluent containing a mixture of methanol/H2O was necessary. In addition, the developed two dimensional IC method was hyphenated to an inductively coupled plasma mass spectrometer (ICP-MS) using aqueous NaOH without organic modifiers. This proof of principle measurement was carried out for future quantitative investigation regarding the concentration of the ionic organophosphates. Furthermore, the chemical stability of several ionic organophosphates in water and acetonitrile at room temperature over a period of 10h was investigated. In both solvents no decomposition of the investigated analytes was observed and therefore water as solvent for dilution of samples was proved as suitable. Copyright © 2015 Elsevier B.V. All rights reserved.

Three-dimensional elastic wave analysis of the October 2, 2004 tremor at Mount St. Helens, Washington.

NASA Astrophysics Data System (ADS)

Denlinger, R. P.

2006-12-01

On October 2, 2004, three component, broad-frequency band seismometers as far as 250 km away from Mount St. Helens volcano detected a prominent low-frequency resonance associated with the onset of eruptive volcanic activity. The energy is dominantly in the 0.5 to 10 Hz range. Since gas emissions were low, I investigate a gas-free tremor mechanism generated by sudden extension of a pressurized, cylindrical, visco- elastic magma conduit beneath the mountain as it forces its way through a brittle crust. The concept is that rapid faulting of the crust around and above the magma results in a sudden drop in resistance and, consequently, a concurrent extension of the magma in the magma column at a rate greater than magma can resupply the column. The result is a rapid pressure drop in the magma, causing the column to oscillate and radiate elastic energy into the surrounding crust. The full wavefield generated by this physical mechanism is analyzed using the finite volume method of Leveque (2002), with the approximation outlined in Langseth and Leveque (2000) for hyperbolic conservation laws. In this method, the three-dimensional equations of elasticity are written as a first order set of conservation equations, with a solution vector composed of 3 velocity components and 6 stress components. The eigenvectors of the jacobian matrices of these conservation equations are used in a fourth-order Taylors series expansion of the solution vector around a small increment in time. This method is robust, allows waves to cleanly propagate off of a finite computational grid, and includes surface and interface waves. The method also allows for extremely large contrasts in elastic moduli across internal boundaries in the grid, necessary to accommodate the large variations in rigidity between a hot, visco-elastic magma at depth and the Earth's crust. Analyzing the October 2, 2004 tremor observed at Johnson Ridge Observatory, 9 km north of the mountain, for pressure drop in a 10 km long conduit, I obtain 0.3 +/- .05 MPa, which is consistent with elastic analysis of crustal deformation around the mountain during this time period. Langseth, J.O., and R.J. LeVeque, 2000, A wave propagation method for 3D hyperbolic conservation laws, J. Comp. Phys., 165, 126-166. Leveque, R.J., 2002, Finite volume methods for hyperbolic problems, Cambridge U. Press, 558 p.

Countercurrent flow of supercritical anti-solvent in the production of pure xanthophylls from Nannochloropsis oculata.

PubMed

Cho, Yueh-Cheng; Wang, Yuan-Chuen; Shieh, Chwen-Jen; Lin, Justin Chun-Te; Chang, Chieh-Ming J; Han, Esther

2012-08-10

This study examined pilot scaled elution chromatography coupled with supercritical anti-solvent precipitation (using countercurrent flow) in generating zeaxanthin-rich particulates from a micro-algal species. Ultrasonic agitated acetone extract subjected to column fractionation successfully yielded a fraction containing 349.4 mg/g of zeaxanthin with a recovery of 85%. Subsequently, supercritical anti-solvent (SAS) precipitation of the column fraction at 150 bar and 343 K produced submicron-sized particulates with a concentration of 845.5mg/g of zeaxanthin with a recovery of 90%. Experimental results from a two-factor response surface method SAS precipitation indicated that purity, mean size and morphology of the precipitates were significantly affected by the flow type configuration, feed flow rate and injection time. Copyright © 2012 Elsevier B.V. All rights reserved.

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

NASA Astrophysics Data System (ADS)

Rahai, A. R.; Kazemi, S.

2008-10-01

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

Stationary phase deposition based on onium salts

DOEpatents

Wheeler, David R [Albuquerque, NM; Lewis, Patrick R [Albuquerque, NM; Dirk, Shawn M [Albuquerque, NM; Trudell, Daniel E [Albuquerque, NM

2008-01-01

Onium salt chemistry can be used to deposit very uniform thickness stationary phases on the wall of a gas chromatography column. In particular, the stationary phase can be bonded to non-silicon based columns, especially microfabricated metal columns. Non-silicon microfabricated columns may be manufactured and processed at a fraction of the cost of silicon-based columns. In addition, the method can be used to phase-coat conventional capillary columns or silicon-based microfabricated columns.

Hydrogen sulfide generation in simulated construction and demolition debris landfills: impact of waste composition.

PubMed

Yang, Kenton; Xu, Qiyong; Townsend, Timothy G; Chadik, Paul; Bitton, Gabriel; Booth, Matthew

2006-08-01

Hydrogen sulfide (H2S) generation in construction and demolition (C&D) debris landfills has been associated with the biodegradation of gypsum drywall. Laboratory research was conducted to observe H2S generation when drywall was codisposed with different C&D debris constituents. Two experiments were conducted using simulated landfill columns. Experiment 1 consisted of various combinations of drywall, wood, and concrete to determine the impact of different waste constituents and combinations on H2S generation. Experiment 2 was designed to examine the effect of concrete on H2S generation and migration. The results indicate that decaying drywall, even alone, leached enough sulfate ions and organic matter for sulfate-reducing bacteria (SRB) to generate large H2S concentrations as high as 63,000 ppmv. The codisposed wastes show some effect on H2S generation. At the end of experiment 1, the wood/drywall and drywall alone columns possessed H2S concentrations > 40,000 ppmv. Conversely, H2S concentrations were < 1 ppmv in those columns containing concrete. Concrete plays a role in decreasing H2S by increasing pH out of the range for SRB growth and by reacting with H2S. This study also showed that wood lowered H2S concentrations initially by decreasing leachate pH values. Based on the results, two possible control mechanisms to mitigate H2S generation in C&D debris landfills are suggested.

Method for making a non-extractable stationary phase of polymer within a capillary column

DOEpatents

Springston, S.R.

1990-10-30

A method is described for coating interior capillary column surfaces, or packing material of a packed column, used for gas chromatography, with a stationary polymer phase that is cross-linked by exposing it to a low-temperature plasma that is uniformly distributed over the column or packing material for a predetermined period of time to effect the desired degree of cross-linking of the coating. 7 figs.

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.

Characterization of retentivity of reversed phase liquid chromatography columns.

PubMed

Ying, P T; Dorsey, J G

1991-03-01

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

[Comparison of acetonitrile, ethanol and chromatographic column to eliminate high-abundance proteins in human serum].

PubMed

Li, Yin; Liao, Ming; He, Xiao; Zhou, Yi; Luo, Rong; Li, Hongtao; Wang, Yun; He, Min

2012-11-01

To compare the effects of acetonitrile precipitation, ethanol precipitation and multiple affinity chromatography column Human 14 removal to eliminate high-abundance proteins in human serum. Elimination of serum high-abundance proteins performed with acetonitrile precipitation, ethanol precipitation and multiple affinity chromatography column Human 14 removal. Bis-Tris Mini Gels electrophoresis and two-dimensional gel electrophoresis to detect the effect. Grey value analysis from 1-DE figure showed that after serum processed by acetonitrile method, multiple affinity chromatography column Human 14 removal method and ethanol method, the grey value of albumin changed into 157.2, 40.8 and 8.2 respectively from the original value of 19. 2-DE analysis results indicated that using multiple affinity chromatography column Human 14 method, the protein points noticeable increased by 137 compared to the original serum. After processed by acetonitrile method and ethanol method, the protein point reduced, but the low abundance protein point emerged. The acetonitrile precipitation could eliminate the vast majority of high abundance proteins in serum and gain more proteins of low molecular weight, ethanol precipitation could eliminate part of high abundance proteins in serum, but low abundance proteins less harvested, and multiple affinity chromatography column Human 14 method could effectively removed the high abundance proteins, and keep a large number of low abundance proteins.

The perils of pathogen discovery: origin of a novel parvovirus-like hybrid genome traced to nucleic acid extraction spin columns.

PubMed

Naccache, Samia N; Greninger, Alexander L; Lee, Deanna; Coffey, Lark L; Phan, Tung; Rein-Weston, Annie; Aronsohn, Andrew; Hackett, John; Delwart, Eric L; Chiu, Charles Y

2013-11-01

Next-generation sequencing was used for discovery and de novo assembly of a novel, highly divergent DNA virus at the interface between the Parvoviridae and Circoviridae. The virus, provisionally named parvovirus-like hybrid virus (PHV), is nearly identical by sequence to another DNA virus, NIH-CQV, previously detected in Chinese patients with seronegative (non-A-E) hepatitis. Although we initially detected PHV in a wide range of clinical samples, with all strains sharing ∼99% nucleotide and amino acid identity with each other and with NIH-CQV, the exact origin of the virus was eventually traced to contaminated silica-binding spin columns used for nucleic acid extraction. Definitive confirmation of the origin of PHV, and presumably NIH-CQV, was obtained by in-depth analyses of water eluted through contaminated spin columns. Analysis of environmental metagenome libraries detected PHV sequences in coastal marine waters of North America, suggesting that a potential association between PHV and diatoms (algae) that generate the silica matrix used in the spin columns may have resulted in inadvertent viral contamination during manufacture. The confirmation of PHV/NIH-CQV as laboratory reagent contaminants and not bona fide infectious agents of humans underscores the rigorous approach needed to establish the validity of new viral genomes discovered by next-generation sequencing.

Method for determination of aflatoxin M₁ in cheese and butter by HPLC using an immunoaffinity column.

PubMed

Sakuma, Hisako; Kamata, Yoichi; Sugita-Konishi, Yoshiko; Kawakami, Hiroshi

2011-01-01

A rapid, sensitive convenient method for determination of aflatoxin M₁ (AFM₁) in cheese and butter by HPLC was developed and validated. The method employs a safe extraction solution (mixture of acetonitrile, methanol and water) and an immunoaffinity column (IAC) for clean-up. Compared with the widely used method employing chloroform and a Florisil column, the IAC method has a short analytical time and there are no interference peaks. The limits of quantification (LOQ) of the IAC method were 0.12 and 0.14 µg/kg, while those of the Florisil column method were 0.47 and 0.23 µg/kg in cheese and buffer, respectively. The recovery and relative standard deviation (RSD) for cheese (spiked at 0.5 µg/kg) in the IAC method were 92% and 7%, respectively, while for the Florisil column method the corresponding values were 76% and 10%. The recovery and RSD for butter (spiked at 0.5 µg/kg) in the IAC method were 97% and 9%, and those in the Florisil method were 74% and 9%, respectively. In the IAC method, the values of in-house precision (n=2, day=5) of cheese and butter (spiked at 0.5 µg/kg) were 9% and 13%, respectively. The IAC method is superior to the Florisil column method in terms of safety, ease of handling, sensitivity and reliability. A survey of AFM₁ contamination in imported cheese and butter in Japan was conducted by the IAC method. AFM₁ was not detected in 60 samples of cheese and 30 samples of butter.

A LC/UV/Vis method for determination of cyanocobalamin in multivitamin dietary supplements with on-line sample clean-up

USDA-ARS?s Scientific Manuscript database

A HPLC-UV method using a two-column strategy with a switching valve for on-line sample clean-up was developed for the determination of cyanocobalamin (CN-CBL-vitamin B12, in dietary supplements. The method uses two columns, an Agilent Zorbax C8 (150 mm x 4.6 mm, 5 um particle) reversed-phase column...

Cellufine sulfate column chromatography as a simple, rapid, and effective method to purify dengue virus.

PubMed

Kanlaya, Rattiyaporn; Thongboonkerd, Visith

2016-08-01

Conventional method to purify/concentrate dengue virus (DENV) is time-consuming with low virus recovery yield. Herein, we applied cellufine sulfate column chromatography to purify/concentrate DENV based on the mimicry between heparan sulfate and DENV envelope protein. Comparative analysis demonstrated that this new method offered higher purity (as determined by less contamination of bovine serum albumin) and recovery yield (as determined by greater infectivity). Moreover, overall duration used for cellufine sulfate column chromatography to purify/concentrate DENV was approximately 1/20 of that of conventional method. Therefore, cellufine sulfate column chromatography serves as a simple, rapid, and effective alternative method for DENV purification/concentration. Copyright © 2016 Elsevier B.V. All rights reserved.

Leaching of heavy metals from E-waste in simulated landfill columns

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

Li Yadong; Richardson, Jay B.; Mark Bricka, R.

2009-07-15

In recent history the volume of electronic products purchased by consumers has dramatically escalated. As a result this has produced an ever-increasing electronic waste (E-waste) stream, which has generated concerns regarding the E-waste's potential for adversely impacting the environment. The leaching of toxic substances from obsolete personal computers (PCs) and cathode ray tubes (CRTs) of televisions and monitors, which are the most significant components in E-waste stream, was studied using landfill simulation in columns. Five columns were employed. One column served as a control which was filled with municipal solid waste (MSW), two columns were filled with a mixture ofmore » MSW and CRTs, and the other two were filled with MSW and computer components including printed wire boards, hard disc drives, floppy disc drives, CD/DVD drives, and power supply units. The leachate generated from the columns was monitored for toxic materials throughout the two-year duration of the study. Results indicate that lead (Pb) and various other heavy metals that were of environmental and health concern were not detected in the leachate from the simulators. When the samples of the solids were collected from underneath the E-waste in the columns and were analyzed, significant amount of Pb was detected. This indicates that Pb could readily leach from the E-waste, but was absorbed by the solids around the E-waste materials. While Pb was not observed in the leachate in this study, it is likely that the Pb would eventually enter the leachate after a long term transport.« less

D.C. - ARC plasma generator for nonequilibrium plasmachemical processes

NASA Astrophysics Data System (ADS)

Kvaltin, J.

1990-06-01

The analysis of conditions for generation of nonequilibrium plasma to plasmachemical processes is made and the design of d.c.-arc plasma generator on the base of integral criterion is suggested. The measurement of potentials on the plasma column of that generator is presented.

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

PubMed Central

Plenis, Alina; Rekowska, Natalia; Bączek, Tomasz

2016-01-01

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

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

PubMed

Plenis, Alina; Rekowska, Natalia; Bączek, Tomasz

2016-01-21

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

Multi-GPU implementation of a VMAT treatment plan optimization algorithm.

PubMed

Tian, Zhen; Peng, Fei; Folkerts, Michael; Tan, Jun; Jia, Xun; Jiang, Steve B

2015-06-01

Volumetric modulated arc therapy (VMAT) optimization is a computationally challenging problem due to its large data size, high degrees of freedom, and many hardware constraints. High-performance graphics processing units (GPUs) have been used to speed up the computations. However, GPU's relatively small memory size cannot handle cases with a large dose-deposition coefficient (DDC) matrix in cases of, e.g., those with a large target size, multiple targets, multiple arcs, and/or small beamlet size. The main purpose of this paper is to report an implementation of a column-generation-based VMAT algorithm, previously developed in the authors' group, on a multi-GPU platform to solve the memory limitation problem. While the column-generation-based VMAT algorithm has been previously developed, the GPU implementation details have not been reported. Hence, another purpose is to present detailed techniques employed for GPU implementation. The authors also would like to utilize this particular problem as an example problem to study the feasibility of using a multi-GPU platform to solve large-scale problems in medical physics. The column-generation approach generates VMAT apertures sequentially by solving a pricing problem (PP) and a master problem (MP) iteratively. In the authors' method, the sparse DDC matrix is first stored on a CPU in coordinate list format (COO). On the GPU side, this matrix is split into four submatrices according to beam angles, which are stored on four GPUs in compressed sparse row format. Computation of beamlet price, the first step in PP, is accomplished using multi-GPUs. A fast inter-GPU data transfer scheme is accomplished using peer-to-peer access. The remaining steps of PP and MP problems are implemented on CPU or a single GPU due to their modest problem scale and computational loads. Barzilai and Borwein algorithm with a subspace step scheme is adopted here to solve the MP problem. A head and neck (H&N) cancer case is then used to validate the authors' method. The authors also compare their multi-GPU implementation with three different single GPU implementation strategies, i.e., truncating DDC matrix (S1), repeatedly transferring DDC matrix between CPU and GPU (S2), and porting computations involving DDC matrix to CPU (S3), in terms of both plan quality and computational efficiency. Two more H&N patient cases and three prostate cases are used to demonstrate the advantages of the authors' method. The authors' multi-GPU implementation can finish the optimization process within ∼ 1 min for the H&N patient case. S1 leads to an inferior plan quality although its total time was 10 s shorter than the multi-GPU implementation due to the reduced matrix size. S2 and S3 yield the same plan quality as the multi-GPU implementation but take ∼4 and ∼6 min, respectively. High computational efficiency was consistently achieved for the other five patient cases tested, with VMAT plans of clinically acceptable quality obtained within 23-46 s. Conversely, to obtain clinically comparable or acceptable plans for all six of these VMAT cases that the authors have tested in this paper, the optimization time needed in a commercial TPS system on CPU was found to be in an order of several minutes. The results demonstrate that the multi-GPU implementation of the authors' column-generation-based VMAT optimization can handle the large-scale VMAT optimization problem efficiently without sacrificing plan quality. The authors' study may serve as an example to shed some light on other large-scale medical physics problems that require multi-GPU techniques.

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

PubMed Central

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

2011-01-01

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

SO2 columns over China: Temporal and spatial variations using OMI and GOME-2 observations

NASA Astrophysics Data System (ADS)

Huanhuan, Yan; Liangfu, Chen; Lin, Su; Jinhua, Tao; Chao, Yu

2014-03-01

Enhancements of SO2 column amounts due to anthropogenic emission sources over China were shown in this paper by using OMI and GOME-2 observations. The temporal and spatial variations of SO2 columns over China were analyzed for the time period 2005-2010. Beijing and Chongqing showed a high concentration in the SO2 columns, attributable to the use of coal for power generation in China and the characteristic of terrain and meteorology. The reduction of SO2 columns over Beijing and surrounding provinces in 2008 was observed by OMI, which confirms the effectiveness of strict controls on pollutant emissions and motor vehicle traffic before and during 2008 Olympic and Paralympic Games. The SO2 columns over China from GOME-2 (0.2-0.5 DU) were lower than those from OMI (0.6-1 DU), but both showed a decrease in SO2 columns over northern China since 2008 (except an increase in OMI SO2 in 2010).

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

NASA Technical Reports Server (NTRS)

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

1971-01-01

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

Tropical intercontinental optical measurement network of aerosol, precipitable water and total column ozone

NASA Technical Reports Server (NTRS)

Holben, B. N.; Tanre, D.; Reagan, J. A.; Eck, T. F.; Setzer, A.; Kaufman, Y. A.; Vermote, E.; Vassiliou, G. D.; Lavenu, F.

1992-01-01

A new generation of automatic sunphotometers is used to systematically monitor clear sky total column aerosol concentration and optical properties, precipitable water and total column ozone diurnally and annually in West Africa and South America. The instruments are designed to measure direct beam sun, solar aureole and sky radiances in nine narrow spectral bands from the UV to the near infrared on an hourly basis. The instrumentation and the algorithms required to reduce the data for subsequent analysis are described.

Surfactant-induced flow compromises determination of air-water interfacial areas by surfactant miscible-displacement.

PubMed

Costanza-Robinson, Molly S; Henry, Eric J

2017-03-01

Surfactant miscible-displacement (SMD) column experiments are used to measure air-water interfacial area (A I ) in unsaturated porous media, a property that influences solute transport and phase-partitioning. The conventional SMD experiment results in surface tension gradients that can cause water redistribution and/or net drainage of water from the system ("surfactant-induced flow"), violating theoretical foundations of the method. Nevertheless, the SMD technique is still used, and some suggest that experimental observations of surfactant-induced flow represent an artifact of improper control of boundary conditions. In this work, we used numerical modeling, for which boundary conditions can be perfectly controlled, to evaluate this suggestion. We also examined the magnitude of surfactant-induced flow and its impact on A I measurement during multiple SMD flow scenarios. Simulations of the conventional SMD experiment showed substantial surfactant-induced flow and consequent drainage of water from the column (e.g., from 75% to 55% S W ) and increases in actual A I of up to 43%. Neither horizontal column orientation nor alternative boundary conditions resolved surfactant-induced flow issues. Even for simulated flow scenarios that avoided surfactant-induced drainage of the column, substantial surfactant-induced internal water redistribution occurred and was sufficient to alter surfactant transport, resulting in up to 23% overestimation of A I . Depending on the specific simulated flow scenario and data analysis assumptions used, estimated A I varied by nearly 40% and deviated up to 36% from the system's initial A I . We recommend methods for A I determination that avoid generation of surface-tension gradients and urge caution when relying on absolute A I values measured via SMD. Copyright © 2016 Elsevier Ltd. All rights reserved.

A two-column formalism for time-dependent modelling of stellar convection. I. Description of the method

NASA Astrophysics Data System (ADS)

Stökl, A.

2008-11-01

Context: In spite of all the advances in multi-dimensional hydrodynamics, investigations of stellar evolution and stellar pulsations still depend on one-dimensional computations. This paper devises an alternative to the mixing-length theory or turbulence models usually adopted in modelling convective transport in such studies. Aims: The present work attempts to develop a time-dependent description of convection, which reflects the essential physics of convection and that is only moderately dependent on numerical parameters and far less time consuming than existing multi-dimensional hydrodynamics computations. Methods: Assuming that the most extensive convective patterns generate the majority of convective transport, the convective velocity field is described using two parallel, radial columns to represent up- and downstream flows. Horizontal exchange, in the form of fluid flow and radiation, over their connecting interface couples the two columns and allows a simple circulating motion. The main parameters of this convective description have straightforward geometrical meanings, namely the diameter of the columns (corresponding to the size of the convective cells) and the ratio of the cross-section between up- and downdrafts. For this geometrical setup, the time-dependent solution of the equations of radiation hydrodynamics is computed from an implicit scheme that has the advantage of being unaffected by the Courant-Friedrichs-Lewy time-step limit. This implementation is part of the TAPIR-Code (short for The adaptive, implicit RHD-Code). Results: To demonstrate the approach, results for convection zones in Cepheids are presented. The convective energy transport and convective velocities agree with expectations for Cepheids and the scheme reproduces both the kinetic energy flux and convective overshoot. A study of the parameter influence shows that the type of solution derived for these stars is in fact fairly robust with respect to the constitutive numerical parameters.

Comprehensive two-dimensional gas chromatography applied to illicit drug analysis.

PubMed

Mitrevski, Blagoj; Wynne, Paul; Marriott, Philip J

2011-11-01

Multidimensional gas chromatography (MDGC), and especially its latest incarnation--comprehensive two-dimensional gas chromatography (GC × GC)--have proved advantageous over and above classic one-dimensional gas chromatography (1D GC) in many areas of analysis by offering improved peak capacity, often enhanced sensitivity and, especially in the case of GC × GC, the unique feature of 'structured' chromatograms. This article reviews recent advances in MDGC and GC × GC in drug analysis with special focus on ecstasy, heroin and cocaine profiling. Although 1D GC is still the method of choice for drug profiling in most laboratories because of its simplicity and instrument availability, GC × GC is a tempting proposition for this purpose because of its ability to generate a higher net information content. Effluent refocusing due to the modulation (compression) process, combined with the separation on two 'orthogonal' columns, results in more components being well resolved and therefore being analytically and statistically useful to the profile. The spread of the components in the two-dimensional plots is strongly dependent on the extent of retention 'orthogonality' (i.e. the extent to which the two phases possess different or independent retention mechanisms towards sample constituents) between the two columns. The benefits of 'information-driven' drug profiling, where more points of reference are usually required for sample differentiation, are discussed. In addition, several limitations in application of MDGC in drug profiling, including data acquisition rate, column temperature limit, column phase orthogonality and chiral separation, are considered and discussed. Although the review focuses on the articles published in the last decade, a brief chronological preview of the profiling methods used throughout the last three decades is given.

Plasma column and nano-powder generation from solid titanium by localized microwaves in air

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

Popescu, Simona; Jerby, Eli, E-mail: jerby@eng.tau.ac.il; Meir, Yehuda

2015-07-14

This paper studies the effect of a plasma column ejected from solid titanium by localized microwaves in an ambient air atmosphere. Nanoparticles of titanium dioxide (titania) are found to be directly synthesized in this plasma column maintained by the microwave energy in the cavity. The process is initiated by a hotspot induced by localized microwaves, which melts the titanium substrate locally. The molten hotspot emits ionized titanium vapors continuously into the stable plasma column, which may last for more than a minute duration. The characterization of the dusty plasma obtained is performed in-situ by small-angle X-ray scattering (SAXS), optical spectroscopy,more » and microwave reflection analyses. The deposited titania nanoparticles are structurally and morphologically analyzed by ex-situ optical and scanning-electron microscope observations, and also by X-ray diffraction. Using the Boltzmann plot method combined with the SAXS results, the electron temperature and density in the dusty plasma are estimated as ∼0.4 eV and ∼10{sup 19 }m{sup −3}, respectively. The analysis of the plasma product reveals nanoparticles of titania in crystalline phases of anatase, brookite, and rutile. These are spatially arranged in various spherical, cubic, lamellar, and network forms. Several applications are considered for this process of titania nano-powder production.« less

Electrodic voltages in the presence of dissolved sulfide: Implications for monitoring natural microbial activity

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

Slater, L.; Ntarlagiannis, D.; Yee, N.

2008-10-01

There is growing interest in the development of new monitoring strategies for obtaining spatially extensive data diagnostic of microbial processes occurring in the earth. Open-circuit potentials arising from variable redox conditions in the fluid local-to-electrode surfaces (electrodic potentials) were recorded for a pair of silver-silver chloride electrodes in a column experiment, whereby a natural wetland soil containing a known community of sulfate reducers was continuously fed with a sulfate-rich nutrient medium. Measurements were made between five electrodes equally spaced along the column and a reference electrode placed on the column inflow. The presence of a sulfate reducing microbial population, coupledmore » with observations of decreasing sulfate levels, formation of black precipitate (likely iron sulfide),elevated solid phase sulfide, and a characteristic sulfurous smell, suggest microbial-driven sulfate reduction (sulfide generation) in our column. Based on the known sensitivity of a silver electrode to dissolved sulfide concentration, we interpret the electrodic potentials approaching 700 mV recorded in this experiment as an indicator of the bisulfide (HS-) concentration gradients in the column. The measurement of the spatial and temporal variation in these electrodic potentials provides a simple and rapid method for monitoring patterns of relative HS- concentration that are indicative of the activity of sulfate-reducing bacteria. Our measurements have implications both for the autonomous monitoring of anaerobic microbial processes in the subsurface and the performance of self-potential electrodes, where it is critical to isolate, and perhaps quantify, electrochemical interfaces contributing to observed potentials.« less

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

PubMed

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

2016-03-01

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

Optimized fractional cloudiness determination from five ground-based remote sensing techniques

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

Boers, R.; de Haij, M. J.; Wauben, W.M.F.

2010-12-23

A one-year record of fractional cloudiness at 10 minute intervals was generated for the Cabauw Experimental Site for Atmospheric Research [CESAR] (51°58’N, 4° 55’E) using an integrated assessment of five different observational methods. The five methods are based on active as well as passive systems and use either a hemispheric or column remote sensing technique. The one-year instrumental cloudiness data were compared against a 30 year climatology of Observer data in the vicinity of CESAR [1971- 2000]. In the intermediate 2 - 6 octa range, most instruments, but especially the column methods, report lower frequency of occurrence of cloudiness thanmore » the absolute minimum values from the 30 year Observer climatology. At night, the Observer records less clouds in the 1, 2 octa range than during the day, while the instruments registered more clouds. During daytime the Observer also records much more 7 octa cloudiness than the instruments. One column method combining a radar with a lidar outstrips all other techniques in recording cloudiness, even up to height in excess of 9 km. This is mostly due to the high sensitivity of the radar that is used in the technique. A reference algorithm was designed to derive a continuous and optimized record of fractional cloudiness. Output from individual instruments were weighted according to the cloud base height reported at the observation time; the larger the height, the lower the weight. The algorithm was able to provide fractional cloudiness observations every 10 minutes for 98% of the total period of 12 months [15 May 2008 - 14 May 2009].« less

Finite Element Analysis of Increasing Column Section and CFRP Reinforcement Method under Different Axial Compression Ratio

NASA Astrophysics Data System (ADS)

Jinghai, Zhou; Tianbei, Kang; Fengchi, Wang; Xindong, Wang

2017-11-01

Eight less stirrups in the core area frame joints are simulated by ABAQUS finite element numerical software. The composite reinforcement method is strengthened with carbon fiber and increasing column section, the axial compression ratio of reinforced specimens is 0.3, 0.45 and 0.6 respectively. The results of the load-displacement curve, ductility and stiffness are analyzed, and it is found that the different axial compression ratio has great influence on the bearing capacity of increasing column section strengthening method, and has little influence on carbon fiber reinforcement method. The different strengthening schemes improve the ultimate bearing capacity and ductility of frame joints in a certain extent, composite reinforcement joints strengthening method to improve the most significant, followed by increasing column section, reinforcement method of carbon fiber reinforced joints to increase the minimum.

On Entropy Generation and the Effect of Heat and Mass Transfer Coupling in a Distillation Process

NASA Astrophysics Data System (ADS)

Burgos-Madrigal, Paulina; Mendoza, Diego F.; López de Haro, Mariano

2018-01-01

The entropy production rates as obtained from the exergy analysis, entropy balance and the nonequilibrium thermodynamics approach are compared for two distillation columns. The first case is a depropanizer column involving a mixture of ethane, propane, n-butane and n-pentane. The other is a weighed sample of Mexican crude oil distilled with a pilot scale fractionating column. The composition, temperature and flow profiles, for a given duty and operating conditions in each column, are obtained with the Aspen Plus V8.4 software by using the RateFrac model with a rate-based nonequilibrium column. For the depropanizer column the highest entropy production rate is found in the central trays where most of the mass transfer occurs, while in the second column the highest values correspond to the first three stages (where the vapor mixture is in contact with the cold liquid reflux), and to the last three stages (where the highest temperatures take place). The importance of the explicit inclusion of thermal diffusion in these processes is evaluated. In the depropanizer column, the effect of the coupling between heat and mass transfer is found to be negligible, while for the fractionating column it becomes appreciable.

Impact of NO2 horizontal heterogeneity on tropospheric NO2 vertical columns retrieved from satellite, multi-axis differential optical absorption spectroscopy, and in situ measurements

NASA Astrophysics Data System (ADS)

Mendolia, D.; D'Souza, R. J. C.; Evans, G. J.; Brook, J.

2013-01-01

Tropospheric NO2 vertical column densities were retrieved for the first time in Toronto, Canada using three methods of differing spatial scales. Remotely-sensed NO2 vertical column densities, retrieved from multi-axis differential optical absorption spectroscopy and satellite remote sensing, were evaluated by comparison with in situ vertical column densities derived using a pair of chemiluminescence monitors situated 0.01 and 0.5 km above ground level. The chemiluminescence measurements were corrected for the influence of NOz, which reduced the NO2 concentrations at 0.01 and 0.5 km by 8 ± 1% and 12 ± 1%, respectively. The average absolute decrease in the chemiluminescence NO2 measurement as a result of this correction was less than 1 ppb. Good correlation was observed between the remotely sensed and in situ NO2 vertical column densities (Pearson R ranging from 0.68 to 0.79), but the in situ vertical column densities were 27% to 55% greater than the remotely-sensed columns. These results indicate that NO2 horizontal heterogeneity strongly impacted the magnitude of the remotely-sensed columns. The in situ columns reflected an urban environment with major traffic sources, while the remotely-sensed NO2 vertical column densities were representative of the region, which included spatial heterogeneity introduced by residential neighbourhoods and Lake Ontario. Despite the difference in absolute values, the reasonable correlation between the vertical column densities determined by three distinct methods increased confidence in the validity of the values provided by each of the methods.

Systematic generation of buffer systems for pH gradient ion exchange chromatography and their application.

PubMed

Kröner, Frieder; Hubbuch, Jürgen

2013-04-12

pH gradient protein separations are widely used techniques in the field of protein analytics, of which isoelectric focusing is the most well known application. The chromatographic variant, based on the formation of pH gradients in ion exchange columns is only rarely applied due to the difficulties to form controllable, linear pH gradients over a broad pH range. This work describes a method for the systematic generation of buffer compositions with linear titration curves, resulting in well controllable pH gradients. To generate buffer compositions with linear titration curves an in silico method was successfully developed. With this tool, buffer compositions for pH gradient ion exchange chromatography with pH ranges spanning up to 7.5 pH units were established and successfully validated. Subsequently, the buffer systems were used to characterize the elution behavior of 22 different model proteins in cation and anion exchange pH gradient chromatography. The results of both chromatographic modes as well as isoelectric focusing were compared to describe differences in between the methods. Copyright © 2013 Elsevier B.V. All rights reserved.

The study on the extraction method of indirubin from Indigo Naturalis.

PubMed

Cheng, Li-hui

2007-01-01

To discuss how to extract the indirubin of the higher purity from Indigo Naturalis. After extracting the indirubin from Indigo Naturalis by acetic ether, compare the separation effect of the extract in Si gel column with that in alumina column. The indirubin in Indigo Naturalis by Si gel column chromatography is chosen. The purity of indirubin is 98.3% after Si gel column chromatography. The indiruhbin of the higher purity was attained by the simple experimental method.

On-line gas chromatographic analysis of airborne particles

DOEpatents

Hering, Susanne V [Berkeley, CA; Goldstein, Allen H [Orinda, CA

2012-01-03

A method and apparatus for the in-situ, chemical analysis of an aerosol. The method may include the steps of: collecting an aerosol; thermally desorbing the aerosol into a carrier gas to provide desorbed aerosol material; transporting the desorbed aerosol material onto the head of a gas chromatography column; analyzing the aerosol material using a gas chromatograph, and quantizing the aerosol material as it evolves from the gas chromatography column. The apparatus includes a collection and thermal desorption cell, a gas chromatograph including a gas chromatography column, heated transport lines coupling the cell and the column; and a quantization detector for aerosol material evolving from the gas chromatography column.

Molecular column densities in selected model atmospheres. [chemical analysis of carbon stars

NASA Technical Reports Server (NTRS)

Johnson, H. R.; Beebe, R. F.; Sneden, C.

1974-01-01

From an examination of predicted column densities, the following conclusions were drawn: (1) The SiO ought to be visible in carbon stars which were generated from triple alpha burning, but absent from carbon stars generated from the CNO bi-cycle. (2) Variation in the observed relative strengths of TiO and ZrO is indicative of real differences in the ratio Ti/Zr. (3) The TiO/ZrO ratio shows a small variation as C/O and effective temperature is changed. (4) Column density of silicon dicarbide (SiC2) is sensitive to abundance, temperature, and gravity; hence all relationships between the strength of SiC2 and other stellar parameters will show appreciable scatter. There is however, a substantial luminosity effect present in the SiC2 column densities. (5) Unexpectedly, SiC2 is anti-correlated with C2. (6) The presence of SiC2 in a carbon star eliminates the possibility of these stars having temperatures greater than or equal to 3000 K, or being produced through the CNO bi-cycle.

Stress Degradation Studies on Varenicline Tartrate and Development of a Validated Stability-Indicating HPLC Method

PubMed Central

Pujeri, Sudhakar S.; Khader, Addagadde M. A.; Seetharamappa, Jaldappagari

2012-01-01

A simple, rapid and stability-indicating reversed-phase liquid chromatographic method was developed for the assay of varenicline tartrate (VRT) in the presence of its degradation products generated from forced decomposition studies. The HPLC separation was achieved on a C18 Inertsil column (250 mm × 4.6 mm i.d. particle size is 5 μm) employing a mobile phase consisting of ammonium acetate buffer containing trifluoroacetic acid (0.02M; pH 4) and acetonitrile in gradient program mode with a flow rate of 1.0 mL min−1. The UV detector was operated at 237 nm while column temperature was maintained at 40 °C. The developed method was validated as per ICH guidelines with respect to specificity, linearity, precision, accuracy, robustness and limit of quantification. The method was found to be simple, specific, precise and accurate. Selectivity of the proposed method was validated by subjecting the stock solution of VRT to acidic, basic, photolysis, oxidative and thermal degradation. The calibration curve was found to be linear in the concentration range of 0.1–192 μg mL−1 (R2 = 0.9994). The peaks of degradation products did not interfere with that of pure VRT. The utility of the developed method was examined by analyzing the tablets containing VRT. The results of analysis were subjected to statistical analysis. PMID:22396908

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.

Computer systems and methods for the query and visualization of multidimensional databases

DOEpatents

Stolte, Chris; Tang, Diane L; Hanrahan, Patrick

2015-03-03

A computer displays a graphical user interface on its display. The graphical user interface includes a schema information region and a data visualization region. The schema information region includes multiple operand names, each operand corresponding to one or more fields of a multi-dimensional database that includes at least one data hierarchy. The data visualization region includes a columns shelf and a rows shelf. The computer detects user actions to associate one or more first operands with the columns shelf and to associate one or more second operands with the rows shelf. The computer generates a visual table in the data visualization region in accordance with the user actions. The visual table includes one or more panes. Each pane has an x-axis defined based on data for the one or more first operands, and each pane has a y-axis defined based on data for the one or more second operands.

Computer systems and methods for the query and visualization of multidimensional databases

DOEpatents

Stolte, Chris; Tang, Diane L.; Hanrahan, Patrick

2015-11-10

A computer displays a graphical user interface on its display. The graphical user interface includes a schema information region and a data visualization region. The schema information region includes a plurality of fields of a multi-dimensional database that includes at least one data hierarchy. The data visualization region includes a columns shelf and a rows shelf. The computer detects user actions to associate one or more first fields with the columns shelf and to associate one or more second fields with the rows shelf. The computer generates a visual table in the data visualization region in accordance with the user actions. The visual table includes one or more panes. Each pane has an x-axis defined based on data for the one or more first fields, and each pane has a y-axis defined based on data for the one or more second fields.

Variable speed control in wells turbine-based oscillating water column devices: optimum rotational speed

NASA Astrophysics Data System (ADS)

Lekube, J.; Garrido, A. J.; Garrido, I.

2018-03-01

The effects of climate change and global warming reveal the need to find alternative sources of clean energy. In this sense, wave energy power plants, and in particular Oscillating Water Column (OWC) devices, offer a huge potential of energy harnessing. Nevertheless, the conversion systems have not reached a commercially mature stage yet so as to compete with conventional power plants. At this point, the use of new control methods over the existing technology arises as a doable way to improve the efficiency of the system. Due to the non-uniform response that the turbine shows to the rotational speed variation, the speed control of the turbo-generator may offer a feasible solution for efficiency improvement during the energy conversion. In this context, a novel speed control approach for OWC systems is presented in this paper, demonstrating its goodness and affording promising results when particularized to the Mutriku’s wave power plant.

[Study on the analysis of organogermanium compounds by ion chromatography].

PubMed

Chen, Q; Mou, S; Hou, X; Ni, Z

1997-05-01

A new high performance ion exchange chromatographic method for separation and determination of three organogermanium compounds beta-carboxyethylgermanium sesquioxide (I), beta-(alpha-methyl) carboxyethylgermanium sesquioxide (II) and di-(beta-carboxyethyl) germanium hydroxide (III) has been developed. A Dionex DX-300 Ion Chromatograph equipped with a Dionex PED-II pulsed electrochemical detector (conductivity mode), a Dionex AMMS-1 anion micromembrane suppressor, and a Dionex ACI advanced computer interface coupled with AI-450 chromatographic software was employed. The separation was achieved by using a Dionex IonPac AS4A-SC column as analytical column, sodium tetraborate solution as eluent, and sulfuric acid solution as regenerant. For reducing run time, a gradient program was chosen. The detection limits (S/N = 3, expressed as germanium) for the three compounds were 0.038mg/L (I), 0.035mg/L (II) and 0.025mg/L (III), respectively. The method has been applied to the analysis of two tonic oral drinks, and the average recoveries for the three compounds ranged from 95%-101%. The results obtained were in agreement with those of hydride generation atomic fluorescence spectrometry (HG-AFS).

Design of Tactical Support Strategies in Military Logistics: Trade-offs Between Efficiency and Effectiveness. A Column and Cut Generation Modeling Methods

DTIC Science & Technology

2011-12-01

problems need to be addressed in the design of military logis- tics networks. The design problem includes strategic decisions, such as the location of...military strategic logistics [11–13]. In this study, we focus on the design of tactical logistics strategies, which achieve different optimal balances...is clear that our problem is N P−Hard 1 since it generalizes the CVPR and the BPP . Different solutions to handle the loading and routing of

40 CFR 799.6786 - TSCA water solubility: Generator column method.

Code of Federal Regulations, 2011 CFR

2011-07-01

..., concentrations expressed in milligrams per liter (mg/L) are approximately equal to 10−3 g/103 g or parts per... section. (E) Two 6-port high-pressure rotary switching valves in paragraph (c)(3)(ii) of this section. (F... Seawater1 Chemical Amount NaF 3 mg SrCl2.6H2O 20 mg H3BO3 30 mg KBr 100 mg KCl 700 mg CaCl2.2H2O 1.47 gram...

Practical issues relating to soil column chromatography for sorption parameter determination.

PubMed

Bi, Erping; Schmidt, Torsten C; Haderlein, Stefan B

2010-08-01

Determination of sorption distribution coefficients (K(d)) of organic compounds by a dynamic soil column chromatography (SCC) method was developed and validated. Eurosoil 4, quartz, and alumina were chosen as exemplary packing materials. Heterocyclic aromatic compounds were selected in the validation of SCC. The prerequisites of SCC with regard to column dimension, packing procedure, and sample injection volume are discussed. Reproducible soil column packing was achieved by addition of a pre-column and an HPLC pump for subsequent compression of the packed material. Various methods to determine retention times from breakthrough curves are discussed and the use of the half mass method is recommended. To dilute soil with inert material can prevent column-clogging and help to complete experiments in a reasonable period of time. For the chosen probe compounds, quartz rather than alumina proved a suitable dilution material. Non-equilibrium issue can be overcome by conducting the experiments under different flowrates and/or performing numerical simulation. Copyright 2010 Elsevier Ltd. All rights reserved.

A Better Method for Filling Pasteur Pipet Chromatography Columns

ERIC Educational Resources Information Center

Ruekberg, Ben

2006-01-01

An alternative method for the preparation of Pasteur pipet chromatography columns is presented that allows the column to be filled with solvent without bubbles and allows greater control of fluid flow while the materials to be separated are added. Students are required to wear gloves and goggles and caution should be used while handling glass…

Enantioselective ultra-high and high performance liquid chromatography: a comparative study of columns based on the Whelk-O1 selector.

PubMed

Kotoni, Dorina; Ciogli, Alessia; D'Acquarica, Ilaria; Kocergin, Jelena; Szczerba, Ted; Ritchie, Harald; Villani, Claudio; Gasparrini, Francesco

2012-12-21

This paper reports on the thermodynamic and kinetic evaluation of a new ultra-high performance liquid chromatography broad-spectrum Pirkle-type chiral stationary phase (CSP) for enantioselective applications (eUHPLC). The well-known Whelk-O1 selector was covalently immobilized onto 1.7-μm high-surface-area, porous spherical silica particles to produce a totally synthetic, covalently bonded CSP that was packed into 150 mm, 100mm, 75 mm and 50mm columns, either 4.6 or 3.0mm ID. A 100 mm × 4.6 mm ID column was fully characterized from a kinetic and thermodynamic point of view, using as reference a conventional HPLC Whelk-O1 column, 250 mm×4.6mm ID, based on 5-μm porous silica particles. On the eUHPLC column, van Deemter plots generated H(min) values of 3.53 μm for 1,3-dinitrobenzene, at an interstitial mobile phase linear velocity (μ(inter)) of 5.07 mm/s, and H(min) of 4.26 and 4.17 μm for the two enantiomers of acenaphthenol, at μ(inter) of 4.85 mm/s and 4.24 mm/s, respectively. Resolution of 21 enantiomeric pairs including alcohols, epoxides, sulfoxides, phosphine oxides, benzodiazepines and 2-aryloxyproprionic esters used as herbicides, were obtained with significant advantages in terms of efficiency and analysis time. Speed gain factors were calculated for the different column geometries (150 mm, 100mm, 75 mm and 50mm, either 4.6 or 3.0mm ID), with respect to the standard HPLC column (250 mm ×4.6 mm ID), and were as high as 13, in the case of the 50-mm-long column, affording sub-minute separations of enantiomers with excellent resolution factors. In particular, trans-stilbene oxide was resolved in only 10s, while a 50 mm×3.0 mm ID column was used as a compromise between reduced mobile phase consumption (less than 1 mL per analysis) and smaller extra-column band-broadening effect. Given the relatively low viscosity in NP mode, and the excellent permeability of these eUHPLC columns, with backpressure values under 600 bar for a wide range of flow rates, the use of standard HPLC hardware is possible. In this case, however, a significant loss in resolution is observed, compared to the UHPLC instrumentation, if no modifications are introduced in the HPLC apparatus to reduce extra-column variance. The excellent efficiency and selectivity, conjugated with the very high-throughput and the ultra-fast analysis time, prove the potentials of the eUHPLC Whelk-O1 columns in the development of enantioselective UHPLC methods. Copyright © 2012 Elsevier B.V. All rights reserved.

Validation of an HPLC method for the determination of fleroxacin and its photo-degradation products in pharmaceutical forms.

PubMed

Djurdjevic, Predrag; Laban, Aleksandra; Jelikic-Stankov, Milena

2004-01-01

HPLC determination of fleroxacin in dosage forms was carried out using either reversed-phase column YMC pack ODS-AQ or Supelco LC Hisep shielded hydrophobic phase column, with UV detection at 280 nm. The mobile phase for ODS column consisted of 50:50:0.5 v/v/v and for Hisep column 15:85:0.5 v/v/v acetonitrile-water-triethylamine. The pH of the mobile phase was adjusted to 6.30 for ODS column and to 6.85 for Hisep column, with H3PO4. Linear response was obtained in the concentration range of fleroxacin between 0.01 and 1.30 micrograms/mL. Detection limit was 4.8 ng/mL. Recovery test in the determination of fleroxacin in "Quinodis" tablets (Hoffmann La Roche, nominal mass 400 or 200 mg) was 98-101% for both columns. The effect of the composition and pH of the mobile phase on spectra, retention time and dissociation constants of fleroxacin was discussed. The proposed method could be also used for separation of the photo-degradation products of fleroxacin. Ten degradation products were separated on the ODS-AQ column, thus confirming the suitability of the proposed method for stability study of fleroxacin in pharmaceuticals.

Pretreatment method for immunoassay of polychlorinated biphenyls in transformer oil using multilayer capillary column and microfluidic liquid-liquid partitioning.

PubMed

Aota, Arata; Date, Yasumoto; Terakado, Shingo; Ohmura, Naoya

2013-01-01

Polychlorinated biphenyls (PCBs) are persistent organic pollutants that are present in the insulating oil inside a large number of transformers. To aid in eliminating PCB-contaminated transformers, PCBs in oil need to be measured using a rapid and cost-effective analytical method. We previously reported a pretreatment method for the immunoassay of PCBs in oil using a large-scale multilayer column and a microchip with multiple microrecesses, which permitted concentrated solvent extraction. In this paper, we report on a more rapid and facile pretreatment method, without an evaporation process, by improving the column and the microchip. In a miniaturized column, the decomposition and separation of oil were completed in 2 min. PCBs can be eluted from the capillary column at concentrations seven-times higher than those from the previous column. The total volume of the microrecesses was increased by improving the microrecess structure, the enabling extraction of four-times the amount of PCBs achieved with the previous system. By interfacing the capillary column with the improved microchip, PCBs in the eluate from the column were extracted into dimethyl sulfoxide in microrecesses with high enrichment and without the need for evaporation. Pretreatment was completed within 20 min. The pretreated oil was analyzed using a flow-based kinetic exclusion immunoassay. The limit of detection of PCBs in oil was 0.15 mg kg(-1), which satisfies the criterion set in Japan of 0.5 mg kg(-1).

The Perils of Pathogen Discovery: Origin of a Novel Parvovirus-Like Hybrid Genome Traced to Nucleic Acid Extraction Spin Columns

PubMed Central

Naccache, Samia N.; Greninger, Alexander L.; Lee, Deanna; Coffey, Lark L.; Phan, Tung; Rein-Weston, Annie; Aronsohn, Andrew; Hackett, John; Delwart, Eric L.

2013-01-01

Next-generation sequencing was used for discovery and de novo assembly of a novel, highly divergent DNA virus at the interface between the Parvoviridae and Circoviridae. The virus, provisionally named parvovirus-like hybrid virus (PHV), is nearly identical by sequence to another DNA virus, NIH-CQV, previously detected in Chinese patients with seronegative (non-A-E) hepatitis. Although we initially detected PHV in a wide range of clinical samples, with all strains sharing ∼99% nucleotide and amino acid identity with each other and with NIH-CQV, the exact origin of the virus was eventually traced to contaminated silica-binding spin columns used for nucleic acid extraction. Definitive confirmation of the origin of PHV, and presumably NIH-CQV, was obtained by in-depth analyses of water eluted through contaminated spin columns. Analysis of environmental metagenome libraries detected PHV sequences in coastal marine waters of North America, suggesting that a potential association between PHV and diatoms (algae) that generate the silica matrix used in the spin columns may have resulted in inadvertent viral contamination during manufacture. The confirmation of PHV/NIH-CQV as laboratory reagent contaminants and not bona fide infectious agents of humans underscores the rigorous approach needed to establish the validity of new viral genomes discovered by next-generation sequencing. PMID:24027301

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.

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

NASA Astrophysics Data System (ADS)

Jivkov, Venelin S.; Zahariev, Evtim V.

2016-12-01

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

MAMAP - a new spectrometer system for column-averaged methane and carbon dioxide observations from aircraft: retrieval algorithm and first inversions for point source emission rates

NASA Astrophysics Data System (ADS)

Krings, T.; Gerilowski, K.; Buchwitz, M.; Reuter, M.; Tretner, A.; Erzinger, J.; Heinze, D.; Burrows, J. P.; Bovensmann, H.

2011-04-01

MAMAP is an airborne passive remote sensing instrument designed for measuring columns of methane (CH4) and carbon dioxide (CO2). The MAMAP instrument consists of two optical grating spectrometers: One in the short wave infrared band (SWIR) at 1590-1690 nm to measure CO2 and CH4 absorptions and another one in the near infrared (NIR) at 757-768 nm to measure O2 absorptions for reference purposes. MAMAP can be operated in both nadir and zenith geometry during the flight. Mounted on an airplane MAMAP can effectively survey areas on regional to local scales with a ground pixel resolution of about 29 m × 33 m for a typical aircraft altitude of 1250 m and a velocity of 200 km h-1. The retrieval precision of the measured column relative to background is typically ≲ 1% (1σ). MAMAP can be used to close the gap between satellite data exhibiting global coverage but with a rather coarse resolution on the one hand and highly accurate in situ measurements with sparse coverage on the other hand. In July 2007 test flights were performed over two coal-fired powerplants operated by Vattenfall Europe Generation AG: Jänschwalde (27.4 Mt CO2 yr-1) and Schwarze Pumpe (11.9 Mt CO2 yr-1), about 100 km southeast of Berlin, Germany. By using two different inversion approaches, one based on an optimal estimation scheme to fit Gaussian plume models from multiple sources to the data, and another using a simple Gaussian integral method, the emission rates can be determined and compared with emissions as stated by Vattenfall Europe. An extensive error analysis for the retrieval's dry column results (XCO2 and XCH4) and for the two inversion methods has been performed. Both methods - the Gaussian plume model fit and the Gaussian integral method - are capable of delivering reliable estimates for strong point source emission rates, given appropriate flight patterns and detailed knowledge of wind conditions.

[Preparation and applications of a supported liquid-liquid extraction column with a composite diatomite material].

PubMed

Bao, Jianmin; Ma, Zhishuang; Sun, Ying; Wang, Yongzun; Li, Youxin

2012-08-01

A rapid and special supported liquid-liquid extraction (SLE) column was developed with a composite diatomite material. The SLE column was evaluated by high performance liquid chromatography (HPLC) with acidic, neutral and alkaline compounds dissolved in water. Furthermore, some real complex samples were also analyzed by HPLC with the SLE method. The recoveries of benzoic acid (acidic), p-nitroaniline (alkaline) and 4-hydroxy-benzoic methyl ester (neutral) treated by the SLE column were 90.6%, 98.1% and 97.7%. However, the recoveries of the three compounds treated by traditional liquid-liquid extraction (LLE) method were 71.9%, 81.9% and 83.9%. The results showed that the SLE technique had higher recoveries than the traditional LLE method. The spiked recoveries of the complex samples, such as benzoic acid in Sprite and dexamethasone acetate, chlorphenamine maleate, indomethacin in bovine serum, were between 80% and 110% and the relative standard deviations (RSDs) were less than 15%. For biological specimen, the results could be accepted. Meantime, many disadvantages associated with traditional LLE method, such as emulsion formation, didn't occur using SLE column. The SLE column technique is a good sample preparation method with many advantages, such as rapid, simple, robust, easily automated, high recovery and high-throughput, which would be widely used in the future.

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

PubMed

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

2014-01-01

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

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.

A Rapid Spin Column-Based Method to Enrich Pathogen Transcripts from Eukaryotic Host Cells Prior to Sequencing

DOE PAGES

Bent, Zachary W.; Poorey, Kunal; LaBauve, Annette E.; ...

2016-12-21

When analyzing pathogen transcriptomes during the infection of host cells, the signal-to-background (pathogen-to-host) ratio of nucleic acids (NA) in infected samples is very small. Despite the advancements in next-generation sequencing, the minute amount of pathogen NA makes standard RNA-seq library preps inadequate for effective gene-level analysis of the pathogen in cases with low bacterial loads. In order to provide a more complete picture of the pathogen transcriptome during an infection, we developed a novel pathogen enrichment technique, which can enrich for transcripts from any cultivable bacteria or virus, using common, readily available laboratory equipment and reagents. To evenly enrich formore » pathogen transcripts, we generate biotinylated pathogen-targeted capture probes in an enzymatic process using the entire genome of the pathogen as a template. The capture probes are hybridized to a strand-specific cDNA library generated from an RNA sample. The biotinylated probes are captured on a monomeric avidin resin in a miniature spin column, and enriched pathogen-specific cDNA is eluted following a series of washes. To test this method, we performed an in vitro time-course infection using Klebsiella pneumoniae to infect murine macrophage cells. K. pneumoniae transcript enrichment efficiency was evaluated using RNA-seq. Bacterial transcripts were enriched up to ~400-fold, and allowed the recovery of transcripts from ~2000–3600 genes not observed in untreated control samples. These additional transcripts revealed interesting aspects of K. pneumoniae biology including the expression of putative virulence factors and the expression of several genes responsible for antibiotic resistance even in the absence of drugs.« less

A Rapid Spin Column-Based Method to Enrich Pathogen Transcripts from Eukaryotic Host Cells Prior to Sequencing

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

Bent, Zachary W.; Poorey, Kunal; LaBauve, Annette E.

When analyzing pathogen transcriptomes during the infection of host cells, the signal-to-background (pathogen-to-host) ratio of nucleic acids (NA) in infected samples is very small. Despite the advancements in next-generation sequencing, the minute amount of pathogen NA makes standard RNA-seq library preps inadequate for effective gene-level analysis of the pathogen in cases with low bacterial loads. In order to provide a more complete picture of the pathogen transcriptome during an infection, we developed a novel pathogen enrichment technique, which can enrich for transcripts from any cultivable bacteria or virus, using common, readily available laboratory equipment and reagents. To evenly enrich formore » pathogen transcripts, we generate biotinylated pathogen-targeted capture probes in an enzymatic process using the entire genome of the pathogen as a template. The capture probes are hybridized to a strand-specific cDNA library generated from an RNA sample. The biotinylated probes are captured on a monomeric avidin resin in a miniature spin column, and enriched pathogen-specific cDNA is eluted following a series of washes. To test this method, we performed an in vitro time-course infection using Klebsiella pneumoniae to infect murine macrophage cells. K. pneumoniae transcript enrichment efficiency was evaluated using RNA-seq. Bacterial transcripts were enriched up to ~400-fold, and allowed the recovery of transcripts from ~2000–3600 genes not observed in untreated control samples. These additional transcripts revealed interesting aspects of K. pneumoniae biology including the expression of putative virulence factors and the expression of several genes responsible for antibiotic resistance even in the absence of drugs.« 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.

Highly Sensitive Determination of 2,4,6-Trinitrotoluene and Related Byproducts Using a Diol Functionalized Column for High Performance Liquid Chromatography

PubMed Central

Gumuscu, Burcu; Erdogan, Zeynep; Guler, Mustafa O.; Tekinay, Turgay

2014-01-01

In this work, a new detection method for complete separation of 2,4,6-trinitrotoluene (TNT); 2,4-dinitrotoluene (2,4-DNT); 2,6-dinitrotoluene (2,6-DNT); 2-aminodinitrotoluene (2-ADNT) and 4-aminodinitrotoluene (4-ADNT) molecules in high-performance liquid-chromatography (HPLC) with UV sensor has been developed using diol column. This approach improves on cost, time, and sensitivity over the existing methods, providing a simple and effective alternative. Total analysis time was less than 13 minutes including column re-equilibration between runs, in which water and acetonitrile were used as gradient elution solvents. Under optimized conditions, the minimum resolution between 2,4-DNT and 2,6-DNT peaks was 2.06. The recovery rates for spiked environmental samples were between 95–98%. The detection limits for diol column ranged from 0.78 to 1.17 µg/L for TNT and its byproducts. While the solvent consumption was 26.4 mL/min for two-phase EPA and 30 mL/min for EPA 8330 methods, it was only 8.8 mL/min for diol column. The resolution was improved up to 49% respect to two-phase EPA and EPA 8330 methods. When compared to C-18 and phenyl-3 columns, solvent usage was reduced up to 64% using diol column and resolution was enhanced approximately two-fold. The sensitivity of diol column was afforded by the hydroxyl groups on polyol layer, joining the formation of charge-transfer complexes with nitroaromatic compounds according to acceptor-donor interactions. Having compliance with current requirements, the proposed method demonstrates sensitive and robust separation. PMID:24905826

Highly sensitive determination of 2,4,6-trinitrotoluene and related byproducts using a diol functionalized column for high performance liquid chromatography.

PubMed

Gumuscu, Burcu; Erdogan, Zeynep; Guler, Mustafa O; Tekinay, Turgay

2014-01-01

In this work, a new detection method for complete separation of 2,4,6-trinitrotoluene (TNT); 2,4-dinitrotoluene (2,4-DNT); 2,6-dinitrotoluene (2,6-DNT); 2-aminodinitrotoluene (2-ADNT) and 4-aminodinitrotoluene (4-ADNT) molecules in high-performance liquid-chromatography (HPLC) with UV sensor has been developed using diol column. This approach improves on cost, time, and sensitivity over the existing methods, providing a simple and effective alternative. Total analysis time was less than 13 minutes including column re-equilibration between runs, in which water and acetonitrile were used as gradient elution solvents. Under optimized conditions, the minimum resolution between 2,4-DNT and 2,6-DNT peaks was 2.06. The recovery rates for spiked environmental samples were between 95-98%. The detection limits for diol column ranged from 0.78 to 1.17 µg/L for TNT and its byproducts. While the solvent consumption was 26.4 mL/min for two-phase EPA and 30 mL/min for EPA 8330 methods, it was only 8.8 mL/min for diol column. The resolution was improved up to 49% respect to two-phase EPA and EPA 8330 methods. When compared to C-18 and phenyl-3 columns, solvent usage was reduced up to 64% using diol column and resolution was enhanced approximately two-fold. The sensitivity of diol column was afforded by the hydroxyl groups on polyol layer, joining the formation of charge-transfer complexes with nitroaromatic compounds according to acceptor-donor interactions. Having compliance with current requirements, the proposed method demonstrates sensitive and robust separation.

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.

Places to Go: Google's Search Results for "Net Generation"

ERIC Educational Resources Information Center

Downes, Stephen

2007-01-01

In his Places to Go column for a special issue on the Net Generation, Stephen Downes takes an unexpected trip--to Google. According to Downes, Google epitomizes the essence of the Net Generation. Infinitely searchable and adaptable, Google represents the spirit of a generation raised in the world of the Internet, a generation that adapts…

Stress Analysis of Columns and Beam Columns by the Photoelastic Method

NASA Technical Reports Server (NTRS)

Ruffner, B F

1946-01-01

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

Trip report. Eurochemic company assistance: Hanford Atomic Products Operation spent fuel processing technology

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

Shank, E.M.

1959-06-23

Information obtained from HAPO during visit by M.K. Twichell, UCNC, and E.M. Shank, ORNL, is given. Included are the tentative procedures for obtaining and transmitting information to the Eurochemic company. Discussions are given on pulsed columns, corrosion, puse generators, centrifuges, valves, in-line instrumentation, evaporators, resin column design, off-gas processing, solvent recovery, liquid-waste handling, process control, equipment decontamination, criticality, radiation protection, diluent, and solvent stability, backmixing in a pulsed column, and use of 40% TBP in the purex flowsheet.

Feeding Currents generated by Cassiopea jellyfish

NASA Astrophysics Data System (ADS)

Gaddam, M. G.; Santhanakrishnan, A.

2016-02-01

Feeding currents generated by organisms dwelling in the benthic boundary layer can enhance nutrient fluxes in coastal habitats with low-speed ambient flows. Patchy aggregations of Cassiopea medusae, commonly referred to as the "upside-down" jellyfish, are seen in sheltered marine environments such as mangrove forests and coral reefs in shallow regions saturated with sunlight. They exhibit a sessile, non-swimming lifestyle, and are oriented such that their bells are attached to the substrate and oral arms directed toward the free surface. Pulsations of their bells drive flow toward and away from the body, assisting in suspension feeding and for exchange of inorganic and organic matter across the water column. The feeding currents generated by aggregations of these medusae and subsequent effects on mixing in the water column have not been examined. We experimentally investigated currents generated by groups of Cassiopea medusae in a low-speed recirculating water tunnel. Multiple medusae grouping arrangements were tested in the tunnel based on time-lapse videos of the organisms obtained overnight in laboratory aquaria. Fluorescent dye introduced underneath the substrate was used to investigate release of porewater via bell motion. Quantitative flow visualization studies of Cassiopea currents were conducted using 2D high-speed particle image velocimetry. Vertical mixing of medusa-induced jets were observed in the presence of minimal background flow. The implications of feeding currents generated by groups of Cassiopea medusae on mixing in the water column will be presented.

Fully integrated and encapsulated micro-fabricated vacuum diode and method of manufacturing same

DOEpatents

Resnick, Paul J.; Langlois, Eric

2015-12-01

Disclosed is an encapsulated micro-diode and a method for producing same. The method comprises forming a plurality columns in the substrate with a respective tip disposed at a first end of the column, the tip defining a cathode of the diode; disposing a sacrificial oxide layer on the substrate, plurality of columns and respective tips; forming respective trenches in the sacrificial oxide layer around the columns; forming an opening in the sacrificial oxide layer to expose a portion of the tips; depositing a conductive material in of the opening and on a surface of the substrate to form an anode of the diode; and removing the sacrificial oxide layer.

Method of manufacturing a fully integrated and encapsulated micro-fabricated vacuum diode

DOEpatents

Resnick, Paul J.; Langlois, Eric

2014-08-26

Disclosed is an encapsulated micro-diode and a method for producing same. The method comprises forming a plurality columns in the substrate with a respective tip disposed at a first end of the column, the tip defining a cathode of the diode; disposing a sacrificial oxide layer on the substrate, plurality of columns and respective tips; forming respective trenches in the sacrificial oxide layer around the columns; forming an opening in the sacrificial oxide layer to expose a portion of the tips; depositing a conductive material in of the opening and on a surface of the substrate to form an anode of the diode; and removing the sacrificial oxide layer.

A New Resonance Tube

ERIC Educational Resources Information Center

Bates, Alan

2017-01-01

The measurement of the speed of sound in air with the resonance tube is a popular experiment that often yields accurate results. One approach is to hold a vibrating tuning fork over an air column that is partially immersed in water. The column is raised and lowered in the water until the generated standing wave produces resonance: this occurs at…

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.

Simultaneous Liquid Chromatographic Determination of 10 Ultra-Violet Filters in Sunscreens.

PubMed

Wharton, Mary; Geary, Michael; O'Connor, Niamh; Curtin, Laura; Ketcher, Krystal

2015-09-01

A rapid HPLC method was developed for the simultaneous determination of 10 UV filters found in sunscreen. The following UV filters were analyzed in this method; 2-phenylbenzimidazole-5-sulfonic acid, benzophenone-3, isoamyl p-methoxycinnamate, 4-methylbenzylidene camphor, octocrylene, ethylhexyl dimethyl 4-aminobenzoic acid, ethylhexyl methoxycinnamate, butyl methoxydibenzoylmethane, ethylhexyl salicylate and homosalate. The method was developed on two columns; a Thermo Hypersil C18 BDS, 3 µm column (4.6 × 100 mm) and a Chromolith RP-18e Monolithic column (4.6 × 100 mm). The same mobile phase of ethanol and 1% acetic acid (70:30, v/v) was employed for both columns. The separation of the 10 UV filters was carried out successfully on both columns; the optimal resolution was obtained on the Thermo Scientific Hypersil column in a time frame of 7 min. An isocratic elution utilizing ethanol and acetic acid (70:30, v/v) at a temperature of 35°C was employed. The method was applied to a number of commercial samples of sunscreen and lotions and was validated according to International Conference on Harmonisation guidelines for selectivity, linearity, accuracy, precision and robustness. A comparison of the performances of both columns was also carried out. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Atmospheric electron x-ray spectrometer

NASA Technical Reports Server (NTRS)

Feldman, Jason E. (Inventor); George, Thomas (Inventor); Wilcox, Jaroslava Z. (Inventor)

2002-01-01

The present invention comprises an apparatus for performing in-situ elemental analyses of surfaces. The invention comprises an atmospheric electron x-ray spectrometer with an electron column which generates, accelerates, and focuses electrons in a column which is isolated from ambient pressure by a:thin, electron transparent membrane. After passing through the membrane, the electrons impinge on the sample in atmosphere to generate characteristic x-rays. An x-ray detector, shaping amplifier, and multi-channel analyzer are used for x-ray detection and signal analysis. By comparing the resultant data to known x-ray spectral signatures, the elemental composition of the surface can be determined.

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

Kaczmarski, Krzysztof; Guiochon, Georges A

The adsorption isotherms of selected compounds are our main source of information on the mechanisms of adsorption processes. Thus, the selection of the methods used to determine adsorption isotherm data and to evaluate the errors made is critical. Three chromatographic methods were evaluated, frontal analysis (FA), frontal analysis by characteristic point (FACP), and the pulse or perturbation method (PM), and their accuracies were compared. Using the equilibrium-dispersive (ED) model of chromatography, breakthrough curves of single components were generated corresponding to three different adsorption isotherm models: the Langmuir, the bi-Langmuir, and the Moreau isotherms. For each breakthrough curve, the best conventionalmore » procedures of each method (FA, FACP, PM) were used to calculate the corresponding data point, using typical values of the parameters of each isotherm model, for four different values of the column efficiency (N = 500, 1000, 2000, and 10,000). Then, the data points were fitted to each isotherm model and the corresponding isotherm parameters were compared to those of the initial isotherm model. When isotherm data are derived with a chromatographic method, they may suffer from two types of errors: (1) the errors made in deriving the experimental data points from the chromatographic records; (2) the errors made in selecting an incorrect isotherm model and fitting to it the experimental data. Both errors decrease significantly with increasing column efficiency with FA and FACP, but not with PM.« less

High-throughput sample preparation and simultaneous column regeneration liquid chromatography-tandem mass spectrometry method for determination of nitrogen mustard metabolites in human urine.

PubMed

Reddy, Muntha K; Mills, Grier; Nixon, Christopher; Wyatt, Shane A; Croley, Timothy R

2011-08-15

Nitrogen mustards (NMs) are known to have DNA alkylation and strong vesicant properties. Their availability to terrorist organizations makes them a potential choice for chemical attacks on civilian populations. After an exposure, it is difficult to measure NMs directly because of their rapid metabolism in the human body. Therefore to determine an individual's level of exposure to NMs, it is necessary to analyze for NM metabolites being excreted by the body. The metabolites of NMs are generated by a hydrolysis reaction, and are easily detectable by liquid chromatography tandem mass spectrometry (LC-MS/MS). This work is focused on the development of a high-throughput assay for the quantitation of N-ethyldiethanolamine (EDEA) and N-methyldiethanolamine (MDEA) metabolites of bis (2-chloroethyl) ethylethanamine (HN1) and bis (2-chloroethyl) methylethanamine (HN2), respectively. The method uses automated 96-well plate sample preparation of human urine samples and a 2-position 10-port switching valve to allow for simultaneous regeneration of the liquid chromatography (LC) columns. Using this method, over 18 h was saved through the reduction of sample preparation and analysis time when compared to a conventional method for 96 samples. The validated method provided excellent accuracy for both EDEA (100.9%) and MDEA (100.6%) with precision better than 5.27% for each analyte. Copyright © 2011 Elsevier B.V. All rights reserved.

Simplified and Efficient Quantification of Low-abundance Proteins at Very High Multiplex via Targeted Mass Spectrometry*

PubMed Central

Burgess, Michael W.; Keshishian, Hasmik; Mani, D. R.; Gillette, Michael A.; Carr, Steven A.

2014-01-01

Liquid chromatography–multiple reaction monitoring mass spectrometry (LC-MRM-MS) of plasma that has been depleted of abundant proteins and fractionated at the peptide level into six to eight fractions is a proven method for quantifying proteins present at low nanogram-per-milliliter levels. A drawback of fraction-MRM is the increased analysis time due to the generation of multiple fractions per biological sample. We now report that the use of heated, long, fused silica columns (>30 cm) packed with 1.9 μm of packing material can reduce or eliminate the need for fractionation prior to LC-MRM-MS without a significant loss of sensitivity or precision relative to fraction-MRM. We empirically determined the optimal column length, temperature, gradient duration, and sample load for such assays and used these conditions to study detection sensitivity and assay precision. In addition to increased peak capacity, longer columns packed with smaller beads tolerated a 4- to 6-fold increase in analyte load without a loss of robustness or reproducibility. The longer columns also provided a 4-fold improvement in median limit-of-quantitation values with increased assay precision relative to the standard 12 cm columns packed with 3 μm material. Overall, the optimized chromatography provided an approximately 3-fold increase in analysis throughput with excellent robustness and less than a 2-fold reduction in quantitative sensitivity relative to fraction-MRM. The value of the system for increased multiplexing was demonstrated by the ability to configure an 800-plex MRM-MS assay, run in a single analysis, comprising 2400 transitions with retention time scheduling to monitor 400 unlabeled and heavy labeled peptide pairs. PMID:24522978

Multi-GPU implementation of a VMAT treatment plan optimization algorithm

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

Tian, Zhen, E-mail: Zhen.Tian@UTSouthwestern.edu, E-mail: Xun.Jia@UTSouthwestern.edu, E-mail: Steve.Jiang@UTSouthwestern.edu; Folkerts, Michael; Tan, Jun

Purpose: Volumetric modulated arc therapy (VMAT) optimization is a computationally challenging problem due to its large data size, high degrees of freedom, and many hardware constraints. High-performance graphics processing units (GPUs) have been used to speed up the computations. However, GPU’s relatively small memory size cannot handle cases with a large dose-deposition coefficient (DDC) matrix in cases of, e.g., those with a large target size, multiple targets, multiple arcs, and/or small beamlet size. The main purpose of this paper is to report an implementation of a column-generation-based VMAT algorithm, previously developed in the authors’ group, on a multi-GPU platform tomore » solve the memory limitation problem. While the column-generation-based VMAT algorithm has been previously developed, the GPU implementation details have not been reported. Hence, another purpose is to present detailed techniques employed for GPU implementation. The authors also would like to utilize this particular problem as an example problem to study the feasibility of using a multi-GPU platform to solve large-scale problems in medical physics. Methods: The column-generation approach generates VMAT apertures sequentially by solving a pricing problem (PP) and a master problem (MP) iteratively. In the authors’ method, the sparse DDC matrix is first stored on a CPU in coordinate list format (COO). On the GPU side, this matrix is split into four submatrices according to beam angles, which are stored on four GPUs in compressed sparse row format. Computation of beamlet price, the first step in PP, is accomplished using multi-GPUs. A fast inter-GPU data transfer scheme is accomplished using peer-to-peer access. The remaining steps of PP and MP problems are implemented on CPU or a single GPU due to their modest problem scale and computational loads. Barzilai and Borwein algorithm with a subspace step scheme is adopted here to solve the MP problem. A head and neck (H and N) cancer case is then used to validate the authors’ method. The authors also compare their multi-GPU implementation with three different single GPU implementation strategies, i.e., truncating DDC matrix (S1), repeatedly transferring DDC matrix between CPU and GPU (S2), and porting computations involving DDC matrix to CPU (S3), in terms of both plan quality and computational efficiency. Two more H and N patient cases and three prostate cases are used to demonstrate the advantages of the authors’ method. Results: The authors’ multi-GPU implementation can finish the optimization process within ∼1 min for the H and N patient case. S1 leads to an inferior plan quality although its total time was 10 s shorter than the multi-GPU implementation due to the reduced matrix size. S2 and S3 yield the same plan quality as the multi-GPU implementation but take ∼4 and ∼6 min, respectively. High computational efficiency was consistently achieved for the other five patient cases tested, with VMAT plans of clinically acceptable quality obtained within 23–46 s. Conversely, to obtain clinically comparable or acceptable plans for all six of these VMAT cases that the authors have tested in this paper, the optimization time needed in a commercial TPS system on CPU was found to be in an order of several minutes. Conclusions: The results demonstrate that the multi-GPU implementation of the authors’ column-generation-based VMAT optimization can handle the large-scale VMAT optimization problem efficiently without sacrificing plan quality. The authors’ study may serve as an example to shed some light on other large-scale medical physics problems that require multi-GPU techniques.« less

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.

Void fraction, bubble size and interfacial area measurements in co-current downflow bubble column reactor with microbubble dispersion

DOE PAGES

Hernandez-Alvarado, Freddy; Kalaga, Dinesh V.; Turney, Damon; ...

2017-05-06

Micro-bubbles dispersed in bubble column reactors have received great interest in recent years, due to their small size, stability, high gas-liquid interfacial area concentrations and longer residence times. The high gas-liquid interfacial area concentrations lead to high mass transfer rates compared to conventional bubble column reactors. In the present work, experiments have been performed in a down-flow bubble column reactor with micro-bubbles generated and dispersed by a novel mechanism to determine the gas-liquid interfacial area concentrations by measuring the void fraction and bubble size distributions. Gamma-ray densitometry has been employed to determine the axial and radial distributions of void fractionmore » and a high speed camera equipped with a borescope is used to measure the axial and radial variations of bubble sizes. Also, the effects of superficial gas and liquid velocities on the two-phase flow characteristics have been investigated. Further, reconstruction techniques of the radial void fraction profiles from the gamma densitometry's chordal measurements are discussed and compared for a bubble column reactor with dispersed micro-bubbles. The results demonstrate that the new bubble generation technique offers high interfacial area concentrations (1,000 to 4,500 m 2/m 3) with sub-millimeter bubbles (500 to 900 µm) and high overall void fractions (10% – 60%) in comparison with previous bubble column reactor designs. The void fraction data was analyzed using slip velocity model and empirical correlation has been proposed to predict the Sauter mean bubble diameter.« less

Void fraction, bubble size and interfacial area measurements in co-current downflow bubble column reactor with microbubble dispersion

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

Hernandez-Alvarado, Freddy; Kalaga, Dinesh V.; Turney, Damon

Micro-bubbles dispersed in bubble column reactors have received great interest in recent years, due to their small size, stability, high gas-liquid interfacial area concentrations and longer residence times. The high gas-liquid interfacial area concentrations lead to high mass transfer rates compared to conventional bubble column reactors. In the present work, experiments have been performed in a down-flow bubble column reactor with micro-bubbles generated and dispersed by a novel mechanism to determine the gas-liquid interfacial area concentrations by measuring the void fraction and bubble size distributions. Gamma-ray densitometry has been employed to determine the axial and radial distributions of void fractionmore » and a high speed camera equipped with a borescope is used to measure the axial and radial variations of bubble sizes. Also, the effects of superficial gas and liquid velocities on the two-phase flow characteristics have been investigated. Further, reconstruction techniques of the radial void fraction profiles from the gamma densitometry's chordal measurements are discussed and compared for a bubble column reactor with dispersed micro-bubbles. The results demonstrate that the new bubble generation technique offers high interfacial area concentrations (1,000 to 4,500 m 2/m 3) with sub-millimeter bubbles (500 to 900 µm) and high overall void fractions (10% – 60%) in comparison with previous bubble column reactor designs. The void fraction data was analyzed using slip velocity model and empirical correlation has been proposed to predict the Sauter mean bubble diameter.« less

Damage Detection of a Concrete Column Subject to Blast Loads Using Embedded Piezoceramic Transducers.

PubMed

Xu, Kai; Deng, Qingshan; Cai, Lujun; Ho, Siuchun; Song, Gangbing

2018-04-28

Some of the most severe structural loadings come in the form of blast loads, which may be caused by severe accidents or even terrorist activities. Most commonly after exposure to explosive forces, a structure will suffer from different degrees of damage, and even progress towards a state of collapse. Therefore, damage detection of a structure subject to explosive loads is of importance. This paper proposes a new approach to damage detection of a concrete column structure subjected to blast loads using embedded piezoceramic smart aggregates (SAs). Since the sensors are embedded in the structure, the proposed active-sensing based approach is more sensitive to internal or through cracks than surface damage. In the active sensing approach, the embedded SAs act as actuators and sensors, that can respectively generate and detect stress waves. If the stress wave propagates across a crack, the energy of the wave attenuates, and the reduction of the energy compared to the healthy baseline is indicative of a damage. With a damage index matrix constructed by signals obtained from an array of SAs, cracks caused by blast loads can be detected throughout the structure. Conventional sensing methods such as the measurement of dynamic strain and acceleration were included in the experiment. Since columns are critical elements needed to prevent structural collapse, knowledge of their integrity and damage conditions is essential for safety after exposure to blast loads. In this research, a concrete column with embedded SAs was chosen as the specimen, and a series of explosive tests were conducted on the column. Experimental results reveal that surface damages, though appear severe, cause minor changes in the damage index, and through cracks result in significant increase of the damage index, demonstrating the effectiveness of the active sensing, enabled by embedded SAs, in damage monitoring of the column under blast loads, and thus providing a reliable indication of structural integrity in the event of blast loads.

Damage Detection of a Concrete Column Subject to Blast Loads Using Embedded Piezoceramic Transducers

PubMed Central

Deng, Qingshan; Cai, Lujun; Ho, Siuchun; Song, Gangbing

2018-01-01

Some of the most severe structural loadings come in the form of blast loads, which may be caused by severe accidents or even terrorist activities. Most commonly after exposure to explosive forces, a structure will suffer from different degrees of damage, and even progress towards a state of collapse. Therefore, damage detection of a structure subject to explosive loads is of importance. This paper proposes a new approach to damage detection of a concrete column structure subjected to blast loads using embedded piezoceramic smart aggregates (SAs). Since the sensors are embedded in the structure, the proposed active-sensing based approach is more sensitive to internal or through cracks than surface damage. In the active sensing approach, the embedded SAs act as actuators and sensors, that can respectively generate and detect stress waves. If the stress wave propagates across a crack, the energy of the wave attenuates, and the reduction of the energy compared to the healthy baseline is indicative of a damage. With a damage index matrix constructed by signals obtained from an array of SAs, cracks caused by blast loads can be detected throughout the structure. Conventional sensing methods such as the measurement of dynamic strain and acceleration were included in the experiment. Since columns are critical elements needed to prevent structural collapse, knowledge of their integrity and damage conditions is essential for safety after exposure to blast loads. In this research, a concrete column with embedded SAs was chosen as the specimen, and a series of explosive tests were conducted on the column. Experimental results reveal that surface damages, though appear severe, cause minor changes in the damage index, and through cracks result in significant increase of the damage index, demonstrating the effectiveness of the active sensing, enabled by embedded SAs, in damage monitoring of the column under blast loads, and thus providing a reliable indication of structural integrity in the event of blast loads. PMID:29710807

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.

Validated HPLC method for determination of sennosides A and B in senna tablets.

PubMed

Sun, Shao Wen; Su, Hsiu Ting

2002-07-31

This study developed an efficient and reliable ion-pair liquid chromatographic method for quantitation of sennosides A and B in commercial senna tablets. Separation was conducted on a Hypersil C 18 column (250 x 4.6 mm, 5 microm) at a temperature of 40 degrees C, using a mixture of 0.1 M acetate buffer (pH 6.0) and acetonitrile (70:30, v/v) containing 5 mM tetrahexylammonium bromide as mobile phase. Sennosides A and B were completely separated from other constituents within 14 min. The developed method was validated. Both run-to-run repeatability (n=10) and day-to-day reproducibility (n=3) of peak area were below 0.4% RSD. Linearity of peak area was tested in the range 30-70 microg/ml (r>0.9997). Accuracy was assessed with recovery and the recoveries for sennosides A and B were 101.73+/-1.30% and 101.81+/-2.18% (n=3 x 6), respectively. Robustness of the analytical method was tested using a three-leveled Plackett-Burman design in which 11 factors were assessed with 23 experiments. Eight factors (column, concentration of ion pair reagent, % of organic modifier (acetonitrile), buffer pH, column temperature, flow rate, time constant and detection wavelength) were investigated in a specified range above and below the nominal method conditions. It was found that: (1) column and % acetonitrile affected significantly resolution and retention time, (2) column, % acetonitrile, column temperature, flow rate and time constant affected significantly the plate number of sennoside A, and (3) column and time constant affected significantly the tailing factor.

In-situ polymerization PLOT columns I: divinylbenzene

NASA Technical Reports Server (NTRS)

Shen, T. C.

1992-01-01

A novel method for preparation of porous-layer open-tubular (PLOT) columns is described. The method involves a simple and reproducible, straight-forward in-situ polymerization of monomer directly on the metal tube.

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.

Detecting overpressure using the Eaton and Equivalent Depth methods in Offshore Nova Scotia, Canada

NASA Astrophysics Data System (ADS)

Ernanda; Primasty, A. Q. T.; Akbar, K. A.

2018-03-01

Overpressure is an abnormal high subsurface pressure of any fluids which exceeds the hydrostatic pressure of column of water or formation brine. In Offshore Nova Scotia Canada, the values and depth of overpressure zone are determined using the eaton and equivalent depth method, based on well data and the normal compaction trend analysis. Since equivalent depth method is using effective vertical stress principle and Eaton method considers physical property ratio (velocity). In this research, pressure evaluation only applicable on Penobscot L-30 well. An abnormal pressure is detected at depth 11804 feet as possibly overpressure zone, based on pressure gradient curve and calculation between the Eaton method (7241.3 psi) and Equivalent Depth method (6619.4 psi). Shales within Abenaki formation especially Baccaro Member is estimated as possible overpressure zone due to hydrocarbon generation mechanism.

Evaluation of ODS-AQ stationary phase for use in capillary electrochromatography.

PubMed

Djordjevic, N M; Fitzpatrick, F; Houdiere, F

2001-04-01

The aim of this study was to evaluate the applicability of ODS-AQ packing material as a stationary phase in capillary electrochromatography (CEC). The electroosmotic flow created on an ODS-AQ stationary phase was measured at different mobile phase compositions and at different column temperatures. It was observed that the electroosmotic flow generated in the column increased by 50% when the temperature of the system was raised from 20 degrees C to 60 degrees C, while all other conditions were kept constant. The electroosmotic flow produced by the ODS-AQ stationary phase was found to be comparable to the flow generated in a column packed with Nucleosil bare-silica material. In addition, a set of polar compounds (D-lysergic acid diethylamide derivatives) was utilized to determine the influence of temperature and mobile phase composition on their chromatographic behavior on an ODS-AQ stationary phase in a CEC mode. A linear relationship between the solute retention factor and column temperatures was seen over the temperature range studied (20 degrees C to 60 degrees C). A quadratic function was used to describe the changes in the solute retention factors with variation of acetonitrile concentration in the mobile phase.

Using the fundamentals of adsorption to understand peak distortion due to strong solvent effect in hydrophilic interaction chromatography.

PubMed

Gritti, Fabrice; Sehajpal, Jyotsna; Fairchild, Jacob

2017-03-17

The peak distortion observed in hydrophilic interaction chromatography (HILIC) may be caused by the sample diluent to mobile phase mismatch. The United States Pharmacopeia (USP) method for organic impurities in cetirizine HCl tablets calls for such a mismatch, having a higher concentration of strong solvent in the sample diluent than in the mobile phase. A significant peak deformation is reported for cetirizine (a second-generation antihistamine) when it is purified on a Ethylene Bridged Hybrid (BEH) HILIC column (4.6mm×100mm, 2.5μm particles) using an acetonitrile-water eluent mixture and a sample diluent containing 7% and 9% water (in volume), respectively. The mechanism and physical origin of such peak distortion are related to (1) the diluent-to-eluent excess of water that propagates along the column at a velocity similar to that of the analyte, (2) the significant drop of the Henry's constant of the analyte upon increasing water concentration in the eluent, (3) the sample volume injected, and (4) to the pre-column sample dilution factor that depends on the characteristics of the LC instrument used. This proposed mechanism is validated from the calculation of the concentration profiles of cetirizine and water by using the equilibrium-dispersive (ED) model of chromatography. The observed distortion of cetirizine peaks is successfully predicted from the measurement of (1) the excess adsorption isotherm of water from acetonitrile onto the BEH HILIC adsorbent, (2) the retention factor of cetirizine as a function of the volume fraction (7, 8, and 9%) of water in the mobile phase, and (3) of the pre-column sample dispersion related to the instrument used (HPLC or UHPLC). The results of the calculations enables the user to anticipate the impacts of the diluent-to-eluent mismatch in water content, the injection volume, the analyte retention under infinite dilution, and of the pre-column sample dispersion on the amplitude of peak distortion in HILIC. Appropriate and permitted alterations of the USP method are then suggested based on a sound physico-chemical approach. Copyright © 2017 Elsevier B.V. All rights reserved.

Rapid column heating method for subcritical water chromatography.

PubMed

Fogwill, Michael O; Thurbide, Kevin B

2007-01-19

A novel resistive heating method is presented for subcritical water chromatography (SWC) that provides higher column heating rates than those conventionally obtained from temperature-programmed gas chromatography (GC) convection ovens. Since the polarity of water reduces dramatically with increasing temperature, SWC employs column heating to achieve gradient elution. As such, the rate at which the mobile phase is heated directly impacts the magnitude of such gradients applied in SWC. Data from the current study demonstrate that the maximum column heating rate attainable in a typical SWC apparatus (i.e. using a GC convection oven) is around 10 degrees C/min, even at instrument oven settings of over three times this value. Conversely, by wrapping the separation column with ceramic insulation and a resistively heated wire, the column heating rates are increased five-fold. As a result, elution times can be greatly decreased in SWC employing gradients. Separations of standard alcohol test mixtures demonstrate that the retention time of the latest eluting component decreases by 35 to 50% using the prototype method. Additionally, solute retention times in this mode deviate by less than 1% RSD over several trials, which compares very well to those obtained using a conventional GC convection oven. Results suggest that the developed method can be a useful alternative heating technique in SWC.

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

PubMed

Ren, Yu; Schlager, Hans; Martin, Damien

2014-01-01

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

Next Generation Clustered Heat Maps | Informatics Technology for Cancer Research (ITCR)

Cancer.gov

Next-Generation (Clustered) Heat Maps are interactive heat maps that enable the user to zoom and pan across the heatmap, alter its color scheme, generate production quality PDFs, and link out from rows, columns, and individual heatmap entries to related statistics, databases and other information.

Investigation of radioactivity concentration in spent technetium generators

NASA Astrophysics Data System (ADS)

Idriss, Hajo; Salih, Isam; Alaamer, Abdulaziz S.; Eisa, M. H.; Sam, A. K.

2014-04-01

This study was carried out to survey and measure radioactivity concentration and estimate radiation dose level at the surface of spent technetium generator columns for the safe final disposal of radioactive waste. High resolution γ-spectrometry with the aid of handheld radiation survey meters has been used. The radioactivity measurements has shown that 238U, 40K and 137Cs were only measurable in one sample whereas 125Sb was found in 14 samples out of total of 20 samples with an activity concentration which ranged from 21 to 7404 with an average value of 1095 Bq/kg. The activity concentration of 125Sb is highly variable indicating that the spent 99mTc generator columns are of different origin. This investigation highlighted the importance of radiation monitoring of spent technetium generators in the country in order to protect workers, and the public from the dangers posed by radioactive waste.

Optimization of Feasibility Stage for Hydrogen/Deuterium Exchange Mass Spectrometry

NASA Astrophysics Data System (ADS)

Hamuro, Yoshitomo; Coales, Stephen J.

2018-03-01

The practice of HDX-MS remains somewhat difficult, not only for newcomers but also for veterans, despite its increasing popularity. While a typical HDX-MS project starts with a feasibility stage where the experimental conditions are optimized and the peptide map is generated prior to the HDX study stage, the literature usually reports only the HDX study stage. In this protocol, we describe a few considerations for the initial feasibility stage, more specifically, how to optimize quench conditions, how to tackle the carryover issue, and how to apply the pepsin specificity rule. Two sets of quench conditions are described depending on the presence of disulfide bonds to facilitate the quench condition optimization process. Four protocols are outlined to minimize carryover during the feasibility stage: (1) addition of a detergent to the quench buffer, (2) injection of a detergent or chaotrope to the protease column after each sample injection, (3) back-flushing of the trap column and the analytical column with a new plumbing configuration, and (4) use of PEEK (or PEEK coated) frits instead of stainless steel frits for the columns. The application of the pepsin specificity rule after peptide map generation and not before peptide map generation is suggested. The rule can be used not only to remove falsely identified peptides, but also to check the sample purity. A well-optimized HDX-MS feasibility stage makes subsequent HDX study stage smoother and the resulting HDX data more reliable. [Figure not available: see fulltext.

Intrinsic advantages of packed capillaries over narrow-bore columns in very high-pressure gradient liquid chromatography.

PubMed

Gritti, Fabrice; McDonald, Thomas; Gilar, Martin

2016-06-17

250μm×100mm fused silica glass capillaries were packed with 1.8μm high-strength silica (HSS) fully porous particles. They were prepared without bulky stainless steel endfittings and metal frits, which both generate significant sample dispersion. The isocratic efficiencies and gradient peak capacities of these prototype capillary columns were measured for small molecules (n-alkanophenones) using a home-made ultra-low dispersive micro-HPLC instrument. Their resolution power was compared to that of standard 2.1mm×100mm very high-pressure liquid chromatography (vHPLC) narrow-bore columns packed with the same particles. The results show that, for the same column efficiency (25000 plates) and gradient steepness (0.04min(-1)), the peak capacity of the 250μm i.d. capillary columns is systematically 15-20% higher than that of the 2.1mm i.d. narrow-bore columns. A validated model of gradient chromatography enabled one to predict accurately the observed peak capacities of the capillary columns for non-linear solvation strength retention behavior and under isothermal conditions. Thermodynamics applied to the eluent quantified the temperature difference for the thermal gradients in both capillary and narrow-bore columns. Experimental data revealed that the gradient peak capacity is more affected by viscous heating than the column efficiency. Unlike across 2.1mm i.d. columns, the changes in eluent composition across the 250μm i.d. columns during the gradient is rapidly relaxed by transverse dispersion. The combination of (1) the absence of viscous heating and (2) the high uniformity of the eluent composition across the diameter of capillary columns explains the intrinsic advantage of capillary over narrow-bore columns in gradient vHPLC. Copyright © 2016 Elsevier B.V. All rights reserved.

Mobile autonomous robotic apparatus for radiologic characterization

DOEpatents

Dudar, Aed M.; Ward, Clyde R.; Jones, Joel D.; Mallet, William R.; Harpring, Larry J.; Collins, Montenius X.; Anderson, Erin K.

1999-01-01

A mobile robotic system that conducts radiological surveys to map alpha, beta, and gamma radiation on surfaces in relatively level open areas or areas containing obstacles such as stored containers or hallways, equipment, walls and support columns. The invention incorporates improved radiation monitoring methods using multiple scintillation detectors, the use of laser scanners for maneuvering in open areas, ultrasound pulse generators and receptors for collision avoidance in limited space areas or hallways, methods to trigger visible alarms when radiation is detected, and methods to transmit location data for real-time reporting and mapping of radiation locations on computer monitors at a host station. A multitude of high performance scintillation detectors detect radiation while the on-board system controls the direction and speed of the robot due to pre-programmed paths. The operators may revise the preselected movements of the robotic system by ethernet communications to remonitor areas of radiation or to avoid walls, columns, equipment, or containers. The robotic system is capable of floor survey speeds of from 1/2-inch per second up to about 30 inches per second, while the on-board processor collects, stores, and transmits information for real-time mapping of radiation intensity and the locations of the radiation for real-time display on computer monitors at a central command console.

Mobile autonomous robotic apparatus for radiologic characterization

DOEpatents

Dudar, A.M.; Ward, C.R.; Jones, J.D.; Mallet, W.R.; Harpring, L.J.; Collins, M.X.; Anderson, E.K.

1999-08-10

A mobile robotic system is described that conducts radiological surveys to map alpha, beta, and gamma radiation on surfaces in relatively level open areas or areas containing obstacles such as stored containers or hallways, equipment, walls and support columns. The invention incorporates improved radiation monitoring methods using multiple scintillation detectors, the use of laser scanners for maneuvering in open areas, ultrasound pulse generators and receptors for collision avoidance in limited space areas or hallways, methods to trigger visible alarms when radiation is detected, and methods to transmit location data for real-time reporting and mapping of radiation locations on computer monitors at a host station. A multitude of high performance scintillation detectors detect radiation while the on-board system controls the direction and speed of the robot due to pre-programmed paths. The operators may revise the preselected movements of the robotic system by ethernet communications to remonitor areas of radiation or to avoid walls, columns, equipment, or containers. The robotic system is capable of floor survey speeds of from 1/2-inch per second up to about 30 inches per second, while the on-board processor collects, stores, and transmits information for real-time mapping of radiation intensity and the locations of the radiation for real-time display on computer monitors at a central command console. 4 figs.

High performance liquid chromatographic method for the determination of cetirizine and ambroxol in human plasma and urine--a boxcar approach.

PubMed

Dharuman, J; Vasudhevan, M; Ajithlal, T

2011-09-01

A column switching high performance liquid chromatographic method with estimable sensitivity and accuracy was developed for the determination of cetirizine and ambroxol in human plasma using nebivolol as the internal standard. Plasma samples were prepared by liquid-liquid extraction in methylene chloride and a mixture of diethylether (80:20, v/v). The extracted samples were injected into a multifunctional clean-up column Supelcosil LCABZ (50 mm × 4.6 mm, 5 μm particle size) using mobile phase 1 comprising acetonitrile-phosphate buffer (pH 3.5; 20 mM) (20:80, v/v). The eluate of cetirizine and ambroxol were separated to an analytical Kromasil C(8) micro bore column (50 mm × 0.3 mm, 5 μm particle size) via a column switching device. A Kromasil C(18) analytical column (250 mm × 2.1 mm, 5 μm particle size) was used as a separation column. Mobile phase 2 consisting acetonitrile-triethylamine (0.5%) in phosphate buffer (pH 3.5; 20mM) (55:45, v/v) was used for the compound elution. The eluents were detected at 230 nm with photodiode array detector. An aliquot of 150 μl of plasma sample was introduced into the pretreatment column via the auto sampler using mobile phase 1 at a flow rate of 0.5 ml/min, column switching valve being positioned at A. The pretreatment column retained cetirizine, ambroxol and nebivolol (IS) in the column leaving the residual proteins of plasma eluted in void volume and drained out. The switching valve was shifted to position B at 7.5 min. Cetirizine, ambroxol and IS were eluted from the pretreatment column between 7. 5 and 11.5 min and introduced to the concentration column. Finally, cetirizine, ambroxol and IS were introduced to the separation column by switching valve using mobile phase 2 at a flow rate of 0.4 ml/min. During the analysis the pretreatment column was washed for the next analysis and resume to the position A. The total run time was 25 min for a sample. The procedure was repeated for urine analysis also. The method was linear from 2 to 450 ng/ml and 7-300 ng/ml for cetirizine and ambroxol respectively in plasma and 1-500 ng/ml and 5-400 ng/ml, respectively for cetirizine and ambroxol in urine. Intra-day and inter-day precision of cetirizine and ambroxol was below 15% in terms of coefficient of variation and accuracy of cetirizine and ambroxol was ranged from 94 to 101.6% and 91.1 to 100.2%, respectively. The method demonstrated high sensitivity and selectivity and therefore, applied to evaluate pharmacokinetics of cetirizine and ambroxol in healthy human volunteer after a single oral administration. Urine samples obtained from healthy human volunteers and clinical subjects with renal impairment have also been analyzed by the method to compare the elimination pattern. The method was precise and accurate for the estimation of cetirizine and ambroxol both in blood and in urine. Copyright © 2011 Elsevier B.V. All rights reserved.

Theoretical study of the accuracy of the pulse method, frontal analysis, and frontal analysis by characteristic points for the determination of single component adsorption isotherms.

PubMed

Andrzejewska, Anna; Kaczmarski, Krzysztof; Guiochon, Georges

2009-02-13

The adsorption isotherms of selected compounds are our main source of information on the mechanisms of adsorption processes. Thus, the selection of the methods used to determine adsorption isotherm data and to evaluate the errors made is critical. Three chromatographic methods were evaluated, frontal analysis (FA), frontal analysis by characteristic point (FACP), and the pulse or perturbation method (PM), and their accuracies were compared. Using the equilibrium-dispersive (ED) model of chromatography, breakthrough curves of single components were generated corresponding to three different adsorption isotherm models: the Langmuir, the bi-Langmuir, and the Moreau isotherms. For each breakthrough curve, the best conventional procedures of each method (FA, FACP, PM) were used to calculate the corresponding data point, using typical values of the parameters of each isotherm model, for four different values of the column efficiency (N=500, 1000, 2000, and 10,000). Then, the data points were fitted to each isotherm model and the corresponding isotherm parameters were compared to those of the initial isotherm model. When isotherm data are derived with a chromatographic method, they may suffer from two types of errors: (1) the errors made in deriving the experimental data points from the chromatographic records; (2) the errors made in selecting an incorrect isotherm model and fitting to it the experimental data. Both errors decrease significantly with increasing column efficiency with FA and FACP, but not with PM.

Fourier-space combination of Planck and Herschel images

NASA Astrophysics Data System (ADS)

Abreu-Vicente, J.; Stutz, A.; Henning, Th.; Keto, E.; Ballesteros-Paredes, J.; Robitaille, T.

2017-08-01

Context. Herschel has revolutionized our ability to measure column densities (NH) and temperatures (T) of molecular clouds thanks to its far infrared multiwavelength coverage. However, the lack of a well defined background intensity level in the Herschel data limits the accuracy of the NH and T maps. Aims: We aim to provide a method that corrects the missing Herschel background intensity levels using the Planck model for foreground Galactic thermal dust emission. For the Herschel/PACS data, both the constant-offset as well as the spatial dependence of the missing background must be addressed. For the Herschel/SPIRE data, the constant-offset correction has already been applied to the archival data so we are primarily concerned with the spatial dependence, which is most important at 250 μm. Methods: We present a Fourier method that combines the publicly available Planck model on large angular scales with the Herschel images on smaller angular scales. Results: We have applied our method to two regions spanning a range of Galactic environments: Perseus and the Galactic plane region around l = 11deg (HiGal-11). We post-processed the combined dust continuum emission images to generate column density and temperature maps. We compared these to previously adopted constant-offset corrections. We find significant differences (≳20%) over significant ( 15%) areas of the maps, at low column densities (NH ≲ 1022 cm-2) and relatively high temperatures (T ≳ 20 K). We have also applied our method to synthetic observations of a simulated molecular cloud to validate our method. Conclusions: Our method successfully corrects the Herschel images, including both the constant-offset intensity level and the scale-dependent background variations measured by Planck. Our method improves the previous constant-offset corrections, which did not account for variations in the background emission levels. The image FITS files used in this paper are only available at the CDS via anonymous ftp to http://cdsarc.u-strasbg.fr (http://130.79.128.5) or via http://cdsarc.u-strasbg.fr/viz-bin/qcat?J/A+A/604/A65

Systems and methods for reactive distillation with recirculation of light components

DOEpatents

Stickney, Michael J [Nassau Bay, TX; Jones, Jr., Edward M.

2011-07-26

Systems and methods for producing gas-to-liquids products using reactive distillation are provided. The method for producing gas-to-liquids products can include reacting a feedstock in a column having a distillation zone and a reaction zone to provide a bottoms stream and an overhead stream. A first portion of the overhead stream can be recycled to the column at the top of the reaction zone and second portion of the overhead stream can be recycled to the column at the bottom of the reaction zone.

Method for converting sucrose to .beta.-D-glucose

DOEpatents

Simmons, Blake A [San Francisco, CA; Volponi, Joanne V [Livermore, CA; Ingersoll, David [Albuquerque, NM; Walker, Andrew [Woodinville, WA

2009-07-07

Disclosed is an apparatus and method for continuously converting sucrose to .beta.-D-glucose. The method comprises a three-stage enzymatic reactor in which an aqueous solution of sucrose is first converted into a solution of fructose and .alpha.-D-glucose by passing it through a porous, packed column containing an inert media on which invertase is immobilized. This solution is then sent through a second packed column containing glucose isomerase and finally a third packed column containing mutarotase. Solution temperature and pH are adjusted to maximize glucose output.

A comparison of in situ methods for measuring net nitrogen mineralization rates of organic soil amendments.

PubMed

Hanselman, Travis A; Graetz, Donald A; Obreza, Thomas A

2004-01-01

In situ incubation methods may help provide site-specific estimates of N mineralization from land-applied wastes. However, there are concerns about the reliability of the data generated by the various methods due to containment artifacts. We amended a sandy soil with either poultry manure, biosolids, or yard-waste compost and incubated the mixtures using four in situ methods (buried bags, covered cylinders, standard resin traps, and "new" soil-resin traps) and a conventional laboratory technique in plastic bags. Each incubation device was destructively sampled at 45-d intervals for 180 d and net N mineralization was determined by measuring the amount of inorganic N that accumulated in the soil or soil plus resin traps. Containment effects were evaluated by comparing water content of the containerized soil to a field-reference soil column. In situ incubation methods provided reasonable estimates of short-term (< 45 d) N mineralization, but long-term (> 45 d) mineralization data were not accurate due to a variety of problems specific to each technique. Buried bags and covered cylinders did not retain mineralized N due to water movement into and out of the containers. Neither resin method captured all of the mineralized N that leached through the soil columns, but the new soil-resin trap method tracked field soil water content better than all other in situ methods evaluated. With further refinement and validation, the new soil-resin trap method may be a useful in situ incubation technique for measuring net N mineralization rates of organic soil amendments.

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.

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.

Improvement of pre-treatment method for 36Cl/Cl measurement of Cl in natural groundwater by AMS

NASA Astrophysics Data System (ADS)

Nakata, Kotaro; Hasegawa, Takuma

2011-02-01

Estimation of 36Cl/Cl by accelerator mass spectrometry (AMS) is a useful method to trace hydrological processes in groundwater. For accurate estimation, separation of SO42- from Cl - in groundwater is required because 36S affects AMS measurement of 36Cl. Previous studies utilized the difference in solubility between BaSO 4 and BaCl 2 (BaSO 4 method) to chemically separate SO42- from Cl -. However, the accuracy of the BaSO 4 method largely depends on operator skill, and consequently Cl - recovery is typically incomplete (70-80%). In addition, the method is time consuming (>1 week), and cannot be applied directly to dilute solutions. In this study, a method based on ion-exchange column chromatography (column method) was developed for separation of Cl - and SO42-. Optimum conditions were determined for the diameter and height of column, type and amount of resin, type and concentration of eluent, and flow rate. The recovery of Cl - was almost 100%, which allowed complete separation from SO42-. The separation procedure was short (<6 h), and was successfully applied to dilute (1 mg/L Cl) solution. Extracted pore water and diluted seawater samples were processed by the column and BaSO 4 methods, and then analyzed by AMS to estimate 36S counts and 36Cl/Cl values. 36S counts in samples processed by the column method were stable and lower than those from the BaSO 4 method. The column method has the following advantages over the BaSO 4 method: (1) complete and stable separation of Cl - and SO42-, (2) less operator influence on results, (3) short processing time (<6 h), (4) high (almost 100%) recovery of Cl -, and (5) concentration of Cl - and separation from SO42- in the one system for dilute solutions.

Application of Snyder-Dolan classification scheme to the selection of "orthogonal" columns for fast screening of illicit drugs and impurity profiling of pharmaceuticals--I. Isocratic elution.

PubMed

Fan, Wenzhe; Zhang, Yu; Carr, Peter W; Rutan, Sarah C; Dumarey, Melanie; Schellinger, Adam P; Pritts, Wayne

2009-09-18

Fourteen judiciously selected reversed phase columns were tested with 18 cationic drug solutes under the isocratic elution conditions advised in the Snyder-Dolan (S-D) hydrophobic subtraction method of column classification. The standard errors (S.E.) of the least squares regressions of logk' vs. logk'(REF) were obtained for a given column against a reference column and used to compare and classify columns based on their selectivity. The results are consistent with those obtained with a study of the 16 test solutes recommended by Snyder and Dolan. To the extent these drugs are representative, these results show that the S-D classification scheme is also generally applicable to pharmaceuticals under isocratic conditions. That is, those columns judged to be similar based on the 16 S-D solutes were similar based on the 18 drugs; furthermore those columns judged to have significantly different selectivities based on the 16 S-D probes appeared to be quite different for the drugs as well. Given that the S-D method has been used to classify more than 400 different types of reversed phases the extension to cationic drugs is a significant finding.

Self-Interaction Chromatography of mAbs: Accurate Measurement of Dead Volumes.

PubMed

Hedberg, S H M; Heng, J Y Y; Williams, D R; Liddell, J M

2015-12-01

Measurement of the second virial coefficient B22 for proteins using self-interaction chromatography (SIC) is becoming an increasingly important technique for studying their solution behaviour. In common with all physicochemical chromatographic methods, measuring the dead volume of the SIC packed column is crucial for accurate retention data; this paper examines best practise for dead volume determination. SIC type experiments using catalase, BSA, lysozyme and a mAb as model systems are reported, as well as a number of dead column measurements. It was observed that lysozyme and mAb interacted specifically with Toyopearl AF-Formyl dead columns depending upon pH and [NaCl], invalidating their dead volume usage. Toyopearl AF-Amino packed dead columns showed no such problems and acted as suitable dead columns without any solution condition dependency. Dead volume determinations using dextran MW standards with protein immobilised SIC columns provided dead volume estimates close to those obtained using Toyopearl AF-Amino dead columns. It is concluded that specific interactions between proteins, including mAbs, and select SIC support phases can compromise the use of some standard approaches for estimating the dead volume of SIC columns. Two other methods were shown to provide good estimates for the dead volume.

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

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.

Deconvolution of gas chromatographic data

NASA Technical Reports Server (NTRS)

Howard, S.; Rayborn, G. H.

1980-01-01

The use of deconvolution methods on gas chromatographic data to obtain an accurate determination of the relative amounts of each material present by mathematically separating the merged peaks is discussed. Data were obtained on a gas chromatograph with a flame ionization detector. Chromatograms of five xylenes with differing degrees of separation were generated by varying the column temperature at selected rates. The merged peaks were then successfully separated by deconvolution. The concept of function continuation in the frequency domain was introduced in striving to reach the theoretical limit of accuracy, but proved to be only partially successful.

SU-E-T-395: Multi-GPU-Based VMAT Treatment Plan Optimization Using a Column-Generation Approach

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

Tian, Z; Shi, F; Jia, X

Purpose: GPU has been employed to speed up VMAT optimizations from hours to minutes. However, its limited memory capacity makes it difficult to handle cases with a huge dose-deposition-coefficient (DDC) matrix, e.g. those with a large target size, multiple arcs, small beam angle intervals and/or small beamlet size. We propose multi-GPU-based VMAT optimization to solve this memory issue to make GPU-based VMAT more practical for clinical use. Methods: Our column-generation-based method generates apertures sequentially by iteratively searching for an optimal feasible aperture (referred as pricing problem, PP) and optimizing aperture intensities (referred as master problem, MP). The PP requires accessmore » to the large DDC matrix, which is implemented on a multi-GPU system. Each GPU stores a DDC sub-matrix corresponding to one fraction of beam angles and is only responsible for calculation related to those angles. Broadcast and parallel reduction schemes are adopted for inter-GPU data transfer. MP is a relatively small-scale problem and is implemented on one GPU. One headand- neck cancer case was used for test. Three different strategies for VMAT optimization on single GPU were also implemented for comparison: (S1) truncating DDC matrix to ignore its small value entries for optimization; (S2) transferring DDC matrix part by part to GPU during optimizations whenever needed; (S3) moving DDC matrix related calculation onto CPU. Results: Our multi-GPU-based implementation reaches a good plan within 1 minute. Although S1 was 10 seconds faster than our method, the obtained plan quality is worse. Both S2 and S3 handle the full DDC matrix and hence yield the same plan as in our method. However, the computation time is longer, namely 4 minutes and 30 minutes, respectively. Conclusion: Our multi-GPU-based VMAT optimization can effectively solve the limited memory issue with good plan quality and high efficiency, making GPUbased ultra-fast VMAT planning practical for real clinical use.« less

Optimization of SHINE Process: Design and Verification of Plant-Scale AG 1 Anion-Exchange Concentration Column and Titania Sorbent Pretreatment

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

Stepinski, Dominique C.; Abdul, Momen; Youker, Amanda J.

2016-06-01

Argonne National Laboratory has developed a Mo-recovery and -purification system for the SHINE medical technologies process, which uses a uranyl sulfate solution for the accelerator-driven production of Mo-99. The objective of this effort is to reduce the processing time for the acidification of the Mo-99 product prior to loading onto a concentration column and concentration of the Mo-99 product solution. Two methods were investigated: (1) the replacement of the titania concentration column by an anion-exchange column to decrease processing time and increase the radioiodine-decontamination efficiency and (2) pretreatment of the titania sorbent to improve its effectiveness for the Mo-recovery andmore » -concentration columns. Promising results are reported for both methods.« less

In situ iron activated persulfate oxidative fluid sparging treatment of TCE contamination--a proof of concept study.

PubMed

Liang, Chenju; Lee, I-Ling

2008-09-10

In situ chemical oxidation (ISCO) is considered a reliable technology to treat groundwater contaminated with high concentrations of organic contaminants. An ISCO oxidant, persulfate anion (S(2)O(8)(2-)) can be activated by ferrous ion (Fe(2+)) to generate sulfate radicals (E(o)=2.6 V), which are capable of destroying trichloroethylene (TCE). The property of polarity inhibits S(2)O(8)(2-) or sulfate radical (SO(4)(-)) from effectively oxidizing separate phase TCE, a dense non-aqueous phase liquid (DNAPL). Thus the oxidation primarily takes place in the aqueous phase where TCE is dissolved. A bench column study was conducted to demonstrate a conceptual remediation method by flushing either S(2)O(8)(2-) or Fe(2+) through a soil column, where the TCE DNAPL was present, and passing the dissolved mixture through either a Fe(2+) or S(2)O(8)(2-) fluid sparging curtain. Also, the effect of a solubility enhancing chemical, hydroxypropyl-beta-cyclodextrin (HPCD), was tested to evaluate its ability to increase the aqueous TCE concentration. Both flushing arrangements may result in similar TCE degradation efficiencies of 35% to 42% estimated by the ratio of TCE degraded/(TCE degraded+TCE remained in effluent) and degradation byproduct chloride generation rates of 4.9 to 7.6 mg Cl(-) per soil column pore volume. The addition of HPCD did greatly increase the aqueous TCE concentration. However, the TCE degradation efficiency decreased because the TCE degradation was a lower percentage of the relatively greater amount of dissolved TCE by HPCD. This conceptual treatment may serve as a reference for potential on-site application.

A set-covering based heuristic algorithm for the periodic vehicle routing problem.

PubMed

Cacchiani, V; Hemmelmayr, V C; Tricoire, F

2014-01-30

We present a hybrid optimization algorithm for mixed-integer linear programming, embedding both heuristic and exact components. In order to validate it we use the periodic vehicle routing problem (PVRP) as a case study. This problem consists of determining a set of minimum cost routes for each day of a given planning horizon, with the constraints that each customer must be visited a required number of times (chosen among a set of valid day combinations), must receive every time the required quantity of product, and that the number of routes per day (each respecting the capacity of the vehicle) does not exceed the total number of available vehicles. This is a generalization of the well-known vehicle routing problem (VRP). Our algorithm is based on the linear programming (LP) relaxation of a set-covering-like integer linear programming formulation of the problem, with additional constraints. The LP-relaxation is solved by column generation, where columns are generated heuristically by an iterated local search algorithm. The whole solution method takes advantage of the LP-solution and applies techniques of fixing and releasing of the columns as a local search, making use of a tabu list to avoid cycling. We show the results of the proposed algorithm on benchmark instances from the literature and compare them to the state-of-the-art algorithms, showing the effectiveness of our approach in producing good quality solutions. In addition, we report the results on realistic instances of the PVRP introduced in Pacheco et al. (2011)  [24] and on benchmark instances of the periodic traveling salesman problem (PTSP), showing the efficacy of the proposed algorithm on these as well. Finally, we report the new best known solutions found for all the tested problems.

A set-covering based heuristic algorithm for the periodic vehicle routing problem

PubMed Central

Cacchiani, V.; Hemmelmayr, V.C.; Tricoire, F.

2014-01-01

We present a hybrid optimization algorithm for mixed-integer linear programming, embedding both heuristic and exact components. In order to validate it we use the periodic vehicle routing problem (PVRP) as a case study. This problem consists of determining a set of minimum cost routes for each day of a given planning horizon, with the constraints that each customer must be visited a required number of times (chosen among a set of valid day combinations), must receive every time the required quantity of product, and that the number of routes per day (each respecting the capacity of the vehicle) does not exceed the total number of available vehicles. This is a generalization of the well-known vehicle routing problem (VRP). Our algorithm is based on the linear programming (LP) relaxation of a set-covering-like integer linear programming formulation of the problem, with additional constraints. The LP-relaxation is solved by column generation, where columns are generated heuristically by an iterated local search algorithm. The whole solution method takes advantage of the LP-solution and applies techniques of fixing and releasing of the columns as a local search, making use of a tabu list to avoid cycling. We show the results of the proposed algorithm on benchmark instances from the literature and compare them to the state-of-the-art algorithms, showing the effectiveness of our approach in producing good quality solutions. In addition, we report the results on realistic instances of the PVRP introduced in Pacheco et al. (2011)  [24] and on benchmark instances of the periodic traveling salesman problem (PTSP), showing the efficacy of the proposed algorithm on these as well. Finally, we report the new best known solutions found for all the tested problems. PMID:24748696

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.

Iridium 191-m generator

DOEpatents

Treves, S.; Cheng, C.C.

1988-03-08

Potassium osmate, of the formula K[sub 2]OsO[sub 2](OH)[sub 4], is used to make a column for the generation of Ir-191 m, which is used in first pass angiography to detect cardiac defects in patients. 2 figs.

The analysis of carbohydrates in milk powder by a new "heart-cutting" two-dimensional liquid chromatography method.

PubMed

Ma, Jing; Hou, Xiaofang; Zhang, Bing; Wang, Yunan; He, Langchong

2014-03-01

In this study, a new"heart-cutting" two-dimensional liquid chromatography method for the simultaneous determination of carbohydrate contents in milk powder was presented. In this two dimensional liquid chromatography system, a Venusil XBP-C4 analysis column was used in the first dimension ((1)D) as a pre-separation column, a ZORBAX carbohydrates analysis column was used in the second dimension ((2)D) as a final-analysis column. The whole process was completed in less than 35min without a particular sample preparation procedure. The capability of the new two dimensional HPLC method was demonstrated in the determination of carbohydrates in various brands of milk powder samples. A conventional one dimensional chromatography method was also proposed. The two proposed methods were both validated in terms of linearity, limits of detection, accuracy and precision. The comparison between the results obtained with the two methods showed that the new and completely automated two dimensional liquid chromatography method is more suitable for milk powder sample because of its online cleanup effect involved. Crown Copyright © 2013. Published by Elsevier B.V. All rights reserved.

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.

Myocardial segmentation based on coronary anatomy using coronary computed tomography angiography: Development and validation in a pig model.

PubMed

Chung, Mi Sun; Yang, Dong Hyun; Kim, Young-Hak; Kang, Soo-Jin; Jung, Joonho; Kim, Namkug; Heo, Seung-Ho; Baek, Seunghee; Seo, Joon Beom; Choi, Byoung Wook; Kang, Joon-Won; Lim, Tae-Hwan

2017-10-01

To validate a method for performing myocardial segmentation based on coronary anatomy using coronary CT angiography (CCTA). Coronary artery-based myocardial segmentation (CAMS) was developed for use with CCTA. To validate and compare this method with the conventional American Heart Association (AHA) classification, a single coronary occlusion model was prepared and validated using six pigs. The unstained occluded coronary territories of the specimens and corresponding arterial territories from CAMS and AHA segmentations were compared using slice-by-slice matching and 100 virtual myocardial columns. CAMS more precisely predicted ischaemic area than the AHA method, as indicated by 95% versus 76% (p < 0.001) of the percentage of matched columns (defined as percentage of matched columns of segmentation method divided by number of unstained columns in the specimen). According to the subgroup analyses, CAMS demonstrated a higher percentage of matched columns than the AHA method in the left anterior descending artery (100% vs. 77%; p < 0.001) and mid- (99% vs. 83%; p = 0.046) and apical-level territories of the left ventricle (90% vs. 52%; p = 0.011). CAMS is a feasible method for identifying the corresponding myocardial territories of the coronary arteries using CCTA. • CAMS is a feasible method for identifying corresponding coronary territory using CTA • CAMS is more accurate in predicting coronary territory than the AHA method • The AHA method may underestimate the ischaemic territory of LAD stenosis.

Recent Progress in Monolithic Silica Columns for High-Speed and High-Selectivity Separations.

PubMed

Ikegami, Tohru; Tanaka, Nobuo

2016-06-12

Monolithic silica columns have greater (through-pore size)/(skeleton size) ratios than particulate columns and fixed support structures in a column for chemical modification, resulting in high-efficiency columns and stationary phases. This review looks at how the size range of monolithic silica columns has been expanded, how high-efficiency monolithic silica columns have been realized, and how various methods of silica surface functionalization, leading to selective stationary phases, have been developed on monolithic silica supports, and provides information on the current status of these columns. Also discussed are the practical aspects of monolithic silica columns, including how their versatility can be improved by the preparation of small-sized structural features (sub-micron) and columns (1 mm ID or smaller) and by optimizing reaction conditions for in situ chemical modification with various restrictions, with an emphasis on recent research results for both topics.

Chamber for Aerosol Deposition of Bioparticles

NASA Technical Reports Server (NTRS)

Kern, Roger; Kirschner, Larry

2008-01-01

Laboratory apparatus is depicted that is a chamber for aerosol deposition of bioparticles on surfaces of test coupons. It is designed for primary use in inoculating both flat and three-dimensional objects with approximately reproducible, uniform dispersions of bacterial spores of the genus Bacillus so that the objects could be used as standards for removal of the spores by quantitative surface sampling and/or cleaning processes. The apparatus is also designed for deposition of particles other than bacterial spores, including fungal spores, viruses, bacteriophages, and standard micron-sized beads. The novelty of the apparatus lies in the combination of a controllable nebulization system with a settling chamber large enough to contain a significant number of test coupons. Several companies market other nebulizer systems, but none are known to include chambers for deposition of bioparticles to mimic the natural fallout of bioparticles. The nebulization system is an expanded and improved version of commercially available aerosol generators that include nebulizers and drying columns. In comparison with a typical commercial aerosol generator, this system includes additional, higher-resolution flowmeters and an additional pressure regulator. Also, unlike a typical commercial aerosol generator, it includes stopcocks for separately controlling flows of gases to the nebulizer and drying column. To maximize the degree of uniformity of dispersion of bioaerosol, the chamber is shaped as an axisymmetrical cylinder and the aerosol generator is positioned centrally within the chamber and aimed upward like a fountain. In order to minimize electric charge associated with the aerosol particles, the drying column is made of aluminum, the drying column is in direct contact with an aluminum base plate, and three equally spaced Po-210 antistatic strips are located at the exit end of the drying column. The sides and top of the chamber are made of an acrylic polymer; to prevent accumulation of electric charge on them, they are spray-coated with an anti-static material. During use, the base plate and the sides and top of the chamber are grounded as a further measure to minimize the buildup of electric charge.

Robust Operation of Soft Open Points in Active Distribution Networks with High Penetration of Photovoltaic Integration

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

Ding, Fei; Ji, Haoran; Wang, Chengshan

Distributed generators (DGs) including photovoltaic panels (PVs) have been integrated dramatically in active distribution networks (ADNs). Due to the strong volatility and uncertainty, the high penetration of PV generation immensely exacerbates the conditions of voltage violation in ADNs. However, the emerging flexible interconnection technology based on soft open points (SOPs) provides increased controllability and flexibility to the system operation. For fully exploiting the regulation ability of SOPs to address the problems caused by PV, this paper proposes a robust optimization method to achieve the robust optimal operation of SOPs in ADNs. A two-stage adjustable robust optimization model is built tomore » tackle the uncertainties of PV outputs, in which robust operation strategies of SOPs are generated to eliminate the voltage violations and reduce the power losses of ADNs. A column-and-constraint generation (C&CG) algorithm is developed to solve the proposed robust optimization model, which are formulated as second-order cone program (SOCP) to facilitate the accuracy and computation efficiency. Case studies on the modified IEEE 33-node system and comparisons with the deterministic optimization approach are conducted to verify the effectiveness and robustness of the proposed method.« less

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.

Interpretation of the lime column penetration test

NASA Astrophysics Data System (ADS)

Liyanapathirana, D. S.; Kelly, R. B.

2010-06-01

Dry soil mix (DSM) columns are used to reduce the settlement and to improve the stability of embankments constructed on soft clays. During construction the shear strength of the columns needs to be confirmed for compliance with technical assumptions. A specialized blade shaped penetrometer known as the lime column probe, has been developed for testing DSM columns. This test can be carried out as a pull out resistance test (PORT) or a push in resistance test (PIRT). The test is considered to be more representative of average column shear strength than methods that test only a limited area of the column. Both PORT and PIRT tests require empirical correlations of measured resistance to an absolute measure of shear strength, in a similar manner to the cone penetration test. In this paper, finite element method is used to assess the probe factor, N, for the PORT test. Due to the large soil deformations around the probe, an Arbitrary Lagrangian Eulerian (ALE) based finite element formulation has been used. Variation of N with rigidity index and the friction at the probe-soil interface are investigated to establish a range for the probe factor.

The ability of endotoxin adsorption during a longer duration of direct hemoperfusion with a polymyxin B-immobilized fiber column in patients with septic shock.

PubMed

Shimizu, Tomoharu; Obata, Toru; Sonoda, Hiromichi; Akabori, Hiroya; Tabata, Takahisa; Eguchi, Yutaka; Endo, Yoshihiro; Tani, Tohru

2013-12-01

The patients' hemodynamic conditions of septic shock due to intra-abdominal infection were improved by the longer duration of direct hemoperfusion with a polymyxin B-immobilized fiber column (PMX), reducing plasma endotoxins measured by the novel endotoxin detection method, named endotoxin scattering photometry (ESP) method; however, turbidimetric method could not detect endotoxins. We also observed the reduction in the endotoxin after passing through column by ESP method even after the longer duration of PMX. ESP method may more sensitively detect endotoxins than the ordinary turbidimetric method. Moreover, we demonstrated the ability of endotoxin adsorption in spite of the longer duration of PMX. Copyright © 2013 Elsevier Ltd. All rights reserved.

Device and method for treatment of gases

DOEpatents

Vegge, Olaf Trygve; Brinch, Jon Christian

2007-01-30

The device and method of the present invention employs a column having a gas inlet in its lower part and a gas outlet in its upper part. Carbon particles are introduced into the column through a supply pipe. The supply pipe is movable so that by manipulating the height of the supply pipe in conjunction with discharging particulate matter through the column, the height of the bed of particulate matter in the column can be adjusted so that the retention time of the off gas in the particulate bed is constant. By maintaining a constant retention time of the off gas in the bed, complete conversion of the off gas is achieved.

Rapid, economical qualitative method for separation of aflatoxins B-1, B-2 & G-1, G-2 by dry column chromatography.

PubMed

Megalla, S E

1983-12-01

A good correlation of four components of aflatoxins was accomplished by using the dry column chromatography method. The decolorization process of interfering substances, by 0.01 N KOH and defatting the extract with petroleum ether yields a clean residue for DCC separation. It is clear that the dry column chromatography is a very simple and time-saving procedure for separation of aflatoxins. DCC columns are more economical than precoated 'thick layer' preparative plates and, in DCC, no large developing tanks need to be used. Hazards associated with the use of large volumes of flammable solvents are greatly reduced.

The potential for geostationary remote sensing of NO2 to improve weather prediction

NASA Astrophysics Data System (ADS)

Liu, X.; Mizzi, A. P.; Anderson, J. L.; Fung, I. Y.; Cohen, R. C.

2017-12-01

Observations of surface winds remain sparse making it challenging to simulate and predict the weather in circumstances of light winds that are most important for poor air quality. Direct measurements of short-lived chemicals from space might be a solution to this challenge. Here we investigate the application of data assimilation of NO­2 columns as will be observed from geostationary orbit to improve predictions and retrospective analysis of surface wind fields. Specifically, synthetic NO2 observations are sampled from a "nature run (NR)" regarded as the true atmosphere. Then NO2 observations are assimilated using EAKF methods into a "control run (CR)" which differs from the NR in the wind field. Wind errors are generated by introducing (1) errors in the initial conditions, (2) creating a model error by using two different formulations for the planetary boundary layer, (3) and by combining both of these effects. Assimilation of NO2 column observations succeeds in reducing wind errors, indicating the prospects for future geostationary atmospheric composition measurements to improve weather forecasting are substantial. We find that due to the temporal heterogeneity of wind errors, the success of this application favors chemical observations of high frequency, such as those from geostationary platform. We also show the potential to improve soil moisture field by assimilating NO­2 columns.

Processing and Analysis of Multibeam Sonar Data and Images near the Yellow River Estuary

NASA Astrophysics Data System (ADS)

Tang, Q.

2017-12-01

Yellow River Estuary is a typical high-suspended particulate matter estuary in the world. A lot of sediments from Yellow River and other substances produced by human activity cause high-concentration suspended matter and depositional system in the estuary and adjacent water area. Multibeam echo sounder (MBES) was developed in the 1970s, and it not only provided high-precision bathymetric data, but also provided seabed backscatter strength data and water column data with high temporal and spatial resolution. Here, based on high-precision sonar data of the seabed and water column collected by SeaBat7125 MBES system near the Yellow River Estuary, we use advanced data and image processing methods to generate seabed sonar images and water suspended particulate matter acoustic images. By analyzing these data and images, we get a lot of details of the seabed and whole water column features, and we also acquire their shape, size and basic physical characteristics of suspended particulate matters in the experiment area near the Yellow River Estuary. This study shows great potential for monitoring suspended particulate matter use MBES, and the research results will contribute to a comprehensive understanding of sediment transportation, evolution of river trough and shoal in Yellow River Estuary.

An experiment for determining the Euler load by direct computation

NASA Technical Reports Server (NTRS)

Thurston, Gaylen A.; Stein, Peter A.

1986-01-01

A direct algorithm is presented for computing the Euler load of a column from experimental data. The method is based on exact inextensional theory for imperfect columns, which predicts two distinct deflected shapes at loads near the Euler load. The bending stiffness of the column appears in the expression for the Euler load along with the column length, therefore the experimental data allows a direct computation of bending stiffness. Experiments on graphite-epoxy columns of rectangular cross-section are reported in the paper. The bending stiffness of each composite column computed from experiment is compared with predictions from laminated plate theory.

Simultaneous determination of intracellular UDP-sugars in hyaluronic acid-producing Streptococcus zooepidemicus.

PubMed

Franke, Lukáš; Čožíková, Dagmar; Smirnou, Dzianis; Hermannová, Martina; Hanová, Tereza; Růžičková, Andrea; Velebný, Vladimír

2015-08-01

Two chromatographic methods for the quantitative analysis of uridine diphosphate (UDP) sugars involved in hyaluronan pathway of Streptococcus zooepidemicus (SEZ) were developed and compared. The sample preparation protocol using centrifugation and extraction in hot ethanol was employed prior to the analyses. Separation was achieved using an anion exchange Spherisorb SAX column or a Shodex QA-825 column connected with a photodiode array (PDA) detector. To increase the throughput of the chromatography method employing the Spherisorb SAX column, the solid phase extraction (SPE) procedure was introduced. Method validation results displayed that limits of detection (LODs) of UDP-glucose (UDP-Glc), UDP-N-acetylglucosamine (UDP-GlcNAc) and UDP-glucuronic acid (UDP-GlcA) calculated according to QC Expert software were in the low micromolar range and the coefficient of correlation (R(2)) was above 0.997. However, the analytical technique using the Spherisorb SAX column resulted in 80-90% recoveries and low LODs (≤6.19μM), the Shodex QA-825 column showed better long-term stability and reproducible chromatographic properties (RSD≤5.60%). The Shodex QA-825 column was successfully used to monitor UDP-sugar levels during the growth rate of SEZ cells. Copyright © 2015 Elsevier B.V. All rights reserved.

Enhancement of soft X-ray lasing action with thin blade radiators

DOEpatents

Suckewer, Szymon; Skinner, Charles H.; Voorhees, David R.

1988-01-01

An enhancement of approximately 100 of stimulated emission over spontaneous emission of the CVI 182 Angstrom line was obtained in a recombining magnetically confined plasma column. The plasma was formed by focusing a CO.sub.2 laser beam on a carbon disc. A magnetic solenoid produced a strong magnetic field which confined the plasma to the shape of a column. A single thin carbon blade extended parallel to the plasma column and served to make the column axially more uniform and also acted as a heat sink. Axial and transverse measurements of the soft X-ray lasing action were made from locations off-set from the central axis of the plasma column. Multiple carbon blades located at equal intervals around the plasma column were also found to produce acceptable results. According to another embodiment 10 a thin coating of aluminum or magnesium was placed on the carbon disc and blade. The Z of the coating should preferably be at least 5 greater than the Z of the target. Measurements of the soft X-rays generated at 182 Angstroms showed a significant increase in intensity enhancement.

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

A dynamic pressure calibration standard

NASA Technical Reports Server (NTRS)

Schutte, P. C.; Cate, K. H.; Young, S. D.

1985-01-01

A dynamic pressure calibration standard has been developed for calibrating flush diaphragm mounted pressure transducers. Pressures up to 20 kPa (3 psi) have been accurately generated over a frequency range of 50 to 1800 hz. The uncertainty of the standard is +/-5 pct to 5kPa (.75 psi) and +/-10 pct from 5 kPa (.75 psi) to 20 kPa (3 psi). The system consists of two conically shaped, aluminum columns, one 5 cm (2 in.) high for low pressures and another 11 cm (4.3 in.) high for higher pressures, each filled with a viscous fluid. A column is mounted on the armature of a vibration exciter which imparts a sinusoidally varying acceleration to the fluid column. Two pressure transducers mounted at the base of the column sense the sinusoidally varying pressure. This pressure is determined from measurements of the density of the fluid, the height of the fluid, and the acceleration of the column. A section of the taller column is filled with steel balls to control the damping of the fluid to extend its useful frequency range.

Production and purification of lentiviral vectors generated in 293T suspension cells with baculoviral vectors.

PubMed

Lesch, H P; Laitinen, A; Peixoto, C; Vicente, T; Makkonen, K-E; Laitinen, L; Pikkarainen, J T; Samaranayake, H; Alves, P M; Carrondo, M J T; Ylä-Herttuala, S; Airenne, K J

2011-06-01

Lentivirus can be engineered to be a highly potent vector for gene therapy applications. However, generation of clinical grade vectors in enough quantities for therapeutic use is still troublesome and limits the preclinical and clinical experiments. As a first step to solve this unmet need we recently introduced a baculovirus-based production system for lentiviral vector (LV) production using adherent cells. Herein, we have adapted and optimized the production of these vectors to a suspension cell culture system using recombinant baculoviruses delivering all elements required for a safe latest generation LV preparation. High-titer LV stocks were achieved in 293T cells grown in suspension. Produced viruses were accurately characterized and the functionality was also tested in vivo. Produced viruses were compared with viruses produced by calcium phosphate transfection method in adherent cells and polyethylenimine transfection method in suspension cells. Furthermore, a scalable and cost-effective capture purification step was developed based on a diethylaminoethyl monolithic column capable of removing most of the baculoviruses from the LV pool with 65% recovery.

Treatment of zinc-rich acid mine water in low residence time bioreactors incorporating waste shells and methanol dosing.

PubMed

Mayes, W M; Davis, J; Silva, V; Jarvis, A P

2011-10-15

Bioreactors utilising bacterially mediated sulphate reduction (BSR) have been widely tested for treating metal-rich waters, but sustained treatment of mobile metals (e.g. Zn) can be difficult to achieve in short residence time systems. Data are presented providing an assessment of alkalinity generating media (shells or limestone) and modes of metal removal in bioreactors receiving a synthetic acidic metal mine discharge (pH 2.7, Zn 15 mg/L, SO(4)(2-) 200mg/L, net acidity 103 mg/L as CaCO(3)) subject to methanol dosing. In addition to alkalinity generating media (50%, v.v.), the columns comprised an organic matrix of softwood chippings (30%), manure (10%) and anaerobic digested sludge (10%). The column tests showed sustained alkalinity generation, which was significantly better in shell treatments. The first column in each treatment was effective throughout the 422 days in removing >99% of the dissolved Pb and Cu, and effective for four months in removing 99% of the dissolved Zn (residence time: 12-14 h). Methanol was added to the feedstock after Zn breakthrough and prompted almost complete removal of dissolved Zn alongside improved alkalinity generation and sulphate attenuation. While there was geochemical evidence for BSR, sequential extraction of substrates suggests that the bulk (67-80%) of removed Zn was associated with Fe-Mn oxide fractions. Copyright © 2011 Elsevier B.V. All rights reserved.

Applications of neural network methods to the processing of earth observation satellite data.

PubMed

Loyola, Diego G

2006-03-01

The new generation of earth observation satellites carries advanced sensors that will gather very precise data for studying the Earth system and global climate. This paper shows that neural network methods can be successfully used for solving forward and inverse remote sensing problems, providing both accurate and fast solutions. Two examples of multi-neural network systems for the determination of cloud properties and for the retrieval of total columns of ozone using satellite data are presented. The developed algorithms based on multi-neural network are currently being used for the operational processing of European atmospheric satellite sensors and will play a key role in related satellite missions planed for the near future.

Stability Study on Steel Structural Columns with Initial Blast Damage under High Temperatures

NASA Astrophysics Data System (ADS)

Baoxin, Qi; Yan, Shi; Li, Peng

2018-03-01

Blast may bring light-weight steel columns with initial damages, resulting in lowering its critical fire-resistance temperature whose reduced amplitude is relevant to the form and degree of the damages. Finite element analysis software ANSYS was used in the paper to analyze the issue of the fire-resistance temperature of the column with the blast damages, and the coupling method for heat and structure was applied during the simulation. The emphasis was laid on parametric factors of axial compression ratio, the form and the degree of the initial damages, as well as the confined condition at the ends of the columns. The numerical results showed that the fire-resistance temperature will lower as increasing of the axial compression ratio, the form and the degree of the initial damages and it will be also affected by the restraint conditions at the ends of the columns. The critical stress formula with initial bending damage under elevated temperature was set up under flexural small deformation condition, then the stability coefficient was determined and the method for evaluating the limit temperature of the column was put forward. The theoretical result was also compared with that of the finite element method (FEM). The results both showed that the stability capacity for the damaged columns was dramatically reduced as increasing the temperature and the initial damage level.

Analysis of clonazepam in a tablet dosage form using smallbore HPLC.

PubMed

Spell, J C; Stewart, J T

1998-11-01

A stability indicating, reversed phase high-performance liquid chromatographic method utilizing a smallbore HPLC column has been developed for the determination of clonazepam in a commercial tablet dosage form. The use of a small bore column results in a substantial solvent savings, as well as a greater mass sensitivity, especially in the identification of degradation peaks in a chromatogram. The method involves ultraviolet detection at 254 nm and utilized a 150 x 3.0 mm i.d. column packed with 3 microm octyldecylsilane particles with a mobile phase of water methanol acetonitrile (40:30:30, v/v/v) at a flow rate of 400 microl min(-1) at ambient temperature, with and without the use of 1,2-dichlorobenzene as the internal standard. The current USP method for the analysis of clonazepam using a 300 x 3.9 mm i.d. conventional octyldecylsilane column was utilized as a comparison to the smallbore method. The retention times for clonazepam and the internal standard on the 3.0 mm i.d. column were 4.0 and 12.5 min, respectively. The intra- and interday RSDs on the 3.0 mm i.d. column were < 0.55% (n =4) using the internal standard, and < 0.19% (n = 4) without the internal standard at the lower limit of the standard curve, 50 microg ml(-1) and had a limit of detection of 24 ng ml(-1). The assay using the 3.0 mm i.d. column was shown to be suitable for measuring clonazepam in a tablet dosage form.

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

NASA Technical Reports Server (NTRS)

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

2001-01-01

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

Liquid gallium columns sheathed with carbon: Bulk synthesis and manipulation.

PubMed

Zhan, Jinhua; Bando, Yoshio; Hu, Junqing; Golberg, Dmitri; Nakanishi, Haruyuki

2005-06-16

It is impossible to fabricate isolated gallium nanomaterials due to the low melting point of Ga (29.8 degrees C) and its high reactivity. We report the bulk synthesis of uniform liquid Ga columns encapsulated into carbon nanotubes through high-temperature chemical reaction between Ga and CH4. The diameter of filled Ga liquid columns is approximately 25 nm, and their length is up to several micrometers. The thickness of the carbon sheaths is approximately 6 nm. Simultaneous condensation of a Ga vapor and carbon clusters results in the generation of Ga-filled carbon nanotubes. A convergent 300 kV electron beam generated in a field emission high-resolution electron microscope is demonstrated to be a powerful tool for delicate manipulation of the liquid Ga nanocolumns: they can be gently joined, cut, and sealed within carbon nanotubes. The self-organization of a carbon sheath during the electron-beam irradiation is discussed. The electron-beam irradiation may also become a decent tool for Ga-filled carbon nanotube thermometer calibration.

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.

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

Mastren, Tara; Radchenko, Valery; Hopkins, Philip D.

Ruthenium-103 is the parent isotope of 103mRh (t1/2 56.1 min), an isotope of interest for Auger electron therapy. During the proton irradiation of thorium targets, large amounts of 103Ru are generated through proton induced fission. Furthermore, the development of a two part chemical separation process to isolate 103Ru in high yield and purity from a proton irradiated thorium matrix on an analytical scale is described herein. The first part employed an anion exchange column to remove cationic actinide/lanthanide impurities along with the majority of the transition metal fission products. Secondly, an extraction chromatographic column utilizing diglycolamide functional groups was usedmore » to decontaminate 103Ru from the remaining impurities. This method then resulted in a final radiochemical yield of 83 ± 5% of 103Ru with a purity of 99.9%. Additionally, measured nuclear reaction cross sections for the formation of 103Ru and 106Ru via the 232Th(p,f) 103,106Ru reactions are reported within.« less

Optimization of elutriation device for filtration of microplastic particles from sediment.

PubMed

Zhu, X

2015-03-15

The increasing presence of plastic pollution in marine ecosystems has become a major concern. In the environment, plastics break down into smaller and smaller pieces of microplastics. Methods of microplastic recovery are needed to reduce the dangers they can pose to a variety of organisms. An elutriation device was manufactured and optimized to achieve maximum microplastic recovery. The parameters flow rate and diameter of elutriation column were varied and their domain of variation was determined. A composite factorial experimental design was generated using MODDE 10.1 and was undergone. The optimal values of flow rate and column diameter were determined to be 385 L h(-1) and 5.06 cm respectively, under constraints, to achieve a maximum feasible microplastics recovery percentage of 50.2%. The elutriation process can be improved through further testing, and can be tested in the field to compare its efficiency to that of manual microplastics filtration. Copyright © 2015 Elsevier Ltd. All rights reserved.

The Next-generation Berkeley High Resolution NO2 (BEHR NO2) Retrieval: Design and Preliminary Emissions Constraints

NASA Astrophysics Data System (ADS)

Laughner, J.; Cohen, R. C.

2017-12-01

Recent work has identified a number of assumptions made in NO2 retrievals that lead to biases in the retrieved NO2 column density. These include the treatment of the surface as an isotropic reflector, the absence of lightning NO2 in high resolution a priori profiles, and the use of monthly averaged a priori profiles. We present a new release of the Berkeley High Resolution (BEHR) OMI NO2 retrieval based on the new NASA Standard Product (version 3) that addresses these assumptions by: accounting for surface anisotropy by using a BRDF albedo product, using an updated method of regridding NO2 data, and revised NO2 a priori profiles that better account for lightning NO2 and daily variation in the profile shape. We quantify the effect these changes have on the retrieved NO2 column densities and the resultant impact these updates have on constraints of urban NOx emissions for select cities throughout the United States.

The presence of sodium nitrate in generator eluate decreases the radiochemical purity of 99mTc-sestamibi.

PubMed

Métayé, Thierry; Rosenberg, Thierry; Guilhot, Joëlle; Bouin-Pineau, Marie-Hélène; Perdrisot, Rémy

2012-09-01

A high radiochemical purity (RCP) is recommended for radiopharmaceutical compounds used in the clinical practice of nuclear medicine. However, some preparations of (99m)Tc-sestamibi contain excess impurities (>6%). To understand the origin of these impurities, we investigated the effect of sodium nitrate on the RCP of sestamibi preparations by testing eluates from 3 commercially available (99m)Tc generators. The sestamibi kits (Stamicis) were reconstituted with (99m)Tc eluate from nitrate-containing wet-column (NCWC), nitrate-free wet-column (NFWC), and nitrate-free dry-column (NFDC) generators. Sodium nitrate was 0.05 mg/mL in eluates from the NCWC generators. The RCP was determined using aluminum oxide sheets as the stationary phase and absolute ethanol as the mobile phase. Succimer, tetrofosmin, oxidronate, exametazine, albumin nanocolloid, and soluble albumin were also tested for their RCP values with eluates from the 3 different (99m)Tc generators. The RCP assessment of (99m)Tc-sestamibi was performed on 127 Stamicis preparations. Significantly lower RCP values were found for Stamicis kits prepared with the NCWC generator than for Stamicis prepared with the NFWC (P < 0.0001) and NFDC (P < 0.0001) generators. The number of Stamicis preparations with an RCP under 94% was greater with the NCWC generator (32 of 53 kits) than with the NFDC (2 of 51 kits) or NFWC (0 of 23 kits) generator. Furthermore, the addition of a 0.05 mg/mL concentration of nitrate in NFWC generator eluates significantly decreased the RCP of the Stamicis preparation. In the absence of nitrate in (99m)Tc eluate, no difference was observed between the RCP values of Stamicis kits prepared with the NFWC and NFDC generators. The (99m)Tc impurities generated by nitrates did not modify the quality of myocardial imaging (normal heart-to-lung ratio, 2.2), probably because these impurities are not in the heart field of view. No other tested (99m)Tc-radiopharmaceutical interfered with nitrates. We recommend using nitrate-free generator eluates in (99m)Tc-sestamibi preparations to improve the product quality and prevent unnecessary exposure of the patient to radiation.

Electron beam generation in the turbulent plasma of Z-pinch discharges

NASA Astrophysics Data System (ADS)

Vikhrev, Victor V.; Baronova, Elena O.

1997-05-01

Numerical modeling of the process of electron beam generation in z-pinch discharges are presented. The proposed model represents the electron beam generation under turbulent plasma conditions. Strong current distribution inhomogeneity in the plasma column has been accounted for the adequate generation process investigation. Electron beam is generated near the maximum of compression due to run away mechanism and it is not related with the current break effect.

WATER CHEMISTRY ASSESSMENT METHODS

EPA Science Inventory

This section summarizes and evaluates the surfce water column chemistry assessment methods for USEPA/EMAP-SW, USGS-NAQA, USEPA-RBP, Oho EPA, and MDNR-MBSS. The basic objective of surface water column chemistry assessment is to characterize surface water quality by measuring a sui...

Seismic Tremors and Three-Dimensional Magma Wagging

NASA Astrophysics Data System (ADS)

Liao, Y.; Bercovici, D.

2015-12-01

Seismic tremor is a feature shared by many silicic volcanoes and is a precursor of volcanic eruption. Many of the characteristics of tremors, including their frequency band from 0.5 Hz to 7 Hz, are common for volcanoes with very different geophysical and geochemical properties. The ubiquitous characteristics of tremor imply that it results from some generation mechanism that is common to all volcanoes, instead of being unique to each volcano. Here we present new analysis on the magma-wagging mechanism that has been proposed to generate tremor. The model is based on the suggestion given by previous work (Jellinek & Bercovici 2011; Bercovici et.al. 2013) that the magma column is surrounded by a compressible, bubble-rich foam annulus while rising inside the volcanic conduit, and that the lateral oscillation of the magma inside the annulus causes observable tremor. Unlike the previous two-dimensional wagging model where the displacement of the magma column is restricted to one vertical plane, the three-dimensional model we employ allows the magma column to bend in different directions and has angular motion as well. Our preliminary results show that, without damping from viscous deformation of the magma column, the system retains angular momentum and develops elliptical motion (i.e., the horizontal displacement traces an ellipse). In this ''inviscid'' limit, the magma column can also develop instabilities with higher frequencies than what is found in the original two-dimensional model. Lateral motion can also be out of phase for various depths in the magma column leading to a coiled wagging motion. For the viscous-magma model, we predict a similar damping rate for the uncoiled magma column as in the two-dimensional model, and faster damping for the coiled magma column. The higher damping thus requires the existence of a forcing mechanism to sustain the oscillation, for example the gas-driven Bernoulli effect proposed by Bercovici et al (2013). Finally, using our new 3-D model, the spectrum of displacement and unsynchronized cross-correlation between displacements measured from different locations can be calculated, and this can be compared to more detailed seismic measurements on well monitored volcanoes.

Comparison of a gel column blood typing method and a point-of-care cartridge for dog erythrocyte antigen 1.1.

PubMed

Blois, Shauna L; Richardson, Danielle M; Abrams-Ogg, Anthony C G

2013-01-01

Blood typing for the presence of Dog Erythrocyte Antigen (DEA) 1.1 is recommended in all donor and recipient dogs prior to transfusion of blood products. The objective of this study was to determine if a point-of-care DEA 1.1 blood typing cartridge could be used in place of the gel column typing method. Detection of DEA 1.1 was performed using a laboratory-based gel column method and a point-of-care cartridge. A convenience sample of 30 healthy blood donors, 13 dogs with immune-mediated hemolytic anemia (IMHA) (3 of which had concurrent immune-mediated thrombocytopenia [IMT]), and 44 dogs with other diseases was included in the study. Agreement was observed between the tests for normal dogs and dogs with nonimmune-mediated disease in 74/74 cases. Two dogs in the IMHA group had indeterminate gel column blood typing results; 1 dog in this group had a negative gel column test result but a positive cartridge test result. There was good agreement between the 2 methods for normal dogs and dogs with nonimmune-mediated disease. Blood typing methods in dogs with IMHA should be further investigated. © Veterinary Emergency and Critical Care Society 2013.

Enhanced reductive dechlorination in columns treated with edible oil emulsion

NASA Astrophysics Data System (ADS)

Long, Cameron M.; Borden, Robert C.

2006-09-01

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

Automated statistical experimental design approach for rapid separation of coenzyme Q10 and identification of its biotechnological process related impurities using UHPLC and UHPLC-APCI-MS.

PubMed

Talluri, Murali V N Kumar; Kalariya, Pradipbhai D; Dharavath, Shireesha; Shaikh, Naeem; Garg, Prabha; Ramisetti, Nageswara Rao; Ragampeta, Srinivas

2016-09-01

A novel ultra high performance liquid chromatography method development strategy was ameliorated by applying quality by design approach. The developed systematic approach was divided into five steps (i) Analytical Target Profile, (ii) Critical Quality Attributes, (iii) Risk Assessments of Critical parameters using design of experiments (screening and optimization phases), (iv) Generation of design space, and (v) Process Capability Analysis (Cp) for robustness study using Monte Carlo simulation. The complete quality-by-design-based method development was made automated and expedited by employing sub-2 μm particles column with an ultra high performance liquid chromatography system. Successful chromatographic separation of the Coenzyme Q10 from its biotechnological process related impurities was achieved on a Waters Acquity phenyl hexyl (100 mm × 2.1 mm, 1.7 μm) column with gradient elution of 10 mM ammonium acetate buffer (pH 4.0) and a mixture of acetonitrile/2-propanol (1:1) as the mobile phase. Through this study, fast and organized method development workflow was developed and robustness of the method was also demonstrated. The method was validated for specificity, linearity, accuracy, precision, and robustness in compliance to the International Conference on Harmonization, Q2 (R1) guidelines. The impurities were identified by atmospheric pressure chemical ionization-mass spectrometry technique. Further, the in silico toxicity of impurities was analyzed using TOPKAT and DEREK software. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Behaviour of Reinforced Concrete Columns of Various Cross-Sections Subjected to Fire

NASA Astrophysics Data System (ADS)

Balaji, Aneesha; Muhamed Luquman, K.; Nagarajan, Praveen; Madhavan Pillai, T. M.

2016-09-01

Fire resistance is one of the crucial design regulations which are now mandatory in most of the design codes. Therefore, a thorough knowledge of behaviour of structures exposed to fire is required in this aspect. Columns are the most vulnerable structural member to fire as it can be exposed to fire from all sides. However, the data available for fire resistant design for columns are limited. Hence the present work is focused on the effect of cross-sectional shape of column in fire resistance design. The various cross-sections considered are Square, Ell (L), Tee (T), and Plus (`+') shape. Also the effect of size and shape and distribution of steel reinforcement on fire resistance of columns is studied. As the procedure for determining fire resistance is not mentioned in Indian Standard code IS 456 (2000), the simplified method (500 °C isotherm method) recommended in EN 1992-1-2:2004 (E) (Eurocode 2) is adopted. The temperature profiles for various cross-sections are developed using finite element method and these profiles are used to predict fire resistance capability of compression members. The fire resistance based on both numerical and code based methods are evaluated and compared for various types of cross-section.

A practical approach for predicting retention time shifts due to pressure and temperature gradients in ultra-high-pressure liquid chromatography.

PubMed

Åsberg, Dennis; Chutkowski, Marcin; Leśko, Marek; Samuelsson, Jörgen; Kaczmarski, Krzysztof; Fornstedt, Torgny

2017-01-06

Large pressure gradients are generated in ultra-high-pressure liquid chromatography (UHPLC) using sub-2μm particles causing significant temperature gradients over the column due to viscous heating. These pressure and temperature gradients affect retention and ultimately result in important selectivity shifts. In this study, we developed an approach for predicting the retention time shifts due to these gradients. The approach is presented as a step-by-step procedure and it is based on empirical linear relationships describing how retention varies as a function of temperature and pressure and how the average column temperature increases with the flow rate. It requires only four experiments on standard equipment, is based on straightforward calculations, and is therefore easy to use in method development. The approach was rigorously validated against experimental data obtained with a quality control method for the active pharmaceutical ingredient omeprazole. The accuracy of retention time predictions was very good with relative errors always less than 1% and in many cases around 0.5% (n=32). Selectivity shifts observed between omeprazole and the related impurities when changing the flow rate could also be accurately predicted resulting in good estimates of the resolution between critical peak pairs. The approximations which the presented approach are based on were all justified. The retention factor as a function of pressure and temperature was studied in an experimental design while the temperature distribution in the column was obtained by solving the fundamental heat and mass balance equations for the different experimental conditions. We strongly believe that this approach is sufficiently accurate and experimentally feasible for this separation to be a valuable tool when developing a UHPLC method. After further validation with other separation systems, it could become a useful approach in UHPLC method development, especially in the pharmaceutical industry where demands are high for robustness and regulatory oversight. Copyright © 2016 Elsevier B.V. All rights reserved.

RP-HPLC×HILIC chromatography for quantifying ertapenem sodium with a look at green chemistry.

PubMed

Pedroso, Tahisa M; Medeiros, Ana C D; Salgado, Herida R N

2016-11-01

Ertapenem sodium is a polar and ionizable compound; therefore, it has little retention on traditional C18 columns in reverse-phase high-performance liquid chromatography, even using a highly-aqueous mobile phase that can result in dewetting in the stationary phase. Thus, the most coherent process for ERTM is to develop a method for Hydrophilic Interaction Chromatography. However, for the traditional methods in HILIC, the use of a highly organic mobile phase is necessary; usually an amount exceeding 80% acetonitrile is necessary. On the other hand, the RP-HPLC mode is considered for the analysis technique, which is more often used for quantification of substances, and new columns are often introduced to analyze different groups of compounds. Two new analytical methods have been developed for routine analysis. The proposed chromatographic method was adequate and advantageous by presenting simplicity, linearity, precision, accuracy, robustness, detection limits, and satisfactory quantification. Analytical methods are constantly undergoing changes and improvements. Researchers worldwide are rapidly adopting Green Chemistry. The development of new pharmaceutical methods based in Green chemistry has been encouraged by universities and the pharmaceutical industry. Issues related to green chemistry are in evidence and they have been featured in international journals of high impact. The methods described here have economic advantages and they feature an eco-friendly focus, which is discussed in this work. This work was developed with an environmental conscience, always looking to minimize the possible generated organic waste. Therefore, discussion on this aspect is included. Copyright © 2016 Elsevier B.V. All rights reserved.

Regulation of Electrochemically Generated H2O2 in Situ from a Novel CB-PTFE Cathode for Transformation of Chlorine Benzene in Groundwater

NASA Astrophysics Data System (ADS)

Jiang, J.; Zhang, X.; Li, G.

2014-12-01

Fenton's reagents (H2O2 and Fe2+ catalyst commonly) have been widely used in soil and groundwater remediation. But the excessive H2O2 decomposition and the pH modification (acidification) problem have been limitations for Fenton based remediation strategies. The Electro-Fenton (E- Fenton) processes has been recently developed to solve the problems, in which Fe2+ or H2O2are generated in situ as continuing source of Fenton's reagents. In this study, a novel CB-PTFE cathode and a Fe cathode were employed to generate H2O2 and Fe2+ in situ simultaneously. The generated reactive oxidizing species, i.e., O2,H2O2 and hydroxyl radical (HO•), oxidized bio-refractory organics to nontoxic matters in groundwater. Automatic pH adjustments are achieved by appropriately arraying the electrodes. Laboratory batch tests and column tests for the E-Fenton oxidation and hybrid electrolysis system were conducted to evaluate the transformation efficiency of chlorine benzene. Results from batch experiments suggested the CB-PTFE cathode was effective for reducing O2 to H2O2. The H2O2 concentration reached 468 mg/L under the condition of pH 3.0 and 30mA/cm2 in 60 minutes, which was 5 and 10 times of that with a graphite and C-felt cathode. The removal efficiency of chlorine benzene reached 80% in 20 minutes. Both chlorine benzene degradation and H2O2 production increased with decreasing solution pH and increasing current density. The results from the columns tests proved that the in situ E-Fenton system is a feasible method for groundwater remediation.

Quantitative structure-retention relationships of flavonoids unraveled by immobilized artificial membrane chromatography.

PubMed

Santoro, Adriana Leandra; Carrilho, Emanuel; Lanças, Fernando Mauro; Montanari, Carlos Alberto

2016-06-10

The pharmacokinetic properties of flavonoids with differing degrees of lipophilicity were investigated using immobilized artificial membranes (IAMs) as the stationary phase in high performance liquid chromatography (HPLC). For each flavonoid compound, we investigated whether the type of column used affected the correlation between the retention factors and the calculated octanol/water partition (log Poct). Three-dimensional (3D) molecular descriptors were calculated from the molecular structure of each compound using i) VolSurf software, ii) the GRID method (computational procedure for determining energetically favorable binding sites in molecules of known structure using a probe for calculating the 3D molecular interaction fields, between the probe and the molecule), and iii) the relationship between partition and molecular structure, analyzed in terms of physicochemical descriptors. The VolSurf built-in Caco-2 model was used to estimate compound permeability. The extent to which the datasets obtained from different columns differ both from each other and from both the calculated log Poct and the predicted permeability in Caco-2 cells was examined by principal component analysis (PCA). The immobilized membrane partition coefficients (kIAM) were analyzed using molecular descriptors in partial least square regression (PLS) and a quantitative structure-retention relationship was generated for the chromatographic retention in the cholesterol column. The cholesterol column provided the best correlation with the permeability predicted by the Caco-2 cell model and a good fit model with great prediction power was obtained for its retention data (R(2)=0.96 and Q(2)=0.85 with four latent variables). Copyright © 2015 Elsevier B.V. All rights reserved.

Application of Snyder-Dolan Classification Scheme to the Selection of “Orthogonal” Columns for Fast Screening for Illicit Drugs and Impurity Profiling of Pharmaceuticals - I. Isocratic Elution

PubMed Central

Fan, Wenzhe; Zhang, Yu; Carr, Peter W.; Rutan, Sarah C.; Dumarey, Melanie; Schellinger, Adam P.; Pritts, Wayne

2011-01-01

Fourteen judiciously selected reversed-phase columns were tested with 18 cationic drug solutes under the isocratic elution conditions advised in the Snyder-Dolan (S-D) hydrophobic subtraction method of column classification. The standard errors (S.E.) of the least squares regressions of log k′ vs. log k′REF were obtained for a given column against a reference column and used to compare and classify columns based on their selectivity. The results are consistent with those obtained with a study of the 16 test solutes recommended by Snyder and Dolan. To the extent that these drugs are representative these results show that the S-D classification scheme is also generally applicable to pharmaceuticals under isocratic conditions. That is, those columns judged to be similar based on the S-D 16 solutes were similar based on the 18 drugs; furthermore those columns judged to have significantly different selectivities based on the 16 S-D probes appeared to be quite different for the drugs as well. Given that the S-D method has been used to classify more than 400 different types of reversed phases the extension to cationic drugs is a significant finding. PMID:19698948

Data-driven probability concentration and sampling on manifold

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

Soize, C., E-mail: christian.soize@univ-paris-est.fr; Ghanem, R., E-mail: ghanem@usc.edu

2016-09-15

A new methodology is proposed for generating realizations of a random vector with values in a finite-dimensional Euclidean space that are statistically consistent with a dataset of observations of this vector. The probability distribution of this random vector, while a priori not known, is presumed to be concentrated on an unknown subset of the Euclidean space. A random matrix is introduced whose columns are independent copies of the random vector and for which the number of columns is the number of data points in the dataset. The approach is based on the use of (i) the multidimensional kernel-density estimation methodmore » for estimating the probability distribution of the random matrix, (ii) a MCMC method for generating realizations for the random matrix, (iii) the diffusion-maps approach for discovering and characterizing the geometry and the structure of the dataset, and (iv) a reduced-order representation of the random matrix, which is constructed using the diffusion-maps vectors associated with the first eigenvalues of the transition matrix relative to the given dataset. The convergence aspects of the proposed methodology are analyzed and a numerical validation is explored through three applications of increasing complexity. The proposed method is found to be robust to noise levels and data complexity as well as to the intrinsic dimension of data and the size of experimental datasets. Both the methodology and the underlying mathematical framework presented in this paper contribute new capabilities and perspectives at the interface of uncertainty quantification, statistical data analysis, stochastic modeling and associated statistical inverse problems.« less

Determination of Total Biotin by Liquid Chromatography Coupled with Immunoaffinity Column Cleanup Extraction: Multilaboratory Testing, Final Action 2016.02.

PubMed

Joseph, George; Devi, Ranjani; Marley, Elaine C; Leeman, David

2018-05-01

Single- and multilaboratory testing data have provided systematic scientific evidence that a simple, selective, accurate, and precise method can be used as a potential candidate reference method for dispute resolution in determining total biotin in all forms of infant, adult, and/or pediatric formula. Using LC coupled with immunoaffinity column cleanup extraction, the method fully meets the intended purpose and applicability statement in AOAC Standard Method Performance Requirement 2014.005. The method was applied to a cross-section of infant formula and adult nutritional matrixes, and acceptable precision and accuracy were established. The analytical platform is inexpensive, and the method can be used in almost any laboratory worldwide with basic facilities. The immunoaffinity column cleanup extraction is the key step to successful analysis.

Measurement of menadione in urine by HPLC

USDA-ARS?s Scientific Manuscript database

Mammals convert phylloquinone to MK-4, with menadione as a possible intermediate. We developed and validated a method measuring urinary menadione. A high performance liquid chromatography (HPLC) method with a C30 column, fluorescence detection and post-column zinc reduction was developed. The mobile...

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

NASA Technical Reports Server (NTRS)

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

1974-01-01

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

Survey of simulation methods for modeling pulsed sieve-plate extraction columns

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

Burkhart, L.

1979-03-01

The report first considers briefly the use of liquid-liquid extraction in nuclear fuel reprocessing and then describes the operation of the pulse column. Currently available simulation models of the column are reviewed, and followed by an analysis of the information presently available from which the necessary parameters can be obtained for use in a model of the column. Finally, overall conclusions are given regarding the information needed to develop an accurate model of the column for materials accountability in fuel reprocessing plants. 156 references.

Enzymatic cascade bioreactor

DOEpatents

Simmons, Blake A.; Volponi, Joanne V.; Ingersoll, David; Walker, Andrew

2007-09-04

Disclosed is an apparatus and method for continuously converting sucrose to .beta.-D-glucose. The method comprises a three stage enzymatic reactor in which an aqueous solution of sucrose is first converted into a solution of fructose and .alpha.-D-glucose by passing it through a porous, packed column containing an inert media on which invertase is immobilized. This solution is then sent through a second packed column containing glucose isomerase and finally a third packed column containing mutarotase. Solution temperature and pH are adjusted to maximize glucose output.

Validated high-performance anion-exchange chromatography with pulsed amperometric detection method for the determination of residual keratan sulfate and other glucosamine impurities in sodium chondroitin sulfate.

PubMed

Bottelli, Susanna; Grillo, Gianluca; Barindelli, Edoardo; Nencioni, Alessandro; Di Maria, Alessandro; Fossati, Tiziano

2017-07-07

An efficient and sensitive analytical method based on high-performance anion exchange chromatography with pulsed amperometric detection (HPAEC-PAD) was devised for the determination of glucosamine (GlcN) in sodium chondroitin sulfate (CS). Glucosamine (GlcN) is intended as marker of residual keratan sulfate (KS) and other impurities generating glucosamine by acidic hydrolyzation. The latter brings CS and KS to their respective monomers. Since GlcN is present only in KS we developed a method that separates GlcN from GalN, the principal hydrolytic product of CS, and then we validated it in order to quantify GlcN. Method validation was performed by spiking CS raw material with known amounts of KS. Detection limit was 0.5% of KS in CS (corresponding to 0.1μg/ml), and the linear range was 0.5-5% of KS in CS (corresponding to 0.1-1μg/ml). The optimized analysis was carried out on an ICS-5000 system (Dionex, Sunnyvale, CA, USA) equipped with a Dionex Amino Trap guard column (3mm×30mm), Dionex CarboPac-PA20 (3mm×30mm) and a Dionex CarboPac-PA20 analytical column (3mm×150mm) using gradient elution at a 0.5ml/min flow rate. Regression equations revealed good linear relationship (R 2 =0.99, n=5) within the test ranges. Quality parameters, including precision and accuracy, were fully validated and found to be satisfactory. The fully validated HPAEC-PAD method was readily applied for the quantification of residual KS in CS in several raw materials and USP/EP reference substance. Results confirmed that the HPAEC-PAD method is more specific than the electrophoretic method for related substance reported in EP and provides sensitive determination of KS in acid-hydrolyzed CS samples, enabling the quantitation of KS and other impurities (generating glucosamine) in CS. Copyright © 2017 Elsevier B.V. All rights reserved.

Graphene oxide sheets immobilized polystyrene for column preconcentration and sensitive determination of lead by flame atomic absorption spectrometry.

PubMed

Islam, Aminul; Ahmad, Hilal; Zaidi, Noushi; Kumar, Suneel

2014-08-13

A novel solid-phase extractant was synthesized by coupling graphene oxide (GO) on chloromethylated polystyrene through an ethylenediamine spacer unit to develop a column method for the preconcentration/separation of lead prior to its determination by flame atomic absorption spectrometry. It was characterized by Fourier transform infrared spectroscopy, far-infrared spectroscopy, thermogravimetric analysis/differential thermal analysis, scanning electron microscopy, energy-dispersive spectrometry, and transmission electron microscopy. The abundant oxygen-containing surface functional groups form a strong complex with lead, resulting in higher sorption capacity (227.92 mg g(-1)) than other nanosorbents used for sorption studies of the column method. Using the column procedure here is an alternative to the direct use of GO, which restricts irreversible aggregation of GO and its escape into the ecosystem, making it an environmentally sustainable method. The column method was optimized by varying experimental variables such as pH, flow rate for sorption/desorption, and elution condition and was observed to exhibit a high preconcentration factor (400) with a low preconcentration limit (2.5 ppb) and a high degree of tolerance for matrix ions. The accuracy of the proposed method was verified by determining the Pb content in the standard reference materials and by recovery experiments. The method showed good precision with a relative standard deviation <5%. The proposed method was successfully applied for the determination of lead in tap water, electroplating wastewater, river water, and food samples after preconcentration.

Effect of keyswitch design of desktop and notebook keyboards related to key stiffness and typing force.

PubMed

Bufton, Marcia J; Marklin, Richard W; Nagurka, Mark L; Simoneau, Guy G

2006-08-15

This study aimed to compare and analyse rubber-dome desktop, spring-column desktop and notebook keyboards in terms of key stiffness and fingertip typing force. The spring-column keyboard resulted in the highest mean peak contact force (0.86N), followed by the rubber dome desktop (0.68N) and the notebook (0.59N). All these differences were statistically significant. Likewise, the spring-column keyboard registered the highest fingertip typing force and the notebook keyboard the lowest. A comparison of forces showed the notebook (rubber dome) keyboard had the highest fingertip-to-peak contact force ratio (overstrike force), and the spring-column generated the least excess force (as a ratio of peak contact force). The results of this study could aid in optimizing computer key design that could possibly reduce subject discomfort and fatigue.

A new 68Ge/68Ga generator system using an organic polymer containing N-methylglucamine groups as adsorbent for 68Ge.

PubMed

Nakayama, M; Haratake, M; Ono, M; Koiso, T; Harada, K; Nakayama, H; Yahara, S; Ohmomo, Y; Arano, Y

2003-01-01

A macroporous styrene-divinylbenzene copolymer containing N-methylglucamine groups was selected for a new 68Ge/68Ga generator system. This resin packed into a column effectively adsorbed the parent nuclide 68Ge. The daughter 68Ga was eluted from the resin with a solution of a low-affinity gallium chelating ligand such as citric or phosphoric acid. The 68Ge leakage was less than 0.0004% of the 68Ge adsorbed on the resin. By simple mixing of transferrin and desferoxamine conjugated HSA and IgG with the eluate from the column, 68Ga-labeling was completed in high yield. Copyright 2002 Elsevier Science Ltd.

A hybrid Dantzig-Wolfe, Benders decomposition and column generation procedure for multiple diet production planning under uncertainties

NASA Astrophysics Data System (ADS)

Udomsungworagul, A.; Charnsethikul, P.

2018-03-01

This article introduces methodology to solve large scale two-phase linear programming with a case of multiple time period animal diet problems under both nutrients in raw materials and finished product demand uncertainties. Assumption of allowing to manufacture multiple product formulas in the same time period and assumption of allowing to hold raw materials and finished products inventory have been added. Dantzig-Wolfe decompositions, Benders decomposition and Column generations technique has been combined and applied to solve the problem. The proposed procedure was programmed using VBA and Solver tool in Microsoft Excel. A case study was used and tested in term of efficiency and effectiveness trade-offs.

Molecular Analysis of Bacterial Community Dynamics During Bioaugmentation Studies in a Soil Column and at a Field Test Site

DTIC Science & Technology

2004-06-03

82 4.14 A GelComparII-generated UPGMA clustering dendrogram and corresponding normalized restriction...A GelComparII-generated UPGMA clustering dendrogram and corresponding normalized restriction profiles from the community...A GelComparII-generated UPGMA clustering dendrogram and corresponding normalized restriction profiles from the community

The value of automated gel column agglutination technology in the identification of true inherited D blood types in massively transfused patients.

PubMed

Summers, Thomas; Johnson, Viviana V; Stephan, John P; Johnson, Gloria J; Leonard, George

2009-08-01

Massive transfusion of D- trauma patients in the combat setting involves the use of D+ red blood cells (RBCs) or whole blood along with suboptimal pretransfusion test result documentation. This presents challenges to the transfusion service of tertiary care military hospitals who ultimately receive these casualties because initial D typing results may only reflect the transfused RBCs. After patients are stabilized, mixed-field reaction results on D typing indicate the patient's true inherited D phenotype. This case series illustrates the utility of automated gel column agglutination in detecting mixed-field reactions in these patients. The transfusion service test results, including the automated gel column agglutination D typing results, of four massively transfused D- patients transfused D+ RBCs is presented. To test the sensitivity of the automated gel column agglutination method in detecting mixed-field agglutination reactions, a comparative analysis of three automated technologies using predetermined mixtures of D+ and D- RBCs is also presented. The automated gel column agglutination method detected mixed-field agglutination in D typing in all four patients and in the three prepared control specimens. The automated microwell tube method identified one of the three prepared control specimens as indeterminate, which was subsequently manually confirmed as a mixed-field reaction. The automated solid-phase method was unable to detect any mixed fields. The automated gel column agglutination method provides a sensitive means for detecting mixed-field agglutination reactions in the determination of the true inherited D phenotype of combat casualties transfused massive amounts of D+ RBCs.

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...

Enhanced reactive metal wall for dehalogenation of hydrocarbons

DOEpatents

Howson, P.E.; Mackenzie, P.D.; Horney, D.P.

1996-08-06

A method is provided for remediation of contaminated solutions using a tiered metal wall or column. The tiered metal wall or column has at least three zones with graduated sizes of reducing metal particles. Contaminated solutions pass through the tiered wall or column to dehalogenate contaminant halogenated hydrocarbons. 3 figs.

Enhanced reactive metal wall for dehalogenation of hydrocarbons

DOEpatents

Howson, Paul E.; Mackenzie, Patricia D.; Horney, David P.

1996-01-01

A method is provided for remediation of contaminated solutions using a tiered metal wall or column. The tiered metal wall or column has at least three zones with graduated sizes of reducing metal particles. Contaminated solutions pass through the tiered wall or column to dehalogenate contaminant halogenated hydrocarbons.

Quantitative analysis of cell columns in the cerebral cortex.

PubMed

Buxhoeveden, D P; Switala, A E; Roy, E; Casanova, M F

2000-04-01

We present a quantified imaging method that describes the cell column in mammalian cortex. The minicolumn is an ideal template with which to examine cortical organization because it is a basic unit of function, complete in itself, which interacts with adjacent and distance columns to form more complex levels of organization. The subtle details of columnar anatomy should reflect physiological changes that have occurred in evolution as well as those that might be caused by pathologies in the brain. In this semiautomatic method, images of Nissl-stained tissue are digitized or scanned into a computer imaging system. The software detects the presence of cell columns and describes details of their morphology and of the surrounding space. Columns are detected automatically on the basis of cell-poor and cell-rich areas using a Gaussian distribution. A line is fit to the cell centers by least squares analysis. The line becomes the center of the column from which the precise location of every cell can be measured. On this basis several algorithms describe the distribution of cells from the center line and in relation to the available surrounding space. Other algorithms use cluster analyses to determine the spatial orientation of every column.

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.

Use of a polystyrene-divinylbenzene-based weakly acidic cation-exchange resin column and propionic acid as an eluent in ion-exclusion/adsorption chromatography of aliphatic carboxylic acids and ethanol in food samples.

PubMed

Mori, Masanobu; Hironaga, Takahiro; Kajiwara, Hiroe; Nakatani, Nobutake; Kozaki, Daisuke; Itabashi, Hideyuki; Tanaka, Kazuhiko

2011-01-01

We developed an ion-exclusion/adsorption chromatography (IEAC) method employing a polystyrene-divinylbenzene-based weakly acidic cation-exchange resin (PS-WCX) column with propionic acid as the eluent for the simultaneous determination of multivalent aliphatic carboxylic acids and ethanol in food samples. The PS-WCX column well resolved mono-, di-, and trivalent carboxylic acids in the acidic eluent. Propionic acid as the eluent gave a higher signal-to-noise ratio, and enabled sensitive conductimetric detection of analyte acids. We found the optimal separation condition to be the combination of a PS-WCX column and 20-mM propionic acid. Practical applicability of the developed method was confirmed by using a short precolumn with a strongly acidic cation-exchange resin in the H(+)-form connected before the separation column; this was to remove cations from food samples by converting them to hydrogen ions. Consequently, common carboxylic acids and ethanol in beer, wine, and soy sauce were successfully separated by the developed method.

Measurement of bromate in bread by liquid chromatography with post-column flow reactor detection.

PubMed

Himata, K; Noda, M; Ando, S; Yamada, Y

2000-01-01

This method is suitable for the determination of bromate residues in a variety of baked goods. The peer-verified method trial was performed on white bread, multigrain bread, and coffee cake spiked with known levels of potassium bromate. The analytical portion is extracted with deionized water to remove bromate from the bulk of the baked product. The aqueous extract is carried through a series of steps to remove co-extractives that would interfere with the liquid chromatography (LC) in the determinative step or hasten the deterioration of the LC column. The extract is filtered before passing it through a reversed-phase solid-phase extraction (SPE) column and a cation-exchange column in the silver form to remove lipids and chloride, respectively. Ultrafiltration is then used to remove proteins with molecular weights of >30,000 daltons. Finally, a cation-exchange column in the sodium form is used to remove silver ions from the extract. The determinative step uses LC with a reversed-phase column and an ion-pairing agent in the mobile phase. Detection is based on the post-column reaction of bromate with o-dianisidine to form an oxidation product that is quantitated spectrophotometrically at 450 nm. Overall agreement between the submitting and peer laboratories was quite good. For bromate levels of 10-52 ppb, overall mean recoveries were 76.9 and 78.8% for the submitting and peer laboratories, respectively. The standard deviations were higher for the results of the peer laboratory, probably because of the generally higher level of baseline noise present in the chromatograms. The results demonstrate that the method provides adequate accuracy with low-fat as well as high-fat foods. Bromate at levels as low as 5 ppb (ng/g) can be detected with the method.

Chromatographic test methods for characterizing alkylsiloxane-bonded silica columns for reversed-phase liquid chromatography.

PubMed

Poole, Colin F

2018-06-07

Major obstacles to formulating a simple retention mechanism for reversed-phase liquid chromatography have a direct impact on the development of experimental methods for column characterization as they limit our capability to understand observed differences in retention at a system level. These problems arise from the heterogeneous composition of the stationary phase, the difficulty of providing a working definition for the phase ratio, and uncertainty as to whether the distribution mechanism for varied compounds is a partition, adsorption or mixed (combination) of these models. Retention factor and separation factor measurements offer little guidance as they represent an average of various and variable contributing factors that can only be interpreted by assuming a specific model. Column characterization methods have tended to ignore these difficulties by inventing a series of terms to describe column properties, such as hydrophobicity, hydrophilicity, silanol activity, steric resistance, etc., without proper definition. This has allowed multiple scales to be proposed for the same property which generally are only weakly correlated. Against this background we review the major approaches for the characterization of alkylsiloxane-bonded silica stationary phases employing prototypical compounds, the hydrophobic-subtraction model and the solvation parameter model. Those methods using prototypical compounds are limited by the lack of compounds with a singular dominant interaction. The multivariate approaches that extract column characteristic properties from the retention of varied compounds are more hopeful but it is important to be more precise in defining the characteristic column properties and cognizant that general interpretation of these properties for varied columns cannot escape the problem of a poor understanding of the distribution mechanism. Copyright © 2018 Elsevier B.V. All rights reserved.

ANIONIC EXCHANGE PROCESS FOR THE RECOVERY OF URANIUM AND VANADIUM FROM CARBONATE SOLUTIONS

DOEpatents

Bailes, R.H.; Ellis, D.A.; Long, R.S.

1958-12-16

Uranium and vanadium can be economically purified and recovered from non- salt roast carbonate leach liquors by adsorption on a strongly basic anionic exchange resin and subsequent selective elution by one of three alternative methods. Method 1 comprises selectively eluting uranium from the resin with an ammonium sulfate solution followed by eluting vanadium from the resin with either 5 M NaCl, saturated (NH/sub 4/)/sub 2/CO/sub 3/, saturated NaHCO/sub 3/, 1 M NaOH, or saturated S0/sub 2/ solutions. Method II comprises selectively eluting vanadium from the resin with either concentrated NaCl or S0/sub 2/ solutions subsequent to pretreatment of the column with either S0/sub 2/ gas, 1 N HCl, or 0.1 N H/sub 2/8O/sub 4/ followed by eluting uranium from the resin with solutions containing 0.9 M NH/sub 4/Cl or NaCl and 0.1 Cl. Method III comprises flowing the carbonate leac solutlon through a first column of a strongly basic anlonlc exchange resin untll vanadium breakthrough occurs, so that the effluent solution is enriched ln uranium content and the vanadium is chiefly retalned by the resln, absorbing the uranlum from the enriched effluent solution on a second column of a strongly basic anionic exchange resin, pretreating the first column with either 0.1 N HCl, 0.1 H/sub 2/SO/sub 4/, C0/sub 2/ gas, or ammonium sulfate, selectively eluting the vanadlum from the column with saturated S0/sub 2/ solution, pretreatlng the second column with either 0.1 N HCl or S0/sub 2/ gas, selectively eluting residual vanadium from the column with saturated S0/sub 2/ solution, and then eluting the uranium from the column with either 0.1 N HCl and 1 N NaCl orO.l N HCl and 1 N NH/sub 4/Cl.

A simple method for HPLC retention time prediction: linear calibration using two reference substances.

PubMed

Sun, Lei; Jin, Hong-Yu; Tian, Run-Tao; Wang, Ming-Juan; Liu, Li-Na; Ye, Liu-Ping; Zuo, Tian-Tian; Ma, Shuang-Cheng

2017-01-01

Analysis of related substances in pharmaceutical chemicals and multi-components in traditional Chinese medicines needs bulk of reference substances to identify the chromatographic peaks accurately. But the reference substances are costly. Thus, the relative retention (RR) method has been widely adopted in pharmacopoeias and literatures for characterizing HPLC behaviors of those reference substances unavailable. The problem is it is difficult to reproduce the RR on different columns due to the error between measured retention time (t R ) and predicted t R in some cases. Therefore, it is useful to develop an alternative and simple method for prediction of t R accurately. In the present study, based on the thermodynamic theory of HPLC, a method named linear calibration using two reference substances (LCTRS) was proposed. The method includes three steps, procedure of two points prediction, procedure of validation by multiple points regression and sequential matching. The t R of compounds on a HPLC column can be calculated by standard retention time and linear relationship. The method was validated in two medicines on 30 columns. It was demonstrated that, LCTRS method is simple, but more accurate and more robust on different HPLC columns than RR method. Hence quality standards using LCTRS method are easy to reproduce in different laboratories with lower cost of reference substances.

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.

An automated online turboflow cleanup LC/MS/MS method for the determination of 11 plasticizers in beverages and milk.

PubMed

Ates, Ebru; Mittendorf, Klaus; Senyuva, Hamide

2013-01-01

An automated sample preparation technique involving cleanup and analytical separation in a single operation using an online coupled TurboFlow (RP-LC system) is reported. This method eliminates time-consuming sample preparation steps that can be potential sources for cross-contamination in the analysis of plasticizers. Using TurboFlow chromatography, liquid samples were injected directly into the automated system without previous extraction or cleanup. Special cleanup columns enabled specific binding of target compounds; higher MW compounds, i.e., fats and proteins, and other matrix interferences with different chemical properties were removed to waste, prior to LC/MS/MS. Systematic stepwise method development using this new technology in the food safety area is described. Selection of optimum columns and mobile phases for loading onto the cleanup column followed by transfer onto the analytical column and MS detection are critical method parameters. The method was optimized for the assay of 10 phthalates (dimethyl, diethyl, dipropyl, butyl benzyl, diisobutyl, dicyclohexyl, dihexyl, diethylhexyl, diisononyl, and diisododecyl) and one adipate (diethylhexyl) in beverages and milk.

Methods of forming a fluidized bed of circulating particles

DOEpatents

Marshall, Douglas W [Blackfoot, ID

2011-05-24

There is disclosed an apparatus for forming a fluidized bed of circulating particles. In an embodiment, the apparatus includes a bottom portion having a sidewall, the sidewall defining a curvilinear profile, and the bottom portion configured to contain a bed of particles; and a gas inlet configured to produce a column of gas to carry entrained particles therein. There is disclosed a method of forming a fluidized bed of circulating particles. In an embodiment, the method includes positioning particles within a bottom portion having a sidewall, the sidewall defining a curvilinear profile; producing a column of gas directed upwardly through a gas inlet; carrying entrained particles in the column of gas to produce a fountain of particles over the fluidized bed of circulating particles and subside in the particle bed until being directed inwardly into the column of gas within the curvilinear profile.

Method for maximizing shale oil recovery from an underground formation

DOEpatents

Sisemore, Clyde J.

1980-01-01

A method for maximizing shale oil recovery from an underground oil shale formation which has previously been processed by in situ retorting such that there is provided in the formation a column of substantially intact oil shale intervening between adjacent spent retorts, which method includes the steps of back filling the spent retorts with an aqueous slurry of spent shale. The slurry is permitted to harden into a cement-like substance which stabilizes the spent retorts. Shale oil is then recovered from the intervening column of intact oil shale by retorting the column in situ, the stabilized spent retorts providing support for the newly developed retorts.

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of chlorinated pesticides in aquatic tissue by capillary-column gas chromatography with electron-capture detection

USGS Publications Warehouse

Leiker, Thomas J.; Madsen, J.E.; Deacon, J.R.; Foreman, W.T.

1995-01-01

A method for the determination of chlorinated organic compounds in aquatic tissue by dual capillary-column gas chromatography with electron-capture detection is described. Whole-body-fish or corbicula tissue is homogenized, Soxhlet extracted, lipid removed by gel permeation chromatography, and fractionated using alumina/silica adsorption chromatography. The extracts are analyzed by dissimilar capillary-column gas chromatography with electron-capture detection. The method reporting limits are 5 micrograms per kilogram (μg/kg) for chlorinated compounds, 50 μg/kg for polychlorinated biphenyls, and 200 μg/kg for toxaphene.

Apparatus and method for plasma processing of SRF cavities

NASA Astrophysics Data System (ADS)

Upadhyay, J.; Im, Do; Peshl, J.; Bašović, M.; Popović, S.; Valente-Feliciano, A.-M.; Phillips, L.; Vušković, L.

2016-05-01

An apparatus and a method are described for plasma etching of the inner surface of superconducting radio frequency (SRF) cavities. Accelerator SRF cavities are formed into a variable-diameter cylindrical structure made of bulk niobium, for resonant generation of the particle accelerating field. The etch rate non-uniformity due to depletion of the radicals has been overcome by the simultaneous movement of the gas flow inlet and the inner electrode. An effective shape of the inner electrode to reduce the plasma asymmetry for the coaxial cylindrical rf plasma reactor is determined and implemented in the cavity processing method. The processing was accomplished by moving axially the inner electrode and the gas flow inlet in a step-wise way to establish segmented plasma columns. The test structure was a pillbox cavity made of steel of similar dimension to the standard SRF cavity. This was adopted to experimentally verify the plasma surface reaction on cylindrical structures with variable diameter using the segmented plasma generation approach. The pill box cavity is filled with niobium ring- and disk-type samples and the etch rate of these samples was measured.

40 CFR 1065.275 - N2O measurement devices.

Code of Federal Regulations, 2012 CFR

2012-07-01

... for interpretation of infrared spectra. For example, EPA Test Method 320 is considered a valid method... uncompensated signal's bias. Examples of laser infrared analyzers are pulsed-mode high-resolution narrow band.... Examples of acceptable columns are a PLOT column consisting of bonded polystyrene-divinylbenzene or a...

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.

Towards Reconstructing a Doric Column in a Virtual Construction Site

NASA Astrophysics Data System (ADS)

Bartzis, D.

2017-02-01

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

Solution methods for one-dimensional viscoelastic problems

NASA Technical Reports Server (NTRS)

Stubstad, John M.; Simitses, George J.

1987-01-01

A recently developed differential methodology for solution of one-dimensional nonlinear viscoelastic problems is presented. Using the example of an eccentrically loaded cantilever beam-column, the results from the differential formulation are compared to results generated using a previously published integral solution technique. It is shown that the results obtained from these distinct methodologies exhibit a surprisingly high degree of correlation with one another. A discussion of the various factors affecting the numerical accuracy and rate of convergence of these two procedures is also included. Finally, the influences of some 'higher order' effects, such as straining along the centroidal axis are discussed.

Nitrogen removal from landfill leachate using single or combined processes.

PubMed

He, P J; Shao, L M; Guo, H D; Li, G J; Lee, D J

2005-04-01

The municipal solids waste (MSW) collected at Shanghai includes a high proportion of food waste, which is easily hydrolyzed to generate ammonia-nitrogen in leachate. This study investigated the efficiency of nitrogen removal from landfill leachate employing four different treatment processes. The simulated rainfall and direct leachate recycling produced strong leachate with high ammonia-nitrogen content, and resulted in the removal of only a small amount of nitrogen. Although pretreating the leachate using an aerobic reactor removed some nitrogen, most of which was transformed to biomass because of the high organic loading applied. Using the three-compartment system, which comprises a landfill column with fresh MSW, a column with well-decomposed refuse layer as the methane generator, and a nitrifier, the ammonia-nitrogen was converted into nitrogen gas and hence removed. Experimental results demonstrated the feasibility of adopting the three-compartment system for managing nitrogen in landfill leachate generated from high-nitrogen-content MSW.

76 FR 2109 - Next Generation Risk Assessment Public Dialogue Conference

Federal Register 2010, 2011, 2012, 2013, 2014

2011-01-12

... ENVIRONMENTAL PROTECTION AGENCY [FRL-9246-7] Next Generation Risk Assessment Public Dialogue Conference Correction In notice document 2010-32977 appearing on page 82387 in the issue of Thursday, December 30, 2010, make the following correction: In the second column, below the signature date, the...

Rapid micro-scale proteolysis of proteins for MALDI-MS peptide mapping using immobilized trypsin

NASA Astrophysics Data System (ADS)

Gobom, Johan; Nordhoff, Eckhard; Ekman, Rolf; Roepstorff, Peter

1997-12-01

In this study we present a rapid method for tryptic digestion of proteins using micro-columns with enzyme immobilized on perfusion chromatography media. The performance of the method is exemplified with acyl-CoA-binding protein and reduced carbamidomethylated bovine serum albumin. The method proved to be significantly faster and yielded a better sequence coverage and an improved signal-to-noise ratio for the MALDI-MS peptide maps, compared to in-solution- and on-target digestion. Only a single sample transfer step is required, and therefore sample loss due to adsorption to surfaces is reduced, which is a critical issue when handling low picomole to femtomole amounts of proteins. An example is shown with on-column proteolytic digestion and subsequent elution of the digest into a reversed-phase micro-column. This is useful if the sample contains large amounts of salt or is too diluted for MALDI-MS analysis. Furthermore, by step-wise elution from the reversedphase column, a complex digest can be fractionated, which reduces signal suppression and facilitates data interpretation in the subsequent MS-analysis. The method also proved useful for consecutive digestions with enzymes of different cleavage specificity. This is exemplified with on-column tryptic digestion, followed by reversed-phase step-wise elution, and subsequent on-target V8 protease digestion.

Freeze drying for gas chromatography stationary phase deposition

DOEpatents

Sylwester, Alan P [Livermore, CA

2007-01-02

The present disclosure relates to methods for deposition of gas chromatography (GC) stationary phases into chromatography columns, for example gas chromatography columns. A chromatographic medium is dissolved or suspended in a solvent to form a composition. The composition may be inserted into a chromatographic column. Alternatively, portions of the chromatographic column may be exposed or filled with the composition. The composition is permitted to solidify, and at least a portion of the solvent is removed by vacuum sublimation.

Isolation by cell-column chromatography of immunoglobulins specific for cell surface carbohydrates

PubMed Central

1977-01-01

A new method of affinity chromatography using glutaraldehyde-fixed cells immobilized on Sephadex beads has been used to isolate immunoglobulins (Ig's) specific for cell surface glycoproteins. Ig's that specifically bound and agglutinated the same cells as those originally fixed on the columns were isolated from nonimmune sera of various species. Periodate treatment of the cell-columns and the free cells destroyed their ability to bind the Ig's, and the binding of the Ig's to untreated cells was inhibited by monosaccharides such as D- galactose and sialic acid. The binding of antibodies directed against cell surfaces obtained by immunizing animals with the same mouse tumor cell lines used on the columns (P388 and EL4) was not inhibited by various saccharides. Surface glycoproteins obtained from the mouse tumor cells by immunoprecipitation with the column-isolated Ig's yielded specific electrophoretic patterns that differed from those obtained using Ig's from the sera of rabbits immunized with the tumor cells. The data suggest that the Ig's isolated by cell-column chromatography were directed against carbohydrates, probably those in terminal positions of the polysaccharide portions of the tumor cell surface glycoproteins. Column-isolated Ig's specific for carbohydrates were also useful in studies of cell interactions in nonmammalian systems including Dictyostelium discoideum and Saccharomyces cerevisiae. The cell-column method appears to be adaptable to the isolation of a variety of molecules in addition to antibodies. PMID:833547

The behavior of compression and degradation for municipal solid waste and combined settlement calculation method.

PubMed

Shi, Jianyong; Qian, Xuede; Liu, Xiaodong; Sun, Long; Liao, Zhiqiang

2016-09-01

The total compression of municipal solid waste (MSW) consists of primary, secondary, and decomposition compressions. It is usually difficult to distinguish between the three parts of compressions. In this study, the odeometer test was used to distinguish between the primary and secondary compressions to determine the primary and secondary compression coefficient. In addition, the ending time of the primary compressions were proposed based on municipal solid waste compression tests in a degradation-inhibited condition by adding vinegar. The amount of the secondary compression occurring in the primary compression stage has a relatively high percentage to either the total compression or the total secondary compression. The relationship between the degradation ratio and time was obtained from the tests independently. Furthermore, a combined compression calculation method of municipal solid waste for all three parts of compressions including considering organics degradation is proposed based on a one-dimensional compression method. The relationship between the methane generation potential L0 of LandGEM model and degradation compression index was also discussed in the paper. A special column compression apparatus system, which can be used to simulate the whole compression process of municipal solid waste in China, was designed. According to the results obtained from 197-day column compression test, the new combined calculation method for municipal solid waste compression was analyzed. The degradation compression is the main part of the compression of MSW in the medium test period. Copyright © 2015 Elsevier Ltd. All rights reserved.

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

PubMed

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

2014-08-15

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

ANALYSIS OF FERRIC AND FERROUS IONS IN SOIL EXTRACTS BY ION CHROMATOGRAPHY

EPA Science Inventory

A method using ion chromatography (IC) for the analysis of ferrous (Fe 2+) and ferric (Fe 3+) ions in soil extracts has been developed. This method uses an ion exchange column with detection at 520 nm after post-column derivatization. Selectivity is achieved by using an anionic...

Developing a Method for Resolving NOx Emission Inventory Biases Using Discrete Kalman Filter Inversion, Direct Sensitivities, and Satellite-Based Columns

EPA Science Inventory

An inverse method was developed to integrate satellite observations of atmospheric pollutant column concentrations and direct sensitivities predicted by a regional air quality model in order to discern biases in the emissions of the pollutant precursors.

Clean-up of a pesticide-lanolin mixture by gel permeation chromatography.

PubMed

López-Mesas, M; Crespi, M; Brach, J; Mullender, J P

2000-12-01

In this study, the efficiency of a clean-up method by gel permeation chromatography (GPC) for the separation of pesticides from lanolin is analyzed. The pesticides analyzed belong to two different families, organophosphorous and synthetic pyrethroids. Lanolin, a standard mixture of the pesticides, and a lanolin-pesticides mixture are injected in a GPC column. The recoveries and elution times from the GPC column of lanolin (by a gravimetric method) and pesticides (by gas chromatography-electron capture detector) are determined. From this column, a good separation of the lanolin-pesticides mixture is observed.

METHOD OF OPERATING A HEAVY WATER MODERATED REACTOR

DOEpatents

Vernon, H.C.

1962-08-14

A method of removing fission products from the heavy water used in a slurry type nuclear reactor is described. According to the process the slurry is steam distilled with carbon tetrachloride so that at least a part of the heavy water and carbon tetrachloride are vaporized; the heavy water and carbon tetrachloride are separated; the carbon tetrachloride is returned to the steam distillation column at different points in the column to aid in depositing the slurry particles at the bottom of the column; and the heavy water portion of the condensate is purified. (AEC)

Deterministic Modeling of the High Temperature Test Reactor with DRAGON-HEXPEDITE

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

J. Ortensi; M.A. Pope; R.M. Ferrer

2010-10-01

The Idaho National Laboratory (INL) is tasked with the development of reactor physics analysis capability of the Next Generation Nuclear Power (NGNP) project. In order to examine the INL’s current prismatic reactor analysis tools, the project is conducting a benchmark exercise based on modeling the High Temperature Test Reactor (HTTR). This exercise entails the development of a model for the initial criticality, a 19 fuel column thin annular core, and the fully loaded core critical condition with 30 fuel columns. Special emphasis is devoted to physical phenomena and artifacts in HTTR that are similar to phenomena and artifacts in themore » NGNP base design. The DRAGON code is used in this study since it offers significant ease and versatility in modeling prismatic designs. DRAGON can generate transport solutions via Collision Probability (CP), Method of Characteristics (MOC) and Discrete Ordinates (Sn). A fine group cross-section library based on the SHEM 281 energy structure is used in the DRAGON calculations. The results from this study show reasonable agreement in the calculation of the core multiplication factor with the MC methods, but a consistent bias of 2–3% with the experimental values is obtained. This systematic error has also been observed in other HTTR benchmark efforts and is well documented in the literature. The ENDF/B VII graphite and U235 cross sections appear to be the main source of the error. The isothermal temperature coefficients calculated with the fully loaded core configuration agree well with other benchmark participants but are 40% higher than the experimental values. This discrepancy with the measurement partially stems from the fact that during the experiments the control rods were adjusted to maintain criticality, whereas in the model, the rod positions were fixed. In addition, this work includes a brief study of a cross section generation approach that seeks to decouple the domain in order to account for neighbor effects. This spectral interpenetration is a dominant effect in annular HTR physics. This analysis methodology should be further explored in order to reduce the error that is systematically propagated in the traditional generation of cross sections.« less

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

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.

Effects of ethanol-based fuel contamination: microbial community changes, production of regulated compounds, and methane generation.

PubMed

Nelson, Denice K; Lapara, Timothy M; Novak, Paige J

2010-06-15

Ethanol-based fuels are becoming more heavily used, increasing the likelihood of ethanol-based fuel spills during transportation and storage. Although ethanol is well-known to be readily biodegradable, very little is known about the effects that such a spill might have on an indigenous microbial community. Of particular concern is that ethanol contamination could stimulate the growth of organisms that can generate regulated compounds and/or produce explosive quantities of methane gas. A column-based study was performed to elucidate the potential impacts of ethanol-based fuel (E85) on the indigenous microbial community during a simulated fuel spill. A continuous dilute supply of E85 resulted in profound shifts in both the bacterial and archaeal communities. The shift was accompanied by the production of high concentrations of volatile fatty acids and butanol, a compound that is regulated in groundwater by some states. Results also indicated that a continuous feed of dilute E85 generated explosive levels of methane within one month of column operation. Quantitative PCR data showed a statistically significant increase in methanogenic populations when compared to a control column. The elevated population numbers correlated to areas of the column receiving a sustained carbon load. Toxicity data indicated that microbial growth was completely inhibited (as evidenced by absence of ethanol breakdown products) at ethanol levels above 6% (v/v). These data suggest that ethanol from ethanol-based fuel can be readily degraded, but can also produce metabolic products that are regulated as well as explosive levels of methane. The core of an E85 spill may serve as a long-term source of contamination as it cannot be degraded until significant dilution has occurred.

Global Free Tropospheric NO2 Abundances Derived Using a Cloud Slicing Technique Applied to Satellite Observations from the Aura Ozone Monitoring Instrument (OMI)

NASA Technical Reports Server (NTRS)

Choi, S.; Joiner, J.; Choi, Y.; Duncan, B. N.; Bucsela, E.

2014-01-01

We derive free-tropospheric NO2 volume mixing ratios (VMRs) and stratospheric column amounts of NO2 by applying a cloud slicing technique to data from the Ozone Monitoring Instrument (OMI) on the Aura satellite. In the cloud-slicing approach, the slope of the above-cloud NO2 column versus the cloud scene pressure is proportional to the NO2 VMR. In this work, we use a sample of nearby OMI pixel data from a single orbit for the linear fit. The OMI data include cloud scene pressures from the rotational-Raman algorithm and above-cloud NO2 vertical column density (VCD) (defined as the NO2 column from the cloud scene pressure to the top-of-the-atmosphere) from a differential optical absorption spectroscopy (DOAS) algorithm. Estimates of stratospheric column NO2 are obtained by extrapolating the linear fits to the tropopause. We compare OMI-derived NO2 VMRs with in situ aircraft profiles measured during the NASA Intercontinental Chemical Transport Experiment Phase B (INTEX-B) campaign in 2006. The agreement is generally within the estimated uncertainties when appropriate data screening is applied. We then derive a global seasonal climatology of free-tropospheric NO2 VMR in cloudy conditions. Enhanced NO2 in the free troposphere commonly appears near polluted urban locations where NO2 produced in the boundary layer may be transported vertically out of the boundary layer and then horizontally away from the source. Signatures of lightning NO2 are also shown throughout low and middle latitude regions in summer months. A profile analysis of our cloud slicing data indicates signatures of uplifted and transported anthropogenic NO2 in the middle troposphere as well as lightning-generated NO2 in the upper troposphere. Comparison of the climatology with simulations from the Global Modeling Initiative (GMI) for cloudy conditions (cloud optical thicknesses > 10) shows similarities in the spatial patterns of continental pollution outflow. However, there are also some differences in the seasonal variation of free-tropospheric NO2 VMRs near highly populated regions and in areas affected by lightning-generated NOx. Stratospheric column NO2 obtained from cloud slicing agrees well with other independently-generated estimates, providing further confidence in the free-tropospheric results.

Ranking nano-enabled hybrid media for simultaneous removal of contaminants with different chemistries: Pseudo-equilibrium sorption tests versus column tests.

PubMed

Custodio, Tomas; Garcia, Jose; Markovski, Jasmina; McKay Gifford, James; Hristovski, Kiril D; Olson, Larry W

2017-12-15

The underlying hypothesis of this study was that pseudo-equilibrium and column testing conditions would provide the same sorbent ranking trends although the values of sorbents' performance descriptors (e.g. sorption capacity) may vary because of different kinetics and competition effects induced by the two testing approaches. To address this hypothesis, nano-enabled hybrid media were fabricated and its removal performances were assessed for two model contaminants under multi-point batch pseudo-equilibrium and continuous-flow conditions. Calculation of simultaneous removal capacity indices (SRC) demonstrated that the more resource demanding continuous-flow tests are able to generate the same performance rankings as the ones obtained by conducing the simpler pseudo-equilibrium tests. Furthermore, continuous overlap between the 98% confidence boundaries for each SRC index trend, not only validated the hypothesis that both testing conditions provide the same ranking trends, but also pointed that SRC indices are statistically the same for each media, regardless of employed method. In scenarios where rapid screening of new media is required to obtain the best performing synthesis formulation, use of pseudo-equilibrium tests proved to be reliable. Considering that kinetics induced effects on sorption capacity must not be neglected, more resource demanding column test could be conducted only with the top performing media that exhibit the highest sorption capacity. Copyright © 2017 Elsevier B.V. All rights reserved.

Increasing Flexibility in Two-Dimensional Liquid Chromatography by Pulsed Elution of the First Dimension: A Proof of Concept.

PubMed

Jakobsen, Simon S; Christensen, Jan H; Verdier, Sylvain; Mallet, Claude R; Nielsen, Nikoline J

2017-09-05

This work demonstrates the development of an online two-dimensional liquid chromatography (2D-LC) method where the first dimension column is eluted by a sequence of pulses of increasing eluotropic strength generated by the LC pumps (pulsed-elution 2D-LC). Between the pulses, the first dimension is kept in a no-elution state using low eluent strength. The eluate from the first dimension is actively modulated using trap columns and subsequently analyzed in the second dimension. We demonstrate that by tuning the length and eluotropic strength of the pulses, peaks with retention factors in water, k w , above 150 can be manipulated to elute in 3-4 pulses. The no-elution state can be kept for 1-10 min with only minor changes as to which and how many pulses the peaks elute in. Pulsed-elution 2D-LC combined with active modulation tackles three of the main challenges encountered in 2D-LC and specifically online comprehensive 2D-LC: undersampling, difficulties in refocusing, and lack of flexibility in the selection of column dimensions and flow rates because the two dimensions constrain each other. The pulsed-elution 2D-LC was applied for the analysis of a basic fraction of vacuum gas oil. Peak capacity was 4018 for a 540 min analysis and 4610 for a 1040 min analysis.

Recovery of isopropyl alcohol from waste solvent of a semiconductor plant.

PubMed

Lin, Sheng H; Wang, Chuen S

2004-01-30

An important waste solvent generated in the semiconductor manufacturing process was characterized by high isopropyl alcohol (IPA) concentration over 65%, other organic pollutants and strong color. Because of these characteristics, IPA recovery was deemed as a logic choice for tackling this waste solvent. In the present work, an integrated method consisting of air stripping in conjunction with condensation and packed activated carbon fiber (ACF) adsorption for dealing with this waste solvent. The air stripping with proper stripping temperature control was employed to remove IPA from the waste solvent and the IPA vapor in the gas mixture was condensed out in a side condenser. The residual IPA remaining in the gas mixture exiting the side condenser was efficiently removed in a packed ACF column. The air stripping with condensation was able to recover up to 93% of total IPA in the initial waste solvent. The residual IPA in the gas mixture, representing less than 3% of the initial IPA, was efficiently captured in the packed ACF column. Experimental tests were conducted to examine the performances of each unit and to identify the optimum operating conditions. Theoretical modeling of the experimental IPA breakthrough curves was also undertaken using a macroscopic model. The verified breakthrough model significantly facilitates the adsorption column design. The recovered IPA was found to be of high purity and could be considered for reuse. Copyright 2003 Elsevier B.V.

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.

Enrichment isolation of adipose-derived stem/stromal cells from the liquid portion of liposuction aspirates with the use of an adherent column.

PubMed

Doi, Kentaro; Kuno, Shinichiro; Kobayashi, Akira; Hamabuchi, Takahisa; Kato, Harunosuke; Kinoshita, Kahori; Eto, Hitomi; Aoi, Noriyuki; Yoshimura, Kotaro

2014-03-01

Adipose-derived stem/progenitor cells (ASCs) are typically obtained from the lipoaspirates; however, a smaller number of ASCs can be isolated without enzymatic digestion from the infranatant liposuction aspirate fluid (LAF). We evaluated the effectiveness of an adherent column, currently used to isolate mesenchymal stromal cells from bone marrow, to isolate LAF cells. We applied peripheral blood (PB), PB mixed with cultured ASCs (PB-ASC), and LAF solution to the column and divided it into two fractions, the adherent (positive) and the non-adherent (negative) fractions. We compared this method with hypotonic hemolysis (lysis) for the red blood cell count, nucleated cells count and cell compositions as well as functional properties of isolated mesenchymal cells. The column effectively removed red blood cells, though the removal efficiency was slightly inferior to hemolysis. After column processing of PB-ASC, 60.5% of ASCs (53.2% by lysis) were selectively collected in the positive fraction, and the negative fraction contained almost no ASCs. After processing of LAF solution, nucleated cell yields were comparable between the column and hemolysis; however, subsequent adherent culture indicated that a higher average ASC yield was obtained from the column-positive samples than from the lysis samples, suggesting that the column method may be superior to hemolysis for obtaining viable ASCs. Mesenchymal differentiation and network formation assays showed no statistical differences in ASC functions between the lysis and column-positive samples. Our results suggest that a column with non-woven rayon and polyethylene fabrics is useful for isolating stromal vascular fraction cells from LAF solutions for clinical applications. Copyright © 2014 International Society for Cellular Therapy. Published by Elsevier Inc. All rights reserved.

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.

Calcium Isotope Analysis with "Peak Cut" Method on Column Chemistry

NASA Astrophysics Data System (ADS)

Zhu, H.; Zhang, Z.; Liu, F.; Li, X.

2017-12-01

To eliminate isobaric interferences from elemental and molecular isobars (e.g., 40K+, 48Ti+, 88Sr2+, 24Mg16O+, 27Al16O+) on Ca isotopes during mass determination, samples should be purified through ion-exchange column chemistry before analysis. However, large Ca isotopic fractionation has been observed during column chemistry (Russell and Papanastassiou, 1978; Zhu et al., 2016). Therefore, full recovery during column chemistry is greatly needed, otherwise uncertainties would be caused by poor recovery (Zhu et al., 2016). Generally, matrix effects could be enhanced by full recovery, as other elements might overlap with Ca cut during column chemistry. Matrix effects and full recovery are difficult to balance and both need to be considered for high-precision analysis of stable Ca isotopes. Here, we investigate the influence of poor recovery on δ44/40Ca using TIMS with the double spike technique. The δ44/40Ca values of IAPSO seawater, ML3B-G and BHVO-2 in different Ca subcats (e.g., 0-20, 20-40, 40-60, 60-80, 80-100%) with 20% Ca recovery on column chemistry display limited variation after correction by the 42Ca-43Ca double spike technique with the exponential law. Notably, δ44/40Ca of each Ca subcut is quite consistent with δ44/40Ca of Ca cut with full recovery within error. Our results indicate that the 42Ca-43Ca double spike technique can simultaneously correct both of the Ca isotopic fractionation that occurred during column chemistry and thermal ionization mass spectrometry (TIMS) determination properly, because both of the isotopic fractionation occurred during analysis follow the exponential law well. Therefore, we propose the "peak cut" method on Ca column chemistry for samples with complex matrix effects. Briefly, for samples with low Ca contents, we can add the double spike before column chemistry, and only collect the middle of the Ca eluate and abandon the both sides of Ca eluate that might overlap with other elements (e.g., K, Sr). This method would eliminate matrix effects and improve efficiency for the column chemistry.

Osmium-191/iridium-191m radionuclide

DOEpatents

Knapp, Jr., Furn F.; Butler, Thomas A.; Brihaye, Claude

1987-01-01

A generator system to provide iridium-191m for clinical imaging applications comprises an activated carbon adsorbent loaded with a compound containing the parent nuclide, osmium-191. The generator, which has a shelf-life in excess of two weeks and does not require a scavenger column, can be eluted with physiologically compatible saline.

Method of Forming Three-Dimensional Semiconductors Structures

NASA Technical Reports Server (NTRS)

Fathauer, Robert W. (Inventor)

2002-01-01

Silicon and metal are coevaporated onto a silicon substrate in a molecular beam epitaxy system with a larger than stoichiometric amount of silicon so as to epitaxially grow columns of metal silicide embedded in a matrix of single crystal, epitaxially grown silicon. Higher substrate temperatures and lower deposition rates yield larger columns that are farther apart while more silicon produces smaller columns. Column shapes and locations are selected by seeding the substrate with metal silicide starting regions. A variety of 3-dimensional, exemplary electronic devices are disclosed.

Twisting of thin walled columns perfectly restrained at one end

NASA Technical Reports Server (NTRS)

Lazzarino, Lucio

1938-01-01

Proceeding from the basic assumptions of the Batho-Bredt theory on twisting failure of thin-walled columns, the discrepancies most frequently encountered are analyzed. A generalized approximate method is suggested for the determination of the disturbances in the stress condition of the column, induced by the constrained warping in one of the end sections.

Improved quality-by-design compliant methodology for method development in reversed-phase liquid chromatography.

PubMed

Debrus, Benjamin; Guillarme, Davy; Rudaz, Serge

2013-10-01

A complete strategy dedicated to quality-by-design (QbD) compliant method development using design of experiments (DOE), multiple linear regressions responses modelling and Monte Carlo simulations for error propagation was evaluated for liquid chromatography (LC). The proposed approach includes four main steps: (i) the initial screening of column chemistry, mobile phase pH and organic modifier, (ii) the selectivity optimization through changes in gradient time and mobile phase temperature, (iii) the adaptation of column geometry to reach sufficient resolution, and (iv) the robust resolution optimization and identification of the method design space. This procedure was employed to obtain a complex chromatographic separation of 15 antipsychotic basic drugs, widely prescribed. To fully automate and expedite the QbD method development procedure, short columns packed with sub-2 μm particles were employed, together with a UHPLC system possessing columns and solvents selection valves. Through this example, the possibilities of the proposed QbD method development workflow were exposed and the different steps of the automated strategy were critically discussed. A baseline separation of the mixture of antipsychotic drugs was achieved with an analysis time of less than 15 min and the robustness of the method was demonstrated simultaneously with the method development phase. Copyright © 2013 Elsevier B.V. All rights reserved.

Temperature-enhanced alumina HPLC method for the analysis of wax esters, sterol esters, and methyl esters.

PubMed

Moreau, Robert A; Kohout, Karen; Singh, Vijay

2002-12-01

Previous attempts at separating nonpolar lipid esters (including wax esters, sterol esters, and methyl esters) have achieved only limited success. Among the several normal-phase methods tested, a single recent report of a method employing an alumina column at 30 degrees C with a binary gradient system was the most promising. In the current study, modification of the alumina method by increasing the column temperature to 75 degrees C improved the separation of standards of wax esters and sterol esters. Elevated column temperature also enhanced the separation of FAME with differing degrees of unsaturation. Evidence was also presented to indicate that the method similarly separated phytosterol esters, based on their levels of unsaturation. With the increased interest in phytosterol- and phytostanol-ester enriched functional foods, this method should provide a technique to characterize and compare these products.

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of organophosphate pesticides in filtered water by gas chromatography with flame photometric detection

USGS Publications Warehouse

Jha, Virendra K.; Wydoski, Duane S.

2002-01-01

A method for the isolation of 20 parent organophosphate pesticides and 5 pesticide degradates from filtered natural-water samples is described. Seven of these compounds are reported permanently with an estimated concentration because of performance issues. Water samples are filtered to remove suspended particulate matter, and then 1 liter of filtrate is pumped through disposable solid-phase extraction columns that contain octadecyl-bonded porous silica to extract the compounds. The C-18 columns are dried with nitrogen gas, and method compounds are eluted from the columns with ethyl acetate. The extract is analyzed by dual capillary-column gas chromatography with flame photometric detection. Single-operator method detection limits in all three water-matrix samples ranged from 0.004 to 0.012 microgram per liter. Method performance was validated by spiking all compounds into three different matrices at three different concentrations. Eight replicates were analyzed at each concentration level in each matrix. Mean recoveries of method compounds spiked in surface-water samples ranged from 39 to 149 percent and those in ground-water samples ranged from 40 to 124 percent for all pesticides except dimethoate. Mean recoveries of method compounds spiked in reagent-water samples ranged from 41 to 119 percent for all pesticides except dimethoate. Dimethoate exhibited reduced recoveries (mean of 43 percent in low- and medium-concentration level spiked samples and 20 percent in high-concentration level spiked samples) in all matrices because of incomplete collection on the C-18 column. As a result, concen-trations of dimethoate and six other compounds (based on performance issues) in samples are reported in this method with an estimated remark code.

Quantifying the condition of eruption column collapse during explosive volcanic eruptions

NASA Astrophysics Data System (ADS)

Koyaguchi, Takehiro; Suzuki, Yujiro

2016-04-01

During an explosive eruption, a mixture of pyroclasts and volcanic gas forms a buoyant eruption column or a pyroclastic flow. Generation of a pyroclastic flow caused by eruption column collapse is one of the most hazardous phenomena during explosive volcanic eruptions. The quantification of column collapse condition (CCC) is, therefore, highly desired for volcanic hazard assessment. Previously the CCC was roughly predicted by a simple relationship between magma discharge rate and water content (e.g., Carazzo et al., 2008). When a crater is present above the conduit, because of decompression/compression process inside/above the crater, the CCC based on this relationship can be strongly modified (Woods and Bower, 1995; Koyaguchi et al., 2010); however, the effects of the crater on CCC has not been fully understood in a quantitative fashion. Here, we have derived a semi-analytical expression of CCC, in which the effects of the crater is taken into account. The CCC depends on magma properties, crater shape (radius, depth and opening angle) as well as the flow rate at the base of crater. Our semi-analytical CCC expresses all these dependencies by a single surface in a parameter space of the dimensionless magma discharge rate, the dimensionless magma flow rate (per unit area) and the ratio of the cross-sectional areas at the top and the base of crater. We have performed a systematic parameter study of three-dimensional (3D) numerical simulations of eruption column dynamics to confirm the semi-analytical CCC. The results of the 3D simulations are consistent with the semi-analytical CCC, while they show some additional fluid dynamical features in the transitional state (e.g., partial column collapse). Because the CCC depends on such many parameters, the scenario towards the generation of pyroclastic flow during explosive eruptions is considered to be diverse. Nevertheless, our semi-analytical CCC together with the existing semi-analytical solution for the 1D conduit flow model (Koyaguchi, 2005) allows us to intuitively and quantitatively understand how the eruption column dynamics approaches to the CCC as the crater radius increases during the waxing stage of an eruption, or as the magma chamber pressure decreases during the waning stage.

Column-coupling strategies for multidimensional electrophoretic separation techniques.

PubMed

Kler, Pablo A; Sydes, Daniel; Huhn, Carolin

2015-01-01

Multidimensional electrophoretic separations represent one of the most common strategies for dealing with the analysis of complex samples. In recent years we have been witnessing the explosive growth of separation techniques for the analysis of complex samples in applications ranging from life sciences to industry. In this sense, electrophoretic separations offer several strategic advantages such as excellent separation efficiency, different methods with a broad range of separation mechanisms, and low liquid consumption generating less waste effluents and lower costs per analysis, among others. Despite their impressive separation efficiency, multidimensional electrophoretic separations present some drawbacks that have delayed their extensive use: the volumes of the columns, and consequently of the injected sample, are significantly smaller compared to other analytical techniques, thus the coupling interfaces between two separations components must be very efficient in terms of providing geometrical precision with low dead volume. Likewise, very sensitive detection systems are required. Additionally, in electrophoretic separation techniques, the surface properties of the columns play a fundamental role for electroosmosis as well as the unwanted adsorption of proteins or other complex biomolecules. In this sense the requirements for an efficient coupling for electrophoretic separation techniques involve several aspects related to microfluidics and physicochemical interactions of the electrolyte solutions and the solid capillary walls. It is interesting to see how these multidimensional electrophoretic separation techniques have been used jointly with different detection techniques, for intermediate detection as well as for final identification and quantification, particularly important in the case of mass spectrometry. In this work we present a critical review about the different strategies for coupling two or more electrophoretic separation techniques and the different intermediate and final detection methods implemented for such separations.

Dynamic interpretation of slug tests in highly permeable aquifers

USGS Publications Warehouse

Zurbuchen, Brian R.; Zlotnik, Vitaly A.; Butler, James J.

2002-01-01

Considerable progress has been made in developing a theoretical framework for modeling slug test responses in formations with high hydraulic conductivity K. However, several questions of practical significance remain unresolved. Given the rapid and often oscillatory nature of test responses, the traditional hydrostatic relationship between the water level and the transducer‐measured head in the water column may not be appropriate. A general dynamic interpretation is proposed that describes the relationship between water level response and transducer‐measured head. This theory is utilized to develop a procedure for transforming model‐generated water level responses to transducer readings. The magnitude of the difference between the actual water level position and the apparent position based on the transducer measurement is a function of the acceleration and velocity of the water column, test geometry, and depth of the transducer. The dynamic approach explains the entire slug test response, including the often‐noted discrepancy between the actual initial water level displacement and that measured by a transducer in the water column. Failure to use this approach can lead to a significant underestimation of K when the transducer is a considerable distance below the static water level. Previous investigators have noted a dependence of test responses on the magnitude of the initial water level displacement and have developed various approximate methods for analyzing such data. These methods are re‐examined and their limitations clarified. Practical field guidelines are proposed on the basis of findings of this work. The soundness of the dynamic approach is demonstrated through a comparison of K profiles from a series of multilevel slug tests with those from dipole‐flow tests performed in the same wells.

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

PubMed

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

2015-08-28

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

Extracting concrete thermal characteristics from temperature time history of RC column exposed to standard fire.

PubMed

Kim, Jung J; Youm, Kwang-Soo; Reda Taha, Mahmoud M

2014-01-01

A numerical method to identify thermal conductivity from time history of one-dimensional temperature variations in thermal unsteady-state is proposed. The numerical method considers the change of specific heat and thermal conductivity with respect to temperature. Fire test of reinforced concrete (RC) columns was conducted using a standard fire to obtain time history of temperature variations in the column section. A thermal equilibrium model in unsteady-state condition was developed. The thermal conductivity of concrete was then determined by optimizing the numerical solution of the model to meet the observed time history of temperature variations. The determined thermal conductivity with respect to temperature was then verified against standard thermal conductivity measurements of concrete bricks. It is concluded that the proposed method can be used to conservatively estimate thermal conductivity of concrete for design purpose. Finally, the thermal radiation properties of concrete for the RC column were estimated from the thermal equilibrium at the surface of the column. The radiant heat transfer ratio of concrete representing absorptivity to emissivity ratio of concrete during fire was evaluated and is suggested as a concrete criterion that can be used in fire safety assessment.

Extracting Concrete Thermal Characteristics from Temperature Time History of RC Column Exposed to Standard Fire

PubMed Central

2014-01-01

A numerical method to identify thermal conductivity from time history of one-dimensional temperature variations in thermal unsteady-state is proposed. The numerical method considers the change of specific heat and thermal conductivity with respect to temperature. Fire test of reinforced concrete (RC) columns was conducted using a standard fire to obtain time history of temperature variations in the column section. A thermal equilibrium model in unsteady-state condition was developed. The thermal conductivity of concrete was then determined by optimizing the numerical solution of the model to meet the observed time history of temperature variations. The determined thermal conductivity with respect to temperature was then verified against standard thermal conductivity measurements of concrete bricks. It is concluded that the proposed method can be used to conservatively estimate thermal conductivity of concrete for design purpose. Finally, the thermal radiation properties of concrete for the RC column were estimated from the thermal equilibrium at the surface of the column. The radiant heat transfer ratio of concrete representing absorptivity to emissivity ratio of concrete during fire was evaluated and is suggested as a concrete criterion that can be used in fire safety assessment. PMID:25180197

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).

Simultaneous gas chromatographic determination of four toxic gases generally present in combustion atmospheres.

PubMed

Endecott, B R; Sanders, D C; Chaturvedi, A K

1996-01-01

The measurement of combustion gases produced by burning aircraft cabin materials poses a continuing limitation for smoke toxicity research. Because toxic effects of gases depend on both their concentrations and the duration of exposure, frequent atmosphere sampling is necessary to define the gas concentration-exposure time curve. A gas chromatographic (GC) method was developed for the simultaneous analyses of carbon monoxide (CO), hydrogen sulfide (H2S), sulfur dioxide (SO2), and hydrogen cyanide (HCN). The method used an MTI M200 dual-column gas chromatograph equipped with 4-m molecular sieve-5A and 8-m PoraPlot-U wall-coated capillary columns and two low-volume, high-sensitivity thermal conductivity detectors. Detectability (in parts per million [ppm]) and retention times (in seconds) for the gases were as follows: CO, 100 ppm, 28 s; H2S, 50 ppm, 26 s; SO2, 125 ppm, 76 s; and HCN, 60 ppm, 108 s. The method was effective for determining these gases in mixtures and in the combustion atmospheres generated by burning wool (CO, HCN, and H2S) and modacrylic fabrics (CO and HCN). Common atmospheric gaseous or combustion products (oxygen, carbon dioxide, nitrogen, water vapor, and other volatiles) did not interfere with the analyses. However, filtration of the combustion atmospheres was necessary to prevent restriction of the GC sampling inlet by smoke particulates. The speed, sensitivity, and selectivity of this method make it suitable for smoke toxicity research and for evaluating performance of passenger protective breathing equipment. Also, this method can potentially be modified to analyze these gases when they are liberated from biosamples.

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.

Methods and reagents. Degraded DNA and gel tornados.

PubMed

Hengen, P N

1997-04-01

Methods and reagents is a unique monthly column that highlights current discussions in the newsgroup bionet.molbio.methds-reagnts, available on the Internet. This month's column discusses a case of inexplicable DNA degradation and tornados seen in agarose gels. For details on how to partake in the newsgroup, see the accompanying box.

The effects of load history and design variables on performance limit states of circular bridge columns - volume 3 : analysis methods.

DOT National Transportation Integrated Search

2015-01-01

This report is the third of three volumes and presents the numerical portion of the research project on the impacts of loading history on : the behavior of reinforced concrete bridge columns. Two independent finite element methods were utilized to ac...

40 CFR 799.6784 - TSCA water solubility: Column elution method; shake flask method.

Code of Federal Regulations, 2011 CFR

2011-07-01

....053 (3) The column should be connected to a recycling pump capable of controlling flows of... the carrier is not achieved due to partition effects on the surface of the carrier. (2) The loading of... this, the recycling pump is connected and the apparatus allowed to run until equilibration is...

40 CFR 799.6784 - TSCA water solubility: Column elution method; shake flask method.

Code of Federal Regulations, 2013 CFR

2013-07-01

....053 (3) The column should be connected to a recycling pump capable of controlling flows of... the carrier is not achieved due to partition effects on the surface of the carrier. (2) The loading of... this, the recycling pump is connected and the apparatus allowed to run until equilibration is...

40 CFR 799.6784 - TSCA water solubility: Column elution method; shake flask method.

Code of Federal Regulations, 2012 CFR

2012-07-01

....053 (3) The column should be connected to a recycling pump capable of controlling flows of... the carrier is not achieved due to partition effects on the surface of the carrier. (2) The loading of... this, the recycling pump is connected and the apparatus allowed to run until equilibration is...

40 CFR 799.6784 - TSCA water solubility: Column elution method; shake flask method.

Code of Federal Regulations, 2014 CFR

2014-07-01

....053 (3) The column should be connected to a recycling pump capable of controlling flows of... the carrier is not achieved due to partition effects on the surface of the carrier. (2) The loading of... this, the recycling pump is connected and the apparatus allowed to run until equilibration is...

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 ...

High Performance Liquid Chromatographic Analysis of Phytoplankton Pigments Using a C16-Amide Column

EPA Science Inventory

A reverse-phase high performance liquid chromatographic (RP-HPLC) method was developed to analyze in a single run, most polar and non-polar chlorophylls and carotenoids from marine phytoplankton. The method is based on a RP-C16-Amide column and a ternary gradient system consistin...

Systematic Interpolation Method Predicts Antibody Monomer-Dimer Separation by Gradient Elution Chromatography at High Protein Loads.

PubMed

Creasy, Arch; Reck, Jason; Pabst, Timothy; Hunter, Alan; Barker, Gregory; Carta, Giorgio

2018-05-29

A previously developed empirical interpolation (EI) method is extended to predict highly overloaded multicomponent elution behavior on a cation exchange (CEX) column based on batch isotherm data. Instead of a fully mechanistic model, the EI method employs an empirically modified multicomponent Langmuir equation to correlate two-component adsorption isotherm data at different salt concentrations. Piecewise cubic interpolating polynomials are then used to predict competitive binding at intermediate salt concentrations. The approach is tested for the separation of monoclonal antibody monomer and dimer mixtures by gradient elution on the cation exchange resin Nuvia HR-S. Adsorption isotherms are obtained over a range of salt concentrations with varying monomer and dimer concentrations. Coupled with a lumped kinetic model, the interpolated isotherms predict the column behavior for highly overloaded conditions. Predictions based on the EI method showed good agreement with experimental elution curves for protein loads up to 40 mg/mL column or about 50% of the column binding capacity. The approach can be extended to other chromatographic modalities and to more than two components. This article is protected by copyright. All rights reserved.

Ionic liquids as stationary phases for fatty acid analysis by gas chromatography.

PubMed

Fanali, C; Micalizzi, G; Dugo, P; Mondello, L

2017-12-04

The present paper provides an overview of the application of ionic liquid (IL) columns for GC analysis of fatty acid methyl esters (FAMEs). Although their separation can be carried out utilizing GC columns containing polar stationary phases, some ILs have been employed as stationary phases, either commercial or laboratory made, in GC analysis. Monodimensional and bidimensional GC methods have been optimized in order to achieve the best separation especially considering the geometric and positional isomers of unsaturated fatty acids. Several methods for the analysis of trans-fatty acids have also been reported. The use of GC-GC, using either the same IL columns or different columns in the first and second dimensions, allowed the separation of a large number of FAMEs. The application of the IL columns for GC analysis of FAMEs in different types of real samples is described, e.g., oil of different nature (fish, flaxseed, and olive), margarine and butter, biodiesel, milk, bacteria etc.

Evaluation of comprehensive multidimensional separations using reversed-phase, reversed-phase liquid chromatography/mass spectrometry for shotgun proteomics.

PubMed

Nakamura, Tatsuji; Kuromitsu, Junro; Oda, Yoshiya

2008-03-01

Two-dimensional liquid-chromatographic (LC) separation followed by mass spectrometric (MS) analysis was examined for the identification of peptides in complex mixtures as an alternative to widely used two-dimensional gel electrophoresis followed by MS analysis for use in proteomics. The present method involves the off-line coupling of a narrow-bore, polymer-based, reversed-phase column using an acetonitrile gradient in an alkaline mobile phase in the first dimension with octadecylsilanized silica (ODS)-based nano-LC/MS in the second dimension. After the first separation, successive fractions were acidified and dried off-line, then loaded on the second dimension column. Both columns separate peptides according to hydrophobicity under different pH conditions, but more peptides were identified than with the conventional technique for shotgun proteomics, that is, the combination of a strong cation exchange column with an ODS column, and the system was robust because no salts were included in the mobile phases. The suitability of the method for proteomics measurements was evaluated.

Counteracting moment device for reduction of earthquake-induced excursions of multi-level buildings.

PubMed

Nagaya, K; Fukushima, T; Kosugi, Y

1999-05-01

A vibration-control mechanism for beams and columns was presented in our previous report in which the earthquake force was transformed into a vibration-control force by using a gear train mechanism. In our previous report, however, only the principle of transforming the earthquake force into the control force was presented; the discussion for real structures and the design method were not presented. The present article provides a theoretical analysis of the column which is used in multi-layered buildings. Experimental tests were carried out for a model of multi-layered buildings in the frequency range of a principal earthquake wave. Theoretical results are compared to the experimental data. The optimal design of the control mechanism, which is of importance in the column design, is presented. Numerical calculations are carried out for the optimal design. It is shown that vibrations of the column involving the mechanism are suppressed remarkably. The optimal design method and the analytical results are applicable to the design of the column.

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.

Using the liquid nature of the stationary phase in countercurrent chromatography. IV. The cocurrent CCC method.

PubMed

Berthod, Alain; Hassoun, Mahmoud

2006-05-26

The retention volumes of solutes in countercurrent chromatography (CCC) are directly proportional to their distribution coefficients, K(D) in the biphasic liquid system used as mobile and stationary phase in the CCC column. The cocurrent CCC method consists in putting the liquid "stationary" phase in slow motion in the same direction as the mobile phase. A mixture of five steroid compounds of widely differing polarities was used as a test mixture to evaluate the capabilities of the method with the biphasic liquid system made of water/methanol/ethyl acetate/heptane 6/5/6/5 (v/v) and a 53 mL CCC column of the coil planet centrifuge type. It is shown that the chromatographic resolution obtained in cocurrent CCC is very good because the solute band broadening is minimized as long as the solute is located inside the "stationary" phase. Pushing the method at its limits, it is demonstrated that the five steroids can still be (partly) separated when the flow rate of the two liquid phases is the same (2 mL/min). This is due to the higher volume of upper phase (72% of the column volume) contained inside the CCC column producing a lower linear speed compared to the aqueous lower phase linear speed. The capabilities of the cocurrent CCC method compare well with those of the gradient elution method in HPLC. Continuous detection is a problem due to the fact that two immiscible liquid phases elute from the column. It was partly solved using an evaporative light scattering detector.

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.

Possibilities and limitations of the kinetic plot method in supercritical fluid chromatography.

PubMed

De Pauw, Ruben; Desmet, Gert; Broeckhoven, Ken

2013-08-30

Although supercritical fluid chromatography (SFC) is becoming a technique of increasing importance in the field of analytical chromatography, methods to compare the performance of SFC-columns and separations in an unbiased way are not fully developed. The present study uses mathematical models to investigate the possibilities and limitations of the kinetic plot method in SFC as this easily allows to investigate a wide range of operating pressures, retention and mobile phase conditions. The variable column length (L) kinetic plot method was further investigated in this work. Since the pressure history is identical for each measurement, this method gives the true kinetic performance limit in SFC. The deviations of the traditional way of measuring the performance as a function of flow rate (fixed back pressure and column length) and the isopycnic method with respect to this variable column length method were investigated under a wide range of operational conditions. It is found that using the variable L method, extrapolations towards other pressure drops are not valid in SFC (deviation of ∼15% for extrapolation from 50 to 200bar pressure drop). The isopycnic method provides the best prediction but its use is limited when operating closer towards critical point conditions. When an organic modifier is used, the predictions are improved for both methods with respect to the variable L method (e.g. deviations decreases from 20% to 2% when 20mol% of methanol is added). Copyright © 2013 Elsevier B.V. All rights reserved.

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

NASA Technical Reports Server (NTRS)

Huz, Kateryna

2014-01-01

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

Comparison of the release of constituents from granular materials under batch and column testing.

PubMed

Lopez Meza, Sarynna; Garrabrants, Andrew C; van der Sloot, Hans; Kosson, David S

2008-01-01

Column leaching testing can be considered a better basis for assessing field impact data than any other available batch test method and thus provides a fundamental basis from which to estimate constituent release under a variety of field conditions. However, column testing is time-intensive compared to the more simplified batch testing, and may not always be a viable option when making decisions for material reuse. Batch tests are used most frequently as a simple tool for compliance or quality control reasons. Therefore, it is important to compare the release that occurs under batch and column testing, and establish conservative interpretation protocols for extrapolation from batch data when column data are not available. Five different materials (concrete, construction debris, aluminum recycling residue, coal fly ash and bottom ash) were evaluated via batch and column testing, including different column flow regimes (continuously saturated and intermittent unsaturated flow). Constituent release data from batch and column tests were compared. Results showed no significant difference between the column flow regimes when constituent release data from batch and column tests were compared. In most cases batch and column testing agreed when presented in the form of cumulative release. For arsenic in carbonated materials, however, batch testing underestimates the column constituent release for most LS ratios and also on a cumulative basis. For cases when As is a constituent of concern, column testing may be required.

Stability and characterization of perphenazine aerosols generated using the capillary aerosol generator.

PubMed

Li, Xihao; Blondino, Frank E; Hindle, Michael; Soine, William H; Byron, Peter R

2005-10-13

Perphenazine (a potent antiemetic) was aerosolized using capillary aerosol generator to generate respirable condensation aerosols from drug in propylene glycol (PG) solutions, by pumping the liquids through a heated capillary tube. The study characterized the stability of perphenazine during and following aerosol generation. The stability-indicating HPLC method (C-8 column with a mobile phase of 52% 0.01 M pH 3.0 acetate buffer+48% acetonitrile) also enabled the study of perphenazine stability in solution under acidic, basic, oxidizing and photolysing conditions. An LC-MS (ESI+) method was used to characterize the degradation products. Perphenazine was found to be stable in acidic and basic conditions, while perphenazine sulfoxide was the major product formed in dilute peroxide solutions. Two photo-degradation products were formed in PG that were tentatively identified by LC-MS; one of these was synthesized and confirmed to be 2-[4-(3-phenothiazin-10-yl-propyl)-piperazino]-ethanol. Both photolysis products showed that aromatic dechlorination had occurred and one appeared to also result from interaction with the solvent. Within an aerosolization energy window of 84-95 J, fine particle aerosols were generated from perphenazine PG formulations with no significant degradation. Small amounts of degradation products were produced in all samples during aerosolization at elevated (non-optimal) energies. These were largely consistent with those seen to result from oxidation and photolysis in solution, showing that oxidation and dehalogenation appeared to be the main degradation pathways followed when the CAG system was overheated.

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

PubMed

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

2003-02-05

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

Large-scale single-chirality separation of single-wall carbon nanotubes by simple gel chromatography

PubMed Central

Liu, Huaping; Nishide, Daisuke; Tanaka, Takeshi; Kataura, Hiromichi

2011-01-01

Monostructured single-wall carbon nanotubes (SWCNTs) are important in both scientific research and electronic and biomedical applications; however, the bulk separation of SWCNTs into populations of single-chirality nanotubes remains challenging. Here we report a simple and effective method for the large-scale chirality separation of SWCNTs using a single-surfactant multicolumn gel chromatography method utilizing one surfactant and a series of vertically connected gel columns. This method is based on the structure-dependent interaction strength of SWCNTs with an allyl dextran-based gel. Overloading an SWCNT dispersion on the top column results in the adsorption sites of the column becoming fully occupied by the nanotubes that exhibit the strongest interaction with the gel. The unbound nanotubes flow through to the next column, and the nanotubes with the second strongest interaction with the gel are adsorbed in this stage. In this manner, 13 different (n, m) species were separated. Metallic SWCNTs were finally collected as unbound nanotubes because they exhibited the lowest interaction with the gel. PMID:21556063

Method of separating short half-life radionuclides from a mixture of radionuclides

DOEpatents

Bray, Lane A.; Ryan, Jack L.

1999-01-01

The present invention is a method of removing an impurity of plutonium, lead or a combination thereof from a mixture of radionuclides that contains the impurity and at least one parent radionuclide. The method has the steps of (a) insuring that the mixture is a hydrochloric acid mixture; (b) oxidizing the acidic mixture and specifically oxidizing the impurity to its highest oxidation state; and (c) passing the oxidized mixture through a chloride form anion exchange column whereupon the oxidized impurity absorbs to the chloride form anion exchange column and the 22.sup.9 Th or 2.sup.27 Ac "cow" radionuclide passes through the chloride form anion exchange column. The plutonium is removed for the purpose of obtaining other alpha emitting radionuclides in a highly purified form suitable for medical therapy. In addition to plutonium; lead, iron, cobalt, copper, uranium, and other metallic cations that form chloride anionic complexes that may be present in the mixture; are removed from the mixture on the chloride form anion exchange column.

Method of separating short half-life radionuclides from a mixture of radionuclides

DOEpatents

Bray, L.A.; Ryan, J.L.

1999-03-23

The present invention is a method of removing an impurity of plutonium, lead or a combination thereof from a mixture of radionuclides that contains the impurity and at least one parent radionuclide. The method has the steps of (a) insuring that the mixture is a hydrochloric acid mixture; (b) oxidizing the acidic mixture and specifically oxidizing the impurity to its highest oxidation state; and (c) passing the oxidized mixture through a chloride form anion exchange column whereupon the oxidized impurity absorbs to the chloride form anion exchange column and the {sup 229}Th or {sup 227}Ac ``cow`` radionuclide passes through the chloride form anion exchange column. The plutonium is removed for the purpose of obtaining other alpha emitting radionuclides in a highly purified form suitable for medical therapy. In addition to plutonium, lead, iron, cobalt, copper, uranium, and other metallic cations that form chloride anionic complexes that may be present in the mixture are removed from the mixture on the chloride form anion exchange column. 8 figs.

Column strength of tubes elastically restrained against rotation at the ends

NASA Technical Reports Server (NTRS)

Osgood, William R

1938-01-01

Report presents the results of a study made of the effects of known end restraint on commercially available round and streamline tubing of chromium-molybdenum steel, duralumin, stainless steel, and heat-treated chromium-molybdenum steel; and a more accurate method than any previously available, but still a practical method, was developed for designing compression members in riveted or welded structures, particularly aircraft. Two hundred specimens were tested as short, medium-length, and long columns with freely supported ends or elastically restrained ends. Tensile and compressive tests were made on each piece of original tubing from which column specimens were cut.

Improvement in HPLC separation of acetic acid and levulinic acid in the profiling of biomass hydrolysate.

PubMed

Xie, Rui; Tu, Maobing; Wu, Yonnie; Adhikari, Sushil

2011-04-01

5-Hydroxymethylfurfural (HMF) and furfural could be separated by the Aminex HPX-87H column chromatography, however, the separation and quantification of acetic acid and levulinic acid in biomass hydrolysate have been difficult with this method. In present study, the HPLC separation of acetic acid and levulinic acid on Aminex HPX-87H column has been investigated by varying column temperature, flow rate, and sulfuric acid content in the mobile phase. The column temperature was found critical in resolving acetic acid and levulinic acid. The resolution for two acids increased dramatically from 0.42 to 1.86 when the column temperature was lowered from 60 to 30 °C. So did the capacity factors for levulinic acid that was increased from 1.20 to 1.44 as the column temperature dropped. The optimum column temperature for the separation was found at 45 °C. Variation in flow rate and sulfuric acid concentration improved not as much as the column temperature did. Published by Elsevier Ltd.

High‐precision determination of lithium and magnesium isotopes utilising single column separation and multi‐collector inductively coupled plasma mass spectrometry

PubMed Central

Misra, Sambuddha; Lloyd, Nicholas; Elderfield, Henry; Bickle, Mike J.

2017-01-01

Rationale Li and Mg isotopes are increasingly used as a combined tool within the geosciences. However, established methods require separate sample purification protocols utilising several column separation procedures. This study presents a single‐step cation‐exchange method for quantitative separation of trace levels of Li and Mg from multiple sample matrices. Methods The column method utilises the macro‐porous AGMP‐50 resin and a high‐aspect ratio column, allowing quantitative separation of Li and Mg from natural waters, sediments, rocks and carbonate matrices following the same elution protocol. High‐precision isotope determination was conducted by multi‐collector inductively coupled plasma mass spectrometry (MC‐ICPMS) on the Thermo Scientific™ NEPTUNE Plus™ fitted with 1013 Ω amplifiers which allow accurate and precise measurements at ion beams ≤0.51 V. Results Sub‐nanogram Li samples (0.3–0.5 ng) were regularly separated (yielding Mg masses of 1–70 μg) using the presented column method. The total sample consumption during isotopic analysis is <0.5 ng Li and <115 ng Mg with long‐term external 2σ precisions of ±0.39‰ for δ7Li and ±0.07‰ for δ26Mg. The results for geological reference standards and seawater analysed by our method are in excellent agreement with published values despite the order of magnitude lower sample consumption. Conclusions The possibility of eluting small sample masses and the low analytical sample consumption make this method ideal for samples of limited mass or low Li concentration, such as foraminifera, mineral separates or dilute river waters. PMID:29078008

A rapid silica spin column-based method of RNA extraction from fruit trees for RT-PCR detection of viruses.

PubMed

Yang, Fan; Wang, Guoping; Xu, Wenxing; Hong, Ni

2017-09-01

Efficient recovery of high quality RNA is very important for successful RT-PCR detection of plant RNA viruses. High levels of polyphenols and polysaccharides in plant tissues can irreversibly bind to and/or co-precipitate with RNA, which influences RNA isolation. In this study, a silica spin column-based RNA isolation method was developed by using commercially available silica columns combined with the application of a tissue lysis solution, and binding and washing buffers with high concentration guanidinium thiocyanate (GuSCN, 50% w/v), which helps remove plant proteins, polysaccharides and polyphenolic compounds. The method was successfully used to extract high quality RNA from citrus (Citrus aurantifolia), grapevine (Vitis vinifera), peach (Prunus persica), pear (Pyrus spp.), taro (Colocosia esculenta) and tobacco (Nicotiana benthamiana) samples. The method was comparable to conventional CTAB method in RNA isolation efficiency, but it was more sample-adaptable and cost-effective than commercial kits. High quality RNA isolated using silica spin column-based method was successfully used for the RT-PCR and/or multiplex RT-PCR amplification of woody fruit tree viruses and a viroid. The study provided a useful tool for the detection and characterization of plant viruses. Copyright © 2017 Elsevier B.V. All rights reserved.

A New Resonance Tube

NASA Astrophysics Data System (ADS)

Bates, Alan

2017-12-01

The measurement of the speed of sound in air with the resonance tube is a popular experiment that often yields accurate results. One approach is to hold a vibrating tuning fork over an air column that is partially immersed in water. The column is raised and lowered in the water until the generated standing wave produces resonance: this occurs at the point where sound is perceived to have maximum loudness, or at the point where the amplitude of the standing wave has maximum value, namely an antinode. An antinode coincides with the position of the tuning fork, beyond the end of the air column, which consequently introduces an end correction. One way to minimize this end correction is to measure the distance between consecutive antinodes.

Separation of 103Ru from a proton irradiated thorium matrix: A potential source of Auger therapy radionuclide 103mRh

DOE PAGES

Mastren, Tara; Radchenko, Valery; Hopkins, Philip D.; ...

2017-12-22

Ruthenium-103 is the parent isotope of 103mRh (t1/2 56.1 min), an isotope of interest for Auger electron therapy. During the proton irradiation of thorium targets, large amounts of 103Ru are generated through proton induced fission. Furthermore, the development of a two part chemical separation process to isolate 103Ru in high yield and purity from a proton irradiated thorium matrix on an analytical scale is described herein. The first part employed an anion exchange column to remove cationic actinide/lanthanide impurities along with the majority of the transition metal fission products. Secondly, an extraction chromatographic column utilizing diglycolamide functional groups was usedmore » to decontaminate 103Ru from the remaining impurities. This method then resulted in a final radiochemical yield of 83 ± 5% of 103Ru with a purity of 99.9%. Additionally, measured nuclear reaction cross sections for the formation of 103Ru and 106Ru via the 232Th(p,f) 103,106Ru reactions are reported within.« less

Rapid preparative separation of monoclonal antibody charge variants using laterally-fed membrane chromatography.

PubMed

Sadavarte, Rahul; Madadkar, Pedram; Filipe, Carlos Dm; Ghosh, Raja

2018-01-15

Monoclonal antibodies undergo various forms of chemical transformation which have been shown to cause loss in efficacy and alteration in pharmacokinetic properties of these molecules. Such modified antibody molecules are known as variants. They also display physical properties such as charge that are different from intact antibody molecules. However, the difference in charge is very subtle and separation based on it is quite challenging. Charge variants are usually separated using ion-exchange column chromatography or isoelectric focusing. In this paper, we report a rapid and scalable method for fractionating monoclonal antibody charge variants, based on the use of cation exchange laterally-fed membrane chromatography (LFMC). Starting with a sample of monoclonal antibody hIgG1-CD4, three well-resolved fractions were obtained using either pH or salt gradient. These fractions were identified as acidic, neutral and basic variants. Each of these fractions contained intact heavy and light chains and so antibody fragmentation had no role in variant generation. The separation was comparable to that using column chromatography but was an order of magnitude faster. Copyright © 2017 Elsevier B.V. All rights reserved.

Separation of 103Ru from a proton irradiated thorium matrix: A potential source of Auger therapy radionuclide 103mRh

PubMed Central

Hopkins, Philip D.; Engle, Jonathan W.; Weidner, John W.; Copping, Roy; Brugh, Mark; Nortier, F. Meiring; Birnbaum, Eva R.; John, Kevin D.

2017-01-01

Ruthenium-103 is the parent isotope of 103mRh (t1/2 56.1 min), an isotope of interest for Auger electron therapy. During the proton irradiation of thorium targets, large amounts of 103Ru are generated through proton induced fission. The development of a two part chemical separation process to isolate 103Ru in high yield and purity from a proton irradiated thorium matrix on an analytical scale is described herein. The first part employed an anion exchange column to remove cationic actinide/lanthanide impurities along with the majority of the transition metal fission products. Secondly, an extraction chromatographic column utilizing diglycolamide functional groups was used to decontaminate 103Ru from the remaining impurities. This method resulted in a final radiochemical yield of 83 ± 5% of 103Ru with a purity of 99.9%. Additionally, measured nuclear reaction cross sections for the formation of 103Ru and 106Ru via the 232Th(p,f)103,106Ru reactions are reported within. PMID:29272318

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.

Osmium-191/iridium-191m radionuclide

DOEpatents

Knapp, F.F. Jr.; Butler, T.A.; Brihaye, C.

1985-08-26

A generator system to provide iridium-191m for clinical imaging applications comprises an activated carbon adsorbent loaded with a compound containing the parent nuclide, osmium-191. The generator, which has a shelf-life in excess of two weeks and does not require a scavenger column, can be eluted with physiologically compatible saline. 4 figs. 3 tabs.

Vertically migrating swimmers generate aggregation-scale eddies in a stratified column.

PubMed

Houghton, Isabel A; Koseff, Jeffrey R; Monismith, Stephen G; Dabiri, John O

2018-04-01

Biologically generated turbulence has been proposed as an important contributor to nutrient transport and ocean mixing 1-3 . However, to produce non-negligible transport and mixing, such turbulence must produce eddies at scales comparable to the length scales of stratification in the ocean. It has previously been argued that biologically generated turbulence is limited to the scale of the individual animals involved 4 , which would make turbulence created by highly abundant centimetre-scale zooplankton such as krill irrelevant to ocean mixing. Their small size notwithstanding, zooplankton form dense aggregations tens of metres in vertical extent as they undergo diurnal vertical migration over hundreds of metres 3,5,6 . This behaviour potentially introduces additional length scales-such as the scale of the aggregation-that are of relevance to animal interactions with the surrounding water column. Here we show that the collective vertical migration of centimetre-scale swimmers-as represented by the brine shrimp Artemia salina-generates aggregation-scale eddies that mix a stable density stratification, resulting in an effective turbulent diffusivity up to three orders of magnitude larger than the molecular diffusivity of salt. These observed large-scale mixing eddies are the result of flow in the wakes of the individual organisms coalescing to form a large-scale downward jet during upward swimming, even in the presence of a strong density stratification relative to typical values observed in the ocean. The results illustrate the potential for marine zooplankton to considerably alter the physical and biogeochemical structure of the water column, with potentially widespread effects owing to their high abundance in climatically important regions of the ocean 7 .

The Trace Analysis of DEET in Water using an On-line Preconcentration Column and Liquid Chromatography with UV Photodiode Array Detection

EPA Science Inventory

A method for the detection of trace levels of N,N-diethyl-m-toluamide (DEET) in water is discussed. The method utilizes an on-line preconcentration column in series with high performance liquid chromatography (HPLC) and UV photodiode array detection. DEET, a common insect repel...

High-Throughput Analysis of Sucrose Fatty Acid Esters by Supercritical Fluid Chromatography/Tandem Mass Spectrometry

PubMed Central

Hori, Katsuhito; Tsumura, Kazunobu; Fukusaki, Eiichiro; Bamba, Takeshi

2014-01-01

Supercritical fluid chromatography (SFC) coupled with triple quadrupole mass spectrometry was applied to the profiling of sucrose fatty acid esters (SEs). The SFC conditions (column and modifier gradient) were optimized for the effective separation of SEs. In the column test, a silica gel reversed-phase column was selected. Then, the method was used for the detailed characterization of commercial SEs and the successful analysis of SEs containing different fatty acids. The present method allowed for fast and high-resolution separation of monoesters to tetra-esters within a shorter time (15 min) as compared to the conventional high-performance liquid chromatography. The applicability of our method for the analysis of SEs was thus demonstrated. PMID:26819875

[Determination of sennosides and degraded products in the process of sennoside metabolism by HPLC].

PubMed

Sun, Yan; Li, Xuetuo; Yu, Xingju

2004-01-01

A method for the separation and determination of sennosides A and B and the main composition (sennidins A and B) in degraded products of sennosides by linear gradient high performance liquid chromatography has been developed. Separation conditions were as follows: column, a Spherisorb C18 column (250 mm x 4.6 mm i.d., 10 microm); column temperature, 40 degrees C; detection wavelength, 360 nm; mobile phase A, 1.25% acetic acid aqueous solution; mobile phase B, methanol; linear gradient, 100% A --> (20 min) 100% B. The method is effective, quick, accurate and reproducible. The satisfactory results show that this new method has certain practical values as an approach of real-time analysis in the process of sennoside metabolism.

Web-Based Phylogenetic Assignment Tool for Analysis of Terminal Restriction Fragment Length Polymorphism Profiles of Microbial Communities

PubMed Central

Kent, Angela D.; Smith, Dan J.; Benson, Barbara J.; Triplett, Eric W.

2003-01-01

Culture-independent DNA fingerprints are commonly used to assess the diversity of a microbial community. However, relating species composition to community profiles produced by community fingerprint methods is not straightforward. Terminal restriction fragment length polymorphism (T-RFLP) is a community fingerprint method in which phylogenetic assignments may be inferred from the terminal restriction fragment (T-RF) sizes through the use of web-based resources that predict T-RF sizes for known bacteria. The process quickly becomes computationally intensive due to the need to analyze profiles produced by multiple restriction digests and the complexity of profiles generated by natural microbial communities. A web-based tool is described here that rapidly generates phylogenetic assignments from submitted community T-RFLP profiles based on a database of fragments produced by known 16S rRNA gene sequences. Users have the option of submitting a customized database generated from unpublished sequences or from a gene other than the 16S rRNA gene. This phylogenetic assignment tool allows users to employ T-RFLP to simultaneously analyze microbial community diversity and species composition. An analysis of the variability of bacterial species composition throughout the water column in a humic lake was carried out to demonstrate the functionality of the phylogenetic assignment tool. This method was validated by comparing the results generated by this program with results from a 16S rRNA gene clone library. PMID:14602639

A new solid-phase extraction and HPLC method for determination of patulin in apple products and hawthorn juice in China.

PubMed

Zhou, Yuchun; Kong, Weijun; Li, Yan; Logrieco, Antonio F; Xu, Jun; Yang, Meihua

2012-03-01

A new solid-phase extraction (SPE) pretreatment method using a home-made polyvinylpolypyrrolidone-florisil (PVPP-F) column was developed for the analysis of patulin in apple and hawthorn products in China. Fifty samples (25 apple juices, 12 apple jams, and 13 hawthorn juices) were prepared using the new method and then analyzed by high performance liquid chromatography with diode array detection (HPLC-DAD) on an Agela Venusil MP C(18) reversed-phase column (4.6 mm × 250 mm, 5 μm). The cleanup results for all samples using home-made PVPP-F column were compared with those obtained using a MycoSep®228 AflaPat column. The correlation coefficient R (0.9998) fulfilled the requirement of linearity for patulin in the concentration range of 2.5-250 μg/kg. The limits of detection (LODs) and quantification (LOQs) of patulin were 3.99 and 9.64 μg/kg for PVPP-F column, and 3.56 and 8.07 μg/kg for MycoSep®228 AflaPat column, respectively. Samples were spiked with patulin at levels ranging from 25 to 250 μg/kg, and recoveries using PVPP-F and MycoSep®228 AflaPat columns were in the range of 81.9-100.9% and 86.4-103.9%, respectively. Naturally occurring patulin was found in 2 of 25 apple juice samples (8.0%) and 1 of 13 hawthorn juice samples (7.7%) at concentrations ranging from 12.26 to 36.81 μg/kg. The positive results were further confirmed by liquid chromatography electrospray ionization mass spectrometry (LC-ESI-MS). © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

PubMed

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

2013-11-15

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

Prediction of shear critical behavior of high-strength reinforced concrete columns using finite element methods

NASA Astrophysics Data System (ADS)

Alrasyid, Harun; Safi, Fahrudin; Iranata, Data; Chen-Ou, Yu

2017-11-01

This research shows the prediction of shear behavior of High-Strength Reinforced Concrete Columns using Finite-Element Method. The experimental data of nine half scale high-strength reinforced concrete were selected. These columns using specified concrete compressive strength of 70 MPa, specified yield strength of longitudinal and transverse reinforcement of 685 and 785 MPa, respectively. The VecTor2 finite element software was used to simulate the shear critical behavior of these columns. The combination axial compression load and monotonic loading were applied at this prediction. It is demonstrated that VecTor2 finite element software provides accurate prediction of load-deflection up to peak at applied load, but provide similar behavior at post peak load. The shear strength prediction provide by VecTor 2 are slightly conservative compare to test result.

Axial Crushing of Thin-Walled Columns with Octagonal Section: Modeling and Design

NASA Astrophysics Data System (ADS)

Liu, Yucheng; Day, Michael L.

This chapter focus on numerical crashworthiness analysis of straight thinwalled columns with octagonal cross sections. Two important issues in this analysis are demonstrated here: computer modeling and crashworthiness design. In the first part, this chapter introduces a method of developing simplified finite element (FE) models for the straight thin-walled octagonal columns, which can be used for the numerical crashworthiness analysis. Next, this chapter performs a crashworthiness design for such thin-walled columns in order to maximize their energy absorption capability. Specific energy absorption (SEA) is set as the design objective, side length of the octagonal cross section and wall thickness are selected as design variables, and maximum crushing force (Pm) occurs during crashes is set as design constraint. Response surface method (RSM) is employed to formulate functions for both SEA and Pm.

Counter-current motion in counter-current chromatography.

PubMed

Ito, Yoichiro

2014-12-12

After the CCC2012 meeting, I have received an e-mail regarding the terminology of "Countercurrent Chromatography". It stated that the term "Countercurrent" is a misnomer, because its stationary phase is motionless in the column and that the method should be renamed as liquid-liquid separations or centrifugal separations. However, it was found that these names are already used for various other techniques as found via Google search. The term "Countercurrent Chromatography" was originally made after two preparative methods of Countercurrent distribution and liquid Chromatography, both having no countercurrent motion in the column. However, it is surprising to find that this F1 hybrid method "Countercurrent Chromatography" can clearly exhibit countercurrent motion within the separation column in both hydrodynamic and hydrostatic equilibrium systems. This justifies that "Countercurrent Chromatography" is a proper term for this chromatographic method. Published by Elsevier B.V.

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.

Chaotic bubbling and nonstagnant foams.

PubMed

Tufaile, Alberto; Sartorelli, José Carlos; Jeandet, Philippe; Liger-Belair, Gerard

2007-06-01

We present an experimental investigation of the agglomeration of bubbles obtained from a nozzle working in different bubbling regimes. This experiment consists of a continuous production of bubbles from a nozzle at the bottom of a liquid column, and these bubbles create a two-dimensional (2D) foam (or a bubble raft) at the top of this column. The bubbles can assemble in various dynamically stable arrangement, forming different kinds of foams in a liquid mixture of water and glycerol, with the effect that the bubble formation regimes influence the foam obtained from this agglomeration of bubbles. The average number of bubbles in the foam is related to the bubble formation frequency and the bubble mean lifetime. The periodic bubbling can generate regular or irregular foam, while a chaotic bubbling only generates irregular foam.

Activated Carbon-hydrogen based Continuous Sorption Cooling in Single Adsorbent Bed with LN2 Heat Sink

NASA Astrophysics Data System (ADS)

Koley, Susmita; Ghosh, Indranil

Quick and periodic inflow-outflow of adsorbate in an adsorbent column createsa differential temperature between the two ends of it, allowing for the generation of continuous sorption cooling in a single adsorbent tube. The concept has been proven experimentally and theoretically for near room temperature applications using activated carbon-nitrogen. The feasibility of generating continuous solid sorption cooling in a single adsorbent tube in the cryogenic domainhas been studied theoretically with a different adsorbent-adsorbate pair, namely, activated carbon-hydrogen. Precooling of gaseous hydrogen (before it enters the adsorbent column) and removal of the heat of adsorption has been achieved using liquid nitrogen. Theoretical estimation shows nearly 20 K temperature difference between the two ends under no load condition. Finally, parametric variations have been performed.

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.

METHOD OF AND APPARATUS FOR WITHDRAWING LIGHT ISOTOPIC PRODUCT FROM A LIQUID THERMAL DIFFUSION PLANT

DOEpatents

Dole, M.

1959-09-22

An improved process and apparatus are described for removing enriched product from the columns of a thermal diffusion plant for separation of isotopes. In the removal cycle, light product at the top cf the diffusion columns is circulated through the column tops and a shipping cylinder connected thereto unttl the concertation of enriched product in the cylinder reaches the desired point. During the removal, circulation through the bottoms is blocked bv freezing. in the diffusion cycle, the bottom portion is unfrozen, fresh feed is distributed to the bottoms of the columns, ard heavy product is withdrawn from the bottoms, while the tops of the columns are blocked by freezing.

Optimized anion exchange column isolation of zirconium-89 ( 89Zr) 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 abilitymore » to quantitatively capture Zr from a load solution 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 (>10 5) and has been shown to remove Fe, an abundant contaminant in Y foils, from the 89Zr elution fraction. Finally, the method was evaluated using cyclotron bombarded Y foil targets; the method was shown to achieve >95% recovery of the 89Zr present in the foils. The anion exchange column method described here is intended to be the first 89Zr isolation stage in a dual-column purification process.« less

Optimized anion exchange column isolation of zirconium-89 ( 89Zr) from yttrium cyclotron target: Method development and implementation on an automated fluidic platform

DOE PAGES

O’Hara, Matthew J.; Murray, Nathaniel J.; Carter, Jennifer C.; ...

2018-02-24

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 abilitymore » to quantitatively capture Zr from a load solution 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 (>10 5) and has been shown to remove Fe, an abundant contaminant in Y foils, from the 89Zr elution fraction. Finally, the method was evaluated using cyclotron bombarded Y foil targets; the method was shown to achieve >95% recovery of the 89Zr present in the foils. The anion exchange column method described here is intended to be the first 89Zr isolation stage in a dual-column purification process.« less

A variational theorem for creep with applications to plates and columns

NASA Technical Reports Server (NTRS)

Sanders, J Lyell, Jr; Mccomb, Harvey G , Jr; Schlechte, Floyd R

1958-01-01

A variational theorem is presented for a body undergoing creep. Solutions to problems of the creep behavior of plates, columns, beams, and shells can be obtained by means of the direct methods of the calculus of variations in conjunction with the stated theorem. The application of the theorem is illustrated for plates and columns by the solution of two sample problems.

49 CFR Appendix I to Subpart A of... - Revenue Need and Allocation to Traffic at Issue

Code of Federal Regulations, 2014 CFR

2014-10-01

... composite carrier basis comprised of all traffic and cost study carriers. Data in part II, line 14 columns... Issue Traffic Based on Ton and Ton-Mile Method (See Note A) Line No. Item Source for columns 3 and 4..., by using Statement No. 6-68, Highway Form B, Schedule A, Line III. Assign the dollars in columns (6...

49 CFR Appendix I to Subpart A of... - Revenue Need and Allocation to Traffic at Issue

Code of Federal Regulations, 2013 CFR

2013-10-01

... composite carrier basis comprised of all traffic and cost study carriers. Data in part II, line 14 columns... Issue Traffic Based on Ton and Ton-Mile Method (See Note A) Line No. Item Source for columns 3 and 4..., by using Statement No. 6-68, Highway Form B, Schedule A, Line III. Assign the dollars in columns (6...

49 CFR Appendix I to Subpart A of... - Revenue Need and Allocation to Traffic at Issue

Code of Federal Regulations, 2010 CFR

2010-10-01

... composite carrier basis comprised of all traffic and cost study carriers. Data in part II, line 14 columns... Issue Traffic Based on Ton and Ton-Mile Method (See Note A) Line No. Item Source for columns 3 and 4..., by using Statement No. 6-68, Highway Form B, Schedule A, Line III. Assign the dollars in columns (6...

49 CFR Appendix I to Subpart A of... - Revenue Need and Allocation to Traffic at Issue

Code of Federal Regulations, 2011 CFR

2011-10-01

... composite carrier basis comprised of all traffic and cost study carriers. Data in part II, line 14 columns... Issue Traffic Based on Ton and Ton-Mile Method (See Note A) Line No. Item Source for columns 3 and 4..., by using Statement No. 6-68, Highway Form B, Schedule A, Line III. Assign the dollars in columns (6...

49 CFR Appendix I to Subpart A of... - Revenue Need and Allocation to Traffic at Issue

Code of Federal Regulations, 2012 CFR

2012-10-01

... composite carrier basis comprised of all traffic and cost study carriers. Data in part II, line 14 columns... Issue Traffic Based on Ton and Ton-Mile Method (See Note A) Line No. Item Source for columns 3 and 4..., by using Statement No. 6-68, Highway Form B, Schedule A, Line III. Assign the dollars in columns (6...

A New NASA Data Product: Tropospheric and Stratospheric Column Ozone in the Tropics Derived from TOMS Measurements

NASA Technical Reports Server (NTRS)

Ziemke, J. R.; Chandra, S.; Bhartia, P. K.

1999-01-01

Tropospheric column ozone (TCO) and stratospheric column ozone (SCO) gridded data in the tropics for 1979-present are now available from NASA Goddard Space Flight Center via either direct ftp, world-NN,ide-NN,eb, or electronic mail. This note provides a brief overview of the method used to derive the data set including validation and adjustments.

Removal of arsenic from drinking water using rice husk

NASA Astrophysics Data System (ADS)

Asif, Zunaira; Chen, Zhi

2017-06-01

Rice husk adsorption column method has proved to be a promising solution for arsenic (As) removal over the other conventional methods. The present work investigates the potential of raw rice husk as an adsorbent for the removal of arsenic [As(V)] from drinking water. Effects of various operating parameters such as diameter of column, bed height, flow rate, initial arsenic feed concentration and particle size were investigated using continuous fixed bed column to check the removal efficiency of arsenic. This method shows maximum removal of As, i.e., 90.7 % under the following conditions: rice husk amount 42.5 g; 7 mL/min flow rate in 5 cm diameter column at the bed height of 28 cm for 15 ppb inlet feed concentration. Removal efficiency was increased from 83.4 to 90.7 % by reducing the particle size from 1.18 mm to 710 µm for 15 ppb concentration. Langmuir and Freundlich isotherm models were employed to discuss the adsorption behavior. The effect of different operating parameters on the column adsorption was determined using breakthrough curves. In the present study, three kinetic models Adam-Bohart, Thomas and Yoon-Nelson were applied to find out the saturated concentration, fixed bed adsorption capacity and time required for 50 % adsorbate breakthrough, respectively. At the end, solidification was done for disposal of rice husk.

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

PubMed

Liu, Yuzhen; Yu, Hong; Li, Siwen

2011-10-01

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

Combined group ECC protection and subgroup parity protection

DOEpatents

Gara, Alan G.; Chen, Dong; Heidelberger, Philip; Ohmacht, Martin

2013-06-18

A method and system are disclosed for providing combined error code protection and subgroup parity protection for a given group of n bits. The method comprises the steps of identifying a number, m, of redundant bits for said error protection; and constructing a matrix P, wherein multiplying said given group of n bits with P produces m redundant error correction code (ECC) protection bits, and two columns of P provide parity protection for subgroups of said given group of n bits. In the preferred embodiment of the invention, the matrix P is constructed by generating permutations of m bit wide vectors with three or more, but an odd number of, elements with value one and the other elements with value zero; and assigning said vectors to rows of the matrix P.

Exact solutions for the collaborative pickup and delivery problem.

PubMed

Gansterer, Margaretha; Hartl, Richard F; Salzmann, Philipp E H

2018-01-01

In this study we investigate the decision problem of a central authority in pickup and delivery carrier collaborations. Customer requests are to be redistributed among participants, such that the total cost is minimized. We formulate the problem as multi-depot traveling salesman problem with pickups and deliveries. We apply three well-established exact solution approaches and compare their performance in terms of computational time. To avoid unrealistic solutions with unevenly distributed workload, we extend the problem by introducing minimum workload constraints. Our computational results show that, while for the original problem Benders decomposition is the method of choice, for the newly formulated problem this method is clearly dominated by the proposed column generation approach. The obtained results can be used as benchmarks for decentralized mechanisms in collaborative pickup and delivery problems.

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

PubMed

Gritti, Fabrice; Guiochon, Georges

2013-07-05

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

Low-frequency instabilities and plasma turbulence

NASA Technical Reports Server (NTRS)

Ilic, D. B.

1973-01-01

A theoretical and experimental study is reported of steady-state and time-dependent characteristics of the positive column and the hollow cathode discharge (HCD). The steady state of a non-isothermal, cylindrical positive column in an axial magnetic field is described by three moment equations in the plasma approximation. Volume generation of electron-ion pairs by single-stage ionization, the presence of axial current, and collisions with neutrals are considered. The theory covers the range from the low pressure, collisionless regime to the intermediate pressure, collisional regime. It yields radial profiles of the charged particle velocities, density, potential, electron and ion temperatures, and demonstrates similarity laws for the positive column. The results are compared with two moment theories and with experimental data on He, Ar and Hg found in the literature for a wide range of pressures. A simple generalization of the isothermal theory for an infinitely long cylinder in an axial magnetic field to the case of a finite column with axial current flow is also demonstrated.

A Column Experiment To Determine Black Shale Degradation And Colonization By Means of δ13C and 14C Analysis Of Phospholipid Fatty Acids And DNA Extraction

NASA Astrophysics Data System (ADS)

Seifert, A.; Gleixner, G.

2008-12-01

We investigated the degradation of black shale organic matter by microbial communities. We inoculated two columns respectively, with the fungi Schizophyllum commune, the gram-positive bacterium Pseudomonas putida and the gram-negative bacteria Streptomyces griseus and Streptomyces chartreusis. These microorganisms are known to degrade a wide variety of organic macromolecules. Additionally, we had two sets of control columns. To one set the same nutrient solution was added as to the inoculated columns and to the other set only sterile deionised water was supplied. All columns contained 1.5 kg of freshly crushed not autoclaved black shale material with a particle size of 0.63-2 mm. The columns were incubated at 28° C and 60% humidity in the dark. The aim was to investigate, which microorganisms live on black shales and if these microorganisms are able to degrade ancient organic matter. We used compound specific stable isotope measurement techniques and compound specific 14C-dating methods. After 183 days PLFAs were extracted from the columns to investigate the microbial community, furthermore we extracted on one hand total-DNA of column material and on the other hand DNA from pure cultures isolates which grew on Kinks-agar B, Starch-casein-nitrate-agar (SCN) and on complete-yeast-medium-agar (CYM). According to the PLFA analysis bacteria dominated in the columns, whereas in pure cultures more fungi were isolated. A principal component analysis revealed differences between the columns in accordance with the inoculation, but it seems that the inoculated microorganisms were replaced by the natural population. For AMS measurements palmitic acid (C 16:0) was re-isolated from total-PLFA-extract with a preparative fraction collector (PFC). Preliminary results of the study revealed that microorganisms are able to degrade black shale material and that PLFA analysis are useful methods to be combined with analysis of stable isotope and 14C measurements to study microbial degradation processes.

Microbial impacts on 99mTc migration through sandstone under highly alkaline conditions relevant to radioactive waste disposal.

PubMed

Smith, Sarah L; Boothman, Christopher; Williams, Heather A; Ellis, Beverly L; Wragg, Joanna; West, Julia M; Lloyd, Jonathan R

2017-01-01

Geological disposal of intermediate level radioactive waste in the UK is planned to involve the use of cementitious materials, facilitating the formation of an alkali-disturbed zone within the host rock. The biogeochemical processes that will occur in this environment, and the extent to which they will impact on radionuclide migration, are currently poorly understood. This study investigates the impact of biogeochemical processes on the mobility of the radionuclide technetium, in column experiments designed to be representative of aspects of the alkali-disturbed zone. Results indicate that microbial processes were capable of inhibiting 99m Tc migration through columns, and X-ray radiography demonstrated that extensive physical changes had occurred to the material within columns where microbiological activity had been stimulated. The utilisation of organic acids under highly alkaline conditions, generating H 2 and CO 2 , may represent a mechanism by which microbial processes may alter the hydraulic conductivity of a geological environment. Column sediments were dominated by obligately alkaliphilic H 2 -oxidising bacteria, suggesting that the enrichment of these bacteria may have occurred as a result of H 2 generation during organic acid metabolism. The results from these experiments show that microorganisms are able to carry out a number of processes under highly alkaline conditions that could potentially impact on the properties of the host rock surrounding a geological disposal facility for intermediate level radioactive waste. Copyright © 2016. Published by Elsevier B.V.

Solving nonlinear equilibrium equations of deformable systems by method of embedded polygons

NASA Astrophysics Data System (ADS)

Razdolsky, A. G.

2017-09-01

Solving of nonlinear algebraic equations is an obligatory stage of studying the equilibrium paths of nonlinear deformable systems. The iterative method for solving a system of nonlinear algebraic equations stated in an explicit or implicit form is developed in the present work. The method consists of constructing a sequence of polygons in Euclidean space that converge into a single point that displays the solution of the system. Polygon vertices are determined on the assumption that individual equations of the system are independent from each other and each of them is a function of only one variable. Initial positions of vertices for each subsequent polygon are specified at the midpoints of certain straight segments determined at the previous iteration. The present algorithm is applied for analytical investigation of the behavior of biaxially compressed nonlinear-elastic beam-column with an open thin-walled cross-section. Numerical examples are made for the I-beam-column on the assumption that its material follows a bilinear stress-strain diagram. A computer program based on the shooting method is developed for solving the problem. The method is reduced to numerical integration of a system of differential equations and to the solution of a system of nonlinear algebraic equations between the boundary values of displacements at the ends of the beam-column. A stress distribution at the beam-column cross-sections is determined by subdividing the cross-section area into many small cells. The equilibrium path for the twisting angle and the lateral displacements tend to the stationary point when the load is increased. Configuration of the path curves reveals that the ultimate load is reached shortly once the maximal normal stresses at the beam-column fall outside the limit of the elastic region. The beam-column has a unique equilibrium state for each value of the load, that is, there are no equilibrium states once the maximum load is reached.

Analysis of Phenolic Antioxidants in Navy Mobility Fuels by Gas Chromatography-Mass Spectrometry

DTIC Science & Technology

2013-06-19

8.0 LITERATURE CITED .........................................................................................14 APPENDIX A: Calibration Curves for...chromatogram from an F-76 diesel fuel containing 24 ppm of the AO-37 additive package, analyzed using single column GC-MS-SIM method...sulfur diesel fuel containing 6.25 ppm of the AO-37 additive package, analyzed using dual column Deans switch GC-MS-SIM method

A Fixed-Pattern Noise Correction Method Based on Gray Value Compensation for TDI CMOS Image Sensor.

PubMed

Liu, Zhenwang; Xu, Jiangtao; Wang, Xinlei; Nie, Kaiming; Jin, Weimin

2015-09-16

In order to eliminate the fixed-pattern noise (FPN) in the output image of time-delay-integration CMOS image sensor (TDI-CIS), a FPN correction method based on gray value compensation is proposed. One hundred images are first captured under uniform illumination. Then, row FPN (RFPN) and column FPN (CFPN) are estimated based on the row-mean vector and column-mean vector of all collected images, respectively. Finally, RFPN are corrected by adding the estimated RFPN gray value to the original gray values of pixels in the corresponding row, and CFPN are corrected by subtracting the estimated CFPN gray value from the original gray values of pixels in the corresponding column. Experimental results based on a 128-stage TDI-CIS show that, after correcting the FPN in the image captured under uniform illumination with the proposed method, the standard-deviation of row-mean vector decreases from 5.6798 to 0.4214 LSB, and the standard-deviation of column-mean vector decreases from 15.2080 to 13.4623 LSB. Both kinds of FPN in the real images captured by TDI-CIS are eliminated effectively with the proposed method.

Quantitative structure-retention relationship models for the prediction of the reversed-phase HPLC gradient retention based on the heuristic method and support vector machine.

PubMed

Du, Hongying; Wang, Jie; Yao, Xiaojun; Hu, Zhide

2009-01-01

The heuristic method (HM) and support vector machine (SVM) were used to construct quantitative structure-retention relationship models by a series of compounds to predict the gradient retention times of reversed-phase high-performance liquid chromatography (HPLC) in three different columns. The aims of this investigation were to predict the retention times of multifarious compounds, to find the main properties of the three columns, and to indicate the theory of separation procedures. In our method, we correlated the retention times of many diverse structural analytes in three columns (Symmetry C18, Chromolith, and SG-MIX) with their representative molecular descriptors, calculated from the molecular structures alone. HM was used to select the most important molecular descriptors and build linear regression models. Furthermore, non-linear regression models were built using the SVM method; the performance of the SVM models were better than that of the HM models, and the prediction results were in good agreement with the experimental values. This paper could give some insights into the factors that were likely to govern the gradient retention process of the three investigated HPLC columns, which could theoretically supervise the practical experiment.

Development of andrographolide molecularly imprinted polymer for solid-phase extraction

NASA Astrophysics Data System (ADS)

Yin, Xiaoying; Liu, Qingshan; Jiang, Yifan; Luo, Yongming

2011-06-01

A method employing molecularly imprinted polymer (MIP) as selective sorbent for solid-phase extraction (SPE) to pretreat samples was developed. The polymers were prepared by precipitation polymerization with andrographolide as template molecule. The structure of MIP was characterized and its static adsorption capacity was measured by the Scatchard equation. In comparison with C 18-SPE and non-imprinted polymer (NIP) SPE column, MIP-SPE column displays high selectivity and good affinity for andrographolide and dehydroandrographolide for extract of herb Andrographis paniculata ( Burm.f.) Nees (APN). MIP-SPE column capacity was 11.9 ± 0.6 μmol/g and 12.1 ± 0.5 μmol/g for andrographolide and dehydroandrographolide, respectively and was 2-3 times higher than that of other two columns. The precision and accuracy of the method developed were satisfactory with recoveries between 96.4% and 103.8% (RSD 3.1-4.3%, n = 5) and 96.0% and 104.2% (RSD 2.9-3.7%, n = 5) for andrographolide and dehydroandrographolide, respectively. Various real samples were employed to confirm the feasibility of method. This developed method demonstrates the potential of molecularly imprinted solid phase extraction for rapid, selective, and effective sample pretreatment.

Design of a portable gas chromatography with a conducting polymer nanocomposite detector device and a method to analyze a gas mixture.

PubMed

Pirsa, Sajad

2017-04-01

A portable chromatography device and a method were developed to analyze a gas mixture. The device comprises a chromatographic column for separating components of a sample of the gas mixture. It has an air pump coupled to the inlet of a chromatographic column for pumping air and an injector coupled to the inlet of chromatographic column for feeding the sample using the air as a carrier gas. A detector is arranged downstream from and coupled to the outlet of the chromatographic column. The detector is a nanostructure semiconductive microfiber. The device further comprises an evaluation unit arranged and configured to evaluate each detected component to determine the concentration. The designed portable system was used for simultaneous detection of amines. The possibility of applying dispersive liquid-liquid microextraction for the determination of analytes in trace levels is demonstrated. The reproducibility of this method is acceptable, and good standard deviations were obtained. The relative standard deviation value is less than 6% for all analytes. Finally, the method was successfully applied to the extraction and determination of analytes in water samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Open-tubular capillary electrochromatographic determination of ten sulfonamides in tap water and milk by a metal-organic framework-coated capillary column.

PubMed

Wang, Xuan; Ye, Nengsheng; Hu, Xiaoyu; Liu, Qingye; Li, Jian; Peng, Lin; Ma, Xiaotong

2018-05-25

In this study, a metal-organic framework (MOF), [Mn(cam)(bpy)], was synthesized and characterized by thermogravimetric analysis, scanning electron microscopy, and Fourier transform infrared spectrometry. An open-tubular capillary column was fabricated from [Mn(cam)(bpy)] via the amide coupling method. Ten types of sulfonamides were separated through the fabricated capillary column, which showed a good limits of detection (< 0.07 μg·mL -1 ) and a linear ranges (1-100 μg·mL -1 or 5-100 μg·mL -1 ) with a high correlation coefficients (R 2 > 0.9987). The intra-day, inter-day and column-to-column relative standard deviations (RSDs) in the migration times ranged from 0.44% to 4.87%, and the peak area RSDs ranged from 0.80% to 7.28%. The developed capillary electrochromatography method can be successfully utilized for the determination of sulfonamides in tap water and milk samples. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

Ion chromatography for determination of nitrite and nitrate in seawater using monolithic ODS columns.

PubMed

Ito, Kazuaki; Takayama, Yohichi; Makabe, Nobuyuki; Mitsui, Ryo; Hirokawa, Takeshi

2005-08-12

A fast and highly sensitive ion chromatographic method using monolithic ODS columns was developed for the determination of nitrite (NO2-) and nitrate (NO3-) in seawater. Two monolithic ODS columns (50 mm x 4.6 mm i.d. + 100 mm x 4.6 mm i.d.) connected in series were coated and equilibrated with 5 mM cetyltrimethylammonium chloride (CTAC) aqueous solution. The column efficiency with 0.5 M NaCl as the mobile phase did not decrease in spite of the increase in flow rate of the mobile phase. Thus, good chromatograms were obtained within 3 minutes for NO2- and NO3 in artificial seawater without interferences by coexisting ions. The detection limit (S/N = 3) with UV detection at 225 nm was 0.8 and 1.6 microg/L for NO2- and NO3-, respectively. The characteristics of the monolithic CTA(+)-coated ODS columns were discussed. The present method was successfully applied to the fast and sensitive determination of NO2- and NO3- in real seawater samples.

Polymeric monolith column composited with multiwalled carbon nanotubes-β-cyclodextrin for the selective extraction of psoralen and isopsoralen.

PubMed

Ling, Xu; Zou, Li; Chen, Zilin

2017-09-01

A polymeric column that contains multiwalled carbon nanotubes-β-cyclodextrin composite was developed. The composite was wrapped into the poly(butyl methacrylate-ethylene dimethacrylate) monolith column (0.76 mm id and 10 cm in length). The column was then applied for the online solid-phase microextraction of psoralen and isopsoralen from Fructus Psoraleae. Following microextraction, the coumarins were quantified by high-performance liquid chromatography with C 18 separation column and UV detection. The effects of sample flow rate, sample volume, and pH value were optimized. The method showed low limits of detection (20 pg/mL, S/N = 3) for both psoralen and isopsoralen. Finally the method was successfully applied to the determination of psoralen and isopsoralen in spiked herb extracts and rat plasma where it gave recoveries that ranged between 93.2 and 102.1%. The empty hydrophobic cavities of β-cyclodextrin and the hydrophobicity of multiwalled carbon nanotubes provided specific extraction capability for psoralen and isopsoralen. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

In vivo genome-wide analysis of multiple tissues identifies gene regulatory networks, novel functions and downstream regulatory genes for Bapx1 and its co-regulation with Sox9 in the mammalian vertebral column.

PubMed

Chatterjee, Sumantra; Sivakamasundari, V; Yap, Sook Peng; Kraus, Petra; Kumar, Vibhor; Xing, Xing; Lim, Siew Lan; Sng, Joel; Prabhakar, Shyam; Lufkin, Thomas

2014-12-05

Vertebrate organogenesis is a highly complex process involving sequential cascades of transcription factor activation or repression. Interestingly a single developmental control gene can occasionally be essential for the morphogenesis and differentiation of tissues and organs arising from vastly disparate embryological lineages. Here we elucidated the role of the mammalian homeobox gene Bapx1 during the embryogenesis of five distinct organs at E12.5 - vertebral column, spleen, gut, forelimb and hindlimb - using expression profiling of sorted wildtype and mutant cells combined with genome wide binding site analysis. Furthermore we analyzed the development of the vertebral column at the molecular level by combining transcriptional profiling and genome wide binding data for Bapx1 with similarly generated data sets for Sox9 to assemble a detailed gene regulatory network revealing genes previously not reported to be controlled by either of these two transcription factors. The gene regulatory network appears to control cell fate decisions and morphogenesis in the vertebral column along with the prevention of premature chondrocyte differentiation thus providing a detailed molecular view of vertebral column development.

Hierarchy of facies of pyroclastic flow deposits generated by Laacher See type eruptions

NASA Astrophysics Data System (ADS)

Freundt, A.; Schmincke, H.-U.

1985-04-01

The upper Quaternary pyroclastic flow deposits of Laacher See volcano show compositional and structural facies variations on four different scales: (1) eruptive units of pyroclastic flows, composed of many flow units; (2) depositional cycles of as many as five flow units; flow units containing (3) regional intraflow-unit facies; and (4) local intraflow-unit subfacies. These facies can be explained by successively overlapping processes beginning in the magma column and ending with final deposition. The pyroclastic flow deposits thus reflect major aspects of the eruptive history of Laacher See volcano: (a) drastic changes in eruptive mechanism due to increasing access of water to the magma chamber and (b) change in chemical composition and crystal and gas content as evacuation of a compositionally zoned magma column progressed. The four scales of facies result from four successive sets of processes: (1) differentiation in the magma column and external factors governing the mechanism of eruption; (2) temporal variations of factors inducing eruption column collapse; (3) physical conditions in the eruption column and the way in which its collapse proceeds; and (4) interplay of flow-inherent and morphology-induced transport mechanics.

Vertebral anatomy in the Florida manatee, Trichechus manatus latirostris: a developmental and evolutionary analysis.

PubMed

Buchholtz, Emily A; Booth, Amy C; Webbink, Katherine E

2007-06-01

The vertebral column of the Florida manatee presents an unusual suite of morphological traits. Key among these are a small precaudal count, elongate thoracic vertebrae, extremely short neural spines, lack of a sacral series, high lumbar variability, and the presence of six instead of seven cervical vertebrae. This study documents vertebral morphology, size, and lumbar variation in 71 skeletons of Trichechus manatus latirostris (Florida manatee) and uses the skeletons of Trichechus senegalensis (west African manatee) and Dugong dugon (dugong) in comparative analysis. Vertebral traits are used to define morphological, and by inference developmental, column modules and to propose their hierarchical relationships. A sequence of evolutionary innovations in column morphology is proposed. Results suggest that the origin of the fluke and low rates of cervical growth originated before separation of trichechids (manatees) and dugongids (dugongs). Meristic reduction in count is a later, trichechid innovation and is expressed across the entire precaudal column. Elongation of thoracic vertebrae may be an innovative strategy to generate an elongate column in an animal with a small precaudal count. Elimination of the lumbus through both meristic and homeotic reduction is currently in progress. 2007 Wiley-Liss, Inc.

Determination of antioxidants by a novel on-line HPLC-cupric reducing antioxidant capacity (CUPRAC) assay with post-column detection.

PubMed

Celik, Saliha Esin; Ozyürek, Mustafa; Güçlü, Kubilay; Apak, Reşat

2010-07-26

A novel on-line HPLC-cupric reducing antioxidant capacity (CUPRAC) method was developed for the selective determination of polyphenols (flavonoids, simple phenolic and hydroxycinnamic acids) in complex plant matrices. The method combines chromatographic separation, constituent analysis, and post-column identification of antioxidants in plant extracts. The separation of polyphenols was performed on a C18 column using gradient elution with two different mobile phase solutions, i.e., MeOH and 0.2% o-phosphoric acid. The HPLC-separated antioxidant polyphenols in the extracts react with copper(II)-neocuproine (Cu(II)-Nc) reagent in a post-column reaction coil to form a derivative. The reagent is reduced by antioxidants to the copper(I)-neocuproine (Cu(I)-Nc) chelate having maximum absorption at 450 nm. The negative peaks of antioxidant constituents were monitored by measuring the increase in absorbance due to Cu(I)-Nc. The detection limits of polyphenols at 450 nm (in the range of 0.17-3.46 microM) after post-column derivatization were comparable to those at 280 nm UV detection without derivatization. The developed method was successfully applied to the identification of antioxidant compounds in crude extracts of Camellia sinensis, Origanum marjorana and Mentha. The method is rapid, inexpensive, versatile, non-laborious, uses stable reagents, and enables the on-line qualitative and quantitative estimation of antioxidant constituents of complex plant samples. Copyright 2010 Elsevier B.V. All rights reserved.

Ion chromatographic methods for the detection of starch hydrolysis products in ruminal digesta.

PubMed

Barsuhn, K; Kotarski, S F

1991-06-21

Dionex high-performance ion chromatographic methods were evaluated for separation and quantitation of plant sugars and starch digestion products in the ruminal digesta of cattle. Mono- and disaccharides were eluted from a Dionex CarboPac PA1 column with sodium hydroxide used isocratically or as a pH gradient. Maltooligosaccharides which had a degree of polymerization (DP) less than 30 glucose residues were eluted in 60 min by a sodium hydroxide eluent containing a sodium acetate gradient. Carbohydrates were detected amperometrically. Responses were linear (r2 greater than 0.99) for glucose, disaccharides and maltooligosaccharides (DP less than 8). Precipitation and solid-phase extraction methods were evaluated for clean-up of samples of feedstuffs, ruminal contents, and bacterial culture fluids. Perchloric acid precipitation hydrolyzed sucrose but did not affect recoveries of cellobiose, isomaltose or maltose. Ethanol in concentrations of 79 and 86% precipitated maltooligosaccharides having chain lengths larger than 14 and 9 glucose residues, respectively. Maltooligosaccharide recoveries from solid-phase extraction columns varied with maltooligosaccharide size and column packing. Recoveries were greater than 94% for short chains (DP less than 6) eluted from phenyl-substituted columns and variable for all oligosaccharides eluted from C18 columns. Applications of these methods are presented and include: (1) detection of sugars in ruminant feed, (2) monitoring changes in ruminal sugars after feeding and (3) monitoring changes in extracellular sugars and oligosaccharides in the culture fluids of the ruminal bacterium, Bacteroides ruminicola.

Implications of the center of rotation concept for the reconstruction of anterior column lordosis and axial preloads in spinal deformity surgery.

PubMed

Koller, Heiko; Mayer, Michael; Zenner, Juliane; Resch, Herbert; Niederberger, Alfred; Fierlbeck, Johann; Hitzl, Wolfgang; Acosta, Frank L

2012-07-01

In thoracolumbar deformity surgery, anterior-only approaches are used for reconstruction of anterior column failures. It is generally advised that vertebral body replacements (VBRs) should be preloaded by compression. However, little is known regarding the impact of different techniques for generation of preloads and which surgical principle is best for restoration of lordosis. Therefore, the authors analyzed the effect of different surgical techniques to restore spinal alignment and lordosis as well as the ability to generate axial preloads on VBRs in anterior column reconstructions. The authors performed a laboratory study using 7 fresh-frozen specimens (from T-3 to S-1) to assess the ability for lordosis reconstruction of 5 techniques and their potential for increasing preloads on a modified distractable VBR in a 1-level thoracolumbar corpectomy. The testing protocol was as follows: 1) Radiographs of specimens were obtained. 2) A 1-level corpectomy was performed. 3) In alternating order, lordosis was applied using 1 of the 5 techniques. Then, preloads during insertion and after relaxation using the modified distractable VBR were assessed using a miniature load-cell incorporated in the modified distractable VBR. The modified distractable VBR was inserted into the corpectomy defect after lordosis was applied using 1) a lamina spreader; 2) the modified distractable VBR only; 3) the ArcoFix System (an angular stable plate system enabling in situ reduction); 4) a lordosizer (a customized instrument enabling reduction while replicating the intervertebral center of rotation [COR] according to the COR method); and 5) a lordosizer and top-loading screws ([LZ+TLS], distraction with the lordosizer applied on a 5.5-mm rod linked to 2 top-loading pedicle screws inserted laterally into the vertebra). Changes in the regional kyphosis angle were assessed radiographically using the Cobb method. The bone mineral density of specimens was 0.72 ± 22.6 g/cm(2). The maximum regional kyphosis angle reconstructed among the 5 techniques averaged 9.7°-16.1°, and maximum axial preloads averaged 123.7-179.7 N. Concerning correction, in decreasing order the LZ+TLS, lordosizer, and ArcoFix System outperformed the lamina spreader and modified distractable VBR. The order of median values for insertion peak load, from highest to lowest, were lordosizer, LZ+TLS, and ArcoFix, which outperformed the lamina spreader and modified distractable VBR. In decreasing order, the axial preload was highest with the lordosizer and LZ+TLS, which both outperformed the lamina spreader and the modified distractable VBR. The technique enabling the greatest lordosis achieved the highest preloads. With the ArcoFix System and LZ+TLS, compression loads could be applied and were 247.8 and 190.6 N, respectively, which is significantly higher than the insertion peak load and axial preload (p < 0.05). Including the ability for replication of the COR in instruments designed for anterior column reconstructions, the ability for lordosis restoration of the anterior column and axial preloads can increase, which in turn might foster fusion.

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

NASA Astrophysics Data System (ADS)

Ramachandran, Nirmal; Ganguli, Ranjan

2018-06-01

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

Tetrahedral Arrangements of Perylene Bisimide Columns via Supramolecular Orientational Memory.

PubMed

Sahoo, Dipankar; Peterca, Mihai; Aqad, Emad; Partridge, Benjamin E; Heiney, Paul A; Graf, Robert; Spiess, Hans W; Zeng, Xiangbing; Percec, Virgil

2017-01-24

Chiral, shape, and liquid crystalline memory effects are well-known to produce commercial macroscopic materials with important applications as springs, sensors, displays, and memory devices. A supramolecular orientational memory effect that provides complex nanoscale arrangements was only recently reported. This supramolecular orientational memory was demonstrated to preserve the molecular orientation and packing within supramolecular units of a self-assembling cyclotriveratrylene crown at the nanoscale upon transition between its columnar hexagonal and Pm3̅n cubic periodic arrays. Here we report the discovery of supramolecular orientational memory in a dendronized perylene bisimide (G2-PBI) that self-assembles into tetrameric crowns and subsequently self-organizes into supramolecular columns and spheres. This supramolecular orientation memory upon transition between columnar hexagonal and body-centered cubic (BCC) mesophases preserves the 3-fold cubic [111] orientations rather than the 4-fold [100] axes, generating an unusual tetrahedral arrangement of supramolecular columns. These results indicate that the supramolecular orientational memory concept may be general for periodic arrays of self-assembling dendrons and dendrimers as well as for other periodic and quasiperiodic nanoscale organizations comprising supramolecular spheres, generated from other organized complex soft matter including block copolymers and surfactants.

Comparison of field-enhanced and pressure-assisted field-enhanced sample injection techniques for the analysis of water-soluble vitamins using CZE.

PubMed

Liu, Qingqing; Liu, Yaling; Guan, Yu; Jia, Li

2009-04-01

A new online concentration method, namely pressure-assisted field-enhanced sample injection (PA-FESI), was developed and compared with FESI for the analysis of water-soluble vitamins by CZE with UV detection. In PA-FESI, negative voltage and positive pressure were simultaneously applied to initialize PA-FESI. PA-FESI uses the hydrodynamic flow generated by the positive pressure to counterbalance the reverse EOF in the capillary column during electrokinetic sample injection, which allowed a longer injection time than usual FESI mode without compromising the separation efficiency. Using the PA-FESI method, the LODs of the vitamins were at ng/mL level based on the S/N of 3 and the RSDs of migration time and peak area for each vitamin (1 microg/mL) were less than 5.1%. The developed method was applied to the analysis of water-soluble vitamins in corns.

Hydroxylapatite chromatography.

PubMed

Broadhurst, A V

2001-05-01

Hydroxylapatite (also called hydroxyapatite), a form of calcium phosphate, can be used as a matrix for the chromatography of both proteins and nucleic acids. Protocols are provided for both standard low-pressure chromatography of a protein mixture using a hydroxylapatite column prepared in the laboratory, and an HPLC method, applicable to proteins and nucleic acids, that uses a commercially available column. Alternate protocols describe column chromatography using a step gradient or batch binding and step-gradient elution.

Staged fluidized bed

DOEpatents

Mallon, Richard G.

1984-01-01

Method and apparatus for narrowing the distribution of residence times of any size particle and equalizing the residence times of large and small particles in fluidized beds. Particles are moved up one fluidized column and down a second fluidized column with the relative heights selected to equalize residence times of large and small particles. Additional pairs of columns are staged to narrow the distribution of residence times and provide complete processing of the material.

Steel-reinforced concrete-filled steel tubular columns under axial and lateral cyclic loading

NASA Astrophysics Data System (ADS)

Farajpourbonab, Ebrahim; Kute, Sunil Y.; Inamdar, Vilas M.

2018-03-01

SRCFT columns are formed by inserting a steel section into a concrete-filled steel tube. These types of columns are named steel-reinforced concrete-filled steel tubular (SRCFT) columns. The current study aims at investigating the various types of reinforcing steel section to improve the strength and hysteresis behavior of SRCFT columns under axial and lateral cyclic loading. To attain this objective, a numerical study has been conducted on a series of composite columns. First, FEM procedure has been verified by the use of available experimental studies. Next, eight composite columns having different types of cross sections were analyzed. For comparison purpose, the base model was a CFT column used as a benchmark specimen. Nevertheless, the other specimens were SRCFT types. The results indicate that reinforcement of a CFT column through this method leads to enhancement in load-carrying capacity, enhancement in lateral drift ratio, ductility, preventing of local buckling in steel shell, and enhancement in energy absorption capacity. Under cyclic displacement history, it was observed that the use of cross-shaped reinforcing steel section causes a higher level of energy dissipation and the moment of inertia of the reinforcing steel sections was found to be the most significant parameter affecting the hysteresis behavior of SRCFT columns.