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.

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

Back, H. O.; Bottenus, D. R.; Clayton, C.

The next generation of 136Xe neutrinoless double beta decay experiments will require on the order of 5 tons of enriched 136Xe. By estimating the relative volatilities of the xenon isotopes and using standard chemical engineering techniques we explore the feasibility of using cryogenic distillation to produce 5 tons of 80% enriched 136Xe in 5-6 years. With current state-of-the-art distillation column packing materials we can estimate the total height of a traditional cryogenic distillation column. We also, report on how Micro Channel Distillation may reduce the overall size of a distillation system for 136Xe production.

Experimental and Numerical Investigation of Two Dimensional CO2 Adsorption/Desorption in Packed Sorption Beds under Non-Ideal Flows

NASA Technical Reports Server (NTRS)

Mohamadinejad, H.; Knox, J. C.; Smith, J. E.; Croomes, Scott (Technical Monitor)

2001-01-01

The experimental results of CO2 adsorption and desorption in a packed column indicated that the concentration wave front at the center of the packed column differs from those which are close to the wall of column filled with adsorbent material even though the ratio of column diameter to the particle size is greater than 20. The comparison of the experimental results with one dimensional model of packed column shows that in order to simulate the average breakthrough in a packed column a two dimensional (radial and axial) model of packed column is needed. In this paper the mathematical model of a non-slip flow through a packed column with 2 inches in diameter and 18 inches in length filled with 5A zeolite pellets is presented. The comparison of experimental results of CO2 absorption and desorption for the mixed and central breakthrough of the packed column with numerical results is also presented.

MODEL FOR NON-EQUILIBRIUM BINDING AND AFFINITY CHROMATOGRAPHY WITH CHARACTERIZATION OF 8-HYDROXYQUINOLINE IMMOBILIZED ON CONTROLLED PORE GLASS USING A FLOW INJECTION SYSTEM WITH A PACKED MICRO-COLUMN. (R826694C651)

EPA Science Inventory

The perspectives, information and conclusions conveyed in research project abstracts, progress reports, final reports, journal abstracts and journal publications convey the viewpoints of the principal investigator and may not represent the views and policies of ORD and EPA. Concl...

Surface micro-structuring of silicon by excimer-laser irradiation in reactive atmospheres

NASA Astrophysics Data System (ADS)

Pedraza, A. J.; Fowlkes, J. D.; Jesse, S.; Mao, C.; Lowndes, D. H.

2000-12-01

The formation mechanisms of cones and columns by pulsed-laser irradiation in reactive atmospheres were studied using scanning electron microscopy and profilometry. Deep etching takes place in SF6- and O2- rich atmospheres and consequently, silicon-containing molecules and clusters are released. Transport of silicon from the etched/ablated regions to the tip of columns and cones and to the side of the cones is required because both structures, columns and cones, protrude above the initial surface. The laser-induced micro-structure is influenced not only by the nature but also by the partial pressure of the reactive gas in the atmosphere. Irradiation in Ar following cone formation in SF6 produced no additional growth but rather melting and resolidification. Subsequent irradiation using again a SF6 atmosphere lead to cone restructuring and growth resumption. Thus the effects of etching plus re-deposition that produce column/cone formation and growth are clearly separated from the effects of just melting. On the other hand, irradiation continued in air after first performed in SF6 resulted in: (a) an intense etching of the cones and a tendency to transform them into columns; (b) growth of new columns on top of the existing cones and (c) filamentary nano-structures coating the sides of the columns and cones.

Consideration of grain packing in granular iron treatability studies

NASA Astrophysics Data System (ADS)

Firdous, R.; Devlin, J. F.

2014-08-01

Commercial granular iron (GI) is light steel that is used in Permeable Reactive Barriers (PRBs). Investigations into the reactivity of GI have focused on its chemical nature and relatively little direct work has been done to account for the effects of grain shape and packing. Both of these factors are expected to influence available grain surface area, which is known to correlate to reactivity. Commercial granular iron grains are platy and therefore pack in preferential orientations that could affect solution access to the surface. Three packing variations were investigated using Connelly Iron and trichloroethylene (TCE). Experimental kinetic data showed reaction rates 2-4 times higher when grains were packed with long axes preferentially parallel to flow (VP) compared to packings with long axes preferentially perpendicular to flow (HP) or randomly arranged (RP). The variations were found to be explainable by variations in reactive sorption capacities, i.e., sorption to sites where chemical transformations took place. The possibility that the different reactive sorption capacities were related to physical pore-scale differences was assessed by conducting an image analysis of the pore structure of sectioned columns. The analyses suggested that pore-scale factors - in particular the grain surface availability, reflected in the sorption capacity terms of the kinetic model used - could only account for a fraction of the observed reactivity differences between packing types. It is concluded that packing does affect observable reaction rates but that micro-scale features on the grain surfaces, rather than the pore scale characteristics, account for most of the apparent reactivity differences. This result suggests that treatability tests should consider the packing of columns carefully if they are to mimic field performance of PRBs to the greatest extent possible.

High resolution photolithography using arrays of polystyrene and SiO2 micro- and nano-sized spherical lenses

NASA Astrophysics Data System (ADS)

Dvoretckaia, L. N.; Mozharov, A. M.; Mukhin, I. S.

2017-11-01

Photolithography mask made of close-packed array of micro- and nano-sized spherical lenses allows to obtain the ordered structures and provides highest “optical resolution/cost” ratio between all existing photolithography and laser direct writing methods. In this letter, we present results of modeling the propagation of a plane wave falling on the array of quartz (SiO2) microspherical lenses and focusing in the image reverse photoresist layer. We present here experimental results on fabrication of ordered arrays of submicron wells and columns and substrate preparation for growth of monocrystalline nanowires on metal surface using photolithography with mask of SiO2 microspheres. Such ordered nano-sized arrays of wells and columns can be used in fabrication of further growth of monocrystalline nanowires, quantum dots and production of plasmon structures.

Optimization of microfabricated nanoliter-scale solid-phase extraction device for detection of gel-separated proteins in low abundance by matrix-assisted laser desorption/ionization mass spectrometry.

PubMed

Chen, Wenzhang; Shen, Jing; Yin, Xuefeng; Yu, Yingnian

2007-01-01

A nano-scale solid-phase extraction (SPE) device was developed for the detection of gel-separated proteins in low abundance by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS) with a simplified microfabrication technology. By using SU-8 photoresist instead of epoxy glue to connect the microchannel and transfer capillary, polymeric contaminant signals in MS analysis were significantly reduced. Micro SPE columns with different capacities and geometric characteristics were investigated in order to increase the detection sensitivity and decrease spot size for MALDI-TOF-MS analysis. It is shown that enhancements in sensitivities for the detection of proteins in low abundance were correlated with the reduction in column capacity and increase in column aspect ratio. Fifty nanoliters of matrix solution were sufficient to elute the sample completely from the optimized micro SPE column with 3.5 nL capacity. The mass spectrum of a 5 fmol in-gel tryptic digest of bovine serum albumin (BSA), processed by the micro SPE column, demonstrated that 29 peptides matched the protein giving a sequence coverage of 51%, which was better than that obtained from analysis of 25 fmol of the same sample prepared by the dried-droplet method. With the micro SPE column treatment of 2 microL of digestion supernatant of a gel spot of the IQGAP1 protein, 15 peptides were detected from the mass spectrum with the highest individual score of 111, while, with a ZipTip procedure, only nine peaks were detected with the highest individual score of 71. Analytical results demonstrated that this approach greatly improved the sequence coverage and identification specificity for the tested protein. It can serve as a very useful tool in proteomics studies, especially for low abundance proteins. Copyright (c) 2006 John Wiley & Sons, Ltd.

Implementation of high slurry concentration and sonication to pack high-efficiency, meter-long capillary ultrahigh pressure liquid chromatography columns.

PubMed

Godinho, Justin M; Reising, Arved E; Tallarek, Ulrich; Jorgenson, James W

2016-09-02

Slurry packing capillary columns for ultrahigh pressure liquid chromatography is complicated by many interdependent experimental variables. Previous results have suggested that combination of high slurry concentration and sonication during packing would create homogeneous bed microstructures and yield highly efficient capillary columns. Herein, the effect of sonication while packing very high slurry concentrations is presented. A series of six, 1m×75μm internal diameter columns were packed with 200mg/mL slurries of 2.02μm bridged-ethyl hybrid silica particles. Three of the columns underwent sonication during packing and yielded highly efficient separations with reduced plate heights as low as 1.05. Copyright © 2016 Elsevier B.V. All rights reserved.

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

PubMed

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

2009-06-01

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

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

PubMed

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

2017-09-01

Column wall effects are well recognized as major limiting factor in achieving high separation efficiency in HPLC. This is especially important for modern analytical columns packed with small particles, where wall effects dominate the band broadening. Detailed knowledge about the packing microstructure of packed analytical columns has so far not been acquired. Here, we present the first three-dimensional reconstruction protocol for these columns utilizing focused ion-beam scanning electron microscopy (FIB-SEM) on a commercial 2.1mm inner diameter×50mm length narrow-bore analytical column packed with 1.7μm bridged-ethyl hybrid silica particles. Two sections from the packed bed are chosen for reconstruction by FIB-SEM: one from the bulk packing region of the column and one from its critical wall region. This allows quantification of structural differences between the wall region and the center of the bed due to effects induced by the hard, confining column wall. Consequences of these effects on local flow velocity in the column are analyzed with flow simulations utilizing the lattice-Boltzmann method. The reconstructions of the bed structures reveal significant structural differences in the wall region (extending radially over approximately 62 particle diameters) compared to the center of the column. It includes the local reduction of the external porosity by up to 10% and an increase of the mean particle diameter by up to 3%, resulting in a decrease of the local flow velocity by up to 23%. In addition, four (more ordered) layers of particles in the direct vicinity of the column wall induce local velocity fluctuations by up to a factor of three regarding the involved velocity amplitudes. These observations highlight the impact of radial variations in packing microstructure on band migration and column performance. This knowledge on morphological peculiarities of column wall effects helps guiding us towards further optimization of the packing process for analytical HPLC columns. Copyright © 2017 Elsevier B.V. All rights reserved.

Bed morphological features associated with an optimal slurry concentration for reproducible preparation of efficient capillary ultrahigh pressure liquid chromatography columns.

PubMed

Reising, Arved E; Godinho, Justin M; Jorgenson, James W; Tallarek, Ulrich

2017-06-30

Column wall effects and the formation of larger voids in the bed during column packing are factors limiting the achievement of highly efficient columns. Systematic variation of packing conditions, combined with three-dimensional bed reconstruction and detailed morphological analysis of column beds, provide valuable insights into the packing process. Here, we study a set of sixteen 75μm i.d. fused-silica capillary columns packed with 1.9μm, C18-modified, bridged-ethyl hybrid silica particles slurried in acetone to concentrations ranging from 5 to 200mg/mL. Bed reconstructions for three of these columns (representing low, optimal, and high slurry concentrations), based on confocal laser scanning microscopy, reveal morphological features associated with the implemented slurry concentration, that lead to differences in column efficiency. At a low slurry concentration, the bed microstructure includes systematic radial heterogeneities such as particle size-segregation and local deviations from bulk packing density near the wall. These effects are suppressed (or at least reduced) with higher slurry concentrations. Concomitantly, larger voids (relative to the mean particle diameter) begin to form in the packing and increase in size and number with the slurry concentration. The most efficient columns are packed at slurry concentrations that balance these counteracting effects. Videos are taken at low and high slurry concentration to elucidate the bed formation process. At low slurry concentrations, particles arrive and settle individually, allowing for rearrangements. At high slurry concentrations, they arrive and pack as large patches (reflecting particle aggregation in the slurry). These processes are discussed with respect to column packing, chromatographic performance, and bed microstructure to help reinforce general trends previously described. Conclusions based on this comprehensive analysis guide us towards further improvement of the packing process. Copyright © 2017 Elsevier B.V. All rights reserved.

Microfluidic direct injection method for analysis of urinary 4-(methylnitrosamino)-1-(3-pyridyl)-1-butanol (NNAL) using molecularly imprinted polymers coupled on-line with LC-MS/MS.

PubMed

Shah, Kumar A; Peoples, Michael C; Halquist, Matthew S; Rutan, Sarah C; Karnes, H Thomas

2011-01-25

The work described in this paper involves development of a high-throughput on-line microfluidic sample extraction method using capillary micro-columns packed with MIP beads coupled with tandem mass spectrometry for the analysis of urinary NNAL. The method was optimized and matrix effects were evaluated and resolved. The method enabled low sample volume (200 μL) and rapid analysis of urinary NNAL by direct injection onto the microfluidic column packed with molecularly imprinted beads engineered to NNAL. The method was validated according to the FDA bioanalytical method validation guidance. The dynamic range extended from 20.0 to 2500.0 pg/mL with a percent relative error of ±5.9% and a run time of 7.00 min. The lower limit of quantitation was 20.0 pg/mL. The method was used for the analysis of NNAL and NNAL-Gluc concentrations in smokers' urine. Copyright © 2010 Elsevier B.V. All rights reserved.

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

PubMed

Yang, Peilin; McCabe, Terry; Pursch, Matthias

2011-11-01

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

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

PubMed

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

2005-12-23

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

Controlled irrigation of a structured packing as a method for increasing the efficiency of liquid mixture separation in the distillation column

NASA Astrophysics Data System (ADS)

Pavlenko, A. N.; Zhukov, V. E.; Pecherkin, N. I.; Nazarov, A. D.; Li, X.; Li, H.; Gao, X.; Sui, H.

2017-09-01

The use of modern structured packing in the distillation columns allows much more even distribution of the liquid film over the packing surface, but it does not completely solve the problem of uniform distribution of flow parameters over the entire height of the packing. Negative stratification of vapor along the packing height caused by different densities of vapor mixture components and higher temperature in the lower part of the column leads to formation of large-scale maldistributions of temperature and mixture composition over the column cross-section even under the conditions of uniform irrigation of packing with liquid. In these experiments, the idea of compensatory action of liquid distributor on the large-scale maldistribution of mixture composition over the column cross-section was implemented. The experiments were carried out in the distillation column with the diameter of 0.9 m on 10 layers of the Mellapak 350Y packing with the total height of 2.1 m. The mixture of R-21 and R-114 was used as the working mixture. To irrigate the packing, the liquid distributorr with 126 independently controlled solenoid valves overlapping the holes with the diameter of 5 mm, specially designed by the authors, was used. Response of the column to the action of liquid distributor was observed in real time according to the indications of 3 groups of thermometers mounted in 3 different cross-sections of the column. The experiments showed that the minimal correction of the drip point pattern in the controlled liquid distributor can significantly affect the pattern of flow parameter distribution over the cross-section and height of the mass transfer surface and increase separation efficiency of the column within 20%.

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.

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.

Mass transfer resistance in narrow-bore columns packed with 1.7 microm particles in very high pressure liquid chromatography.

PubMed

Gritti, Fabrice; Guiochon, Georges

2010-07-30

Surprisingly, the mass transfer kinetic properties of columns packed with superficially porous particles are markedly different from those of columns packed with fully porous particles. The performances of 2.1mmx150mm columns packed with a new type of sub-2microm particles, the superficially porous 1.7microm Kinetex-C(18), and with the classical 1.7microm BEH-C(18) fully porous particles were measured and are discussed. The sample was naphtho[2,3-a]pyrene; the use of different mobile phase compositions allowed a comparison between data measured with retention factors of k(') approximately 2 and k(') approximately 20. The minimum reduced height equivalent to a theoretical plate (HETP) of the two columns were similar, at h(min)=2.0. However, this minimum HETP was observed at a markedly shorter reduced linear velocity for the column packed with totally porous particles, between 5 and 7 for BEH, than for the one packed with shell particles, between 8 and 10 for Kinetex. This result is explained by the combination of (1) a 35% smaller B term for the Kinetex column than for the BEH column, due to the 37% lower porous volume of the former; (2) a larger reduced A term for the Kinetex column (1.6), showing a relatively poorly packed column with significant trans-column velocity biases than for the BEH column (ca. 1.0); and (3) a much lesser dependance of the efficiency on the mobile phase velocity at high velocities for the Kinetex than for the BEH column, when these columns are placed in the oven of the instrument under still-air conditions. The heat friction affects significantly more the efficiency of the BEH column than that of the Kinetex column. This unexpected result is accounted for by the three times smaller heat conductivity of the BEH bed (lambda(BEH) approximately 0.25 W/m/K) than that of the Kinetex bed (lambda(Kinetex) approximately 0.75W/m/K).

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

PubMed

Fekete, Szabolcs; Fekete, Jeno; Ganzler, Katalin

2009-12-05

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

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.

A two-phase flow model for submarine granular flows: With an application to collapse of deeply-submerged granular columns

NASA Astrophysics Data System (ADS)

Lee, Cheng-Hsien; Huang, Zhenhua

2018-05-01

The collapse process of a submerged granular column is strongly affected by its initial packing. Previous models for particle response time, which is used to quantify the drag force between the solid and liquid phases in rheology-based two-phase flow models, have difficulty in simulating the collapse process of granular columns with different initial concentrations (initial packing conditions). This study introduces a new model for particle response time, which enables us to satisfactorily model the drag force between the two phases for a wide range of volume concentration. The present model can give satisfactory results for both loose and dense packing conditions. The numerical results have shown that (i) the initial packing affects the occurrence of contractancy/diltancy behavior during the collapse process, (ii) the general buoyancy and drag force are strongly affected by the initial packing through contractancy and diltancy, and (iii) the general buoyancy and drag force can destabilize the granular material in loose packing condition but stabilize the granular material in dense packing condition. The results have shown that the collapse process of a densely-packed granular column is more sensitive to particle response time than that of a loosely-packed granular column.

Tapered plug foam spray apparatus

NASA Technical Reports Server (NTRS)

Allen, Peter B. (Inventor)

1996-01-01

A two-component foam spray gun is readily disassembled for cleaning. It includes a body (1) with reactant (12, 14) and purge gas (16) inlet ports. A moldable valve packing (32) inside the body has a tapered conical interior surface (142), and apertures which match the reactant ports. A valve/tip (40) has a conical outer surface (48) which mates with the valve packing (32). The valve/tip (40) is held in place by a moldable packing washer (34), held at non-constant pressure by a screw (36, 38). The interior of the valve/tip (40) houses a removable mixing chamber (50). The mixing chamber (50) has direct flow orifices (60) and an auxiliary flow path (58, 60) which ameliorate pressure surges. The spray gun can be disassembled for cleaning without disturbing the seal, by removing the valve/tip (40) to the rear, thereby breaking it free of the conical packing. Rotation of the valve/tip (40) relative to the body (1) shuts off the reactant flow, and starts the purge gas flow.

Microfabricated packed gas chromatographic column

DOEpatents

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

2003-12-16

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

Prevention and suppression of metal packing fires.

PubMed

Roberts, Mark; Rogers, William J; Sam Mannan, M; Ostrowski, Scott W

2003-11-14

Structured packing has been widely used because of large surface area that makes possible columns with high capacity and efficiency. The large surface area also contributes to fire hazards because of hydrocarbon deposits that can easily combust and promote combustion of the thin metal packing materials. Materials of high surface area that can fuel fires include reactive metals, such as titanium, and materials that are not considered combustible, such as stainless steel. Column design and material selection for packing construction is discussed together with employee training and practices for safe column maintenance and operations. Presented also are methods and agents for suppression of metal fires. Guidance for prevention and suppression of metal fires is related to incidents involving packing fires in columns.

Selection of stationary phase particle geometry using X-ray computed tomography and computational fluid dynamics simulations.

PubMed

Schmidt, Irma; Minceva, Mirjana; Arlt, Wolfgang

2012-02-17

The X-ray computed tomography (CT) is used to determine local parameters related to the column packing homogeneity and hydrodynamics in columns packed with spherically and irregularly shaped particles of same size. The results showed that the variation of porosity and axial dispersion coefficient along the column axis is insignificant, compared to their radial distribution. The methodology of using the data attained by CT measurements to perform a CFD simulation of a batch separation of model binary mixtures, with different concentration and separation factors is demonstrated. The results of the CFD simulation study show that columns packed with spherically shaped particles provide higher yield in comparison to columns packed with irregularly shaped particles only below a certain value of the separation factor. The presented methodology can be used for selecting a suited packing material for a particular separation task. Copyright © 2012 Elsevier B.V. All rights reserved.

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

PubMed

Liu, Hong-gao; Wang, Yuan-zhong

2010-01-01

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

Characterisation of RPLC columns packed with porous sub-2 microm particles.

PubMed

Petersson, Patrik; Euerby, Melvin R

2007-08-01

Eight commercially available sub-2 microm octadecyl silane columns (C18 columns) have been characterised by the Tanaka protocol. The columns can be grouped into two groups that display large differences in selectivity and peak shape due to differences in hydrophobicity, degree of surface coverage and silanol activity. Measurements of particle size distributions were made using automated microscopy and electrical sensing zone measurements. Only a weak correlation could be found between efficiency and particle size. Large differences in column backpressure were observed. These differences are not related to particle size distribution. A more likely explanation is differences in packing density. In order to take full advantage of 100-150 mm columns packed with sub-2 microm particles, it is often necessary to employ not only an elevated pressure but also an elevated temperature. A comparison between columns packed with sub-2, 3 and 5 microm versions of the same packing indicates potential method transferability problems for several of the columns due to selectivity differences. Currently, the best alternative for fast high-resolution LC is the use of sub-2 microm particles in combination with elevated pressure and temperature. However, as shown in this study additional efforts are needed to improve transferability as well as column performance.

Root Tip Shape Governs Root Elongation Rate under Increased Soil Strength1[OPEN

PubMed Central

Kirchgessner, Norbert; Walter, Achim

2017-01-01

Increased soil strength due to soil compaction or soil drying is a major limitation to root growth and crop productivity. Roots need to exert higher penetration force, resulting in increased penetration stress when elongating in soils of greater strength. This study aimed to quantify how the genotypic diversity of root tip geometry and root diameter influences root elongation under different levels of soil strength and to determine the extent to which roots adjust to increased soil strength. Fourteen wheat (Triticum aestivum) varieties were grown in soil columns packed to three bulk densities representing low, moderate, and high soil strength. Under moderate and high soil strength, smaller root tip radius-to-length ratio was correlated with higher genotypic root elongation rate, whereas root diameter was not related to genotypic root elongation. Based on cavity expansion theory, it was found that smaller root tip radius-to-length ratio reduced penetration stress, thus enabling higher root elongation rates in soils with greater strength. Furthermore, it was observed that roots could only partially adjust to increased soil strength. Root thickening was bounded by a maximum diameter, and root tips did not become more acute in response to increased soil strength. The obtained results demonstrated that root tip geometry is a pivotal trait governing root penetration stress and root elongation rate in soils of greater strength. Hence, root tip shape needs to be taken into account when selecting for crop varieties that may tolerate high soil strength. PMID:28600344

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

PubMed

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

2009-04-10

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

Capillary trap column with strong cation-exchange monolith for automated shotgun proteome analysis.

PubMed

Wang, Fangjun; Dong, Jing; Jiang, Xiaogang; Ye, Mingliang; Zou, Hanfa

2007-09-01

A 150 microm internal diameter capillary monolithic column with a strong cation-exchange stationary phase was prepared by direct in situ polymerization of ethylene glycol methacrylate phosphate and bisacrylamide in a trinary porogenic solvent consisting dimethylsulfoxide, dodecanol, and N,N'-dimethylformamide. This phosphate monolithic column exhibits higher dynamic binding capacity, faster kinetic adsorption of peptides, and more than 10 times higher permeability than the column packed with commercially available strong cation-exchange particles. It was applied as a trap column in a nanoflow liquid chromatography-tandem mass spectrometry system for automated sample injection and online multidimensional separation. It was observed that the sample could be loaded at a flow rate as high as 40 microL/min with a back pressure of approximately 1300 psi and without compromising the separation efficiency. Because of its good orthogonality to the reversed phase separation mechanism, the phosphate monolithic trap column was coupled with a reversed-phase column for online multidimensional separation of 19 microg of the tryptic digest of yeast proteins. A total of 1522 distinct proteins were identified from 5608 unique peptides (total of 54,780 peptides) at the false positive rate only 0.46%.

Colloidal aspects and packing behaviour of charged microparticulates in high efficiency ion chromatography.

PubMed

Wahab, M Farooq; Pohl, Christopher A; Lucy, Charles A

2012-12-28

The development of small particles in ion chromatography (IC) is a recent phenomenon. Very few studies are available on packing polymeric particles bearing ionizable functional groups. This study explores the colloidal and rheological properties that govern slurry packing to form high efficiency IC columns. The polymeric substrate used was non-porous 4.4 μm sulfonated ethylvinylbenzene–divinylbenzene (1.4 mequiv. SO(3)H/g resin) with 55% crosslink. We developed simple tests optical microscopy and sedimentation tests for predicting the quality of packed columns. The negatively charged particles (zeta potential: −52 mV in water) behave like colloids. The influence of counter-ion charge (Al(3+), Mg(2+), Na(+)) and ionic strength on column efficiency followed the Schulze–Hardy rule. Highly flocculating slurries give poorly packed columns with N ~ 900 whereas under non-agglomerating slurry conditions efficiencies up to N > 10,000 can be achieved. A non-agglomerating slurry also shows non-Newtonian behaviour, specifically shear thickening. Packing at lower flow rate (<1 mL/min) or higher temperature (>50 °C) reduces the shear thickening and produces higher efficiency columns. The packed sulfonated resin column is coated with 72 nm quaternary ammonium bearing latex (AS4A) and used in the separation of F(−), Cl(−), NO(2)(−), Br(−), and NO(3)(−) yielding a reduced plate height of 1.9 under optimum conditions.

Coupled factors influencing detachment of nano- and micro-sized particles from primary minima.

PubMed

Shen, Chongyang; Lazouskaya, Volha; Jin, Yan; Li, Baoguo; Ma, Zhiqiang; Zheng, Wenjuan; Huang, Yuanfang

2012-06-01

This study examined the detachments of nano- and micro-sized colloids from primary minima in the presence of cation exchange by laboratory column experiments. Colloids were initially deposited in columns packed with glass beads at 0.2 M CaCl(2) in the primary minima of Derjaguin-Landau-Verwey-Overbeek (DLVO) interaction energies. Then, the columns were flushed with NaCl solutions with different ionic strengths (i.e., 0.001, 0.01, 0.1 and 0.2 M). Detachments were observed at all ionic strengths and were particularly significant for the nanoparticle. The detachments increased with increasing electrolyte concentration for the nanoparticle whereas increased from 0.001 M to 0.01 M and decreased with further increasing electrolyte concentration for the micro-sized colloid. The observations were attributed to coupled influence of cation exchange, short-range repulsion, surface roughness, surface charge heterogeneity, and deposition in the secondary minima. The detachments of colloids from primary minima challenge the common belief that colloid interaction in primary minimum is irreversible and resistant to disturbance in solution ionic strength and composition. Although the significance of surface roughness, surface charge heterogeneity, and secondary minima on colloid deposition has been widely recognized, our study implies that they also play important roles in colloid detachment. Whereas colloid detachment is frequently associated with decrease of ionic strength, our results show that increase of ionic strength can also cause detachment due to influence of cation exchange. Copyright © 2012 Elsevier B.V. All rights reserved.

Determination of phenylenediamine isomers in hair dyes by coal cinders micro-column extraction and MEKC.

PubMed

Wu, Yiwei; Jiang, Feng; Chen, Lin; Zheng, Jing; Deng, Zhenli; Tao, Qing; Zhang, Jing; Han, Lijuan; Wei, Xiaoshu; Yu, Aimin; Zhang, Haili

2011-06-01

A new micellar electrokinetic chromatography (MEKC) method using beta-cyclodextrins (β-CDs) and 1-butyl-3-methylimidazolium hexafluorophosphates (ionic liquids) as additives was successfully developed for determination of para-, meta-, and ortho-phenylenediamines isomers (p-P, m-P, and o-P) in hair dyes. To improve the sensitivity of the MEKC-UV, a simple and cheap flow injection (FI) technique using a micro-column packed with coal cinders (the by-products from combustion in a boiler) as solid-phase extractant was also investigated. In the presence of 20 mmol L(-1) phosphates at pH 5.5, addition of 12 mmol L(-1) ionic liquids and 8 mmol L(-1) β-CDs greatly improved the separation efficiency. The three analytes could be quantitatively adsorbed by coal cinders, and desorbed readily with 0.15 mL of 0.01 mol L(-1) NaOH. Under the optimum conditions, an enrichment factor (EF) of 33.3 was obtained, and determination limits of p-P, m-P, and o-P were 1.97 × 10(-7), 0.99 × 10(-7), and 0.61 × 10(-7) mol L(-1), respectively. The adsorption capacities of the coal cinders micro-column for p-P, m-P, and o-P were all 1.20 mg g(-1). The presented procedure was successfully applied to the determination of p-P, m-P, and o-P in hair dyes with satisfactory results.

Method for packing chromatographic beds

DOEpatents

Freeman, David H.; Angeles, Rosalie M.; Keller, Suzanne

1991-01-01

Column chromatography beds are packed through the application of static force. A slurry of the chromatography bed material and a non-viscous liquid is filled into the column plugged at one end, and allowed to settle. The column is transferred to a centrifuge, and centrifuged for a brief period of time to achieve a predetermined packing level, at a range generally of 100-5,000 gravities. Thereafter, the plug is removed, other fixtures may be secured, and the liquid is allowed to flow out through the bed. This results in an evenly packed bed, with no channeling or preferential flow characteristics.

Mobility of multiwalled carbon nanotubes in porous media.

PubMed

Liu, Xueying; O'Carroll, Denis M; Petersen, Elijah J; Huang, Qingguo; Anderson, C Lindsay

2009-11-01

Engineered multiwalled carbon nanotubes (MWCNTs) are the subject of intense research and are expected to gain widespread usage in a broad variety of commercial products. However, concerns have been raised regarding potential environmental and human health risks. The mobility of MWCNTs in porous media is examined in this study using one-dimensional flow-through column experiments under conditions representative of subsurface and drinking water treatment systems. Results demonstrate that pore water velocity strongly influenced MWCNT transport, with high MWCNT mobility at pore water velocities greater than 4.0 m/d. A numerical simulator, which incorporated a newly developed theoretical collector efficiency relationship for MWCNTs in spherical porous media, was developed to model observed column results. The model, which incorporated traditional colloid filtration theory in conjunction with a site-blocking term, yielded good agreement with observed results in quartz sand-packed column experiments. Experiments were also conducted in glass bead-packed columns with the same mean grain size as the quartz sand-packed columns. MWCNTs were more mobile in the glass bead-packed columns.

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.

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.

Fabrication and investigation of electrochromatographic columns with a simplex configuration.

PubMed

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

2014-07-04

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

Some results of hemosorption columns development and usage in Czechoslovakia.

PubMed

Kálal, J; Tlustáková, M

Hemoperfusion columns packed with active charcoal and a synthetic resin have been manufactured in Czechoslovakia since 1983. In both cases the sorption packings are coated with a layer of poly(2-hydroxyethyl methacrylate). The columns are manufactured in two sizes: for adults (800 ml) and for children (400 ml). The manufacturer is OPS Kolín: the number of columns manufactured so far is 3400.

Development and evaluation of needle trap device geometry and packing methods for automated and manual analysis.

PubMed

Warren, Jamie M; Pawliszyn, Janusz

2011-12-16

For air/headspace analysis, needle trap devices (NTDs) are applicable for sampling a wide range of volatiles such as benzene, alkanes, and semi-volatile particulate bound compounds such as pyrene. This paper describes a new NTD that is simpler to produce and improves performance relative to previous NTD designs. A NTD utilizing a side-hole needle used a modified tip, which removed the need to use epoxy glue to hold sorbent particles inside the NTD. This design also improved the seal between the NTD and narrow neck liner of the GC injector; therefore, improving the desorption efficiency. A new packing method has been developed and evaluated using solvent to pack the device, and is compared to NTDs prepared using the previous vacuum aspiration method. The slurry packing method reduced preparation time and improved reproducibility between NTDs. To evaluate the NTDs, automated headspace extraction was completed using benzene, toluene, ethylbenzene, p-xylene (BTEX), anthracene, and pyrene (PAH). NTD geometries evaluated include: blunt tip with side-hole needle, tapered tip with side-hole needle, slider tip with side-hole, dome tapered tip with side-hole and blunt with no side-hole needle (expanded desorptive flow). Results demonstrate that the tapered and slider tip NTDs performed with improved desorption efficiency. Copyright © 2011 Elsevier B.V. All rights reserved.

The removal of thermo-tolerant coliform bacteria by immobilized waste stabilization pond algae.

PubMed

Pearson, H W; Marcon, A E; Melo, H N

2011-01-01

This study investigated the potential of laboratory- scale columns of immobilized micro-algae to disinfect effluents using thermo-tolerant coliforms (TTC) as a model system. Cells of a Chlorella species isolated from a waste stabilization pond complex in Northeast Brazil were immobilized in calcium alginate, packed into glass columns and incubated in contact with TTC suspensions for up to 24 hours. Five to six log removals of TTC were achieved in 6 hours and 11 log removals in 12 hours contact time. The results were similar under artificial light and shaded sunlight. However little or no TTC removal occurred in the light in columns of alginate beads without immobilized algae present or when the immobilized algae were incubated in the dark suggesting that the presence of both algae and light were necessary for TTC decay. There was a positive correlation between K(b) values for TTC and increasing pH in the effluent from the immobilized algal columns within the range pH 7.2 and 8.9. The potential of immobilized algal technology for wastewater disinfection may warrant further investigation.

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

PubMed Central

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

2008-01-01

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

Separation of transition metals on a poly-iminodiacetic acid grafted polymeric resin column with post-column reaction detection utilising a paired emitter-detector diode system.

PubMed

Barron, Leon; O'Toole, Martina; Diamond, Dermot; Nesterenko, Pavel N; Paull, Brett

2008-12-05

The selectivity, retention and separation of transition metals on a short (2 mm x 50 mm) column packed with a poly-iminodiacetic acid functionalised polymer 10 microm resin (Dionex ProPac IMAC-10) are presented. This stationary phase, typically used for the separation of proteins, is composed of long chain poly-iminodiacetic acid groups grafted to a hydrophilic layer surrounding a 10 microm polymeric bead. Through the use of a combination of a multi-step pH and picolinic acid gradient, the separation of magnesium, iron, cobalt, cadmium, zinc, lead and copper was possible, followed by post-column reaction with 4-(2-pyridylazo) resorcinol (PAR) and absorbance detection at 510 nm using a novel and inexpensive optical detector, comprised of two light emitting diodes with one acting as a light source and the other as a detector. Column efficiency for selective transition metals was in excess of N=10,000, with the baseline separation of seven metal cations in <3 min possible under optimised conditions. Detection limits of between 5 and 81 microg/L were possible based upon a 50 microL injection volume.

High-performance cation-exchange chromatofocusing of proteins.

PubMed

Kang, Xuezhen; Frey, Douglas D

2003-03-28

Chromatofocusing using high-performance cation-exchange column packings, as opposed to the more commonly used anion-exchange column packings, is investigated with regard to the performance achieved and the range of applications possible. Linear or convex gradients in the range from pH 2.6 to 9 were formed using a variety of commercially available column packings that provide a buffering capacity in different pH ranges, and either polyampholytes or simple mixtures having a small number (three or fewer) of buffering species as the elution buffer. The resolutions achieved using cation-exchange or anion-exchange chromatofocusing were in general comparable, although for certain pairs of proteins better resolution could be achieved using one type of packing as compared to the other, evidently due to the way electrostatic charges are distributed on the protein surface. Several chromatofocusing methods were investigated that take advantage of the acid-base properties of commercially available cation-exchange column packings. These include the use of gradients with a composite shape, the use of very low pH ranges, and the use of elution buffers containing a single buffering species. The advantages of chromatofocusing over ion-exchange chromatography using a salt gradient at constant pH were illustrated by employing the former method and a cation-exchange column packing to separate beta-lactoglobulins A and B, which is a separation reported to be impossible using the latter method and a cation-exchange column packing. Trends in the apparent isoelectric points determined using cation- and anion-exchange chromatofocusing were interpreted using applicable theories. Results of this study indicate that cation-exchange chromatofocusing is a useful technique which is complementary to anion-exchange chromatofocusing and isoelectric focusing for separating proteins at both the analytical and preparative scales.

Enantioseparation of racemic aminoglutethimide using asynchronous simulated moving bed chromatography.

PubMed

Lin, Xiaojian; Gong, Rujin; Li, Jiaxu; Li, Ping; Yu, Jianguo; Rodrigues, Alirio E

2016-10-07

The separation of aminoglutethimide enantiomers by the continuous multicolumn chromatographic processes were investigated experimentally and theoretically, where the columns were packed with cellulose tris 3,5-dimethylphenyl-carbamate stationary phase (brand name Chiralcel OD) and mobile phase was a mixture of n-hexane and ethanol with monoethanolamine additive. The continuous enantioseparation processes included a synchronous shifting process (SMB) and an asynchronous shifting process (VARICOL), which allowed reducing the column number (here from six-column SMB to five-column VARICOL process). Transport-dispersive model with the consideration of both intraparticle mass transfer resistance and axial dispersion was adopted to design and optimize the operation conditions for the separation of aminoglutethimide enantiomers by SMB process and VARICOL process. According to the optimized operation conditions, experiments were carried out on VARICOL-Micro unit using five-column VARICOL process with 1/1.5/1.5/1 configuration and six-column SMB process with 1/2/2/1 configuration. Products of R-aminoglutethimide (R-AG) enantiomer and S-aminoglutethimide (S-AG) enantiomer with more than 99.0% purity were obtained continuously from extract stream and raffinate stream, respectively. Furthermore, the experiemntal data obtained from five-column VARICOL process were compared with that from six-column SMB process, the feasibility and efficiency for the separation of guaifenesin enantiomers by VARICOL processes were evaluated. Copyright © 2016 Elsevier B.V. All rights reserved.

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 Versatile, Automatic Chromatographic Column Packing Device

ERIC Educational Resources Information Center

Barry, Eugene F.; And Others

1977-01-01

Describes an inexpensive apparatus for packing liquid and gas chromatographic columns of high efficiency. Consists of stainless steel support struts, an Automat Getriebmotor, and an associated three-pulley system capable of 10, 30, and 300 rpm. (MLH)

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

PubMed

Park, Sin Young; Cheong, Won Jo

2016-05-01

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

Formation and Growth of Micro and Macro Bubbles on Copper-Graphite Composite Surfaces

NASA Technical Reports Server (NTRS)

Chao, David F.; Sankovic, John M.; Motil, Brian J.; Zhang, Nengli

2007-01-01

Micro scale boiling behavior in the vicinity of graphite micro-fiber tips on the coppergraphite composite boiling surfaces is investigated. It is discovered that a large number of micro bubbles are formed first at the micro scratches and cavities on the copper matrix in pool boiling. In virtue of the non-wetting property of graphite, once the growing micro bubbles touch the graphite tips, the micro bubbles are sucked by the tips and merged into larger micro bubbles sitting on the tips. The micro bubbles grow rapidly and coalesce to form macro bubbles, each of which sitting on several tips. The growth processes of the micro and macro bubbles are analyzed and formulated followed by an analysis of bubble departure on the composite surfaces. Based on these analyses, the enhancement mechanism of the pool boiling heat transfer on the composite surfaces is clearly revealed. Experimental results of pool boiling heat transfer both for water and Freon-113 on the composite surfaces convincingly demonstrate the enhancement effects of the unique structure of Cu-Gr composite surfaces on boiling heat transfer.

Imaging and modeling of flow in porous media using clinical nuclear emission tomography systems and computational fluid dynamics

NASA Astrophysics Data System (ADS)

Boutchko, Rostyslav; Rayz, Vitaliy L.; Vandehey, Nicholas T.; O'Neil, James P.; Budinger, Thomas F.; Nico, Peter S.; Druhan, Jennifer L.; Saloner, David A.; Gullberg, Grant T.; Moses, William W.

2012-01-01

This paper presents experimental and modeling aspects of applying nuclear emission tomography to study fluid flow in laboratory packed porous media columns of the type frequently used in geophysics, geochemistry and hydrology research. Positron emission tomography (PET) and single photon emission computed tomography (SPECT) are used as non-invasive tools to obtain dynamic 3D images of radioactive tracer concentrations. Dynamic sequences obtained using 18F-FDG PET are used to trace flow through a 5 cm diameter × 20 cm tall sand packed column with and without an impermeable obstacle. In addition, a custom-made rotating column setup placed in a clinical two-headed SPECT camera is used to image 99mTc-DTPA tracer propagation in a through-flowing column (10 cm diameter × 30 cm tall) packed with recovered aquifer sediments. A computational fluid dynamics software package FLUENT is used to model the observed flow dynamics. Tracer distributions obtained in the simulations in the smaller column uniformly packed with sand and in the column with an obstacle are remarkably similar to the reconstructed images in the PET experiments. SPECT results demonstrate strongly non-uniform flow patterns for the larger column slurry-packed with sub-surface sediment and slow upward flow. In the numerical simulation of the SPECT study, two symmetric channels with increased permeability are prescribed along the column walls, which result in the emergence of two well-defined preferential flow paths. Methods and results of this work provide new opportunities in hydrologic and biogeochemical research. The primary target application for developed technologies is non-destructive, non-perturbing, quantitative imaging of flow dynamics within laboratory scale porous media systems.

Imaging and modeling of flow in porous media using clinical nuclear emission tomography systems and computational fluid dynamics.

PubMed

Boutchko, Rostyslav; Rayz, Vitaliy L; Vandehey, Nicholas T; O'Neil, James P; Budinger, Thomas F; Nico, Peter S; Druhan, Jennifer L; Saloner, David A; Gullberg, Grant T; Moses, William W

2012-01-01

This paper presents experimental and modeling aspects of applying nuclear emission tomography to study fluid flow in laboratory packed porous media columns of the type frequently used in geophysics, geochemistry and hydrology research. Positron emission tomography (PET) and single photon emission computed tomography (SPECT) are used as non-invasive tools to obtain dynamic 3D images of radioactive tracer concentrations. Dynamic sequences obtained using 18 F-FDG PET are used to trace flow through a 5 cm diameter × 20 cm tall sand packed column with and without an impermeable obstacle. In addition, a custom-made rotating column setup placed in a clinical two-headed SPECT camera is used to image 99m Tc-DTPA tracer propagation in a through-flowing column (10 cm diameter × 30 cm tall) packed with recovered aquifer sediments. A computational fluid dynamics software package FLUENT is used to model the observed flow dynamics. Tracer distributions obtained in the simulations in the smaller column uniformly packed with sand and in the column with an obstacle are remarkably similar to the reconstructed images in the PET experiments. SPECT results demonstrate strongly non-uniform flow patterns for the larger column slurry-packed with sub-surface sediment and slow upward flow. In the numerical simulation of the SPECT study, two symmetric channels with increased permeability are prescribed along the column walls, which result in the emergence of two well-defined preferential flow paths. Methods and results of this work provide new opportunities in hydrologic and biogeochemical research. The primary target application for developed technologies is non-destructive, non-perturbing, quantitative imaging of flow dynamics within laboratory scale porous media systems.

Comparative study of new shell-type, sub-2 micron fully porous and monolith stationary phases, focusing on mass-transfer resistance.

PubMed

Oláh, Erzsébet; Fekete, Szabolcs; Fekete, Jeno; Ganzler, Katalin

2010-06-04

Today sub-2 microm packed columns are very popular to conduct fast chromatographic separations. The mass-transfer resistance depends on the particle size but some practical limits exist not to reach the theoretically expected plate height and mass-transfer resistance. Another approach applies particles with shortened diffusion path to enhance the efficiency of separations. In this study a systematical evaluation of the possibilities of the separations obtained with 5 cm long narrow bore columns packed with new 2.6 microm shell particles (1.9 microm nonporous core surrounded by a 0.35 microm porous shell, Kinetex, Core-Shell), packed with other shell-type particles (Ascentis Express, Fused-Core), totally porous sub-2 microm particles and a 5 cm long narrow bore monolith column is presented. The different commercially available columns were compared by using van Deemter, Knox and kinetic plots. Theoretical Poppe plots were constructed for each column to compare their kinetic performance. Data are presented on polar neutral real-life analytes. Comparison of a low molecular weight compounds (MW=270-430) and a high molecular weight one (MW approximately 900) was conducted. This study proves that the Kinetex column packed with 2.6 microm shell particles is worthy of rivaling to sub-2 microm columns and other commercially available shell-type packings (Ascentis Express or Halo), both for small and large molecule separation. The Kinetex column offers a very flat C term. Utilizing this feature, high flow rates can be applied to accomplish very fast separations without significant loss in efficiency. Copyright 2010 Elsevier B.V. All rights reserved.

Adsorption of hexavalent chromium from synthetic and electroplating effluent on chemically modified Swietenia mahagoni shell in a packed bed column.

PubMed

Rangabhashiyam, S; Nandagopal, M S Giri; Nakkeeran, E; Selvaraju, N

2016-07-01

Packed bed column studies were carried out to evaluate the performance of chemically modified adsorbents for the sequestration of hexavalent chromium from synthetic and electroplating industrial effluent. The effects of parameters such as bed height (3-9 cm), inlet flow rate (5-15 mL/min), and influent Cr(VI) concentration (50-200 mg/L) on the percentage removal of Cr(VI) and the adsorption capacity of the adsorbents in a packed bed column were investigated. The breakthrough time increased with increasing bed height and decreased with the increase of inlet flow rate and influent Cr(VI) concentration. The adsorption column models such as Thomas, Adams-Bohart, Yoon-Nelson, and bed depth service time (BDST) were successfully correlated with the experimental data. The Yoon-Nelson and BDST model showed good agreement with the experimental data for all the studied parameter conditions. Results of the present study indicated that the chemically modified Swietenia mahagoni shell can be used as an adsorbent for the removal of Cr(VI) from industrial wastewater in a packed bed column.

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

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.

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

PubMed

Broeckhoven, Ken; Desmet, Gert

2007-11-16

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

Fast gradient screening of pharmaceuticals with 5 cm long, narrow bore reversed-phase columns packed with sub-3 μm core-shell and sub-2 μm totally porous particles.

PubMed

Fekete, Szabolcs; Fekete, Jeno

2011-04-15

The performance of 5 cm long narrow-bore columns packed with 2.6-2.7 μm core-shell particles and a column packed with 1.7 μm totally porous particles was compared in very fast gradient separations of polar neutral active pharmaceutical compounds. Peak capacities as a function of flow-rate and gradient time were measured. Peak capacities around 160-170 could be achieved within 25 min with these 5 cm long columns. The highest peak capacity was obtained with the Kinetex column however it was found that as the flow-rate increases, the peak capacity of the new Poroshell-120 column is getting closer to that obtained with the Kinetex column. Considering the column permeability, peak capacity per unit time and per unit pressure was also calculated. In this comparison the advantage of sub-3 μm core-shell particles is more significant compared to sub-2 μm totally porous particles. Moreover it was found that the very similar sized (d(p)=2.7 μm) and structured (ρ=0.63) new Poroshell-120 and the earlier introduced Ascentis Express particles showed different efficiency. Results obtained showed that the 5 cm long narrow bore columns packed with sub-3 μm core-shell particles offer the chance of very fast and efficient gradient separations, thus these columns can be applied for fast screening measurements of routine pharmaceutical analysis such as cleaning validation. Copyright © 2011 Elsevier B.V. All rights reserved.

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.

Effect of chemical and physical heterogeneities on colloid-facilitated cesium transport

NASA Astrophysics Data System (ADS)

Rod, Kenton; Um, Wooyong; Chun, Jaehun; Wu, Ning; Yin, Xialong; Wang, Guohui; Neeves, Keith

2018-06-01

A set of column experiments was conducted to investigate the chemical and physical heterogeneity effect on colloid facilitated transport under slow pore velocity conditions. Pore velocities were kept below 100 cm d-1 for all experiments. Glass beads were packed into columns establishing four different conditions: 1) homogeneous, 2) mixed physical heterogeneity, 3) sequentially layered physical heterogeneity, and 4) chemical heterogeneity. The homogeneous column was packed with glass beads (diameter 500-600 μm), and physical heterogeneities were created by sequential layering or mixing two sizes of glass bead (500-600 μm and 300-400 μm). A chemical heterogeneity was created using 25% of the glass beads coated with hydrophobic molecules (1H-1H-2H-2H-perfluorooctyltrichlorosilane) mixed with 75% pristine glass beads (all 500-600 μm). Input solution with 0.5 mM CsI and 50 mg L-1 colloids (1-μm diameter SiO2) was pulsed into columns under saturated conditions. The physical heterogeneity in the packed glass beads retarded the transport of colloids compared to homogeneous (R = 25.0), but showed only slight differences between sequentially layered (R = 60.7) and mixed heterogeneity(R = 62.4). The column with the chemical, hydrophobic/hydrophilic, heterogeneity removed most of the colloids from the input solution. All column conditions stripped Cs from colloids onto the column matrix of packed glass beads.

Determination of dextromethorphan in human plasma using pipette tip solid-phase extraction and gas chromatography-mass spectrometry.

PubMed

Hasegawa, Chika; Kumazawa, Takeshi; Uchigasaki, Seisaku; Lee, Xiao-Pen; Sato, Keizo; Terada, Masaru; Kurosaki, Kunihiko

2011-10-01

Dextromethorphan was extracted from human plasma samples (100 μL) using MonoTip C(18) tips, which are packed with C(18)-bonded monolithic silica gel that is attached to the inside of the tip. The samples, which contained dextromethorphan and trimeprazine as an internal standard (IS), were mixed with 200 μL of distilled water and 50 μL of 1 mol/L glycine-sodium hydroxide buffer (pH 10). The mixture was extracted to the C(18) phase of the tip by 20 sequential aspirating/dispensing cycles using a manual micropipettor. The analytes retained on the C(18) phase were then eluted with methanol by five sequential aspirating/dispensing cycles. The eluate was injected directly into a gas chromatograph and detected by a mass spectrometer with selected ion monitoring in positive electron ionization mode. An Equity-5 fused silica capillary column (30 m × 0.32 mm i.d., film thickness 0.5 μm) gave adequate separation of the dextromethorphan, IS, and impurities. The recoveries of dextromethorphan and the IS spiked into plasma were >87.4%. The regression equation for dextromethorphan showed excellent linearity from 2.5 to 320 ng/mL of plasma, and the limit of detection was 1.25 ng/mL of plasma. The intraday and interday coefficients of variation were less than 10.5% and 14.7%, respectively. The accuracy ranged from 91.9% to 107%. The validated method was successfully used to quantify the plasma concentration of dextromethorphan in a human subject after oral administration of the drug. © Springer-Verlag 2011

Physical reconstruction of packed beds and their morphological analysis: core-shell packings as an example.

PubMed

Bruns, Stefan; Tallarek, Ulrich

2011-04-08

We report a fast, nondestructive, and quantitative approach to characterize the morphology of packed beds of fine particles by their three-dimensional reconstruction from confocal laser scanning microscopy images, exemplarily shown for a 100μm i.d. fused-silica capillary packed with 2.6μm-sized core-shell particles. The presented method is generally applicable to silica-based capillary columns, monolithic or particulate, and comprises column pretreatment, image acquisition, image processing, and statistical analysis of the image data. It defines a unique platform for fundamental comparisons of particulate and monolithic supports using the statistical measures derived from their reconstructions. Received morphological data are column cross-sectional porosity profiles and chord length distributions from the interparticle macropore space, which are a descriptor of local density and can be characterized by a simplified k-gamma distribution. This distribution function provides a parameter of location and a parameter of dispersion which can be correlated to individual chromatographic band broadening processes (i.e., to transchannel and short-range interchannel contributions to eddy dispersion, respectively). Together with the transcolumn porosity profile the presented approach allows to analyze and quantify the packing microstructure from pore to column scale and therefore holds great promise in a comparative study of packing conditions and particle properties, particularly for characterizing and minimizing the packing process-specific heterogeneities in the final bed structure. Copyright © 2011 Elsevier B.V. All rights reserved.

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

NASA Astrophysics Data System (ADS)

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

2013-12-01

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

Leaching of the organophosphorus nematicide fosthiazate.

PubMed

Karpouzas, Dimitrios G; Pantelelis, Ioannis; Menkissoglu-Spiroudi, Urania; Golia, Evangelia; Tsiropoulos, Nikolas G

2007-07-01

Fosthiazate is an organophosphorus nematicide which was recently included in Annex I of the Directive 91/414/EEC under the clause that it should be used with special care in soils vulnerable to leaching. Thus, the leaching of fosthiazate was investigated in columns packed with three different soils which represented situations of high (site 2), intermediate (site 1) and low (site 3) leaching potential. The recommended dose of fosthiazate was applied at the surface of the soil columns and fosthiazate fate and transport was investigated for the next two months. Fosthiazate concentrations in the leachate collected from the bottom of the columns packed with soil from site 2 exceeded 0.1 microgl(-1) in most cases. This soil was characterized as acidic, indicating longer fosthiazate persistence, with low organic matter content, indicating weak adsorption, thus representing a situation vulnerable to leaching. In contrast, the lowest concentrations of fosthiazate in the leachate were evident in the columns packed with soil from site 3. This soil was characterized as alkaline, indicating faster degradation, with higher organic matter content, indicating stronger adsorption, thus representing a situation not favoring leaching of fosthiazate. The highest concentration of fosthiazate in the leachate from the columns packed with soil from site 2 was 3.44 microgl(-1) compared to 1.17 and 0.16 microgl(-1), which were the corresponding maximum values measured in columns packed with soil from sites 1 and 3, respectively. The results of the current study further suggest that fosthiazate is mobile in soil and can leach under conducive soil conditions like acidic soils with low organic matter content.

Effect of chemical and physical heterogeneities on colloid-facilitated cesium transport

DOE PAGES

Rod, Kenton; Um, Wooyong; Chun, Jaehun; ...

2018-03-31

A set of column experiments was conducted to investigate the chemical and physical heterogeneity effect on colloid facilitated transport under slow pore velocity conditions. Pore velocities were kept below 100 cm d -1 for all experiments. Glass beads were packed into columns establishing four different conditions: 1) homogeneous, 2) mixed physical heterogeneity, 3) sequentially layered physical heterogeneity, and 4) chemical heterogeneity. The homogeneous column was packed with glass beads (diameter 500–600 μm), and physical heterogeneities were created by sequential layering or mixing two sizes of glass bead (500–600 μm and 300–400 μm). A chemical heterogeneity was created using 25% ofmore » the glass beads coated with hydrophobic molecules (1H-1H-2H-2H-perfluorooctyltrichlorosilane) mixed with 75% pristine glass beads (all 500–600 μm). Input solution with 0.5 mM CsI and 50 mg L -1 colloids (1-μm diameter SiO 2) was pulsed into columns under saturated conditions. The physical heterogeneity in the packed glass beads retarded the transport of colloids compared to homogeneous (R = 25.0), but showed only slight differences between sequentially layered (R = 60.7) and mixed heterogeneity(R = 62.4). The column with the chemical, hydrophobic/hydrophilic, heterogeneity removed most of the colloids from the input solution. All column conditions stripped Cs from colloids onto the column matrix of packed glass beads.« less

Effect of chemical and physical heterogeneities on colloid-facilitated cesium transport

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

Rod, Kenton; Um, Wooyong; Chun, Jaehun

A set of column experiments was conducted to investigate the chemical and physical heterogeneity effect on colloid facilitated transport under slow pore velocity conditions. Pore velocities were kept below 100 cm d -1 for all experiments. Glass beads were packed into columns establishing four different conditions: 1) homogeneous, 2) mixed physical heterogeneity, 3) sequentially layered physical heterogeneity, and 4) chemical heterogeneity. The homogeneous column was packed with glass beads (diameter 500–600 μm), and physical heterogeneities were created by sequential layering or mixing two sizes of glass bead (500–600 μm and 300–400 μm). A chemical heterogeneity was created using 25% ofmore » the glass beads coated with hydrophobic molecules (1H-1H-2H-2H-perfluorooctyltrichlorosilane) mixed with 75% pristine glass beads (all 500–600 μm). Input solution with 0.5 mM CsI and 50 mg L -1 colloids (1-μm diameter SiO 2) was pulsed into columns under saturated conditions. The physical heterogeneity in the packed glass beads retarded the transport of colloids compared to homogeneous (R = 25.0), but showed only slight differences between sequentially layered (R = 60.7) and mixed heterogeneity(R = 62.4). The column with the chemical, hydrophobic/hydrophilic, heterogeneity removed most of the colloids from the input solution. All column conditions stripped Cs from colloids onto the column matrix of packed glass beads.« less

Bubble Departure from Metal-Graphite Composite Surfaces and Its Effects on Pool Boiling Heat Transfer

NASA Technical Reports Server (NTRS)

Chao, David F.; Sankovic, John M.; Motil, Brian J.; Yang, W-J.; Zhang, Nengli

2010-01-01

The formation and growth processes of a bubble in the vicinity of graphite micro-fiber tips on metal-graphite composite boiling surfaces and their effects on boiling behavior are investigated. It is discovered that a large number of micro bubbles are formed first at the micro scratches and cavities on the metal matrix in pool boiling. By virtue of the non-wetting property of graphite, once the growing micro bubbles touch the graphite tips, the micro bubbles are sucked by the tips and merged into larger micro bubbles sitting on the end of the tips. The micro bubbles grow rapidly and coalesce to form macro bubbles, each spanning several tips. The necking process of a detaching macro bubble is analyzed. It is revealed that a liquid jet is produced by sudden break-off of the bubble throat. The composite surfaces not only have higher temperatures in micro- and macrolayers but also make higher frequency of the bubble departure, which increase the average heat fluxes in both the bubble growth stage and in the bubble departure period. Based on these analyses, the enhancement mechanism of pool boiling heat transfer on composite surfaces is clearly revealed.

Biomass growth restriction in a packed bed reactor

DOEpatents

Griffith, William L.; Compere, Alicia L.

1978-01-01

When carrying out continuous biologically catalyzed reactions with anaerobic microorganisms attached to a support in an upflow packed bed column, growth of the microorganisms is restricted to prevent the microorganisms from plugging the column by limiting the availability of an essential nutrient and/or by the presence of predatory protozoa which consume the anaerobic microorganisms. A membrane disruptive detergent may be provided in the column to lyse dead microorganisms to make them available as nutrients for live microorganisms.

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

PubMed

Gritti, Fabrice; Omamogho, Jesse; Guiochon, Georges

2011-10-07

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

Packed-bed column biosorption of chromium(VI) and nickel(II) onto Fenton modified Hydrilla verticillata dried biomass.

PubMed

Mishra, Ashutosh; Tripathi, Brahma Dutt; Rai, Ashwani Kumar

2016-10-01

The present study represents the first attempt to investigate the biosorption potential of Fenton modified Hydrilla verticillata dried biomass (FMB) in removing chromium(VI) and nickel(II) ions from wastewater using up-flow packed-bed column reactor. Effects of different packed-bed column parameters such as bed height, flow rate, influent metal ion concentration and particle size were examined. The outcome of the column experiments illustrated that highest bed height (25cm); lowest flow rate (10mLmin(-1)), lowest influent metal concentration (5mgL(-1)) and smallest particle size range (0.25-0.50mm) are favourable for biosorption. The maximum biosorption capacity of FMB for chromium(VI) and nickel(II) removal were estimated to be 89.32 and 87.18mgg(-1) respectively. The breakthrough curves were analyzed using Bed Depth Service Time (BDST) and Thomas models. The experimental results obtained agree to both the models. Column regeneration experiments were also carried out using 0.1M HNO3. Results revealed good reusability of FMB during ten cycles of sorption and desorption. Performance of FMB-packed column in treating secondary effluent was also tested under identical experimental conditions. Results demonstrated significant reduction in chromium(VI) and nickel(II) ions concentration after the biosorption process. Copyright © 2016 Elsevier Inc. All rights reserved.

Spindt cold cathode electron gun development program

NASA Technical Reports Server (NTRS)

Spindt, C. A.

1983-01-01

A thin film field emission cathode array and an electron gun based on this emitter array are summarized. Fabricating state of the art cathodes for testing at NASA and NRL, advancing the fabrication technology, developing wedge shaped emitters, and performing emission tests are covered. An anistropic dry etching process (reactive ion beam etching) developed that leads to increasing the packing density of the emitter tips to about 5 x 10 to the 6th power/square cm. Tests with small arrays of emitter tips having about 10 tips has demonstrated current densities of over 100 A/sq cm. Several times using cathodes having a packing density of 1.25 x 10 to the 6th power tips/sq cm. Indications are that the higher packing density achievable with the dry etch process may extend this capability to the 500 A/sq cm range and beyond. The wedge emitter geometry was developed and shown to produce emission. This geometry can (in principle) extend the current density capability of the cathodes beyond the 500 A/sq cm level. An emission microscope was built and tested for use with the cathodes.

7 CFR 923.322 - Washington cherry handling regulation.

Code of Federal Regulations, 2010 CFR

2010-01-01

... solids as determined from a composite sample by refractometer prior to packing, at time of packing, or at.../row size designation the row count/row size marked shall be one of those shown in Column 1 of the... corresponding diameter shown in Column 2 of such table: Provided, That the content of individual containers in...

Heavy metal adsorption changes of EAF steel slag after phosphorus adsorption.

PubMed

Song, Guanling; Cao, Lijing; Chen, Xiao; Hou, Wenhua; Wang, Qunhui

2012-01-01

A kind of electric arc furnace (EAF) steel slag was phosphated, and its isothermal and dynamic adsorptions of copper, cadmium, and lead ions were measured to determine if heavy metal adsorption changes after phosphorus adsorption. The surface area increased greatly after the slag was phosphated. Isothermal adsorption experiments showed that the theoretical Q(max) of the EAF steel slag on Cu(2+), Cd(2+), and Pb(2+) improved 59, 50, and 89% respectively after it was phosphated. Dynamic adsorption results showed that the greatest adsorption capacities of unit volume of Cu(2+), Cd(2+), and Pb(2+) were 2.2, 1.8, and 1.8 times that of the column packed with original EAF steel slag when the column was packed with phosphate EAF steel slag at the same heavy metal ion concentration. The breakthrough time, the exhaustion time and elution efficiency of the column also increased when the column was packed with phosphated EAF steel slag compared with that packed with original EAF steel slag. Phosphorus adsorption could further improve the heavy metal ion adsorption of the EAF steel slag.

Separation of polyethylene glycols and amino-terminated polyethylene glycols by high-performance liquid chromatography under near critical conditions.

PubMed

Wei, Y-Z; Zhuo, R-X; Jiang, X-L

2016-05-20

The separation and characterization of polyethylene glycols (PEGs) and amino-substituted derivatives on common silica-based reversed-phase packing columns using isocratic elution is described. This separation is achieved by liquid chromatography under the near critical conditions (LCCC), based on the number of amino functional end groups without obvious effect of molar mass for PEGs. The mobile phase is acetonitrile in water with an optimal ammonium acetate buffer. The separation mechanism of PEG and amino-substituted PEG under the near LCCC on silica-based packing columns is confirmed to be ion-exchange interaction. Under the LCCC of PEG backbone, with fine tune of buffer concentration, the retention factor ratios for benzylamine and phenol in buffered mobile phases, α(benzylamine/phenol)-values, were used to assess the ion-exchange capacity on silica-based reversed-phase packing columns. To the best of our knowledge, this is the first report on separation of amino-functional PEGs independent of the molar mass by isocratic elution using common C18 or phenyl reversed-phase packing columns. Copyright © 2016 Elsevier B.V. All rights reserved.

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

PubMed

Gritti, Fabrice; Guiochon, Georges

2012-08-24

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

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

Unit operations for gas-liquid mass transfer in reduced gravity environments

NASA Technical Reports Server (NTRS)

Pettit, Donald R.; Allen, David T.

1992-01-01

Basic scaling rules are derived for converting Earth-based designs of mass transfer equipment into designs for a reduced gravity environment. Three types of gas-liquid mass transfer operations are considered: bubble columns, spray towers, and packed columns. Application of the scaling rules reveals that the height of a bubble column in lunar- and Mars-based operations would be lower than terrestrial designs by factors of 0.64 and 0.79 respectively. The reduced gravity columns would have greater cross-sectional areas, however, by factors of 2.4 and 1.6 for lunar and Martian settings. Similar results were obtained for spray towers. In contract, packed column height was found to be nearly independent of gravity.

SU-E-J-81: Beveled Needle Tip Detection Error in Ultrasound-Guided Prostate Brachytherapy.

PubMed

Leu, S; Ruiz, B; Podder, T

2012-06-01

To quantify the needle tip detection errors in ultrasound images due to bevel-tip orientation in relation to the location on template grid. Transrectal ultrasound (TRUS) system (BK Medical) with physical template grid and 18-gauge bevel-tip (20-deg beveled angle) brachytherapy needle (Bard Medical, Covington, GA) were used. The TRUS was set at 6.5MHz in water phantom at 40°C and measurements were taken with 50% and 100% TRUS gains. Needles were oriented with bevel-tip facing up (0-degree) and inserted through template grid-holes. Reference needle depths were measured when needle tip image intensity was bright enough for potentially consistent readings. High-resolution digital vernier caliper was used to measure needle depth. Needle bevel-tip orientation was then changed to bevel down (by rotating 180-degree) and needle depth was adjusted by retracting so that the needle-tip image intensity appeared similar to when the needle bevel-tip was at 0-degree orientation. Clinically relevant locations were considered for needle placement on the template grids (1st row to 9th row, and 'a-f' columns). For 50% TRUS gain, bevel tip detection errors/differences were 0.69±0.30mm (1st row) to 3.23±0.22mm (9th row) and 0.78±0.71mm (1st row) to 4.14±0.56mm (9th row) in columns 'a' and 'D', respectively. The corresponding errors for 100% TRUS gain were 0.57±0.25mm to 5.24±0.36mm and 0.84±0.30mm to 4.2±0.20mm in columns 'a' and 'D', respectively. These errors/differences varied linearly for grid-hole locations on the rows and columns in between, smaller to large depending on distance from the TRUS probe. Observed no effect of gains (50% vs. 100%) along 'D' column, which was directly above the TRUS probe. Experiment results revealed that the beveled needle tip orientation could significantly impact the detection accuracy of the needle tips, based on which the seeds might be delivered. These errors may lead to considerable dosimetric deviations in prostate brachytherapy seed implantation. © 2012 American Association of Physicists in Medicine.

Fundamental Studies on Two-Phase Gas-Liquid Flows Through Packed Beds in Microgravity

NASA Technical Reports Server (NTRS)

Balakotaiah, Vemuri; McCready, Mark J.; Motil, Brian J.

2002-01-01

In the typical operation of a packed-bed reactor, gas and liquid flow simultaneously through a fixed bed of solid particles. Depending on the application, the particles can be of various shapes and sizes and provide for intimate contact and high rates of transport between the phases needed to sustain chemical or biological reactions. The packing may also serve as either a catalyst or as a support for growing biological material. NASA has flown two of these packed-bed systems in a microgravity environment with limited or no success. The goal of this research is to develop models (with scale-up capability) needed for the design of the physicochemical equipment to carry out these unit operations in microgravity. New insight will also lead to improvements in normal gravity operations. Our initial experiment was flown using an existing KC-135 two-phase flow rig with a modified test section. The test section is a clear polycarbonate rectangular column with a depth of 2.54 cm, a width of 5.08 cm, and 60 cm long. The column was randomly packed with spherical glass beads by slowly dropping the beads into the bed. Even though care was taken in handling the column after it was filled with packing, the alternating high and low gravity cycles with each parabola created a slightly tighter packed bed than is typically reported for this type. By the usual method of comparing the weight difference of a completely dry column versus a column filled with water, the void fraction was found to be .345 for both sizes of beads used. Five flush mounted differential pressure transducers are spaced at even intervals with the first location 4 cm from the inlet port and the subsequent pressure transducers spaced at 13 cm intervals along the column. Differential pressure data was acquired at 1000 Hz to adequately observe pulse formation and characteristics. Visual images of the flow were recorded using a high-speed SVHS system at 500 frames per second. Over 250 different test conditions were evaluated along with a companion set of tests in normal gravity. The flow rates, fluid properties and packing properties were selected to provide a range of several orders-of-magnitude for the important dimensionless parameters. Additional information is included in the original extended abstract.

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

PubMed

Frank, H; Senf, L; Welsch, T

1990-12-01

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

7 CFR 923.322 - Washington cherry handling regulation.

Code of Federal Regulations, 2011 CFR

2011-01-01

... solids as determined from a composite sample by refractometer prior to packing, at time of packing, or at... designation the row count/row size marked shall be one of those shown in Column 1 of the following table and... diameter shown in Column 2 of such table: Provided, That the content of individual containers in the lot...

7 CFR 923.322 - Washington cherry handling regulation.

Code of Federal Regulations, 2012 CFR

2012-01-01

... solids as determined from a composite sample by refractometer prior to packing, at time of packing, or at... designation the row count/row size marked shall be one of those shown in Column 1 of the following table and... diameter shown in Column 2 of such table: Provided, That the content of individual containers in the lot...

7 CFR 923.322 - Washington cherry handling regulation.

Code of Federal Regulations, 2014 CFR

2014-01-01

... solids as determined from a composite sample by refractometer prior to packing, at time of packing, or at... designation the row count/row size marked shall be one of those shown in Column 1 of the following table and... diameter shown in Column 2 of such table: Provided, That the content of individual containers in the lot...

7 CFR 923.322 - Washington cherry handling regulation.

Code of Federal Regulations, 2013 CFR

2013-01-01

... solids as determined from a composite sample by refractometer prior to packing, at time of packing, or at... designation the row count/row size marked shall be one of those shown in Column 1 of the following table and... diameter shown in Column 2 of such table: Provided, That the content of individual containers in the lot...

Adsorption of polypropylene from dilute solutions on a zeolite column packing.

PubMed

Macko, Tibor; Pasch, Harald; Denayer, Joeri F

2005-01-01

Faujasite type zeolite CBV-780 was tested as adsorbent for isotactic polypropylene by liquid chromatography. When cyclohexane, cyclohexanol, n-decanol, n-dodecanol, diphenylmethane, or methylcyclohexane was used as mobile phase, polypropylene was fully or partially retained within the column packing. This is the first series of sorbent-solvent systems to show a pronounced retention of isotactic polypropylene. According to the hydrodynamic volumes of polypropylene in solution, macromolecules of polypropylene should be fully excluded from the pore volume of the sorbent. Sizes of polypropylene macromolecules in linear conformations, however, correlate with the pore size of the column packing used. It is presumed that the polypropylene chains partially penetrate into the pores and are retained due to the high adsorption potential in the narrow pores.

Evaluation of columns packed with shell particles with compounds of pharmaceutical interest.

PubMed

Ruta, Joséphine; Zurlino, Daria; Grivel, Candice; Heinisch, Sabine; Veuthey, Jean-Luc; Guillarme, Davy

2012-03-09

The commercial C18 columns packed with sub-3 μm shell particles were tested and compared to a reference UHPLC column, in terms of kinetic performance as well as selectivity, retention capability, peak shape and loading capacity. For this purpose, a set of pharmaceutically relevant molecules was selected, including acidic, neutral and basic drugs. Regarding kinetic performance, h(opt) values for the shell particles were found between 1.7 and 2, while the UHPLC column provided a value of approximately 2.5. However, this impressive performance should be considered with caution, particularly for the construction of kinetic plots since h(opt) values were sometimes related to the column dimensions, depending on the provider (h(opt) comprised between 1.8 and 2.6 for longer columns of 150 mm packed with shell particles). Despite the non-porous inner core of the shell particles representing between 25 and 36% of the particle, we demonstrated that the decrease in retention was on the maximum equal to 15% for Ascentis column while Acquity and Poroshell were strictly equivalent in terms of retention. Concerning loading capacity, it remains comparable to that of fully porous sub-2 μm particles and always more pronounced with 0.1% formic acid vs. phosphate buffer. The loading capacity of the different columns was found to be better correlated to the pore volume or surface coverage than the shell thickness. Experimentally, the most pronounced overloading was observed with the Poroshell. Finally, the selectivity and peak shape were evaluated using a mixture of basic and acidic drugs. It appears that results were very similar between sub-3 μm shell particles and fully porous sub-2-μm particles for our mixture of compounds, showing the ability to transfer existing methods to shell particles, with only limited adjustments. This study confirms the potential of columns packed with shell particles and demonstrates the interest of such column technology with pharmaceutical compounds. Copyright © 2011 Elsevier B.V. All rights reserved.

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

PubMed

Gritti, Fabrice; Guiochon, Georges

2012-08-24

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

A novel technique for micro-hole forming on skull with the assistance of ultrasonic vibration.

PubMed

Li, Zhe; Yang, Daoguo; Hao, Weidong; Wu, Tiecheng; Wu, Song; Li, Xiaoping

2016-04-01

Micro-hole opening on skull is technically challenging and is hard to realize by micro-drilling. Low-stiffness of the drill bit is a serious drawback in micro-drilling. To deal with this problem, a novel ultrasonic vibration assisted micro-hole forming technique has been developed. Tip geometry and vibration amplitude are two key factors affecting the performance of this hole forming technique. To investigate their effects, experiment was carried out with 300μm diameter tools of three different tip geometries at three different vibration amplitudes. Hole forming performance was evaluated by the required thrust force, dimensional accuracy, exit burr and micro-structure of bone tissue around the generated hole. Based on the findings from current study, the 60° conically tipped tool helps generate a micro-hole of better quality at a smaller thrust force, and it is more suitable for hole forming than the 120° conically tipped tool and the blunt tipped tool. As for the vibration amplitude, when a larger amplitude is used, a micro-hole of better quality and higher dimensional accuracy can be formed at a smaller thrust force. Findings from this study would lay a technical foundation for accurately generating a high-quality micro-hole on skull, which enables minimally invasive insertion of a microelectrode into brain for neural activity measuring. Copyright © 2015 Elsevier Ltd. All rights reserved.

Fully automated method for the liquid chromatographic determination of cyproterone acetate in plasma using restricted access material for sample pre-treatment.

PubMed

Christiaens, B; Chiap, P; Rbeida, O; Cello, D; Crommen, J; Hubert, Ph

2003-09-25

A new fully automated method for the quantitative analysis of an antiandrogenic substance, cyproterone acetate (CPA), in plasma samples has been developed using on-line solid-phase extraction (SPE) prior to the determination by reversed-phase liquid chromatography (LC). The automated method was based on the use of a precolumn packed with an internal-surface reversed-phase packing material (LiChrospher RP-4 ADS) for sample clean-up coupled to LC analysis on an octadecyl stationary phase using a column-switching system. A 200-microL volume of plasma sample was injected directly on the precolumn packed with restricted access material using a mixture of water-acetonitrile (90:10, v/v) as washing liquid. The analyte was then eluted in the back-flush mode with the LC mobile phase which consisted of a mixture of phosphate buffer, pH 7.0-acetonitrile (54:46, v/v). The elution profiles of CPA and blank plasma samples on the precolumn and the time needed for analyte transfer from the precolumn to the analytical column were determined. Different compositions of washing liquid and mobile phase were tested to reduce the interference of plasma endogenous components. UV detection was achieved at 280 nm. Finally, the developed method was validated using a new approach, namely the application of the accuracy profile based on the interval confidence at 90% of the total measurement error (bias+standard deviation). The limit of quantification of cyproterone acetate in plasma was determined at 15 ng mL(-1). The validated method should be applicable to the determination of CPA in patients treated by at least 50 mg day(-1).

Aspects of High-Resolution Gas Chromatography as Applied to the Analysis of Hydrocarbon Fuels and Other Complex Organic Mixtures. Volume 2. Survey of Sample Insertion Techniques.

DTIC Science & Technology

1985-06-01

packed column, with low liquid loading (2. 0 mm ID, 4% liquid phase loading on diatomaceous earth *) 0.3 Medium bore analytical packed column, with...moderate liquid loading (4. 5 mm ID, 8%16 liquid phase loading on diatomaceous earth *) 3.0 -3 * diatomaceous earth density 0.24 gm cm 12 associated with the...hydrocarbon fuels. Certain injector inserts have contained packed chromatographic media, e.g., stationary phases coated onto diatomaceous earth . This type

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

PubMed

Gritti, Fabrice; Guiochon, Georges

2012-08-24

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

High speed Deans switch for low duty cycle comprehensive two-dimensional gas chromatography.

PubMed

Ghosh, Abhijit; Bates, Carly T; Seeley, Stacy K; Seeley, John V

2013-05-24

A new high-speed valve-based modulator has been designed and tested for use in comprehensive two-dimensional gas chromatography (GC×GC). The modulator is a Deans switch constructed from two micro-volume fittings and a solenoid valve. Modulator performance was characterized over a wide range of device settings including the magnitude of the switching flow, the gap between the tips of the primary and secondary column, the primary column flow rate, and the carrier gas identity. Under optimized conditions, the modulator was found to be capable of generating narrow pulses (<50ms) of primary effluent with a 2mL/min secondary column flow. This capability will ultimately allow the modulator to be used with GC×GC separations employing a wide range of detectors and secondary column geometries. The main disadvantage of this modulator is that it employs a low sampling duty cycle, and thus it produces separations with sensitivities that are lower than those produced with thermal modulators or differential flow modulators. The efficacy of the new high-speed Deans switch modulator was demonstrated through the GC×GC separation of a hydrocarbon standard and gasoline. Precise quantitation of individual components was possible provided the modulation ratio was kept greater than 2.0. Copyright © 2013 Elsevier B.V. All rights reserved.

Micro-cone targets for producing high energy and low divergence particle beams

DOEpatents

Le Galloudec, Nathalie

2013-09-10

The present invention relates to micro-cone targets for producing high energy and low divergence particle beams. In one embodiment, the micro-cone target includes a substantially cone-shaped body including an outer surface, an inner surface, a generally flat and round, open-ended base, and a tip defining an apex. The cone-shaped body tapers along its length from the generally flat and round, open-ended base to the tip defining the apex. In addition, the outer surface and the inner surface connect the base to the tip, and the tip curves inwardly to define an outer surface that is concave, which is bounded by a rim formed at a juncture where the outer surface meets the tip.

Shell and small particles; evaluation of new column technology.

PubMed

Fekete, Szabolcs; Fekete, Jeno; Ganzler, Katalin

2009-01-15

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

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 initial saturation on properties modification and displacement of tetrachloroethene with aqueous isobutanol.

PubMed

Boyd, Glen R; Ocampo-Gómez, Ana M; Li, Minghua; Husserl, Johana

2006-11-20

Packed column experiments were conducted to study effects of initial saturation of tetrachloroethene (PCE) in the range of 1.0-14% pore volume (PV) on mobilization and downward migration of the non-aqueous phase liquid (NAPL) product upon contact with aqueous isobutanol ( approximately 10 vol.%). This study focused on the consequences of swelling beyond residual saturation. Columns were packed with mixtures of neat PCE, water and glass beads and waterflooded to establish a desired homogeneous residual saturation, and then flooded with aqueous isobutanol under controlled hydraulic conditions. Results showed a critical saturation of approximately 8% PV for these packed column experimental conditions. At low initial PCE saturations (<8% PV), experimental results showed reduced risk of NAPL-product migration upon contact with aqueous isobutanol. At higher initial PCE saturations (>8% PV), results showed NAPL-product mobilization and downward migration which was attributed to interfacial tension (IFT) reduction, swelling of the NAPL-product, and reduced density modification. Packed column results were compared with good agreement to theoretical predictions of NAPL-product mobilization using the total trapping number, N(T). In addition to the packed column study, preliminary batch experiments were conducted to study the effects of PCE volumetric fraction in the range of 0.5-20% on density, viscosity, and IFT modification as a function of time following contact with aqueous isobutanol ( approximately 10 vol.%). Modified NAPL-product fluid properties approached equilibrium within approximately 2 h of contact for density and viscosity. IFT reduction occurred immediately as expected. Measured fluid properties were compared with good agreement to theoretical equilibrium predictions based on UNIQUAC. Overall, this study demonstrates the importance of initial DNAPL saturation, and the associated risk of downward NAPL-product migration, in applying alcohol flooding for remediation of DNAPL contaminated ground water sites.

C(18) columns for the simultaneous determination of oxytetracycline and its related substances by reversed-phase high performance liquid chromatography and UV detection.

PubMed

Smyrniotakis, C G; Archontaki, Helen A

2007-01-17

Simultaneous determination of oxytetracycline, 4-epioxytetracycline, alpha-apooxytetracycline, tetracycline and beta-apooxytetracycline on C(18) columns has been accomplished using a high performance liquid chromatographic method with UV detection. Separation was achieved on a Hypersil BDS RP-C(18) column (250 mm x 4.6 mm) and on a Waters C(18) Symmetry column (150 mm x 3.9mm), 5 microm particle size each. These columns were equilibrated with mobile phases consisted of methanol-acetonitrile-0.1M phosphate buffer pH 8.0 (12.5:12.5:75, v/v/v) and (15:15:70, v/v/v), respectively. The flow rate was 1.0 ml/min and the total elution time was 15 and 5 min, respectively. Both methods were applied to oxytetracycline raw material, human and veterinary formulations, where the excipients did not interfere. External standard calibration curves were linear for 4-epioxytetracycline, oxytetracycline, alpha-apooxytetracycline, tetracycline and beta-apooxytetracycline in the concentration range of 0.27-200 microM, 0.05-200 microM, 0.03-200 microM, 0.35-200 microM and 0.20-200 microM on column A and 0.08-200 microM, 0.15-200 microM, 0.09-200 microM, 0.25-200 microM and 0.47-200 microM on column B, respectively. Day-to-day relative standard deviation of the determination for every component was less than 3%. Concerning the first column, limits of detection and quantification of the above compounds were in the concentration ranges of 10-106 nM and 30-352 nM, respectively, whereas on the second column these ranges became 27-144 nM and 81-475 nM, respectively. Recovery of the separated compounds was 95-105%.

Leaching behaviour of azoxystrobin and metabolites in soil columns.

PubMed

Ghosh, Rakesh Kumar; Singh, Neera

2009-09-01

Azoxystrobin [methyl (E)-2-{2-[6-(2-cyanophenoxy)pyrimidin-4-yloxy]phenyl}-3-methoxyacrylate], a strobilurin fungicide, is a broad-spectrum, systemic and soil-applied fungicide. Azoxystrobin has been registered for rice cultivation in India, but no information is available on its leaching behaviour in Indian soils. Therefore, leaching behaviour of azoxystrobin was studied in packed and intact soil columns under different irrigation regimes. Azoxystrobin did not leach out of the 300 mm long columns after 126 and 362 mm rainfall. After percolating water equivalent to 362 mm rainfall, azoxystrobin leached down to 10-15 cm (packed columns) and 15-20 cm (intact columns) depth. Azoxystrobin was not detected in the leachate from the packed column leached with 94.5 mL water every week (140 mm rainfall per month) during the 28 weeks of the study period. However, azoxystrobin acid, formed by azoxystrobin degradation, was detected in the leachate after 18 weeks. At the end of the study, azoxystrobin had leached down to 5-10 cm depth, and only 60% of initially applied azoxystrobin was recovered from the soil. The results indicate that azoxystrobin is fairly immobile in sandy loam soil, but azoxystrobin acid, a major metabolite of azoxystrobin, is quite mobile and may pose a threat of soil and groundwater contamination. Copyright 2009 Society of Chemical Industry.

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

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

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

1997-08-01

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

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.

Surface confined ionic liquid as a stationary phase for HPLC

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

Wang, Qian; Baker, Gary A; Baker, Sheila N

Trimethoxysilane ionosilane derivatives of room temperature ionic liquids based on alkylimidazolium bromides were synthesized for attachment to silica support material. The derivatives 1-methyl-3-(trimethoxysilylpropyl)imidazolium bromide and 1-butyl-3-(trimethoxysilylpropyl)imidazolium bromide were used to modify the surface of 3 {micro}m diameter silica particles to act as the stationary phase for HPLC. The modified particles were characterized by thermogravimetric analysis (TGA) and {sup 13}C and {sup 29}Si NMR spectroscopies. The surface modification procedure rendered particles with a surface coverage of 0.84 {micro}mol m{sup -2} for the alkylimidazolium bromide. The ionic liquid moiety was predominantly attached to the silica surface through two siloxane bonds of themore » ionosilane derivative (63%). Columns packed with the modified silica material were tested under HPLC conditions. Preliminary evaluation of the stationary phase for HPLC was performed using aromatic carboxylic acids as model compounds. The separation mechanism appears to involve multiple interactions including ion exchange, hydrophobic interaction, and other electrostatic interactions.« less

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

PubMed

Broeckhoven, Ken; Desmet, Gert

2012-10-05

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

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

NASA Astrophysics Data System (ADS)

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

2017-01-01

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

Experiment and modeling for the separation of guaifenesin enantiomers using simulated moving bed and Varicol units.

PubMed

Gong, Rujin; Lin, Xiaojian; Li, Ping; Yu, Jianguo; Rodrigues, Alirio E

2014-10-10

The separation of guaifenesin enantiomers by both simulated moving bed (SMB) process and Varicol process was investigated experimentally and theoretically, where the columns were packed with cellulose tris 3,5-dimethylphenylcarbamate (Chiralcel OD) stationary phase and a mixture of n-hexane and ethanol was used as mobile phase. The operation conditions were designed based on the separation region with the consideration of mass transfer resistance and axial dispersion, and the experiments to separate guaifenesin enantiomers were carried out on VARICOL-Micro unit using SMB process with the column configuration of 1/2/2/1 and Varicol process with the column configuration of 1/1.5/1.5/1, respectively. Single enantiomer with more than 99.0% purity was obtained in both processes with the productivity of 0.42 genantiomer/dcm(3) CSP for SMB process and 054 genantiomer/dcm(3) CSP for Varicol process. These experimental results obtained from SMB and Varicol processes were compared with those reported from literatures. In addition, according to the numerical simulation, the effects of solid-film mass transfer resistance and axial dispersion on the internal profiles were discussed, and the effect of column configuration on the separation performance of SMB and Varicol processes was analyzed for a few columns system. The feasibility and efficiency for the separation of guaifenesin enantiomers by SMB and Varicol processes were evaluated. Copyright © 2014 Elsevier B.V. All rights reserved.

Fabrication and characterization of microelectromechanical systems-based gas chromatography column with embedded micro-posts for separation of environmental carcinogens.

PubMed

Sun, Jianhai; Cui, Dafu; Chen, Xing; Zhang, Lulu; Cai, Haoyuan; Li, Hui

2013-05-24

In this paper, a micro gas chromatography (μGC) column with embedded micro-posts was developed for increasing overall surface area of the columns which is able to support more of the stationary phase and reducing the effective width of the column, leading to higher separation efficiency. The proposed columns have a higher sample capacity as the overall surface area is about 3 times larger than that of open columns with the same dimensions. In order to achieve an even flow velocity in the channels, the location of the micro-posts in the linear channels and the configuration of curved channels were optimized by numerical simulation. The results have indicated that the proposed column separated 5 environmental carcinogens in less than 50s, achieved a separation efficiency of about 9500plates/m and eluted highly symmetrical Gaussian peaks. Copyright © 2013 Elsevier B.V. All rights reserved.

Experimental and numerical investigations of effect of column length on retardation factor determination: a case study of cesium transport in crushed granite.

PubMed

Li, Ming-Hsu; Wang, Tsing-Hai; Teng, Shi-Ping

2009-02-15

This study investigated breakthrough curves (BTCs) from a series of column experiments, including different column lengths and flow rates, of a conservative tracer, tritium oxide (HTO), and a radionuclide, cesium, in crushed granite using a reactive transport model. Results of the short column, with length of 2cm, showed an underestimation of the retardation factor and the corresponding HTO BTCs cannot be successfully modeled even with overestimated fluid dispersivity. Column supporting elements, including filters and rings, on both ends of packed granite were shown to be able to induce additional dispersive mixing, thus significantly affecting BTCs of short columns while those of the long column, with length of 8cm, were less affected. By increasing flow rates from 1mL/min to 5mL/min, the contribution of structural dispersive mixing to the false tilting of short column BTCs still cannot be detached. To reduce the influence of structural dispersivity on BTCs, the equivalent pore volume of column supporting materials should be much smaller than that of packed porous medium. The total length of column supporting structures should be greatly shorter than that of porous medium column.

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.

Zinc oxide crystal whiskers as a novel sorbent for solid-phase extraction of flavonoids.

PubMed

Wang, Licheng; Shangguan, Yangnan; Hou, Xiudan; Jia, Yong; Liu, Shujuan; Sun, Yingxin; Guo, Yong

2017-08-15

As a novel solid-phase extraction material, zinc oxide crystal whiskers were used to extract flavonoid compounds and showed good extraction abilities. X-ray diffraction, scanning electron microscopy with energy dispersive X-ray spectroscopy and surface area/pore volume characterized the sorbent. The zinc oxide was packed into a solid-phase extraction micro-column and its extraction ability was evaluated by four model flavonoid compounds. The sample loading and elution parameters were optimized and the zinc oxide based analytical method for flavonoids was established. It showed that the method has wide linearities from 1 to 150μg/L and low limits of detection at 0.25μg/L. The relative standard deviations of a single column repeatability and column to column reproducibility were less than 6.8% and 10.6%. Several real samples were analyzed by the established method and satisfactory results were obtained. The interactions between flavonoids and zinc oxide were calculated and proved to be from the Van der Waals' forces between the 4p and 5d orbitals from zinc atom and the neighboring π orbitals from flavonoid phenyl groups. Moreover, the zinc oxide crystal whiskers showed good stability and could be reused more than 50 times under the operation conditions. This work proves that the zinc oxide crystal whiskers are a good candidate for flavonoids enrichment. Copyright © 2017. Published by Elsevier B.V.

Synthesis of Energetic Polymers.

DTIC Science & Technology

1981-10-15

demonstrated by a single peak in the gc analysis (injector temperature 2500 C). The reaction will be repeated in a different solvent to avoid the formation of...glass column packed with 10% OV-101 on chrom Q, with n-decane as an internal standard. Rates of polymerization were calculated using the assumption...the Kelen-Tudos method. The disappearance of monomer was monitored by gas chromatography, using a glass column packed with 10% OV-101 on Chrom Q

Catalytic distillation process

DOEpatents

Smith, Jr., Lawrence A.

1982-01-01

A method for conducting chemical reactions and fractionation of the reaction mixture comprising feeding reactants to a distillation column reactor into a feed zone and concurrently contacting the reactants with a fixed bed catalytic packing to concurrently carry out the reaction and fractionate the reaction mixture. For example, a method for preparing methyl tertiary butyl ether in high purity from a mixed feed stream of isobutene and normal butene comprising feeding the mixed feed stream to a distillation column reactor into a feed zone at the lower end of a distillation reaction zone, and methanol into the upper end of said distillation reaction zone, which is packed with a properly supported cationic ion exchange resin, contacting the C.sub.4 feed and methanol with the catalytic distillation packing to react methanol and isobutene, and concurrently fractionating the ether from the column below the catalytic zone and removing normal butene overhead above the catalytic zone.

Catalytic distillation process

DOEpatents

Smith, L.A. Jr.

1982-06-22

A method is described for conducting chemical reactions and fractionation of the reaction mixture comprising feeding reactants to a distillation column reactor into a feed zone and concurrently contacting the reactants with a fixed bed catalytic packing to concurrently carry out the reaction and fractionate the reaction mixture. For example, a method for preparing methyl tertiary butyl ether in high purity from a mixed feed stream of isobutene and normal butene comprising feeding the mixed feed stream to a distillation column reactor into a feed zone at the lower end of a distillation reaction zone, and methanol into the upper end of said distillation reaction zone, which is packed with a properly supported cationic ion exchange resin, contacting the C[sub 4] feed and methanol with the catalytic distillation packing to react methanol and isobutene, and concurrently fractionating the ether from the column below the catalytic zone and removing normal butene overhead above the catalytic zone.

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

PubMed

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

2012-06-01

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

Application of multiwalled carbon nanotubes and its magnetite derivative for emulsified oil removal from produced water.

PubMed

Ibrahim, Taleb H; Sabri, Muhammad A; Khamis, Mustafa I

2018-05-10

Multiwalled carbon nanotubes and their magnetite derivatives were employed as adsorbents for emulsified oil removal from produced water. The experimental parameters for maximum emulsified oil removal efficiency and effective regeneration of these adsorbents were determined. The optimum parameters in terms of adsorbent dosage, contact time, salinity, pH and temperature were 3.0 g/L, 20.0 min, 0 ppm, 7.0 and 25°C for both adsorbents. Due to their low density, multiwalledcarbon nanotubes could not be successfully employed in packed bed columns. The magnetite derivative has a larger density and hence, for the removal of emulsified oil from produced water packed bed column studies were performed utilizing multiwalled carbon magnetite nanotubes. The packed bed column efficiency and behaviour were evaluated using Thomas, Clark, Yan et al. and Bohart and Adams models. The Yan model was found to best describe the column experimental data. The adsorbents were regenerated using n-hexane and reused several times for oil removal from produced water without any significant decrease in their initial adsorption capacities.

A high-performance liquid chromatography assay to monitor the new antiepileptic drug lacosamide in patients with epilepsy.

PubMed

Greenaway, Clare; Ratnaraj, Neville; Sander, Josemir W; Patsalos, Philip N

2010-08-01

A simple high-performance liquid chromatographic micromethod is described for the quantitation of the new antiepileptic drug lacosamide in serum of patients. Serum (100 microL) was first precipitated with 10 microL 60% perchloric acid and 10 microL supernatant injected directly into the high-performance liquid chromatograph. Chromatographic separation was achieved by use of a steel cartridge column (125 x 3 mm inside diameter) packed with Hypersil BDS C-18, at 40 degrees C, and with a gradient elution system comprising methanol, formic acid and water. The eluent was monitored at 215 nm by diode array detection and the calibration curve was linear in the range of 10 to 250 micromol/L. Recovery ranged from 99% to 106%. The limit of quantification was 1 micromol/L and the intrabatch and interbatch coefficients of variation were less than 5%. No interference from commonly prescribed antiepileptic drugs (clobazam, clonazepam, carbamazepine, carbamazepine-10,11-epoxide, gabapentin, lamotrigine, levetiracetam, oxcarbazepine, phenobarbital, phenytoin, primidone, pregabalin, valproic acid, and vigabatrin) was observed, so the method can be used to routinely monitor lacosamide in patients on polytherapy antiepileptic drug regimens.

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

PubMed

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

2018-04-01

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

Efficiency for unretained solutes in packed column supercritical fluid chromatography. I. Theory for isothermal conditions and correction factors for carbon dioxide.

PubMed

Poe, Donald P

2005-06-17

A general theory for efficiency of nonuniform columns with compressible mobile phase fluids is applied to the elution of an unretained solute in packed-column supercritical fluid chromatography (pSFC). The theoretical apparent plate height under isothermal conditions is given by the Knox equation multiplied by a compressibility correction factor f1, which is equal to the ratio of the temporal-to-spatial average densities of the mobile phase. If isothermal conditions are maintained, large pressure drops in pSFC should not result in excessive efficiency losses for elution of unretained solutes.

Evaluating two process scale chromatography column header designs using CFD.

PubMed

Johnson, Chris; Natarajan, Venkatesh; Antoniou, Chris

2014-01-01

Chromatography is an indispensable unit operation in the downstream processing of biomolecules. Scaling of chromatographic operations typically involves a significant increase in the column diameter. At this scale, the flow distribution within a packed bed could be severely affected by the distributor design in process scale columns. Different vendors offer process scale columns with varying design features. The effect of these design features on the flow distribution in packed beds and the resultant effect on column efficiency and cleanability needs to be properly understood in order to prevent unpleasant surprises on scale-up. Computational Fluid Dynamics (CFD) provides a cost-effective means to explore the effect of various distributor designs on process scale performance. In this work, we present a CFD tool that was developed and validated against experimental dye traces and tracer injections. Subsequently, the tool was employed to compare and contrast two commercially available header designs. © 2014 American Institute of Chemical Engineers.

Investigation of quaternary ammonium silane-coated sand filter for the removal of bacteria and viruses from drinking water.

PubMed

Torkelson, A A; da Silva, A K; Love, D C; Kim, J Y; Alper, J P; Coox, B; Dahm, J; Kozodoy, P; Maboudian, R; Nelson, K L

2012-11-01

To develop an anti-microbial filter media using an attached quaternary ammonium compound (QAC) and evaluate its performance under conditions relevant to household drinking water treatment in developing countries. Silica sand was coated with dimethyloctadecyl [3-(trimethoxysilyl) propyl] ammonium chloride via covalent silane chemistry. Filter columns packed with coated media were challenged with micro-organisms under different water quality conditions. The anti-bacterial properties were investigated by visualizing Escherichia coli (E. coli) attachment to coated media under fluorescence microscopy combined with a live/dead stain. A 9-cm columns with a filtration velocity of 18 m h(-1) achieved log(10) removals of 1·7 for E. coli, 1·8 for MS2 coliphage, 1·9 for Poliovirus type 3 and 0·36 for Adenovirus type 2, compared to 0·1-0·3 log(10) removals of E. coli and MS2 by uncoated sand. Removal scaled linearly with column length and decreased with increasing ionic strength, flow velocity, filtration time and humic acid presence. Escherichia coli attached to QAC-coated sand were observed to be membrane-permeable, providing evidence of inactivation. Filtration with QAC-coated sand provided higher removal of bacteria and viruses than filtration with uncoated sand. However, major limitations included rapid fouling by micro-organisms and natural organic matter and low removal of viruses PRD1 and Adenovirus 2. QAC-coated media may be promising for household water treatment. However, more research is needed on long-term performance, options to reduce fouling and inactivation mechanisms. © 2012 The Authors Journal of Applied Microbiology © 2012 The Society for Applied Microbiology.

Interspecies Extrapolations of Halocarbon Respiratory and Tissue Kinetics: Applications to Predicting Toxicity in Different Species

DTIC Science & Technology

1994-08-15

repository for TCE, and thus a critical determinant of TCE’s pharmacokinetics. As previously mentioned, it is advantageous to have quantitative tcxicity...steel columns (182 cm x 0.317 cm) packed with 10% FFAP ( Alltech Associates, Deerfield, IL). The GC operating conditions were: headspace sampler...steel columns (182 cm x 0.317 cm) packed with 10% FFAP ( Alltech Associates, Deerfield, IL). The GC operating conditions were: headspace sampler

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.

Role of Tat-interacting protein of 110 kDa and microRNAs in the regulation of hematopoiesis.

PubMed

Liu, Ying; He, Johnny J

2016-07-01

Hematopoiesis is regulated by cellular factors including transcription factors, microRNAs, and epigenetic modifiers. Understanding how these factors regulate hematopoiesis is pivotal for manipulating them to achieve their desired potential. In this review, we will focus on HIV-1 Tat-interacting protein of 110 kDa (Tip110) and its regulation of hematopoiesis. There are several pathways in hematopoiesis that involve Tip110 regulation. Tip110 is expressed in human cord blood CD34 cells; its expression decreases when CD34 cells begin to differentiate. Tip110 is also expressed in mouse marrow hematopoietic stem cells (HSC) and hematopoietic progenitor cells (HPC). Tip110 expression increases the number, survival, and cell cycling of HPC. Tip110-mediated regulation of hematopoiesis has been linked to its reciprocal control of proto-oncogene expression. Small noncoding microRNAs (miRs) have been shown to play important roles in regulation of hematopoiesis. miR-124 specifically targets 3'-untranslated region of Tip110 and subsequently regulates Tip110 expression in HSC. Our recent findings for manipulating expression levels of Tip110 in HSC and HPC could be useful for expanding HSC and HPC and for improving engraftment of cord blood HSC/HPC.

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

PubMed

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

2012-01-03

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

Establishing column batch repeatability according to Quality by Design (QbD) principles using modeling software.

PubMed

Rácz, Norbert; Kormány, Róbert; Fekete, Jenő; Molnár, Imre

2015-04-10

Column technology needs further improvement even today. To get information of batch-to-batch repeatability, intelligent modeling software was applied. Twelve columns from the same production process, but from different batches were compared in this work. In this paper, the retention parameters of these columns with real life sample solutes were studied. The following parameters were selected for measurements: gradient time, temperature and pH. Based on calculated results, batch-to-batch repeatability of BEH columns was evaluated. Two parallel measurements on two columns from the same batch were performed to obtain information about the quality of packing. Calculating the average of individual working points at the highest critical resolution (R(s,crit)) it was found that the robustness, calculated with a newly released robustness module, had a success rate >98% among the predicted 3(6) = 729 experiments for all 12 columns. With the help of retention modeling all substances could be separated independently from the batch and/or packing, using the same conditions, having high robustness of the experiments. Copyright © 2015 Elsevier B.V. All rights reserved.

EFFECT OF NITRATE-BASED BIOREMEDIATION ON CONTAMINANT DISTRIBUTION AND SEDIMENT TOXICITY-COLUMN STUDY

EPA Science Inventory

A laboratory column study was set up to evaluate changes in contaminant distribution and sediment toxicity following nitrate-based bioremediation and to correlate toxicity reduction with loss of fuel components. Glass columns were packed with sediment from an aquifer that had be...

Frictional and morphological properties of Au-MoS2 films sputtered from a compact target

NASA Technical Reports Server (NTRS)

Spalvins, T.

1984-01-01

AuMoS2 films 0.02 to 1.2 microns thick were sputtered from target compacted from 5 wt % Au + 95 wt % MoS2, to investigate the frictional and morphological film growth characteristics. The gold dispersion effects in MoS2 films are of interest to increase the densitification and strengthening of the film structure. Three microstructural growth stages were identified on the nano-micro-macrostructural level. During sliding both sputtered Au-MoS2 and MoS2 films have a tendency to break within the columner region. The remaining or effective film, about 0.2 microns thick, performs the lubrication. The Au-MoS2 films displayed a lower friction coefficient with a high degree of frictional stability and less wear debris generation as compared to pure MoS2 films. The more favorable frictional characteristics of the Au-MoS2 films are attributed to the effective film thickness and the high density packed columner zone which has a reduced effect on the fragmentation of the tapered crystallites during fracture.

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

PubMed

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

2012-08-01

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

Mineral Separation in a CELSS by Ion-exchange Chromatography

NASA Technical Reports Server (NTRS)

Ballou, E. V.; Spitze, L. A.; Wong, F. W.; Wydeven, T.; Johnson, C. C.

1982-01-01

Operational parameters pertinent to ion exchange chromatography separation were identified. The experiments were performed with 9 mm diameter ion exchange columns and conventional column accessories. The cation separation beds were packed with AG 50W-X2 strong acid cation exchange resin in H(+) form and 200-400 dry mesh particle size. The stripper beds used in some experiments were packed with AG 1-XB strong base cation exchange resin in OH(-) form and 200-400 dry mesh particle size.

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

PubMed

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

2012-11-30

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

Systematic comparison of a new generation of columns packed with sub-2 μm superficially porous particles.

PubMed

Bobály, Balázs; Guillarme, Davy; Fekete, Szabolcs

2014-02-01

The aim of this study was to evaluate the possibilities/limitations of recent RP-LC columns packed with 1.6 μm superficially porous particles (Waters Cortecs) and to compare its potential to other existing sub-2 μm core-shell packings. The kinetic performance of Kinetex 1.3 μm, Kinetex 1.7 μm and Cortecs 1.6 μm stationary phases was assessed. It was found that the Kinetex 1.3 μm phase outperforms its counterparts for ultra-fast separations. Conversely, the Cortecs 1.6 μm packing seemed to be the best stationary phase for assays with longer analysis time in isocratic and gradient modes, considering small molecules and peptides as test probes. This exceptional behaviour was attributed to its favourable permeability and somewhat higher mechanical stability (ΔPmax of 1200 bar). The loading capacity of these three columns was also investigated with basic and neutral drugs analysed under acidic conditions. It appears that the loading capacities of Cortecs 1.6 μm and Kinetex 1.7 μm were very close, while it was reduced by 2-7-fold on the Kinetex 1.3 μm packing. However, this observation is dependent on the nature of the compound and certainly also on mobile phase conditions. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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.

Longitudinal dispersion coefficient depending on superficial velocity of hydrogen isotopes flowing in column packed with zeolite pellets at 77.4 K

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

Kotoh, K.; Graduate School of Engineering, Kyushu University, Nishi-ku, Fukuoka; Kubo, K.

2015-03-15

Authors have been developing a cryogenic pressure swing adsorption system for hydrogen isotope separation. In the problem of its design and operation, it is necessary to predict the concentration profiles developing in packed beds of adsorbent pellets. The profiling is affected by the longitudinal dispersion of gas flowing in packed beds, in addition to the mass transfer resistance in porous media of adsorbent pellets. In this work, an equation is derived for estimating the packed-bed dispersion coefficient of hydrogen isotopes, by analyzing the breakthrough curves of trace D{sub 2} or HD replacing H{sub 2} adsorbed in synthetic zeolite particles packedmore » columns at the liquefied nitrogen temperature 77.4 K. Since specialized for hydrogen isotopes, this equation can be considered to estimate the dispersion coefficients more reliable for the cryogenic hydrogen isotope adsorption process, than the existing equations. (authors)« less

Effect of gravity on colloid transport through water-saturated columns packed with glass beads: modeling and experiments.

PubMed

Chrysikopoulos, Constantinos V; Syngouna, Vasiliki I

2014-06-17

The role of gravitational force on colloid transport in water-saturated columns packed with glass beads was investigated. Transport experiments were performed with colloids (clays: kaolinite KGa-1b, montmorillonite STx-1b). The packed columns were placed in various orientations (horizontal, vertical, and diagonal) and a steady flow rate of Q = 1.5 mL/min was applied in both up-flow and down-flow modes. All experiments were conducted under electrostatically unfavorable conditions. The experimental data were fitted with a newly developed, analytical, one-dimensional, colloid transport model. The effect of gravity is incorporated in the mathematical model by combining the interstitial velocity (advection) with the settling velocity (gravity effect). The results revealed that flow direction influences colloid transport in porous media. The rate of particle deposition was shown to be greater for up-flow than for down-flow direction, suggesting that gravity was a significant driving force for colloid deposition.

Effects of Gravity on Cocurrent Two-Phase Gas-Liquid Flows Through Packed Columns

NASA Technical Reports Server (NTRS)

Motil, Brian J.; Balakotaiah, Vemuri; Kamotani, Yasuhiro

2001-01-01

This work presents the experimental results of research on the influence of gravity on flow pattern transitions, pressure drop and flow characteristics for cocurrent gas-liquid two-phase flow through packed columns. The flow pattern transition data indicates that the pulse flow regime exists over a wider range of gas and liquid flow rates under reduced gravity conditions compared to normal gravity cocurrent down-flow. This is illustrated by comparing the flow regime transitions found in reduced gravity with the transitions predicted by Talmor. Next, the effect of gravity on the total pressure drop in a packed column is shown to depend on the flow regime. The difference is roughly equivalent to the liquid static head for bubbly flow but begins to decrease at the onset of pulse flow. As the spray flow regime is approached by increasing the gas to liquid ratio, the effect of gravity on pressure drop becomes negligible. Finally, gravity tends to suppress the amplitude of each pressure pulse. An example of this phenomenon is presented.

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

Bacteremic complications of intravascular catheter tip colonization with Gram-negative micro-organisms in patients without preceding bacteremia.

PubMed

van Eck van der Sluijs, A; Oosterheert, J J; Ekkelenkamp, M B; Hoepelman, I M; Peters, Edgar J G

2012-06-01

Although Gram-negative micro-organisms are frequently associated with catheter-related bloodstream infections, the prognostic value and clinical implication of a positive catheter tip culture with Gram-negative micro-organisms without preceding bacteremia remains unclear. We determined the outcomes of patients with intravascular catheters colonized with these micro-organisms, without preceding positive blood cultures, and identified risk factors for the development of subsequent Gram-negative bacteremia. All patients with positive intravascular catheter tip cultures with Gram-negative micro-organisms at the University Medical Center, Utrecht, The Netherlands, between 2005 and 2009, were retrospectively studied. Patients with Gram-negative bacteremia within 48 h before catheter removal were excluded. The main outcome measure was bacteremia with Gram-negative micro-organisms. Other endpoints were length of the hospital stay, in-hospital mortality, secondary complications of Gram-negative bacteremia, and duration of intensive care admission. A total of 280 catheters from 248 patients were colonized with Gram-negative micro-organisms. Sixty-seven cases were excluded because of preceding positive blood cultures, leaving 213 catheter tips from 181 patients for analysis. In 40 (19%) cases, subsequent Gram-negative bacteremia developed. In multivariate analysis, arterial catheters were independently associated with subsequent Gram-negative bacteremia (odds ratio [OR] = 5.00, 95% confidence interval [CI]: 1.20-20.92), as was selective decontamination of the digestive tract (SDD) (OR = 2.47, 95% CI: 1.07-5.69). Gram-negative bacteremia in patients who received SDD was predominantly caused by cefotaxime (part of the SDD)-resistant organisms. Mortality was significantly higher in the group with subsequent Gram-negative bacteremia (35% versus 20%, OR = 2.12, 95% CI: 1.00-4.49). Patients with a catheter tip colonized with Gram-negative micro-organisms had a high chance of subsequent Gram-negative bacteremia from any cause. This may be clinically relevant, as starting antibiotic treatment pre-emptively in high-risk patients with Gram-negative micro-organisms cultured from arterial intravenous catheters may be beneficial.

Micro-apparatus for rapid determinations of protein solubilities

NASA Technical Reports Server (NTRS)

Pusey, Marc L.; Munson, Sibyl

1991-01-01

We have developed a column-based micro-technique for rapid determinations of protein solubilities. While retaining a large crystal surface area, the column dead volume has been reduced to equal to or less than 5 micro liters. The technique was tested with tetragonal lysozyme (pH 4.5, 0.1 M acetate, 3.0 percent NaCl, 5-25 C) and column volumes of about 60, 300, and 900 micro liters. Identical solubility data were obtained, indicating that equilibration was obtained even in the smallest columns. In addition, solubility data for Br- and I- salts of lysozyme (pH 4.5, 0.1 M acetate buffer, 0.5 M salt concentrations) were obtained. It appears that the technique can be further miniaturized. The limit in further reducing the crystalline column volume is determined by the minimum solution sample size needed to determine the protein concentration.

Tapered bed bioreactor

DOEpatents

Scott, Charles D.; Hancher, Charles W.

1977-01-01

A vertically oriented conically shaped column is used as a fluidized bed bioreactor wherein biologically catalyzed reactions are conducted in a continuous manner. The column utilizes a packing material a support having attached thereto a biologically active catalytic material.

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

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

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

1998-03-01

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

Simultaneous biosorption of chromium(VI) and copper(II) on Rhizopus arrhizus in packed column reactor: Application of the competitive Freundlich model

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

Sag, Y.; Atacoglu, I.; Kutsal, T.

1999-12-01

The simultaneous biosorption of Cr(VI) and Cu(II) on free Rhizopus arrhizus in a packed column operated in the continuous mode was investigated and compared to the single metal ion situation. The breakthrough curves were measured as a function of feed flow rate, feed pH, and different combinations of metal ion concentrations in the feed solutions. Column competitive biosorption data were evaluated in terms of the maximum (equilibrium) capacity in the column, the amount of metal loading on the R. arrhizus surface, the adsorption yield, and the total adsorption yield. In the single-ion situation the adsorption isotherms were developed for optimummore » conditions, and it was seen that the adsorption equilibrium data fit the noncompetitive Freundlich model. For the multicomponent adsorption equilibrium the competitive adsorption isotherms were also developed. The competitive Freundlich model for binary metal mixtures represented most the column adsorption equilibrium data of Cr(VI) and Cu(II) on R. arrhizus satisfactorily.« less

Centrifugal sedimentation for selectively packing channels with silica microbeads in three-dimensional micro/nanofluidic devices.

PubMed

Gong, Maojun; Bohn, Paul W; Sweedler, Jonathan V

2009-03-01

Incorporation of nanofluidic elements into microfluidic channels is one approach for adding filtration and partition functionality to planar microfluidic devices, as well as providing enhanced biomolecular separations. Here we introduce a strategy to pack microfluidic channels with silica nanoparticles and microbeads, thereby indirectly producing functional nanostructures; the method allows selected channels to be packed, here demonstrated so that a separation channel is packed while keeping an injection channel unpacked. A nanocapillary array membrane is integrated between two patterned microfluidic channels that cross each other in vertically separated layers. The membrane serves both as a frit for bead packing and as a fluid communication conduit between microfluidic channels. Centrifugal force-assisted sedimentation is then used to selectively pack the microfluidic channels using an aqueous silica bead suspension loaded into the appropriate inlet reservoirs. This packing approach may be used to simultaneously pack multiple channels with silica microbeads having different sizes and surface properties. The chip design and packing method introduced here are suitable for packing silica particles in sizes ranging from nanometers to micrometers and allow rapid (approximately 10 min) packing with high quality. The liquid/analyte transport characteristics of these packed micro/nanofluidic devices have potential utility in a wide range of applications, including electroosmotic pumping, liquid chromatographic separations, and electrochromatography.

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.

Filling of high aspect ratio micro features of a microfluidic flow cytometer chip using micro injection moulding

NASA Astrophysics Data System (ADS)

Zhang, Haoyang; Fang, Fengzhou; Gilchrist, Michael D.; Zhang, Nan

2018-07-01

Micro injection moulding has been demonstrated as one of the most efficient mass production technologies for manufacturing polymeric microfluidic devices, which have been widely used in life sciences, environmental and analytical fields and agro-food industries. However, the filling of micro features for typical microfluidic devices is complicated and not yet fully understood, which consequently restricts the chip development. In the present work, a microfluidic flow cytometer chip with essential high aspect ratio micro features was used as a typical model to study their filling process. Short-shot experiments and single factor experiments were performed to examine the filling progress of such features during the injection and packing stages of the micro injection moulding process. The influence of process parameters such as shot size, packing pressure, packing time and mould temperature were systematically monitored, characterised and correlated with 3D measurements and real response of the machine such as screw velocity and screw position. A combined melt flow and creep deformation model was proposed to explain the complex influence of process on replication. An approach of over-shot micro injection moulding was proposed and was shown to be effective at improving the replication quality of high aspect ratio micro features.

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

PubMed

Rocco, Anna; Maruška, Audrius; Fanali, Salvatore

2012-03-01

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

Glycolipid class profiling by packed-column subcritical fluid chromatography.

PubMed

Deschamps, Frantz S; Lesellier, Eric; Bleton, Jean; Baillet, Arlette; Tchapla, Alain; Chaminade, Pierre

2004-06-18

The potential of packed-column subcritical fluid chromatography (SubFC) for the separation of lipid classes has been assessed in this study. Three polar stationary phases were checked: silica, diol, and poly(vinyl alcohol). Carbon dioxide (CO2) with methanol as modifier was used as mobile phase and detection performed by evaporative light scattering detection. The influence of methanol content, temperature, and pressure on the chromatographic behavior of sphingolipids and glycolipids were investigated. A complete separation of lipid classes from a crude wheat lipid extract was achieved using a modifier gradient from 10 to 40% methanol in carbon dioxide. Solute selectivity was improved using coupled silica and diol columns in series. Because the variation of eluotropic strength depending on the fluid density changes, a normalized separation factor product (NSP) was used to select the nature, the number and the order of the columns to reach the optimum glycolipid separation.

Non-planar microfabricated gas chromatography column

DOEpatents

Lewis, Patrick R.; Wheeler, David R.

2007-09-25

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

Determination of erythromycin in human plasma, using column liquid chromatography with a polymeric packing material, alkaline mobile phase and amperometric detection.

PubMed

Nilsson, L G; Walldorf, B; Paulsen, O

1987-12-25

A method based on column liquid chromatography was developed for determination of plasma concentrations of erythromycin. PRP-1, a polymeric type of packing material suitable for chromatography and amperometric detection at high pH, was used. The effect of pH on the column performance and on the electrochemical response was studied. A pH of ca. 10 was found to be optimal. After extraction with tert.-butyl methyl ether, plasma concentrations down to 0.2 mumol/l could be measured, using automated sample injection. Oleandomycin was used as internal standard. The method was used for determination of plasma concentrations in a pharmacokinetic study under steady-state conditions.

Reduction of hydraulic conductivity in column simulations of unconsolidated sediments by growth of in situ microflora

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

Bertetti, F.P.; Birnbaum, S.J.

1992-01-01

Laboratory experiments were employed to determine the effects of microbial growth upon the hydraulic conductivity (K) of unconsolidated sediments at Kelly Air Force Base, Texas. Indigenous microflora were isolated from sediment samples collected at sites contaminated with toxic organic compounds (e.g. dichlorobenzene) by plating on concentrated and dilute media. Plexiglas columns were packed with silica beads or Kelly AFB sediment and used to simulate ground water flow conditions. Grain sizes were selected to yield realistic K values (2.0 [times] 10[sup [minus]1] to 8.0 [times] 10[sup [minus]3] cm/sec) defined by field data from the contaminated sites. Both individual and mixed microbialmore » colonies, selected based on morphological characteristics individual and mixed microbial colonies, selected based on morphological characteristics deemed favorable for porosity obstruction, were injected into sterile, saturated columns. Growth was stimulated by adding sterile liquid nutrient media. Media flow rates were based upon field derived hydraulic conductivity values and water table gradients. Flow rates were controlled using a peristaltic pump. Growth of the microorganisms produced biomass which reduced the column hydraulic conductivity by up to 90% in 11 days. Reduction in K was accomplished via clogging of pore throats by cell attachment and accumulation on bead surfaces, and extracellular biofilm development. Sediment packed columns showed reduction in K values similar to that of bead packed columns of equivalent grain size. Porosity obstruction and corresponding reduction in K persisted in the columns even when subjected to hydraulic gradients significantly exceeding gradients measured in the field thereby demonstrating the robust nature of biological barrier to flow.« less

Electrophoretic fractional elution apparatus employing a rotational seal fraction collector

NASA Technical Reports Server (NTRS)

Bier, M. (Inventor)

1977-01-01

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

Add Sparkle to Your Learning Centers

ERIC Educational Resources Information Center

Miller, Susan

2005-01-01

This brief column offers ten tips on how to revive classroom learning centers by cleaning up, reassessing spaces, and adding fresh materials. Some of the tips include: create colorful banners; provide inspirational materials; and share surprise boxes.

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

PubMed

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

2004-11-01

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

Post-synthetic modification of MIL-101(Cr) with pyridine for high-performance liquid chromatographic separation of tocopherols.

PubMed

Yang, Fang; Yang, Cheng-Xiong; Yan, Xiu-Ping

2015-05-01

Effective separation of tocopherols is challenging and significant due to their structural similarity and important biological role. Here we report the post-synthetic modification of metal-organic framework (MOF) MIL-101(Cr) with pyridine for high-performance liquid chromatographic (HPLC) separation of tocopherols. Baseline separation of four tocopherols was achieved on a pyridine-grafted MIL-101(Cr) packed column within 10 min using hexane/isopropanol (96:4, v/v) as the mobile phase at a flow rate of 0.5 mL min(-1). The pyridine-grafted MIL-101(Cr) packed column gave high column efficiency (85,000 plates m(-1) for δ-tocopherol) and good precision (0.2-0.3% for retention time, 1.8-3.4% for peak area, 2.6-2.7% for peak height), and also offered much better performance than unmodified MIL-101(Cr) and commercial amino-bonded silica packed column for HPLC separation of tocopherols. The results not only show the promising application of pyridine-grafted MIL-101(Cr) as a novel stationary phase for HPLC separation of tocopherols, but also reveal a facile post-modification of MOFs to expand the application of MOFs in separation sciences. Copyright © 2015 Elsevier B.V. All rights reserved.

Effects of distillation system and yeast strain on the aroma profile of Albariño (Vitis vinifera L.) grape pomace spirits.

PubMed

Arrieta-Garay, Y; Blanco, P; López-Vázquez, C; Rodríguez-Bencomo, J J; Pérez-Correa, J R; López, F; Orriols, I

2014-10-29

Orujo is a traditional alcoholic beverage produced in Galicia (northwest Spain) from distillation of grape pomace, a byproduct of the winemaking industry. In this study, the effect of the distillation system (copper charentais alembic versus packed column) and the yeast strain (native yeast L1 versus commercial yeast L2) on the chemical and sensory characteristics of orujo obtained from Albariño (Vitis vinifera L.) grape pomace has been analyzed. Principal component analysis, with two components explaining 74% of the variance, is able to clearly differentiate the distillates according to distillation system and yeast strain. Principal component 1, mainly defined by C6-C12 esters, isoamyl octanoate, and methanol, differentiates L1 from L2 distillates. In turn, principal component 2, mainly defined by linear alcohols, linalool, and 1-hexenol, differentiates alembic from packed column distillates. In addition, an aroma descriptive test reveals that the distillate obtained with a packed column from a pomace fermented with L1 presented the highest positive general impression, which is associated with the highest fruity and smallest solvent aroma scores. Moreover, chemical analysis shows that use of a packed column increases average ethanol recovery by 12%, increases the concentration of C6-C12 esters by 25%, and reduces the concentration of higher alcohols by 21%. In turn, L2 yeast obtained lower scores in the alembic distillates aroma profile. In addition, with L1, 9% higher ethanol yields were achieved, and L2 distillates contained 34%-40% more methanol than L1 distillates.

Mentoring and Coaching Tips: How Educators Can Help Each Other

ERIC Educational Resources Information Center

Waterman, Sheryn Spencer

2013-01-01

This book is for educators at all levels and is packed with creative, use-now tips and activities to support new and struggling teachers. Combining real-life scenarios with current research, the author demonstrates how educators can get the most out of available resources, promote a school culture devoted to helping and caring, and meet common…

[Recent advances and applications of capillary electrochromatography and pressurized capillary electrochromatography].

PubMed

Wu, Yi; Zhang, Xiaohui; Wei, Juan; Xue, Yunyun; Bahatibieke, Marjan; Wang, Yan; Yan, Chao

2009-09-01

Capillary electrochromatography (CEC), in which electroosmotic flow (EOF) created from the electrical double layer is made to act as a pump to drive the mobile phase in a capillary column packed with micro-particulates or coated with stationary phase. Both neutral and charged species can be resolved by CEC. It has been demonstrated that the efficiency of a separation obtained by electroosmotic propulsion is superior to that obtained by pressure-driven flow (as is the case in HPLC). CEC combines the best features of CE and versatile selectivity and large sample capacity of HPLC, promising high efficiency, high resolution, high selectivity and high peak capacity. However, in practice, when CEC is used without pressure, often used on a commercial CE instrument, there are problems and difficulties associated with bubbles formation and column dry-out. These difficulties can be overcome by a pressurized CEC (pCEC) system, in which a supplementary pressure is applied to the column in addition to the EOF. In such a system, a pressure can be applied to the capillary column to suppress bubbles formation. Quantitative sample introduction in pCEC can be easily achieved through a rotary-type injector. Most importantly, it is amenable for a solvent gradient mode, similar to that in HPLC, by programming the composition of mobile phase. The article brings a comprehensive survey of recent development of CEC and pCEC, including the development of instrumentation, capillary columns and stationary phase as well as CEC and pCEC applications in life science, biotechnology, pharmaceutical analysis, food safety and environmental security. Prospects for CEC and pCEC development and application are also discussed.

SURFACE CHEMICAL EFFECTS ON COLLOID STABILITY AND TRANSPORT THROUGH NATURAL POROUS MEDIA

EPA Science Inventory

Surface chemical effects on colloidal stability and transport through porous media were investigated using laboratory column techniques. Approximately 100 nm diameter, spherical, iron oxide particles were synthesized as the mobile colloidal phase. The column packing material was ...

Radial particle-size segregation during packing of particulates into cylindrical containers

USGS Publications Warehouse

Ripple, C.D.; James, R.V.; Rubin, J.

1973-01-01

In a series of experiments, soil materials were placed in long cylindrical containers, using various packing procedures. Soil columns produced by deposition and simultaneous vibratory compaction were dense and axially uniform, but showed significant radial segregation of particle sizes. Similar results were obtained with deposition and simultaneous impact-type compaction when the impacts resulted in significant container "bouncing". The latter procedure, modified to minimize "bouncing" produced dense, uniform soil columns, showing little radial particle-size segregation. Other procedures tested (deposition alone and deposition followed by compaction) did not result in radial segregation, but produced columns showing either relatively low or axially nonuniform densities. Current data suggest that radial particle-size segregation is mainly due to vibration-induced particle circulation in which particles of various sizes have different circulation rates and paths. ?? 1973.

49 CFR 173.240 - Bulk packaging for certain low hazard solid materials.

Code of Federal Regulations, 2014 CFR

2014-10-01

... this subchapter and the special provisions specified in column 7 of the § 172.101 table. (a) Rail cars... the IBC packaging code specified for the specific hazardous material in Column (7) of the § 172.101... subchapter at the Packing Group performance level as specified in Column (5) of the § 172.101 Table of this...

49 CFR 173.240 - Bulk packaging for certain low hazard solid materials.

Code of Federal Regulations, 2012 CFR

2012-10-01

... this subchapter and the special provisions specified in column 7 of the § 172.101 table. (a) Rail cars... the IBC packaging code specified for the specific hazardous material in Column (7) of the § 172.101... subchapter at the Packing Group performance level as specified in Column (5) of the § 172.101 Table of this...

49 CFR 173.240 - Bulk packaging for certain low hazard solid materials.

Code of Federal Regulations, 2011 CFR

2011-10-01

... this subchapter and the special provisions specified in column 7 of the § 172.101 table. (a) Rail cars... the IBC packaging code specified for the specific hazardous material in Column (7) of the § 172.101... subchapter at the Packing Group performance level as specified in Column (5) of the § 172.101 Table of this...

49 CFR 173.240 - Bulk packaging for certain low hazard solid materials.

Code of Federal Regulations, 2013 CFR

2013-10-01

... this subchapter and the special provisions specified in column 7 of the § 172.101 table. (a) Rail cars... the IBC packaging code specified for the specific hazardous material in Column (7) of the § 172.101... subchapter at the Packing Group performance level as specified in Column (5) of the § 172.101 Table of this...

49 CFR 173.240 - Bulk packaging for certain low hazard solid materials.

Code of Federal Regulations, 2010 CFR

2010-10-01

... this subchapter and the special provisions specified in column 7 of the § 172.101 table. (a) Rail cars... the IBC packaging code specified for the specific hazardous material in Column (7) of the § 172.101... subchapter at the Packing Group performance level as specified in Column (5) of the § 172.101 Table of this...

Making a Difference. A Resource Pack for People Who Want To Become More Active Citizens.

ERIC Educational Resources Information Center

Dadzie, Stella, Comp.; Turner, Cheryl, Ed.

This document, which is a resource pack for individuals in the United Kingdom who want to become more active citizens, consists of information for group leaders and five learning modules. The section for group leaders contains the following: basic tips on leading a group; strategies for overcoming barriers to learning; glossary; and overview of…

Process for preparing radiopharmaceuticals

DOEpatents

Barak, Morton; Winchell, Harry S.

1977-01-04

A process for the preparation of technetium-99m labeled pharmaceuticals is disclosed. The process comprises initially isolating technetium-99m pertechnetate by adsorption upon an adsorbent packing in a chromatographic column. The technetium-99m is then eluted from the packing with a biological compound to form a radiopharmaceutical.

Determination of phosphonoformate (foscarnet) in calf and human serum by automated solid-phase extraction and high-performance liquid chromatography with amperometric detection.

PubMed

Ba, B B; Corniot, A G; Ducint, D; Breilh, D; Grellet, J; Saux, M C

1999-03-05

An isocratic high-performance liquid chromatographic method with automated solid-phase extraction has been developed to determine foscarnet in calf and human serums. Extraction was performed with an anion exchanger, SAX, from which the analyte was eluted with a 50 mM potassium pyrophosphate buffer, pH 8.4. The mobile phase consisted of methanol-40 mM disodium hydrogenphosphate, pH 7.6 containing 0.25 mM tetrahexylammonium hydrogensulphate (25:75, v/v). The analyte was separated on a polyether ether ketone (PEEK) column 150x4.6 mm I.D. packed with Kromasil 100 C18, 5 microm. Amperometric detection allowed a quantification limit of 15 microM. The assay was linear from 15 to 240 microM. The recovery of foscarnet from calf serum ranged from 60.65+/-1.89% for 15 microM to 67.45+/-1.24% for 200 microM. The coefficient of variation was < or = 3.73% for intra-assay precision and < or =7.24% for inter-assay precision for calf serum concentrations ranged from 15 to 800 microM. For the same samples, the deviation from the nominal value ranged from -8.97% to +5.40% for same day accuracy and from -4.50% to +2.77% for day-to-day accuracy. Selectivity was satisfactory towards potential co-medications. Replacement of human serum by calf serum for calibration standards and quality control samples was validated. Automation brought more protection against biohazards and increase in productivity for routine monitoring and pharmacokinetic studies.

Separative analyses of a chromatographic column packed with a core-shell adsorbent for lithium isotope separation

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

Sugiyama, T.; Sugura, K.; Enokida, Y.

2015-03-15

Lithium-6 is used as a blanket material for sufficient tritium production in DT fueled fusion reactors. A core-shell type adsorbent was proposed for lithium isotope separation by chromatography. The mass transfer model in a chromatographic column consisted of 4 steps, such as convection and dispersion in the column, transfer through liquid films, intra-particle diffusion and and adsorption or desorption at the local adsorption sites. A model was developed and concentration profiles and time variation in the column were numerically simulated. It became clear that core-shell type adsorbents with thin porous shell were saturated rapidly relatively to fully porous one andmore » established a sharp edge of adsorption band. This is very important feature because lithium isotope separation requires long-distance development of adsorption band. The values of HETP (Height Equivalent of a Theoretical Plate) for core-shell adsorbent packed column were estimated by statistical moments of the step response curve. The value of HETP decreased with the thickness of the porous shell. A core-shell type adsorbent is, then, useful for lithium isotope separation. (authors)« less

Development Of ABEC Column For Separation Of Tc-99 From Northstar Dissolved Target Solution

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

Stepinski, Dominique C.; Bennett, Megan E.; Naik, Seema R.

Batch and column breakthrough experiments were performed to determine isotherms and mass-transfer parameters for adsorption of Tc on aqueous biphasic extraction chromatographic (ABEC) sorbent in two solutions: 200 g/L Mo, 5.1 M K +, 1 M OH -, and 0.1 M NO 3 - (Solution A) and 200 g/L Mo, 9.3 M K +, 5 M OH -, and 0.1 M NO 3 - (Solution B). Good agreement was found between the isotherm values obtained by batch and column breakthrough studies for both Solutions A and B. Potassium-pertechnetate intra-particle diffusivity on ABEC resin was estimated by VERSE simulations, and goodmore » agreement was found among a series of column-breakthrough experiments at varying flow velocities, column sizes, and technetium concentrations. However, testing of 10 cc cartridges provided by NorthStar with Solutions A and B did not give satisfactory results, as significant Tc breakthrough was observed and ABEC cartridge performance varied widely among experiments. These different experimental results are believed to be due to inconsistent preparation of the ABEC resin prior to packing and/or inconsistent packing.« less

Complete temperature profiles in ultra-high-pressure liquid chromatography columns.

PubMed

Gritti, Fabrice; Guiochon, Georges

2008-07-01

The temperature profiles were calculated along and across seven packed columns (lengths 30, 50, 100, and 150 mm, i.d., 1 and 2.1 mm, all packed with Acquity UPLC, BEH-C 18 particles, average d(p) approximately 1.7 microm) and their stainless steel tubes (o.d. 4.53 and 6.35 mm). These columns were kept horizontal and sheltered from forced air convection (i.e., under still air conditions), at room temperature. They were all percolated with pure acetonitrile, either under the maximum pressure drop (1034 bar) or at the maximum flow rate (2 mL/min) permitted by the chromatograph. The heat balance equation of chromatographic columns was discretized and solved numerically with minimum approximation. Both the compressibility and the thermal expansion of the eluent were taken into account. The boundary conditions were determined from the experimental measurements of the column inlet pressure and of the temperature profile along the column wall, which were made with a precision better than +/-0.1 K. These calculation results provide the 3-D temperature profiles along and across the columns. The axial and radial temperature gradients are discussed in relationship with the experimental conditions used. The temperature map obtained permits a prediction of the chromatographic data obtained under a very high pressure gradient.

Silver ion chromatography for peak resolution enhancement: Application to the preparative separation of two sesquiterpenes using online heart-cutting LC-LC technique.

PubMed

Yang, Yang; Zhang, Yongmin; Wei, Chong; Li, Jing; Sun, Wenji

2018-09-01

Silver ion chromatography, utilizing columns packed with silver ions bonded to silica gel, has proved to be an invaluable technique for the analysis of some positional isomers. In this work, silver ion chromatography by combination with online heart-cutting LC-LC technique for the preparative separation of two sesquiterpenes positional isomers from a natural product was investigated. On the basis of the evaluation that silver ion content impacts on the separation, the laboratory-made silver ion columns, utilizing silica gel impregnated with 15% silver nitrate as column packing materials, were used for peak resolution improvement of these two isomers and the preparative separation of them in heart-cutting LC-LC. The relationship among the maximal sample load, flow rate and peak resolution in the silver ion column were optimized, and the performance of the silver ion column was compared with conventional C 18 column and silica gel column. Based on the developed chromatographic conditions, online heart-cutting LC-LC chromatographic separation system in combination with a silica gel column and a silver ion column that was applied to preparative separation of these two isomers from a traditional Chinese medicine, Inula racemosa Hook.f., was established. The results showed that the online heart-cutting LC-LC technique by combination of a silica gel column and a silver ion column for the preparative separation of these two positional isomers from this natural plant was superior to the preparative separation performed on a single-column system with C 18 column or silica gel column. Copyright © 2018 Elsevier B.V. All rights reserved.

Monolithic methacrylate packed 96-tips for high throughput bioanalysis.

PubMed

Altun, Zeki; Skoglund, Christina; Abdel-Rehim, Mohamed

2010-04-16

In the pharmaceutical industry the growing number of samples to be analyzed requires high throughput and fully automated analytical techniques. Commonly used sample-preparation methods are solid-phase extraction (SPE), liquid-liquid extraction (LLE) and protein precipitation. In this paper we will discus a new sample-preparation technique based on SPE for high throughput drug extraction developed and used by our group. This new sample-preparation method is based on monolithic methacrylate polymer as packing sorbent for 96-tip robotic device. Using this device a 96-well plate could be handled in 2-4min. The key aspect of the monolithic phase is that monolithic material can offer both good binding capacity and low back-pressure properties compared to e.g. silica phases. The present paper presents the successful application of monolithic 96-tips and LC-MS/MS by the sample preparation of busulphan, rescovitine, metoprolol, pindolol and local anaesthetics from human plasma samples and cyklophosphamid from mice blood samples. Copyright 2009 Elsevier B.V. All rights reserved.

Fiber-based monolithic columns for liquid chromatography.

PubMed

Ladisch, Michael; Zhang, Leyu

2016-10-01

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

Don’t Let the HumBUG Get Achoo - Tips for a healthy winter at work and home

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

Schlender, Michael H.

2006-12-15

Safety-related article for recurrinig column in the Tri-City Area Journal of Business. Focuses on seasonal wellness tips for employers and employees - namely, cold and flu prevention through personal hygiene.

Laboratory study on leachability of five herbicides in South Australian soils.

PubMed

Ying, G G; Williams, B

2000-03-01

Norflurazon, oxadiazon, oxyfluorfen, trifluralin and simazine are herbicides widely used in the vineyards of the Barossa Valley, South Australia. The leaching behaviour of norflurazon, oxadiazon, oxyfluorfen and trifluralin was investigated on four key soils in the Barossa Valley. Leaching potential on packed soil columns and actual mobility using intact soil columns were investigated. On the packed soil columns, norflurazon was the most leachable herbicide. More of the herbicides were detected in the leachates from the sandy soils (Mountadam and Nuriootpa) than from the clayey soils (Lyndoch and Tanunda). Organic matter is generally low in soils in the Barossa region. Porosity and saturated conductivity significantly affect herbicide movement and in the sandy Mountadam and Nuriootpa soils, the water flux is greater than for the higher clay content Lyndoch and Tanunda soils. Increasing the time interval between herbicide application and the incidence of "rainfall" reduced the amounts of herbicides found in the leachates. The use of intact soil columns and including simazine for comparison showed that both norflurazon and simazine were present in the leachates. Simazine was the first herbicide to appear in leachates. Sectioning of the intact soil columns after leaching clearly demonstrated that norflurazon and simazine reached the bottom of the soil columns for all soils studied. Greater amounts of norflurazon were retained in the soil columns compared with simazine. The other herbicides were mostly retained in the initial sections of the soil columns.

Functionalized nanoparticles based solid-phase membrane micro-tip extraction and high-performance liquid chromatography analyses of vitamin B complex in human plasma.

PubMed

Ali, Imran; Kulsum, Umma; Al-Othman, Zeid A; Alwarthan, Abdulrahman; Saleem, Kishwar

2016-07-01

Iron nanoparticles were prepared by a green method following functionalization using 1-butyl-3-methylimidazolium bromide. 1-Butyl-3-methylimidazole iron nanoparticles were characterized using FTIR spectroscopy, energy dispersive X-ray fluorescence, X-ray diffraction, scanning electron microscopy and transmission electron microscopy. The nanoparticles were used in solid-phase membrane micro-tip extraction to separate vitamin B complex from plasma before high-performance liquid chromatography. The optimum conditions obtained were sorbent (15 mg), agitation time (30 min), pH (9.0), desorbing solvent [water (5 mL) + methanol (5 mL) + sodium hydroxide (0.1 N) + acetic acid (d = 1.05 kg/L, pH 5.5), desorbing volume (10 mL) and desorption time (30 min). The percentage recoveries of all the eight vitamin B complex were from 60 to 83%. A high-performance liquid chromatography method was developed using a PhE column (250 × 4.6 mm, 5.0 μm) and water/acetonitrile (95:5, v/v; pH 4.0 with 0.1% formic acid) mobile phase. The flow rate was 1.0 mL/min with detection at 270 and 210 nm. The values of the capacity, separation and resolution factor were 0.57-39.47, 1.12-6.00 and 1.84-26.26, respectively. The developed sample preparation and chromatographic methods were fast, selective, inexpensive, economic and reproducible. The developed method can be applied for analyzing these drugs in biological and environmental matrices. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Detection biomarkers of lung cancer using mini-GC-PID system integrated with micro GC column and micro pre-concentrator

PubMed Central

2014-01-01

The survival rate of lung cancer can be significantly improved by monitoring biomarkers in exhaled air that indicate diseases in early stage, so it is very important to develop micro analytical systems which can offer a fast, on-site, real-time detecting biomarkers in exhaled air. In this paper, a mini-gas chromatography (GC)-photo-ionization detector (PID) system integrated with a micro GC column and a micro pre-concentrator was developed for forming an inexpensive, fast, and non-invasive diagnostic tool for lung cancer. This system has very strong concentrate ability owing to its integrated micro pre-concentrator, which make the detection of trace components in exhaled air very easy. In addition, the integrated micro GC column can separate complex mixtures, which overcome low resolution and poor anti-interference ability of other instruments. The results indicated that the mini-GC-PID system can effectively separate and detect the biomarkers at parts-per-billion (ppb) level. PMID:25339856

Automated solid-phase extraction and liquid chromatography for assay of cyclosporine in whole blood.

PubMed

Kabra, P M; Wall, J H; Dimson, P

1987-12-01

In this rapid, precise, accurate, cost-effective, automated liquid-chromatographic procedure for determining cyclosporine in whole blood, the cyclosporine is extracted from 0.5 mL of whole blood together with 300 micrograms of cyclosporin D per liter, added as internal standard, by using an Advanced Automated Sample Processing unit. The on-line solid-phase extraction is performed on an octasilane sorbent cartridge, which is interfaced with a RP-8 guard column and an octyl analytical column, packed with 5-microns packing material. Both columns are eluted with a mobile phase containing acetonitrile/methanol/water (53/20/27 by vol) at a flow rate of 1.5 mL/min and column temperature of 70 degrees C. Absolute recovery of cyclosporine exceeded 85% and the standard curve was linear to 5000 micrograms/L. Within-run and day-to-day CVs were less than 8%. Correlation between automated and manual Bond-Elut extraction methods was excellent (r = 0.987). None of 18 drugs and four steroids tested interfered.

Mini-columns for Conducting Breakthrough Experiments. Design and Construction

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

Dittrich, Timothy M.; Reimus, Paul William; Ware, Stuart Douglas

Experiments with moderately and strongly sorbing radionuclides (i.e., U, Cs, Am) have shown that sorption between experimental solutions and traditional column materials must be accounted for to accurately determine stationary phase or porous media sorption properties (i.e., sorption site density, sorption site reaction rate coefficients, and partition coefficients or K d values). This report details the materials and construction of mini-columns for use in breakthrough columns to allow for accurate measurement and modeling of sorption parameters. Material selection, construction techniques, wet packing of columns, tubing connections, and lessons learned are addressed.

Catalyst-induced growth of carbon nanotubes on tips of cantilevers and nanowires

DOEpatents

Lee, James Weifu; Lowndes, Douglas H.; Merkulov, Vladimir I.; Eres, Gyula; Wei, Yayi; Greenbaum, Elias; Lee, Ida

2004-06-29

A method is described for catalyst-induced growth of carbon nanotubes, nanofibers, and other nanostructures on the tips of nanowires, cantilevers, conductive micro/nanometer structures, wafers and the like. The method can be used for production of carbon nanotube-anchored cantilevers that can significantly improve the performance of scaning probe microscopy (AFM, EFM etc). The invention can also be used in many other processes of micro and/or nanofabrication with carbon nanotubes/fibers. Key elements of this invention include: (1) Proper selection of a metal catalyst and programmable pulsed electrolytic deposition of the desired specific catalyst precisely at the tip of a substrate, (2) Catalyst-induced growth of carbon nanotubes/fibers at the catalyst-deposited tips, (3) Control of carbon nanotube/fiber growth pattern by manipulation of tip shape and growth conditions, and (4) Automation for mass production.

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.

Sustainable Blended Cements-Influences of Packing Density on Cement Paste Chemical Efficiency.

PubMed

Knop, Yaniv; Peled, Alva

2018-04-18

This paper addresses the development of blended cements with reduced clinker amount by partial replacement of the clinker with more environmentally-friendly material (e.g., limestone powders). This development can lead to more sustainable cements with reduced greenhouse gas emission and energy consumption during their production. The reduced clicker content was based on improved particle packing density and surface area of the cement powder by using three different limestone particle diameters: smaller (7 µm, 3 µm) or larger (70 µm, 53 µm) than the clinker particles, or having a similar size (23 µm). The effects of the different limestone particle sizes on the chemical reactivity of the blended cement were studied by X-ray diffraction (XRD), thermogravimetry and differential thermogravimetry (TG/DTG), loss on ignition (LOI), isothermal calorimetry, and the water demand for reaching normal consistency. It was found that by blending the original cement with limestone, the hydration process and the reactivity of the limestone itself were increased by the increased surface area of the limestone particles. However, the carbonation reaction was decreased with the increased packing density of the blended cement with limestone, having various sizes.

Multistep continuous-flow synthesis of (R)- and (S)-rolipram using heterogeneous catalysts

NASA Astrophysics Data System (ADS)

Tsubogo, Tetsu; Oyamada, Hidekazu; Kobayashi, Shū

2015-04-01

Chemical manufacturing is conducted using either batch systems or continuous-flow systems. Flow systems have several advantages over batch systems, particularly in terms of productivity, heat and mixing efficiency, safety, and reproducibility. However, for over half a century, pharmaceutical manufacturing has used batch systems because the synthesis of complex molecules such as drugs has been difficult to achieve with continuous-flow systems. Here we describe the continuous-flow synthesis of drugs using only columns packed with heterogeneous catalysts. Commercially available starting materials were successively passed through four columns containing achiral and chiral heterogeneous catalysts to produce (R)-rolipram, an anti-inflammatory drug and one of the family of γ-aminobutyric acid (GABA) derivatives. In addition, simply by replacing a column packed with a chiral heterogeneous catalyst with another column packed with the opposing enantiomer, we obtained antipole (S)-rolipram. Similarly, we also synthesized (R)-phenibut, another drug belonging to the GABA family. These flow systems are simple and stable with no leaching of metal catalysts. Our results demonstrate that multistep (eight steps in this case) chemical transformations for drug synthesis can proceed smoothly under flow conditions using only heterogeneous catalysts, without the isolation of any intermediates and without the separation of any catalysts, co-products, by-products, and excess reagents. We anticipate that such syntheses will be useful in pharmaceutical manufacturing.

Silicon Nanotips Antireflection Surface for Micro Sun Sensor

NASA Technical Reports Server (NTRS)

Bae, Sam Y.; Lee, Choonsup; Mobasser, Sohrab; Manohara, Harish

2006-01-01

We have developed a new technique to fabricate antireflection surface using silicon nano-tips for use on a micro sun sensor for Mars rovers. We have achieved randomly distributed nano-tips of radius spanning from 20 nm to 100 nm and aspect ratio of 200 using a two-step dry etching process. The 30(deg) specular reflectance at the target wavelength of 1 (mu)m is only about 0.09 %, nearly three orders of magnitude lower than that of bare silicon, and the hemispherical reflectance is 8%. By changing the density and aspect ratio of these nanotips, the change in reflectance is demonstrated. Using surfaces covered with these nano-tips, the critical problem of ghost images that are caused by multiple internal reflections in a micro sun sensor was solved.

Improved efficiency of ZnO hierarchical particle based dye sensitized solar cell by incorporating thin passivation layer in photo-anode

NASA Astrophysics Data System (ADS)

Das, Priyanka; Mondal, Biswanath; Mukherjee, Kalisadhan

2018-01-01

Present article describes the DSSC performances of photo-anodes prepared using hydrothermal route derived ZnO particles having dissimilar morphologies i.e. simple micro-rod and nano-tips decorated micro-rod. The surface of nano-tips decorated micro-rod is uneven and patterned which facilitate more dye adsorption and better scattering of the incident light resulting superior photo-conversion efficiency (PCE) ( η 1.09%) than micro-rod ZnO ( η 0.86%). To further improve the efficiency of nano-tips decorated micro-rod ZnO based DSSC, thin passivation layer of ZnO is introduced in the corresponding photo-anode and a higher PCE ( η 1.29%) is achieved. The compact thin passivation layer here expedites the transportation of photo-excited electrons, restricts the undesired recombination reactions and prevents the direct contact of electrolyte with conducting substrates. Attempt is made to understand the effect of passivation layer on the transportation kinetics of photo-excited electrons by analyzing the electrochemical impedance spectra of the developed cells.

How changing the particle structure can speed up protein mass transfer kinetics in liquid chromatography.

PubMed

Gritti, Fabrice; Horvath, Krisztian; Guiochon, Georges

2012-11-09

The mass transfer kinetics of a few compounds (uracil, 112 Da), insulin (5.5 kDa), lysozyme (13.4 kDa), and bovine serum albumin (BSA, 67 kDa) in columns packed with several types of spherical particles was investigated under non-retained conditions, in order to eliminate the poorly known contribution of surface diffusion to overall sample diffusivity across the porous particles in RPLC. Diffusivity across particles is then minimum. Based on the porosity of the particles accessible to analytes, it was accurately estimated from the elution times, the internal obstruction factor (using Pismen correlation), and the hindrance diffusion factor (using Renkin correlation). The columns used were packed with fully porous particles 2.5 μm Luna-C(18) 100 Å, core-shell particles 2.6 μm Kinetex-C(18) 100 Å, 3.6 μm Aeris Widepore-C(18) 200 Å, and prototype 2.7 μm core-shell particles (made of two concentric porous shells with 100 and 300 Å average pore size, respectively), and with 3.3 μm non-porous silica particles. The results demonstrate that the porous particle structure and the solid-liquid mass transfer resistance have practically no effect on the column efficiency for small molecules. For them, the column performance depends principally on eddy dispersion (packing homogeneity), to a lesser degree on longitudinal diffusion (effective sample diffusivity along the packed bed), and only slightly on the solid-liquid mass transfer resistance (sample diffusivity across the particle). In contrast, for proteins, this third HETP contribution, hence the porous particle structure, together with eddy dispersion govern the kinetic performance of columns. Mass transfer kinetics of proteins was observed to be fastest for columns packed with core-shell particles having either a large core-to-particle ratio or having a second, external, shell made of a thin porous layer with large mesopores (200-300 Å) and a high porosity (~/=0.5-0.7). The structure of this external shell seems to speed up the penetration of proteins into the particles. A stochastic model of the penetration of bulky proteins driven by a concentration gradient across an infinitely thin membrane of known porosity and pore size is suggested to explain this mechanism. Yet, under retained conditions, surface diffusion speeds up the mass transfer into the mesopores and levels the kinetic performance of particles built with either one or two porous shells. Copyright © 2012 Elsevier B.V. All rights reserved.

Casingless down-hole for sealing an ablation volume and obtaining a sample for analysis

DOEpatents

Noble, Donald T.; Braymen, Steven D.; Anderson, Marvin S.

1996-10-01

A casing-less down hole sampling system for acquiring a subsurface sample for analysis using an inductively coupled plasma system is disclosed. The system includes a probe which is pushed into the formation to be analyzed using a hydraulic ram system. The probe includes a detachable tip member which has a soil point mad a barb, with the soil point aiding the penetration of the earth, and the barb causing the tip member to disengage from the probe and remain in the formation when the probe is pulled up. The probe is forced into the formation to be tested, and then pulled up slightly, to disengage the tip member and expose a column of the subsurface formation to be tested. An instrumentation tube mounted in the probe is then extended outward from the probe to longitudinally extend into the exposed column. A balloon seal mounted on the end of the instrumentation tube allows the bottom of the column to be sealed. A source of laser radiation is emitted from the instrumentation tube to ablate a sample from the exposed column. The instrumentation tube can be rotated in the probe to sweep the laser source across the surface of the exposed column. An aerosol transport system carries the ablated sample from the probe to the surface for testing in an inductively coupled plasma system. By testing at various levels in the down-hole as the probe is extracted from the soil, a profile of the subsurface formation may be obtained.

The Joule-Thomson coefficient as a criterion for efficient operating conditions in supercritical fluid chromatography.

PubMed

Poe, Donald P; Helmueller, Shawn; Kobany, Stephanie; Feldhacker, Hannah; Kaczmarski, Krzysztof

2017-01-27

When an SFC column is operated in a traditional oven with forced air at low pressures near the critical temperature, severe efficiency losses can occur. The mobile phase cools as it expands along the column, forming axial and radial temperature gradients. In this study we present a simple model based on a virtual fluid to predict the conditions which lead to the onset of efficiency loss. The model shows that the Joule-Thomson coefficient is an important factor leading to efficiency loss in packed columns under forced air conditions. The model was tested experimentally for elution of n-alkylbenzenes on 250×4.6-mm ID columns packed with 5-μm Luna-C18 (fully porous) and Kinetex-C18 (superficially porous) particles at optimum flow rates in a forced air oven at 20-80°C and outlet pressures from 90 to 250bar, with CO 2 mobile phase containing 5, 10 and 20% methanol (v/v). For simplicity, we used a formal J-T coefficient corresponding to the inlet temperature and the outlet pressure to characterize the chromatographic conditions. For 5% methanol, there was no significant loss of efficiency for elution of n-octadecylbenzene as long as the formal J-T coefficient was less than 0.11K/bar for Luna or 0.15K/bar for Kinetex, with minimum reduced plate heights equal to 1.82 and 1.55, respectively, at an average apparent retention factor of approximately 4.0 for both columns. The Kinetex column provided superior efficiency in general, and at 10-20bar lower outlet pressures relative to the Luna column due to the higher thermal conductivity of the packing. Results for 10 and 20% methanol showed similar trends but were less predictable. Copyright © 2016 Elsevier B.V. All rights reserved.

Group-III Nitride Field Emitters

NASA Technical Reports Server (NTRS)

Bensaoula, Abdelhak; Berishev, Igor

2008-01-01

Field-emission devices (cold cathodes) having low electron affinities can be fabricated through lattice-mismatched epitaxial growth of nitrides of elements from group III of the periodic table. Field emission of electrons from solid surfaces is typically utilized in vacuum microelectronic devices, including some display devices. The present field-emission devices and the method of fabricating them were developed to satisfy needs to reduce the cost of fabricating field emitters, make them compatible with established techniques for deposition of and on silicon, and enable monolithic integration of field emitters with silicon-based driving circuitry. In fabricating a device of this type, one deposits a nitride of one or more group-III elements on a substrate of (111) silicon or other suitable material. One example of a suitable deposition process is chemical vapor deposition in a reactor that contains plasma generated by use of electron cyclotron resonance. Under properly chosen growth conditions, the large mismatch between the crystal lattices of the substrate and the nitride causes strains to accumulate in the growing nitride film, such that the associated stresses cause the film to crack. The cracks lie in planes parallel to the direction of growth, so that the growing nitride film becomes divided into microscopic growing single-crystal columns. The outer ends of the fully-grown columns can serve as field-emission tips. By virtue of their chemical compositions and crystalline structures, the columns have low work functions and high electrical conductivities, both of which are desirable for field emission of electrons. From examination of transmission electron micrographs of a prototype device, the average column width was determined to be about 100 nm and the sharpness of the tips was determined to be characterized by a dimension somewhat less than 100 nm. The areal density of the columns was found to about 5 x 10(exp 9)/sq cm . about 4 to 5 orders of magnitude greater than the areal density of tips in prior field-emission devices. The electric field necessary to turn on the emission current and the current per tip in this device are both lower than in prior field-emission devices, such that it becomes possible to achieve longer operational lifetime. Moreover, notwithstanding the lower current per tip, because of the greater areal density of tips, it becomes possible to achieve greater current density averaged over the cathode area. The thickness of the grown nitride film (equivalently, the length of the columns) could lie between about 0.5 microns and a few microns; in any event, a thickness of about 1 micron is sufficient and costs less than do greater thicknesses. It may be possible to grow nitride emitter columns on glass or other substrate materials that cost less than silicon does. What is important in the choice of substrate material is the difference between the substrate and nitride crystalline structures. Inasmuch as the deposition process is nondestructive, an ability to grow emitter columns on a variety of materials would be advantageous in that it would facilitate the integration of field-emitter structures onto previously processed integrated circuits.

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.

Pack A Waste-Free Lunch

EPA Pesticide Factsheets

This page includes EPA's resources for students and teachers interested in hosting a waste-free lunch day at school. These resources include instructions, helpful tips, and directions for tracking success.

Size-exclusion chromatography using core-shell particles.

PubMed

Pirok, Bob W J; Breuer, Pascal; Hoppe, Serafine J M; Chitty, Mike; Welch, Emmet; Farkas, Tivadar; van der Wal, Sjoerd; Peters, Ron; Schoenmakers, Peter J

2017-02-24

Size-exclusion chromatography (SEC) is an indispensable technique for the separation of high-molecular-weight analytes and for determining molar-mass distributions. The potential application of SEC as second-dimension separation in comprehensive two-dimensional liquid chromatography demands very short analysis times. Liquid chromatography benefits from the advent of highly efficient core-shell packing materials, but because of the reduced total pore volume these materials have so far not been explored in SEC. The feasibility of using core-shell particles in SEC has been investigated and contemporary core-shell materials were compared with conventional packing materials for SEC. Columns packed with very small core-shell particles showed excellent resolution in specific molar-mass ranges, depending on the pore size. The analysis times were about an order of magnitude shorter than what could be achieved using conventional SEC columns. Copyright © 2016 Elsevier B.V. All rights reserved.

Novel chiral core-shell silica microspheres with trans-(1R,2R)-diaminocyclohexane bridged in the mesoporous shell: synthesis, characterization and application in high performance liquid chromatography.

PubMed

Wu, Xiabing; You, Linjun; Di, Bin; Hao, Weiqiang; Su, Mengxiang; Gu, Yu; Shen, Lingling

2013-07-19

Novel chiral core-shell silica microspheres with trans-(1R,2R)-diaminocyclohexane (DACH) moiety bridged in the mesoporous shell were synthesized using layer-by-layer method. The chiral mesoporous shell around the nonporous silica core was formed by the co-condensation of N,N'-bis-[(triethoxysilyl)propyl]-trans-(1R,2R)-bis-(ureido)-cyclohexane (DACH-BS) and tetraethoxysilane (TEOS) using octadecyltrimethylammonium chloride (C18TMACl) and triblock poly(ethylene oxide)-b-poly(propylene oxide)-b-poly(ethylene oxide) copolymer (P123) as the templates. The functionalized core-shell silica microspheres were characterized and tested as chiral stationary phases for high performance liquid chromatography (HPLC). R/S-1,1'-bi-2,2'-naphthol, R/S-6,6'-dibromo-1,1'-bi-2-naphthol and R/S-1,1'-bi-2,2'-phenanthrol were enantioseparated rapidly on the column packed with the DACH core-shell silica particles. Moreover, the column packed with core-shell particles exhibited better performance than the column packed with the DACH functionalized periodic mesoporous organosilicas. Copyright © 2013 Elsevier B.V. All rights reserved.

Comparison between the loading capacities of columns packed with partially and totally porous fine particles. What is the effective surface area available for adsorption?

PubMed

Gritti, Fabrice; Guiochon, Georges

2007-12-28

The adsorption isotherms of phenol, caffeine, insulin, and lysozyme were measured on two C(18)-bonded silica columns. The first one was packed with classical totally porous particles (3 microm Luna(2)-C(18)from Phenomenex, Torrance, CA, USA), the second one with shell particles (2.7 microm Halo-C(18) from Advanced Materials Technology, Wilmington, DE, USA). The measurements were made at room temperature (T=295+/-1K), using mainly frontal analysis (FA) and also elution by characteristic points (FACP) when necessary. The adsorption energy distributions (AEDs) were estimated by the iterative numerical expectation-maximization (EM) procedure and served to justify the choice of the best adsorption isotherm model for each compound. The best isotherm parameters were derived from either the best fit of the experimental data to a multi-Langmuir isotherm model (MLRA) or from the AED results (equilibrium constants and saturation capacities), when the convergence of the EM program was achieved. The experiments show than the loading capacity of the Luna column is more than twice that of the Halo column for low-molecular-weight compounds. This result was expected; it is in good agreement with the values of the accessible surface area of these two materials, which were calculated from the pore size volume distributions. The pore size volume distributions are validated by the excellent agreement between the calculated and measured exclusion volumes of polystyrene standards by inverse size exclusion chromatography (ISEC). In contrast, the loading capacity ratio of the two columns is 1.5 or less with insulin and lysozyme. This is due to a significant exclusion of these two proteins from the internal pore volumes of the two packing materials. This result raises the problem of the determination of the effective surface area of the packing material, particularly in the case of proteins. This area is about 40 and 30% of the total surface area for insulin and for lysozyme, respectively, based on the pore size volume distribution validated by the ISEC method. The ISEC experiments showed that the largest and the smallest mesopores have rather a cylindrical and a spherical shape, respectively, for both packing materials.

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

Adams, W.D.

Passive solar heating was used in a still in which a packed column packed with popped popcorn separates the alcohol and water vapors. The still's performance was not satisfactory, and it is concluded that passive solar heating could have been better used to preheat makeup water for the fermentation process and to maintain proper fermentation temperatures during the winter. (LEW)

Continuous, packed-bed, enzymatic bioreactor production and stability of feruloyl soy glycerides

USDA-ARS?s Scientific Manuscript database

The synthesis of feruloyl soy glycerides was demonstrated on a pilot-scale (1 metric ton/year) in a continuous, four-column series, packed-bed, enzymatic bioreactor (herinafter referred to as the bioreactor). Ethyl ferulate and soybean oil were combined and converted at 3.5 kg/d over Candida antarti...

Chemical Oxygen Demand abatement in sewage using Micro-Aeration Enhanced Ecological Floating Bed

NASA Astrophysics Data System (ADS)

Shi, Hongle; Zhou, Gaofeng; Liu, Yiqing; Tan, Jiancong; Fu, Yongsheng

2018-02-01

The traditional ecological floating bed combined with micro-aeration system and artificial medium was developed for the removal of contaminants and remediation of surface water. This micro-aeration enhanced ecological floating bed (MAEEFB) consisted of aeration unit, microbial processing unit and aquatic plant unit. Batch experiments were conducted in different operating conditions on the removal of chemical oxygen demand (COD) in the sewage using MAEEFB. The removal rate of COD by MAEEFB, enhanced ecological floating bed (EEFB) and traditional ecological floating bed (TEFB) in the same reaction conditions was 59.2%, 56.9% and 30.6%, respectively, indicating that the combination of micro-aeration system and artificial medium could enhance the removal efficiency of COD in TEFB. In MAEEFB, the aeration intensity should be designed reasonablely considering both treatment efficiency and operation cost. Only increasing the specific surface area of the packing cannot effectively improve the purification efficiency of water. Factors like packing material, ability of intercepting organics and complicated extent of microorganisms attaching on the packing should also be considered.

A universal piezo-driven ultrasonic cell microinjection system.

PubMed

Huang, Haibo; Mills, James K; Lu, Cong; Sun, Dong

2011-08-01

Over the past decade, the rapid development of biotechnologies such as gene injection, in-vitro fertilization, intracytoplasmic sperm injection (ICSI) and drug development have led to great demand for highly automated, high precision equipment for microinjection. Recently a new cell injection technology using piezo-driven pipettes with a very small mercury column was proposed and successfully applied in ICSI to a variety of mammal species. Although this technique significantly improves the survival rates of the ICSI process, shortcomings due to the toxicity of mercury and damage to the cell membrane due to large lateral tip oscillations of the injector pipette may limit its application. In this paper, a new cell injection system for automatic batch injection of suspended cells is developed. A new design of the piezo-driven cell injector is proposed for automated suspended cell injection. This new piezo-driven cell injector design relocates the piezo oscillation actuator to the injector pipette which eliminates the vibration effect on other parts of the micromanipulator. A small piezo stack is sufficient to perform the cell injection process. Harmful lateral tip oscillations of the injector pipette are reduced substantially without the use of a mercury column. Furthermore, ultrasonic vibration micro-dissection (UVM) theory is utilized to analyze the piezo-driven cell injection process, and the source of the lateral oscillations of the injector pipette is investigated. From preliminary experiments of cell injection of a large number of zebrafish embryos (n = 200), the injector pipette can easily pierce through the cell membrane at a low injection speed and almost no deformation of the cell wall, and with a high success rate(96%) and survival rate(80.7%) This new injection approach shows good potential for precision injection with less damage to the injected cells.

Contexts for Column Addition and Subtraction

ERIC Educational Resources Information Center

Lopez Fernandez, Jorge M.; Velazquez Estrella, Aileen

2011-01-01

In this article, the authors discuss their approach to column addition and subtraction algorithms. Adapting an original idea of Paul Cobb and Erna Yackel's from "A Contextual Investigation of Three-Digit Addition and Subtraction" related to packing and unpacking candy in a candy factory, the authors provided an analogous context by…

[Determination of ten photoinitiators in fruit juices and tea beverages by solid-phase micro-extraction coupled with gas chromatography/mass spectrometry].

PubMed

Liu, Pengyan; Chen, Yanjie; Zhao, Chunxia; Tian, Lei

2013-12-01

A method for the determination of ten photoinitiators (PIs), benzophenone, ethyl 4-dimethylaminobenzoate, 1-hydroxycyclohexyl-phenylketone, 4-methylbenzophenone, 2-ethylhexyl-4-dimethylaminobenzoate, 4-chlorobenzophenone, 2-chlorothioxanthone, 2-isopropylthio-xanthone, 2,2-dimethoxy-2-phenylacetophenone, methyl 2-benzoylbenzoate, in 13 kinds of fruit juice and 3 kinds of tea beverage has been established, using solid-phase micro-extraction (SPME) combined with chromatography/mass spectrometry (GC/MS). At first, the major factors of SPME, extraction time and temperature, were studied through orthogonal experiment. Then the optimal operation conditions were obtained via the refinement of various factors. After the sample was extracted by SPME, it was desorbed for target analytes in sampling inlet for 3 min, and separated on an HP-5MS column, then detected by MS in selected ion monitoring mode, and quantified through calibration curve. The working curves were obtained using sample matrix in order to eliminate the matrix interference. The linear range was from 0.3 microg/L to 60 microg/L and the detection limit range was from 3 ng/L to 16 ng/L. The samples were determined five times with four different spiked levels individually and the relative standard deviations of all the samples were less than 14.5%. This determination method was applied in 16 kinds of packed beverages with different brands and different species. Benzophenone had been detected from all the samples. 4-Methylbenzophenone, 2-ethylhexyl-4-dimethylaminobenzoate, 2-isopropylthioxanthone, 1-hydroxycyclohexyl-phenylketone and 2-chlorothioxanthone had been detected from a portion of samples. Simultaneous determination was achieved for the ten PIs. These results provide a reference to determine the PIs migrated from packing materials in beverage. This method is simple, high sensitive and non-polluting.

Chemical factors influencing colloid-facilitated transport of contaminants in porous media

USGS Publications Warehouse

Roy, Sujoy B.; Dzombak, David A.

1997-01-01

The effects of colloids on the transport of two strongly sorbing solutesa hydrophobic organic compound, phenanthrene, and a metal ion, Ni2+were studied in sand-packed laboratory columns under different pH and ionic strength conditions. Two types of column experiments were performed as follows:  (i) sorption/mobilization experiments where the contaminant was first sorbed in the column under conditions where no colloids were released and mobilized under conditions where colloids were released as a result of ionic strength reduction in the influent; and (ii) transport experiments where the contaminant, dissolved or sorbed on colloids, was injected into columns packed with a strongly sorbing porous medium. In the first type of experiment, contaminant mobilization was significant only when all releasable colloids were flushed from the column. In all other cases, although high colloid particle concentrations were encountered, there was no marked effect on total contaminant concentrations. In the second type of experiment, colloid deposition efficiencies were shown to control the enhancement of transport. The deposition efficiency was a function of the pH (for a high organic content sand) and of the contaminant concentration (for a charged species such as Ni2+).

Linking Water Table Dynamics to Carbon Cycling in Artificial Soil Column Incubations

NASA Astrophysics Data System (ADS)

Geertje, Pronk; Adrian, Mellage; Tatjana, Milojevic; Fereidoun, Rezanezhad; Cappellen Philippe, Van

2016-04-01

The biogeochemistry of wetlands soils is closely tied to their hydrology. Water table fluctuations that cause flooding and drying of these systems may lead to enhanced degradation of organic matter and release of greenhouse gasses (e.g. CO2, CH4) to the atmosphere. However, predicting the influence of water table fluctuations on the biogeochemical functioning of soils requires an understanding of the interactions of soil hydrology with biogeochemical and microbial processes. To determine the effects of water table dynamics on carbon cycling, we are carrying out state-of-the-art automated soil column experiments with fully integrated monitoring of hydro-bio-geophysical process variables under both constant and oscillating water table conditions. An artificial, homogeneous mixture consisting of minerals and organic matter is used to provide a well-defined starting material. The artificial soils are composed of quartz sand, montmorillonite, goethite and humus from a forested riparian zone, from which we also extracted the microbial inoculum added to the soil mixture. The artificial soils are packed into 60 cm high, 7.5 cm wide columns. In the currently ongoing experiment, three replicate columns are incubated while keeping the water table constant water at mid-depth, while another three columns alternate between drained and saturated conditions. Micro-sensors installed at different depths below the soil surface record time-series redox potentials (Eh) varying between oxidizing (~+700 mV) and reducing (~-200 mV) conditions. Continuous O2 levels throughout the soil columns are monitored using high-resolution, luminescence-based, Multi Fiber Optode (MuFO) microsensors. Pore waters are collected periodically with MicroRhizon samplers from different depths, and analyzed for pH, EC, dissolved inorganic and organic carbon and ion/cation compositions. These measurements allow us to track the changes in pore water geochemistry and relate them to differences in carbon cycling between the contrasting water table regimes. Particular attention is given to the mobilization and redistribution of iron from the initially homogeneously distributed goethite. In addition, small solid-phase samples are collected monthly from the saturated and unsaturated zones of the soil columns to characterize the microbial communities and changes in soil microstructure and organo-mineral associations. Headspace gas measurements are used to derive the effluxes of CO2 and CH4 during the experiment. Together, the experimental data will provide a comprehensive picture of the early development of the soil and the accompanying establishment of biogeochemical gradients under dynamic hydrological conditions. They will allow us to relate the degradation of soil organic matter and greenhouse gas emissions to the saturation conditions and redox chemistry under controlled conditions. The experiment is in progress with an expected total duration of 6 months.

Self-regenerating column chromatography

DOEpatents

Park, Woo K.

1995-05-30

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

Transport of viruses through saturated and unsaturated columns packed with sand

USGS Publications Warehouse

Anders, R.; Chrysikopoulos, C.V.

2009-01-01

Laboratory-scale virus transport experiments were conducted in columns packed with sand under saturated and unsaturated conditions. The viruses employed were the male-specific RNA coliphage, MS2, and the Salmonella typhimurium phage, PRD1. The mathematical model developed by Sim and Chrysikopoulos (Water Resour Res 36:173-179, 2000) that accounts for processes responsible for removal of viruses during vertical transport in one-dimensional, unsaturated porous media was used to fit the data collected from the laboratory experiments. The liquid to liquid-solid and liquid to air-liquid interface mass transfer rate coefficients were shown to increase for both bacteriophage as saturation levels were reduced. The experimental results indicate that even for unfavorable attachment conditions within a sand column (e.g., phosphate-buffered saline solution; pH = 7.5; ionic strength = 2 mM), saturation levels can affect virus transport through porous media. ?? Springer Science+Business Media B.V. 2008.

Impact of molecular packing on electronic polarization in organic crystals: the case of pentacene vs TIPS-pentacene.

PubMed

Ryno, Sean M; Risko, Chad; Brédas, Jean-Luc

2014-04-30

Polarization energy corresponds to the stabilization of the cation or anion state of an atom or molecule when going from the gas phase to the solid state. The decrease in ionization energy and increase in electron affinity in the solid state are related to the (electronic and nuclear) polarization of the surrounding atoms and molecules in the presence of a charged entity. Here, through a combination of molecular mechanics and quantum mechanics calculations, we evaluate the polarization energies in two prototypical organic semiconductors, pentacene and 6,13-bis(2-(tri-isopropylsilyl)ethynyl)pentacene (TIPS-pentacene). Comparison of the results for the two systems reveals the critical role played by the molecular packing configurations in the determination of the polarization energies and provides physical insight into the experimental data reported by Lichtenberger and co-workers (J. Amer. Chem. Soc. 2010, 132, 580; J. Phys. Chem. C 2010, 114, 13838). Our results underline that the impact of packing configurations, well established in the case of the charge-transport properties, also extends to the polarization properties of π-conjugated materials.

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

PubMed

Goyon, Alexandre; Guillarme, Davy; Fekete, Szabolcs

2017-02-20

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

Histological examination of the oral mucosa after fractional diode laser irradiation with different power and pulse duration

NASA Astrophysics Data System (ADS)

Belikov, Andrey V.; Ermolaeva, Ludmila A.; Korzhevsky, Dmitriy E.; Sergeeva, Elena S.; Semyashkina, Yulia V.; Antropova, Maria M.; Fedotov, Denis Y.; Zaitseva, Maria A.; Kashina, Tatiana V.

2018-04-01

Optical and histological methods were used to examination of influence the power and pulse duration of 980-nm diode laser to the dimensions and morphology of tissue around fractional micro injuries created by the radiation of that laser in the oral mucosa of rats in vivo. The power of laser radiation (P) varied in the range of 1÷21 W, and its pulse duration (tp) - in the range 50÷500 ms. Histological examination showed that in the mucosa of the oral cavity after the laser fractional irradiation, there following effects are found: a tissue defect, a transudate in the lumen of ablative micro injury, stretching and compacting effect of the nuclei of the basal epithelium, the disappearance of granules of the keratohialin, destroying the structure of the connective tissue, erythrocyte stasis in the vessels, the disappearance of transverse striation in the muscle fibers in muscle layer. It has been found that ablative micro injury begins to form up at P = 5 W, tp = 100 ms and affects only the epithelial layer of the mucosa. At P = 7 W, tp = 120 ms, the ratio of width to depth of ablative micro injury is 1 : 1, and at P = 10 W, tp = 100 ms, an ablative micro column with ratio of 1 : 1.5 is formed in the epithelial and submucosal layers of the mucosa. The laser effect with P = 15 W, tp = 200 ms leads to lengthening of the ablation micro-column to 1 : 2, with the bottom of the ablative micro column reaching the muscular layer. With a further growth of laser power or pulse duration, the width of the micro injury increases, and the growth of the micro injury depth is slowed down so that the micro column buildup is ceased.

Micro heat barrier

DOEpatents

Marshall, Albert C.; Kravitz, Stanley H.; Tigges, Chris P.; Vawter, Gregory A.

2003-08-12

A highly effective, micron-scale micro heat barrier structure and process for manufacturing a micro heat barrier based on semiconductor and/or MEMS fabrication techniques. The micro heat barrier has an array of non-metallic, freestanding microsupports with a height less than 100 microns, attached to a substrate. An infrared reflective membrane (e.g., 1 micron gold) can be supported by the array of microsupports to provide radiation shielding. The micro heat barrier can be evacuated to eliminate gas phase heat conduction and convection. Semi-isotropic, reactive ion plasma etching can be used to create a microspike having a cusp-like shape with a sharp, pointed tip (<0.1 micron), to minimize the tip's contact area. A heat source can be placed directly on the microspikes. The micro heat barrier can have an apparent thermal conductivity in the range of 10.sup.-6 to 10.sup.-7 W/m-K. Multiple layers of reflective membranes can be used to increase thermal resistance.

Reduction of TIP30 in esophageal squamous cell carcinoma cells involves promoter methylation and microRNA-10b

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

Dong, Wenjie, E-mail: dongwenjie200581@126.com; Shen, Ruizhe; Cheng, Shidan

2014-10-31

Highlights: • TIP30 expression is frequently suppressed in ESCC. • TIP30 was hypermethylated in ESCC. • Reduction of TIP30 was significantly correlated with LN metastasis. • miR-10b is a direct regulator of TIP30. - Abstract: TIP30 is a putative tumor suppressor that can promote apoptosis and inhibit angiogenesis. However, the role of TIP30 in esophageal squamous cell carcinoma (ESCC) biology has not been investigated. Immunohistochemistry was used to investigate the expression of TIP30 in 70 ESCC. Hypermethylation of TIP30 was evaluated by the methylation specific PCR (MSP) method in ESCC (tumor and paired adjacent non-tumor tissues). Lost expression of TIP30more » was observed in 50 of 70 (71.4%) ESCC. 61.4% (43 of 70) of primary tumors analyzed displayed TIP30 hypermethylation, indicating that this aberrant characteristic is common in ESCC. Moreover, a statistically significant inverse association was found between TIP30 methylation status and expression of the TIP30 protein in tumor tissues (p = 0.001). We also found that microRNA-10b (miR-10b) targets a homologous DNA region in the 3′untranslated region of the TIP30 gene and represses its expression at the transcriptional level. Reporter assay with 3′UTR of TIP30 cloned downstream of the luciferase gene showed reduced luciferase activity in the presence of miR-10b, providing strong evidence that miR-10b is a direct regulator of TIP30. These results suggest that TIP30 expression is regulated by promoter methylation and miR-10b in ESCC.« less

Treatment of highly polluted groundwater by novel iron removal process.

PubMed

Sim, S J; Kang, C D; Lee, J W; Kim, W S

2001-01-01

The removal of ferrous iron (Fe(II)) in groundwater has been generally achieved by simple aeration, or the addition of an oxidizing agent. Aeration has been shown to be very efficient in insolubilization ferrous iron at a pH level greater than 6.5. In this study, pH was maintained over 6.5 using limestone granules under constant aeration to oxidize ferrous iron in groundwater in a limestone packed column. A sedimentation unit coupled with a membrane filtration was also developed to precipitate and filtrate the oxidized ferric compound simultaneously. Several bench-scale studies, including the effects of the limestone granule sizes, amounts and hydraulic retention time on iron removal in the limestone packed column were investigated. It was found that 550 g/L of the 7-8 mesh size limestone granules, and 20 min of hydraulic retention time in the limestone packed column, were necessary for the sufficient oxidation of 40 mg/L of iron(II) in groundwater. Long-term operation was successfully achieved in contaminated waters by removing the iron deposits on the surface of the limestone granule by continuous aeration from the bottom of the column. Periodic reverse flow helped to remove caking and fouling of membrane surface caused by the continuous filtration. Recycling of the treated water from the membrane right after reverse flow operation made possible an admissible limit of iron concentration of the treated water for drinking. The pilot-scale process was constructed and has been tested in the rural area of Korea.

A novel bench-scale column assay to investigate site-specific nitrification biokinetics in biological rapid sand filters.

PubMed

Tatari, K; Smets, B F; Albrechtsen, H-J

2013-10-15

A bench-scale assay was developed to obtain site-specific nitrification biokinetic information from biological rapid sand filters employed in groundwater treatment. The experimental set-up uses granular material subsampled from a full-scale filter, packed in a column, and operated with controlled and continuous hydraulic and ammonium loading. Flowrates and flow recirculation around the column are chosen to mimic full-scale hydrodynamic conditions, and minimize axial gradients. A reference ammonium loading rate is calculated based on the average loading experienced in the active zone of the full-scale filter. Effluent concentrations of ammonium are analyzed when the bench-scale column is subject to reference loading, from which removal rates are calculated. Subsequently, removal rates above the reference loading are measured by imposing short-term loading variations. A critical loading rate corresponding to the maximum removal rate can be inferred. The assay was successfully applied to characterize biokinetic behavior from a test rapid sand filter; removal rates at reference loading matched those observed from full-scale observations, while a maximum removal capacity of 6.9 g NH4(+)-N/m(3) packed sand/h could easily be determined at 7.5 g NH4(+)-N/m(3) packed sand/h. This assay, with conditions reflecting full-scale observations, and where the biological activity is subject to minimal physical disturbance, provides a simple and fast, yet powerful tool to gain insight in nitrification kinetics in rapid sand filters. Copyright © 2013 Elsevier Ltd. All rights reserved.

Simple determination of betaine, l-carnitine and choline in human urine using self-packed column and column-switching ion chromatography with nonsuppressed conductivity detection.

PubMed

Wei, Dan; Zhu, Yan; Guo, Ming

2018-02-01

A sequential online extraction, clean-up and separation system for the determination of betaine, l-carnitine and choline in human urine using column-switching ion chromatography with nonsuppressed conductivity detection was developed in this work. A self-packed pretreatment column (50 × 4.6 mm, i.d.) was used for the extraction and clean-up of betaine, l-carnitine and choline. The separation was achieved using self-packed cationic exchange column (150 × 4.6 mm, i.d.), followed by nonsuppressed conductivity detection. Under optimized experimental conditions, the developed method presented good analytical performance, with excellent linearity in the range of 0.60-100 μg mL -1 for betaine, 0.75-100 μg mL -1 for l-carnitine and 0.50-100 μg mL -1 for choline, with all correlation coefficients (R 2 ) >0.99 in urine. The limits of detection were 0.15 μg mL -1 for betaine, 0.20 μg mL -1 for l-carnitine and 0.09 μg mL -1 for choline. The intra- and inter-day accuracy and precision for all quality controls were within ±10.32 and ±9.05%, respectively. Satisfactory recovery was observed between 92.8 and 102.0%. The validated method was successfully applied to the detection of urinary samples from 10 healthy people. The values detected in human urine using the proposed method showed good agreement with the measurement reported previously. Copyright © 2017 John Wiley & Sons, Ltd.

Identification of nonvolatile coal derived products via chromatography coupled with on-line FTIR detection. Quarterly progress report, March 1-May 31, 1985. [C/sub 2/H/sub 2/ extracts of ground coal, coffee and paprika

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

Taylor, L.T.

Because it has been our goal to interface the supercritical fluid chromatograph with a Fourier transform infrared spectrometer we have initially chosen packed columns due to their increased sample capacities, and supercritical CO/sub 2/ because of its infrared transparency. This paper compares two sampling techniques that can be utilized in packed column supercritical fluid Chromatography (SFC). Traditional sample introduction is accomplished using an injector with a sample loop. The loop is filled with the appropriate amount of material, and subsequently inserted into the mobile phase path. In most cases the sample must be either dissolved or extracted into an appropriatemore » solvent for such sample introduction. Note that unlike HPLC, where the solvent can be the same as the mobile phase, traditional sampling with SFC must use a solvent that is very different from the mobile phase. As a result, solvent peaks are almost always present, especially with universal detectors like FTIR. An alternative method is described here whereby both extraction of the sample and introduction of the extract onto the column is accomplished on-line using only the supercritical fluid mobile phase. This sampling technique is made possible by a simple valving scheme which ties directly the extraction vessel, the injector, the packed column and the detector. This technique has several advantages over the traditional methods, not the least of which is the absence of a large amount of foreign solvent introduced on the column. 11 refs., 7 figs.« less

Casingless down-hole for sealing an ablation volume and obtaining a sample for analysis

DOEpatents

Noble, D.T.; Braymen, S.D.; Anderson, M.S.

1996-10-01

A casing-less down hole sampling system for acquiring a subsurface sample for analysis using an inductively coupled plasma system is disclosed. The system includes a probe which is pushed into the formation to be analyzed using a hydraulic ram system. The probe includes a detachable tip member which has a soil point and a barb, with the soil point aiding the penetration of the earth, and the barb causing the tip member to disengage from the probe and remain in the formation when the probe is pulled up. The probe is forced into the formation to be tested, and then pulled up slightly, to disengage the tip member and expose a column of the subsurface formation to be tested. An instrumentation tube mounted in the probe is then extended outward from the probe to longitudinally extend into the exposed column. A balloon seal mounted on the end of the instrumentation tube allows the bottom of the column to be sealed. A source of laser radiation is emitted from the instrumentation tube to ablate a sample from the exposed column. The instrumentation tube can be rotated in the probe to sweep the laser source across the surface of the exposed column. An aerosol transport system carries the ablated sample from the probe to the surface for testing in an inductively coupled plasma system. By testing at various levels in the down-hole as the probe is extracted from the soil, a profile of the subsurface formation may be obtained. 9 figs.

A "Greenhouse Gas" Experiment for the Undergraduate Laboratory

ERIC Educational Resources Information Center

Gomez, Elaine; Paul, Melissa; Como, Charles; Barat, Robert

2014-01-01

This experiment and analysis offer an effective experience in greenhouse gas reduction. Ammoniated water is flowed counter-current to a simulated flue gas of air and CO2 in a packed column. The gaseous CO2 concentrations are measured with an on-line, non- dispersive, infrared analyzer. Column operating parameters include total gas flux, dissolved…

Investigation of holdup and axial dispersion of liquid phase in a catalytic exchange column using radiotracer technique.

PubMed

Kumar, Rajesh; Pant, H J; Goswami, Sunil; Sharma, V K; Dash, A; Mishra, S; Bhanja, K; Mohan, Sadhana; Mahajani, S M

2017-03-01

Holdup and axial dispersion of liquid phase in a catalytic exchange column were investigated by measuring residence time distributions (RTD) using a radiotracer technique. RTD experiments were independently carried out with two different types of packings i.e. hydrophobic water-repellent supported platinum catalyst and a mixture (50% (v/v)) of hydrophobic catalyst and a hydrophillic wettable packing were used in the column. Mean residence times and hold-ups of the liquid phase were estimated at different operating conditions. Axial dispersion model (ADM) and axial dispersion with exchange model (ADEM) were used to simulate the measured RTD data. Both the models were found equally suitable to describe the measured data. The degree of axial mixing was estimated in terms of Peclet number (Pe) and Bodenstein number (Bo). Based on the obtained parameters of the ADM, correlations for total liquid hold-up (H T ) and axial mixing in terms of Bo were proposed for design and scale up of the full-scale catalytic exchange column. Copyright © 2016 Elsevier Ltd. All rights reserved.

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

PubMed

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

2011-10-21

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

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

PubMed Central

Xu, Hongjuan; Weber, Stephen G.

2006-01-01

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

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

PubMed

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

2012-08-10

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

The Steerable Microcatheter: A New Device for Selective Catheterisation

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

Soyama, Takeshi; Yoshida, Daisuke; Sakuhara, Yusuke, E-mail: yusaku@med.hokudai.ac.jp

The steerable microcatheter (SwiftNINJA, Sumitomo Bakelite, Tokyo, Japan), which has a remote-controlled flexible tip manipulated using a dial in the handgrip, was recently developed and delivered to the market. This device enables the user to change the angle of the microcatheter tip manually, and potentially makes selective catheterisation easier. We evaluated its unique characteristics and utility in selective catheterisation and coil embolization. This article describes: (1) the advantages of this device in catheterisations involving acute angle branches, and (2) a new technique of compact coil packing with the use of intentional folding by the bendable tip of the catheter.

Future perspectives of using hollow fibers as structured packings in light hydrocarbon distillation

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

Yang, Dali; Orler, Bruce; Tornga, Stephanie

2011-01-26

Olefin and paraffin are the largest chemical commodities. Furthermore, they are major building blocks for the petrochemical industry. Each year, petroleum refining, consumes 4,500 TBtu/yr in separation energy, making it one of the most energy-intensive industries in the United States). Just considering liquefied petroleum gas (ethane/propane/butane) and olefins (ethylene and propylene) alone, the distillation energy consumption is about 400 TBtu/yr in the US. Since petroleum distillation is a mature technology, incremental improvements in column/tray design will only provide a few percent improvements in the performance. However, each percent saving in net energy use amounts to savings of 10 TBtu/yr andmore » reduces CO{sub 2} emissions by 0.2 MTon/yr. In practice, distillation columns require 100 to 200 trays to achieve the desired separation. The height of a transfer unit (HTU) of conventional packings is typical in the range of 36-60 inch. Since 2006, we had explored using several non-selective membranes as the structured packings to replace the conventional packing materials used in propane and propylene distillation. We obtained the lowest HTU of < 8 inch for the hollow fiber column, which was >5 times shorter than that of the conventional packing materials. In 2008, we also investigated this type of packing materials in iso-/n-butane distillation. Because of a slightly larger relative volatility of iso-/n-butane than that of propane/propylene, a wider and a more stable operational range was obtained for the iso-/n-butane pair. However, all of the experiments were conducted on a small scale with flowrate of < 25 gram/min. Recently, we demonstrated this technology on a larger scale (<250 gram/min). Within the loading range of F-factor < 2.2 Pa{sup 0.5}, a pressure drop on the vapor side is below 50 mbar/m, which suggests that the pressure drop of hollow fibers packings is not an engineering barrier for the applications in distillations. The thermal stability study suggests that polypropylene hollow fibers are stable after a long time exposure to C{sub 2} - C{sub 4} mixtures. The effects of packing density on the separation efficiency will be discussed.« less

Optical Fiber-Tip Sensors Based on In-Situ µ-Printed Polymer Suspended-Microbeams.

PubMed

Yao, Mian; Ouyang, Xia; Wu, Jushuai; Zhang, A Ping; Tam, Hwa-Yaw; Wai, P K A

2018-06-05

Miniature optical fiber-tip sensors based on directly µ-printed polymer suspended-microbeams are presented. With an in-house optical 3D μ-printing technology, SU-8 suspended-microbeams are fabricated in situ to form Fabry⁻Pérot (FP) micro-interferometers on the end face of standard single-mode optical fiber. Optical reflection spectra of the fabricated FP micro-interferometers are measured and fast Fourier transform is applied to analyze the cavity of micro-interferometers. The applications of the optical fiber-tip sensors for refractive index (RI) sensing and pressure sensing, which showed 917.3 nm/RIU to RI change and 4.29 nm/MPa to pressure change, respectively, are demonstrated in the experiments. The sensors and their optical µ-printing method unveil a new strategy to integrate complicated microcomponents on optical fibers toward 'lab-on-fiber' devices and applications.

New insights into the effects of support matrix on the removal of organic micro-pollutants and the microbial community in constructed wetlands.

PubMed

Zhang, Liang; Lyu, Tao; Ramírez Vargas, Carlos Andrés; Arias, Carlos A; Carvalho, Pedro N; Brix, Hans

2018-09-01

Constructed wetlands (CWs) are an eco-friendly and cost-effective technology to remove organic micro-pollutants (OMPs) from wastewater. The support matrix is an important component in CWs as it has a primary role in the growth and development of plants and microbes. However, the roles of the support matrix in CWs in removing OMPs have not been systematically studied. Therefore, in this study, six common materials (sand, zeolite, blast iron slag, petcoke, polonite and crushed autoclaved aerated concrete (CAAC)) as support matrixes were firstly investigated by batch tests to explore their adsorption capacities to selected OMPs (ibuprofen, iohexol, tebuconazole and imazalil). Results showed that the adsorption capacities of the materials were low (at the level of μg/g) compared to well-known sorbents (at the level of mg/g), such as activated carbon and carbon nanotubes. Columns packed with the six materials, respectively, were then built up to study the effects of different materials on microbial community. In the medium-term study (66 days), the removal of four OMPs in all the columns increased by 2-58% from day 25 to day 66, and was mainly attributed to microbial degradation. Furthermore, Community-level physiological profiling (CLPP) analysis indicates that material presence shaped the microbial community metabolic function not only in the interstitial water but also in the biofilm. Overall, all the findings demonstrate that although the adsorption capacities of the common materials are low, they may be a driver to improve the removal of OMPs by altering microbial community function in CWs. Copyright © 2018 Elsevier Ltd. All rights reserved.

Increase in the neutron yield from a dense plasma-focus experiment performed with a conical tip placed in the centre of the anode end

NASA Astrophysics Data System (ADS)

Kubes, P.; Paduch, M.; Cikhardt, J.; Cikhardtova, B.; Klir, D.; Kravarik, J.; Rezac, K.; Zielinska, E.; Sadowski, M. J.; Szymaszek, A.; Tomaszewski, K.; Zaloga, D.

2017-09-01

The paper describes the evolution of self-organized structures inside a pinched plasma column during the phase of the effective production of fusion neutrons, as observed in the mega-ampere plasma focus experiment performed with a conical tip placed in the centre of the anode face. In a comparison with the plane anode face configuration, the described anode shape facilitated transformations in the pinch column during the neutron production and increased the neutron yield several times. Simultaneously, it decreased the minimal diameter and the length of the pinched column, and it depressed the first neutron pulse. It also induced shorter pulses of X-rays and neutrons, which enabled the determination of a temporal difference between the emission of electron and deuteron beams. The fast electrons were produced mainly during a disruption of the pinch constriction, while the fast deuterons - during the formation and explosion of plasmoids. The paper also presents the temporal evolution of a current distribution in the plasmoid during the neutron production, as well as the appearance and stable positions of current filaments traces upon the surface of the conical anode tip.

A novel carbon tipped single micro-optrode for combined optogenetics and electrophysiology

PubMed Central

Vizvári, Attila D.; Bali, Zsolt K.; Márki, Balázs; Nagy, Lili V.; Kónya, Zoltán; Madarász, Dániel; Henn-Mike, Nóra; Varga, Csaba; Hernádi, István

2018-01-01

Optical microelectrodes (optrodes) are used in neuroscience to transmit light into the brain of a genetically modified animal to evoke and record electrical activity from light-sensitive neurons. Our novel micro-optrode solution integrates a light-transmitting 125 micrometer optical fiber and a 9 micrometer carbon monofilament to form an electrical lead element, which is contained in a borosilicate glass sheathing coaxial arrangement ending with a micrometer-sized carbon tip. This novel unit design is stiff and slender enough to be used for targeting deep brain areas, and may cause less tissue damage compared with previous models. The center-positioned carbon fiber is less prone to light-induced artifacts than side-lit metal microelectrodes previously presented. The carbon tip is capable of not only recording electrical signals of neuronal origin but can also provide valuable surface area for electron transfer, which is essential in electrochemical (voltammetry, amperometry) or microbiosensor applications. We present details of design and manufacture as well as operational examples of the newly developed single micro-optrode, which includes assessments of 1) carbon tip length–impedance relationship, 2) light transmission capabilities, 3) photoelectric artifacts in carbon fibers, 4) responses to dopamine using fast-scan cyclic voltammetry in vivo, and 5) optogenetic stimulation and spike or local field potential recording from the rat brain transfected with channelrhodopsin-2. With this work, we demonstrate that our novel carbon tipped single micro-optrode may open up new avenues for use in optogenetic stimulation when needing to be combined with extracellular recording, electrochemical, or microbiosensor measurements performed on a millisecond basis. PMID:29513711

Surface chemical effects on colloid stability and transport through natural porous media

USGS Publications Warehouse

Puls, Robert W.; Paul, Cynthia J.; Clark, Donald A.

1993-01-01

Surface chemical effects on colloidal stability and transport through porous media were investigated using laboratory column techniques. Approximately 100 nm diameter, spherical, iron oxide particles were synthesized as the mobile colloidal phase. The column packing material was retrieved from a sand and gravel aquifer on Cape Cod, MA. Previous studies have indicated enhanced stability and transport of iron oxide particles due to specific adsorption of some inorganic anions on the iron oxide surface. This phenomenon was further evaluated with an anionic surfactant, sodium dodecyl sulfate. Surfactants constitute a significant mass of the contaminant loading at the Cape Cod site and their presence may contribute to colloidal transport as a significant transport mechanism at the site. Other studies at the site have previously demonstrated the occurrence of this transport mechanism for iron phosphate particles. Photon correlation spectroscopy, micro-electrophoretic mobility, and scanning electron microscopy were used to evaluate particle stability, mobility and size. Adsorption of negatively charged organic and inorganic species onto the surface of the iron oxide particles was shown to significantly enhance particle stability and transport through alterations of the electrokinetic properties of the particle surface. Particle breakthrough generally occurred simultaneously with tritiated water, a conservative tracer. The extent of particle breakthrough was primarily dependent upon colloidal stability and surface charge.

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.

Treatment of acid rock drainage using a sulfate-reducing bioreactor with zero-valent iron.

PubMed

Ayala-Parra, Pedro; Sierra-Alvarez, Reyes; Field, James A

2016-05-05

This study assessed the bioremediation of acid rock drainage (ARD) in flow-through columns testing zero-valent iron (ZVI) for the first time as the sole exogenous electron donor to drive sulfate-reducing bacteria in permeable reactive barriers. Columns containing ZVI, limestone or a mixture of both materials were inoculated with an anaerobic mixed culture and fed a synthetic ARD containing sulfuric acid and heavy metals (initially copper, and later also cadmium and lead). ZVI significantly enhanced sulfate reduction and the heavy metals were extensively removed (>99.7%). Solid-phase analyses showed that heavy metals were precipitated with biogenic sulfide in the columns packed with ZVI. Excess sulfide was sequestered by iron, preventing the discharge of dissolved sulfide. In the absence of ZVI, heavy metals were also significantly removed (>99.8%) due to precipitation with hydroxide and carbonate ions released from the limestone. Vertical-profiles of heavy metals in the columns packing, at the end of the experiment, demonstrated that the ZVI columns still had excess capacity to remove heavy metals, while the capacity of the limestone control column was approaching saturation. The ZVI provided conditions that enhanced sulfate reduction and generated alkalinity. Collectively, the results demonstrate an innovative passive ARD remediation process using ZVI as sole electron-donor. Copyright © 2016 Elsevier B.V. All rights reserved.

Granular Contact Forces: Proof of "Self-Ergodicity" by Generalizing Boltzmann's Stosszahlansatz and H Theorem

NASA Technical Reports Server (NTRS)

Metzger, Philip T.

2006-01-01

Ergodicity is proved for granular contact forces. To obtain this proof from first principles, this paper generalizes Boltzmann's stosszahlansatz (molecular chaos) so that it maintains the necessary correlations and symmetries of granular packing ensembles. Then it formally counts granular contact force states and thereby defines the proper analog of Boltzmann's H functional. This functional is used to prove that (essentially) all static granular packings must exist at maximum entropy with respect to their contact forces. Therefore, the propagation of granular contact forces through a packing is a truly ergodic process in the Boltzmannian sense, or better, it is self-ergodic. Self-ergodicity refers to the non-dynamic, internal relationships that exist between the layer-by-layer and column-by-column subspaces contained within the phase space locus of any particular granular packing microstate. The generalized H Theorem also produces a recursion equation that may be solved numerically to obtain the density of single particle states and hence the distribution of granular contact forces corresponding to the condition of self-ergodicity. The predictions of the theory are overwhelmingly validated by comparison to empirical data from discrete element modeling.

Studies on the biosorption of hexavalent chromium from aqueous solutions by using boiled mucilaginous seeds of Ocimum americanum.

PubMed

Lakshmanraj, Levankumar; Gurusamy, Ayyanar; Gobinath, M B; Chandramohan, R

2009-09-30

Investigations were carried out to study the chromium removal efficiency of boiled mucilaginous seeds of Ocimum americanum. Batch experiments were conducted to study the biosorption kinetics of chromium removal for the concentrations 10mg/L, 20mg/L and 40 mg/L of chromium(VI) solutions. The biosorbent dosage was 8 g dry seeds/L. The toxic hexavalent chromium was reduced to less toxic chromium(III) in the presence of seeds and the reduced chromium was adsorbed on the mucilage of seeds. Both the chromium(VI) and chromium(III) were present in the aqueous phase. The optimum chromium reduction and adsorption was observed at the pH value 1.5. The biosorption data fitted well with Langmuir isotherm. The biosorption capacity calculated from the Langmuir isotherm was q=32 mg chromium(III)/g of dry seeds. The continuous column study was also carried out at the flow rate of 27 mL/h for the initial concentration 25mg/L of chromium(VI) feed solution using a packed bed column filled with boiled mucilaginous seeds. The maximum reduction of chromium(VI) to chromium(III) in the packed bed was 80%. The percentage removal of reduced chromium from the aqueous solution was 56.25%. This value was maintained constant until 0.52 L of chromium(VI) solution was pumped through the packed bed column. Thus the naturally immobilized polysaccharides on the seeds mimic the microbial polysaccharides in terms of their ability to adsorb heavy metals with an added advantage of making the immobilization step unnecessary which is a major cost factor of the metal removal process when microbial exopolysaccharides used. The uniform size and spherical shape of swollen seeds give an additional advantage to use them in a packed bed column for continuous removal of chromium(VI) from aqueous solutions.

Model study of enhanced oil recovery by flooding with aqueous surfactant solution and comparison with theory.

PubMed

Fletcher, Paul D I; Savory, Luke D; Woods, Freya; Clarke, Andrew; Howe, Andrew M

2015-03-17

With the aim of elucidating the details of enhanced oil recovery by surfactant solution flooding, we have determined the detailed behavior of model systems consisting of a packed column of calcium carbonate particles as the porous rock, n-decane as the trapped oil, and aqueous solutions of the anionic surfactant sodium bis(2-ethylhexyl) sulfosuccinate (AOT). The AOT concentration was varied from zero to above the critical aggregation concentration (cac). The salt content of the aqueous solutions was varied to give systems of widely different, post-cac oil-water interfacial tensions. The systems were characterized in detail by measuring the permeability behavior of the packed columns, the adsorption isotherms of AOT from the water to the oil-water interface and to the water-calcium carbonate interface, and oil-water-calcium carbonate contact angles. Measurements of the percent oil recovery by pumping surfactant solutions into calcium carbonate-packed columns initially filled with oil were analyzed in terms of the characterization results. We show that the measured contact angles as a function of AOT concentration are in reasonable agreement with those calculated from values of the surface energy of the calcium carbonate-air surface plus the measured adsorption isotherms. Surfactant adsorption onto the calcium carbonate-water interface causes depletion of its aqueous-phase concentration, and we derive equations which enable the concentration of nonadsorbed surfactant within the packed column to be estimated from measured parameters. The percent oil recovery as a function of the surfactant concentration is determined solely by the oil-water-calcium carbonate contact angle for nonadsorbed surfactant concentrations less than the cac. For surfactant concentrations greater than the cac, additional oil removal occurs by a combination of solubilization and emulsification plus oil mobilization due to the low oil-water interfacial tension and a pumping pressure increase.

Characterization of an immobilized cell, trickle bed reactor during long term butanol (ABE) fermentation.

PubMed

Park, C H; Okos, M R; Wankat, P C

1990-06-20

Acetone-butanol-ethanol (ABE) fermentation was performed continuously in an immobilized cell, trickle bed reactor for 54 days without, degeneration by maintaining the pH above 4.3. Column clogging was minimized by structured packing of immobilization matrix. The reactor contained two serial glass columns packed with Clostridium acetobutylicum adsorbed on 12- and 20-in.-long polyester sponge strips at total flow rates between 38 and 98.7 mL/h. Cells were initially grown at 20 g/L glucose resulting in low butanol (1.15 g/L) production encouraging cell growth. After the initial cell growth phase a higher glucose concentration (38.7 g/L) improved solvent yield from 13.2 to 24.1 wt%, and butanol production rate was the best. Further improvement in solvent yield and butanol production rate was not observed with 60 g/L of glucose. However, when the fresh nutrient supply was limited to only the first column, solvent yield increased to 27.3 wt% and butanol selectivity was improved to 0.592 as compared to 0.541 when fresh feed was fed to both columns. The highest butanol concentration of 5.2 g/L occurred at 55% conversion of the feed with 60 g/L glucose. Liquid product yield of immobilized cells approached the theoretical value reported in the literature. Glucose and product concentration profiles along the column showed that the columns can be divided into production and inhibition regions. The length of each zone was dependent upon the feed glucose concentration and feed pattern. Unlike batch fermentation, there was no clear distinction between acid and solvent production regions. The pH dropped, from 6.18-6.43 to 4.50-4.90 in the first inch of the reactor. The pH dropped further to 4.36-4.65 by the exit of the column. The results indicate that the strategy for long term stable operation with high solvent yield requires a structured packing of biologically stable porous matrix such as polyester sponge, a pH maintenance above 4.3, glucose concentrations up to 60 g/L and nutrient supply only to the inlet of the reactor.

Packing in Two and Three Dimensions

DTIC Science & Technology

2003-06-01

square on the pallet is either completely covered or uncovered by a box. We first observe there must be at least one unit column with zero waste because...66 ( , , , , )EW N X Y a b X′ ′ ′ ′ ′ ′< . Any such unit column with zero waste must be covered with H-boxes because this corresponds to the

UNDERGRADUATE PROJECT ON VIRUS REMOVAL IN SLOW SAND FILTERS FOR RURAL MAYAN COMMUNITIES

EPA Science Inventory

Long-Term Removal in Columns

To simulate the normal operation of a biosand filter, 4 glass columns (Figure 1) packed with different iron orientations were charged daily with 1 PV of aquifer water containing ~10⁸ pfu/mL of MS-2 bacte...

Biological treatment process of air loaded with an ammonia and hydrogen sulfide mixture.

PubMed

Malhautier, Luc; Gracian, Catherine; Roux, Jean-Claude; Fanlo, Jean-Louis; Le Cloirec, Pierre

2003-01-01

The physico-chemical characteristics of granulated sludge lead us to develop its use as a packing material in air biofiltration. Then, the aim of this study is to investigate the potential of unit systems packed with this support in terms of ammonia and hydrogen sulfide emissions treatment. Two laboratory scale pilot biofilters were used. A volumetric load of 680 g H2S m(-3) empty bed day(-1) and 85 g NH3 m(-3) empty bed day(-1) was applied for eight weeks to a unit called BGSn (column packed with granulated sludge and mainly supplied with hydrogen sulfide); a volumetric load of 170 g H2S m(-3) empty bed day(-1) and 340 g NH3 m(-3) empty bed day(-1) was applied for eight weeks to the other called BGNs (column packed with granulated sludge and mainly supplied with ammonia). Ammonia and hydrogen sulfide elimination occur in the biofilters simultaneously. The hydrogen sulphide and ammonia removal efficiencies reached are very high: 100% and 80% for BGSn; 100% and 80% for BGNs respectively. Hydrogen sulfide is oxidized into sulphate and sulfur. The ammonia oxidation products are nitrite and nitrate. The nitrogen error mass balance is high for BGSn (60%) and BGNs (36%). This result could be explained by the denitrification process which would have occurred in anaerobic zones. High percentages of ammonia or hydrogen sulfide are oxidized on the first half of the column. The oxidation of high amounts of hydrogen sulfide would involve some environmental stress on nitrifying bacterial growth and activity.

Improvements in sparse matrix operations of NASTRAN

NASA Technical Reports Server (NTRS)

Harano, S.

1980-01-01

A "nontransmit" packing routine was added to NASTRAN to allow matrix data to be refered to directly from the input/output buffer. Use of the packing routine permits various routines for matrix handling to perform a direct reference to the input/output buffer if data addresses have once been received. The packing routine offers a buffer by buffer backspace feature for efficient backspacing in sequential access. Unlike a conventional backspacing that needs twice back record for a single read of one record (one column), this feature omits overlapping of READ operation and back record. It eliminates the necessity of writing, in decomposition of a symmetric matrix, of a portion of the matrix to its upper triangular matrix from the last to the first columns of the symmetric matrix, thus saving time for generating the upper triangular matrix. Only a lower triangular matrix must be written onto the secondary storage device, bringing 10 to 30% reduction in use of the disk space of the storage device.

Quantification of micro stickies

Treesearch

Mahendra Doshi; Jeffrey Dyer; Salman Aziz; Kristine Jackson; Said M. Abubakr

1997-01-01

The objective of this project was to compare the different methods for the quantification of micro stickies. The hydrophobic materials investigated in this project for the collection of micro stickies were Microfoam* (polypropylene packing material), low density polyethylene film (LDPE), high density polyethylene (HDPE; a flat piece from a square plastic bottle), paper...

Effects of remediation amendments on vadose zone microorganisms

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

Miller, Hannah M.; Tilton, Fred A.

2012-08-10

Surfactant-based foam delivery technology has been studied to remediate Hanford 200 area deep vadose zone sediment. However, the surfactants and remediation amendments have an unknown effect on indigenous subsurface microorganisms. Microbial populations are important factors to consider in remediation efforts due to their potential to alter soil geochemistry. This project focuses on measuring microbial metabolic responses to remediation amendments in batch and column studies using Deep Vadose Zone Sediments. Initial studies of the microbes from Hanford 200 area deep vadose zone sediment showed surfactants sodium dodecyl sulfate (SDS) and cocamidopropyl betaine (CAPB) and remediation amendment calcium polysulfide (CPS) had nomore » affect on microbial growth using BiologTM Ecoplates. To move towards a more realistic field analog, soil columns were packed with Hanford 200 Area sediment. Once microbial growth in the column was verified by observing growth of the effluent solution on tryptic soy agar plates, remedial surfactants were injected into the columns, and the resulting metabolic diversity was measured. Results suggest surfactant sodium dodecyl sulfate (SDS) stimulates microbial growth. The soil columns were also visualized using X-ray microtomography to inspect soil packing and possibly probe for evidence of biofilms. Overall, BiologTM Ecoplates provide a rapid assay to predict effects of remediation amendments on Hanford 200 area deep vadose zone microorganisms.« less

Experimental Design for One Dimensional Electrolytic Reactive Barrier for Remediation of Munition Constituent in Groundwater

PubMed Central

Gent, David B.; Wani, Altaf; Alshawabkeh, Akram N.

2012-01-01

A combination of direct electrochemical reduction and in-situ alkaline hydrolysis has been proposed to decompose energetic contaminants such as 1,3,5-Trinitroperhydro- 1,3,5-triazine and 2,4,6-Trinitrotoluene (RDX) in deep aquifers. This process utilizes natural groundwater convection to carry hydroxide produced by an upstream cathode to remove the contaminant at the cathode as well as in the pore water downstream as it migrates toward the anode. Laboratory evaluation incorporated fundamental principles of column design coupled with reactive contaminant modeling including electrokinetics transport. Batch and horizontal sand-packed column experiments included both alkaline hydrolysis and electrochemical treatment to determine RDX decomposition reaction rate coefficients. The sand packed columns simulated flow through a contaminated aquifer with a seepage velocity of 30.5 cm/day. Techniques to monitor and record the transient electric potential, hydroxide transport and contaminant concentration within the column were developed. The average reaction rate coefficients for both the alkaline batch (0.0487 hr−1) and sand column (0.0466 hr−1) experiments estimated the distance between the cathode and anode required to decompose 0.5 mg/L RDX to the USEPA drinking water lifetime Health Advisory level of 0.002 mg/L to be 145 and 152 cm. PMID:23472044

Q Sepharose micro-column chromatography: A simple screening method for identifying beta thalassemia traits and hemoglobin E carriers.

PubMed

Wong, Peerapon; Sritippayawan, Suchila; Suwannakhon, Narutchala; Tapprom, Akamon; Deoisares, Rawisut; Sanguansermsri, Torpong

2016-11-01

For beta thalassemia control program in pregnancy, mass screening of the carrier state by determination of the hemoglobin (Hb) A 2 and Hb E proportions and mutation analysis is a preferred method for making prenatal diagnoses. Q Sepharose micro-column chromatography, developed for the determination of Hb A 2 and Hb E for screening purposes, was compared with high performance liquid chromatography (HPLC) to ascertain its relative accuracy and reliability. Results using Q Sepharose micro-column chromatography in 350 blood specimens, including 50 samples genetically proven to be beta thalassemia heterozygotes, were compared to HPLC for validation. An additional study was conducted to test a clinical application on a large-scale survey for beta thalassemia in 1581 pregnant women and their spouses. The mean (±SD) Hb A 2 proportions in the normal and genetically proven beta thalassemia heterozygotes were 2.70±0.40% and 6.30±1.23%, respectively, as determined by Q-Sepharose micro-column chromatography, and 2.65±0.31% and 5.37±0.96%, respectively, as determined by HPLC. The mean Hb E proportions in the Hb E heterozygotes were 23.25±4.13% and 24.72±3.5% as determined by Q Sepharose micro-column chromatography and HPLC, respectively. In the large-scale survey for beta thalassemia, 23 at risk couples were detected. Seven affected fetuses were identified by prenatal diagnosis. Q Sepharose micro-column chromatography was found to be reliable, reproducible and well-suited for large-scale surveys. Additionally, by being reusable and convenient, this simple and economical chromatography method may be an alternative means to screen for beta thalassemia and Hb E carriers in the mass population. Copyright © 2016 The Canadian Society of Clinical Chemists. Published by Elsevier Inc. All rights reserved.

DEVELOPMENT, TESTING, AND DEMONSTRATION OF AN OPTIMAL FINE COAL CLEANING CIRCUIT

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

Steven R. Hadley; R. Mike Mishra; Michael Placha

1999-01-27

The objective of this project was to improve the efficiency of the fine coal froth flotation circuit in commercial coal preparation plants. The plant selected for this project, Cyprus Emerald Coal Preparation Plant, cleans 1200-1400 tph of Pittsburgh seam raw coal and uses conventional flotation cells to clean the minus 100-mesh size fraction. The amount of coal in this size fraction is approximately 80 tph with an average ash content of 35%. The project was carried out in two phases. In Phase I, four advanced flotation cells, i.e., a Jameson cell, an Outokumpu HG tank cell, an open column, andmore » a packed column cell, were subjected to bench-scale testing and demonstration. In Phase II, two of these flotation cells, the Jameson cell and the packed column, were subjected to in-plant, proof-of-concept (POC) pilot plant testing both individually and in two-stage combination in order to ascertain whether a two-stage circuit results in lower levelized production costs. The bench-scale results indicated that the Jameson cell and packed column cell would be amenable to the single- and two-stage flotation approach. POC tests using these cells determined that single-stage coal matter recovery (CMR) of 85% was possible with a product ash content of 5.5-7%. Two-stage operation resulted in a coal recovery of 90% with a clean coal ash content of 6-7.5%. This compares favorably with the plant flotation circuit recovery of 80% at a clean coal ash of 11%.« less

Controlling microstructure of pentacene derivatives by solution processing: impact of structural anisotropy on optoelectronic properties.

PubMed

James, David T; Frost, Jarvist M; Wade, Jessica; Nelson, Jenny; Kim, Ji-Seon

2013-09-24

The consideration of anisotropic structural properties and their impact on optoelectronic properties in small-molecule thin films is vital to understand the performance of devices incorporating crystalline organic semiconductors. Here we report on the important relationship between structural and optoelectronic anisotropy in aligned, functionalized-pentacene thin films fabricated using the solution-based zone-casting technique. The microstructure of thin films composed of 6,13-bis(triisopropylsilylethynyl)pentacene (TIPS-pentacene) and 6,13-bis(triethylsilylethynyl)pentacene (TES-pentacene) is systematically controlled by varying the casting speed. By controlling the structural alignment, we were able to experimentally decouple, for the first time in these films, an intramolecular absorption transition dipole (at ∼440 nm) oriented close to the pentacene short axis and an intermolecular absorption transition dipole (at ∼695 nm) oriented predominantly along the conjugated pentacene-pentacene core stacking axis (crystallographic a-axis) in both films. Using the intermolecular absorption as a signature for intermolecular delocalization, much higher optical dichroism was obtained in TES-pentacene (16 ± 6) than TIPS-pentacene (3.2 ± 0.1), which was attributed to the 1D packing structure of TES-pentacene compared to the 2D packing structure of TIPS-pentacene. This result was also supported by field-effect mobility anisotropy measurements of the films, with TES-pentacene exhibiting a higher anisotropy (∼21-47, depending on the casting speed) than TIPS-pentacene (∼3-10).

Boron isotope fractionation in liquid chromatography with boron-specific resins as column packing material

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

Oi, Takao; Shimazaki, Hiromi; Ishii, Reiko

1997-07-01

Boron-specific resins with n-methyl glucamine as the functional group were used as column packing material of liquid chromatography for boron isotope separation. The shapes of chromatograms in reverse breakthrough experiments were heavily dependent on the pH of the eluents, and there existed a pH value at which a chromatogram of the displacement type was realized nearly ideally. The value of the single-stage separation factor for the boron isotopes varied between 1.010 and 1.022, depending on the temperature and the form of the resins. The existence of the three-coordinate boron species in addition to the four-coordinate species in the resin phasemore » is suggested.« less

SMART micro-scissors with dual motors and OCT sensors (Conference Presentation)

NASA Astrophysics Data System (ADS)

Yeo, Chaebeom; Jang, Seonjin; Park, Hyun-cheol; Gehlbach, Peter L.; Song, Cheol

2017-02-01

Various end-effectors of microsurgical instruments have been developed and studied. Also, many approaches to stabilize the tool-tip using robotics have been studied such as the steady hand robot system, Micron, and SMART system. In our previous study, the horizontal SMART micro-scissors with a common path swept source OCT distance and one linear piezoelectric (PZT) motor was demonstrated as a microsurgical system. Because the outer needle is connected with a mechanical handle and moved to engage the tool tip manually, the tool tip position is instantaneously changed during the engaging. The undesirable motion can make unexpected tissue damages and low surgical accuracy. In this study, we suggest a prototype horizontal SMART micro-scissors which has dual OCT sensors and two motors to improve the tremor cancellation. Dual OCT sensors provide two distance information. Front OCT sensor detects a distance from the sample surface to the tool tip. Rear OCT sensors gives current PZT motor movement, acting like a motor encoder. The PZT motor can compensate the hand tremor with a feedback loop control. The manual engaging of tool tip in previous SMART system is replaced by electrical engaging using a squiggle motor. Compared with previous study, this study showed better performance in the hand tremor reduction. From the result, the SMART with automatic engaging may become increasingly valuable in microsurgical instruments.

Methods for fabricating a micro heat barrier

DOEpatents

Marshall, Albert C.; Kravitz, Stanley H.; Tigges, Chris P.; Vawter, Gregory A.

2004-01-06

Methods for fabricating a highly effective, micron-scale micro heat barrier structure and process for manufacturing a micro heat barrier based on semiconductor and/or MEMS fabrication techniques. The micro heat barrier has an array of non-metallic, freestanding microsupports with a height less than 100 microns, attached to a substrate. An infrared reflective membrane (e.g., 1 micron gold) can be supported by the array of microsupports to provide radiation shielding. The micro heat barrier can be evacuated to eliminate gas phase heat conduction and convection. Semi-isotropic, reactive ion plasma etching can be used to create a microspike having a cusp-like shape with a sharp, pointed tip (<0.1 micron), to minimize the tip's contact area. A heat source can be placed directly on the microspikes. The micro heat barrier can have an apparent thermal conductivity in the range of 10.sup.-6 to 10.sup.-7 W/m-K. Multiple layers of reflective membranes can be used to increase thermal resistance.

Absorption of mercuric cation by tannins in agricultural residues

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

Waiss, A.C. Jr.; Wiley, M.E.; Kuhnle, J.A.

1973-01-01

Two common environmental pollutants are agricultural residues (skins, pits, husks, tannin bark, grape pomace) and waste streams of water containing only traces of heavy metals (such as mercury at 10 or more ppb) from mining or manufacturing operations. Agricultural residues contain tannins, polyphenolic substances, pectin, and other polymers-all with chemically reactive groups that can chelate, reduce, oxidize, demonstrate ion exchange properties, and aid in removing traces of heavy metals from dilute waste water streams at low cost. Finely ground and water-washed agricultural residues were slurried in water and packed into columns for absorption tests with heavy metals. Solutions of knownmore » concentrations of heavy metals were passed through the packed columns which were then eluted with water or with alkaline or acidic solutions. The fractions and the column absorbents were then analyzed by standard atomic absorption methods. The nature of the physical and chemical forces that are effective in metal absorption from agricultural residues is not clear.« less

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.

Do lab-derived distribution coefficient values of pesticides match distribution coefficient values determined from column and field-scale experiments? A critical analysis of relevant literature.

PubMed

Vereecken, H; Vanderborght, J; Kasteel, R; Spiteller, M; Schäffer, A; Close, M

2011-01-01

In this study, we analyzed sorption parameters for pesticides that were derived from batch and column or batch and field experiments. The batch experiments analyzed in this study were run with the same pesticide and soil as in the column and field experiments. We analyzed the relationship between the pore water velocity of the column and field experiments, solute residence times, and sorption parameters, such as the organic carbon normalized distribution coefficient ( ) and the mass exchange coefficient in kinetic models, as well as the predictability of sorption parameters from basic soil properties. The batch/column analysis included 38 studies with a total of 139 observations. The batch/field analysis included five studies, resulting in a dataset of 24 observations. For the batch/column data, power law relationships between pore water velocity, residence time, and sorption constants were derived. The unexplained variability in these equations was reduced, taking into account the saturation status and the packing status (disturbed-undisturbed) of the soil sample. A new regression equation was derived that allows estimating the values derived from column experiments using organic matter and bulk density with an value of 0.56. Regression analysis of the batch/column data showed that the relationship between batch- and column-derived values depends on the saturation status and packing of the soil column. Analysis of the batch/field data showed that as the batch-derived value becomes larger, field-derived values tend to be lower than the corresponding batch-derived values, and vice versa. The present dataset also showed that the variability in the ratio of batch- to column-derived value increases with increasing pore water velocity, with a maximum value approaching 3.5. American Society of Agronomy, Crop Science Society of America, and Soil Science Society of America.

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.

Investigation related to hydrogen isotopes separation by cryogenic distillation

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

Bornea, A.; Zamfirache, M.; Stefanescu, I.

2008-07-15

Research conducted in the last fifty years has shown that one of the most efficient techniques of removing tritium from the heavy water used as moderator and coolant in CANDU reactors (as that operated at Cernavoda (Romania)) is hydrogen cryogenic distillation. Designing and implementing the concept of cryogenic distillation columns require experiments to be conducted as well as computer simulations. Particularly, computer simulations are of great importance when designing and evaluating the performances of a column or a series of columns. Experimental data collected from laboratory work will be used as input for computer simulations run at larger scale (formore » The Pilot Plant for Tritium and Deuterium Separation) in order to increase the confidence in the simulated results. Studies carried out were focused on the following: - Quantitative analyses of important parameters such as the number of theoretical plates, inlet area, reflux flow, flow-rates extraction, working pressure, etc. - Columns connected in series in such a way to fulfil the separation requirements. Experiments were carried out on a laboratory-scale installation to investigate the performance of contact elements with continuous packing. The packing was manufactured in our institute. (authors)« less

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.

Influence of orientation mismatch on charge transport across grain boundaries in tri-isopropylsilylethynyl (TIPS) pentacene thin films.

PubMed

Steiner, Florian; Poelking, Carl; Niedzialek, Dorota; Andrienko, Denis; Nelson, Jenny

2017-05-03

We present a multi-scale model for charge transport across grain boundaries in molecular electronic materials that incorporates packing disorder, electrostatic and polarisation effects. We choose quasi two-dimensional films of tri-isopropylsilylethynyl pentacene (TIPS-P) as a model system representative of technologically relevant crystalline organic semiconductors. We use atomistic molecular dynamics, with a force-field specific for TIPS-P, to generate and equilibrate polycrystalline two-dimensional thin films. The energy landscape is obtained by calculating contributions from electrostatic interactions and polarization. The variation in these contributions leads to energetic barriers between grains. Subsequently, charge transport is simulated using a kinetic Monte-Carlo algorithm. Two-grain systems with varied mutual orientation are studied. We find relatively little effect of long grain boundaries due to the presence of low impedance pathways. However, effects could be more pronounced for systems with limited inter-grain contact areas. Furthermore, we present a lattice model to generalize the model for small molecular systems. In the general case, depending on molecular architecture and packing, grain boundaries can result in interfacial energy barriers, traps or a combination of both with qualitatively different effects on charge transport.

[Comparative evaluation of two kinds of micro-implant system with different size].

PubMed

Wang, Zhen-Dong; Li, Qing-Yi; Wang, Lin; Gu, Yong-Jia

2009-04-01

To offer some reference for micro-implant's development and population by analyzing clinical application of two kinds of micro-implant systems. 38 patients treated with MIA (micro-implant anchorage) and 28 patients treated with SDIA (self-driven titanium implant for orthodontic anchorage) were included. Analyzing the rate of lost implants, the gum's reactivity and the efficiency of moving teeth summarized the excellences and shortcomings of two systems. 1) Six of MIA implants fell off after being inserted. Seven of SDIA implants lost when they had been implanted for a month. But they were stable after being inserted again. 2) The gum around 12 SDIA implants got inflammation symptom, but the gum around MIA implants was normal. 3) Both MIA implants and SDIA implants could move teeth effectively and persistently when they were stable. When we apply micro-implant in clinic, we should prevent it from closing roots of teeth and choose the small tip micro-implant. The embedded position should be in area of attachment gum. At the same time, the areas around the tip of micro-implant should be keeping clean.

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

Medication and volume delivery by gravity-driven micro-drip intravenous infusion: potential variations during "wide-open" flow.

PubMed

Pierce, Eric T; Kumar, Vikram; Zheng, Hui; Peterfreund, Robert A

2013-03-01

Gravity-driven micro-drip infusion sets allow control of medication dose delivery by adjusting drops per minute. When the roller clamp is fully open, flow in the drip chamber can be a continuous fluid column rather than discrete, countable, drops. We hypothesized that during this "wide-open" state, drug delivery becomes dependent on factors extrinsic to the micro-drip set and is therefore difficult to predict. We conducted laboratory experiments to characterize volume delivery under various clinically relevant conditions of wide-open flow in an in vitro laboratory model. A micro-drip infusion set, plugged into a bag of normal saline, was connected to a high-flow stopcock at the distal end. Vertically oriented IV catheters (gauges 14-22) were connected to the stopcock. The fluid meniscus height in the bag was fixed (60-120 cm) above the outflow point. The roller clamp on the infusion set was in fully open position for all experiments resulting in a continuous column of fluid in the drip chamber. Fluid volume delivered in 1 minute was measured 4 times with each condition. To model resistive effects of carrier flow, volumetric infusion pumps were used to deliver various flow rates of normal saline through a carrier IV set into which a micro-drip infusion was "piggybacked." We also compared delivery by micro-drip infusion sets from 3 manufacturers. The volume of fluid delivered by gravity-driven infusion under wide-open conditions (continuous fluid column in drip chamber) varied 2.9-fold (95% confidence interval, 2.84-2.96) depending on catheter size and fluid column height. Total model resistance of the micro-drip with stopcock and catheter varied with flow rate. Volume delivered by the piggybacked micro-drip decreased up to 29.7% ± 0.8% (mean ± SE) as the carrier flow increased from 0 to 1998 mL/min. Delivery characteristics of the micro-drip infusion sets from 3 different manufacturers were similar. Laboratory simulation of clinical situations with gravity-driven micro-drip infusion sets under wide-open flow conditions revealed that infusion rate (drug and/or volume delivery) can vary widely depending on extrinsic factors including catheter size, fluid column height, and carrier flow. The variable resistance implies nonlaminar flow in the micro-drip model that cannot be easily predicted mathematically. These findings support the use of mechanical pumps instead of gravity-driven micro-drips to enhance the precision and safety of IV infusions, especially for vasoactive drugs.

Drill Bit Tip on Mars Rover Curiosity, Head-on View

NASA Image and Video Library

2013-02-04

This head-on view shows the tip of the drill bit on NASA Mars rover Curiosity. The view merges two exposures taken by the remote micro-imager in the rover ChemCam instrument at different focus settings.

California Wild Summer 2003 - Rafflesia

Science.gov Websites

-tipped warts—the anthers—which exuded slimy pollen. In female flowers, which are much rarer, tiny the wound. Other scientists think that tree shrews or ground squirrels gnaw the columns of dead female female, seeds in the remnant of the central column are now available for dispersal. Although long

The effects of intra-particle concentration gradient on consecutive adsorption-desorption of oryzanol from rice bran oil in packed-column

NASA Astrophysics Data System (ADS)

Susanti, Ari Diana; Sediawan, Wahyudi Budi; Wirawan, Sang Kompiang; Budhijanto

2017-05-01

Utilization of valuable trace components in agriculture by product such as rice bran oil is interesting to be explored. Among the valuables, oryzanol, a healthy nutrition for cardiovascular prevention, is the most promising one. Literature studies suggest that adsorption-desorption is a prospective method for oryzanol isolation. Design of commercial scale adsorption-desorption system for oryzanol needs a quantitative description of the phenomena involved. In this study, quantitative modeling of the consecutive adsorption-desorption in packed column has been proposed and verified through experimental data. The offered model takes into account the intra-particle concentration gradient in the adsorbent particle. In this model, the rate of mass transfer from the bulk of the liquid to the surface of the adsorbent particle or vice versa is expressed by film theory. The mass transfer of oryzanol from the liquid in the pore of the particle to the adjacent pore surface is assumed to be instantaneous, so solid-liquid equilibrium on the surface of the pores is always attained. For simplicity, the adsorption equilibrium model applied was coefficient distribution approach. The values of the parameters implicated in the model were obtained by curve fitting to the experimental data. It verified that the model proposed works well to quantitatively describe the consecutive adsorption-desorption of oryzanol from rice bran oil in packed column.

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.

A Micro Ultrasonic Scalpel with Modified Stepped Horn

NASA Astrophysics Data System (ADS)

Kurosawa, Minoru; Umehara, Yuji

A transducer for a micro ultrasonic scalpel has been fabricated. The micro ultrasonic scalpel can be used with an endoscope for a non-abdominal operation or micro surgery, for example, through a microscope. The ultrasonic transducer was 9.8 mm long and 2.7 mm wide and has stepped horn to amplify vibration velocity; tip of the horn is 0.6 mm wide. The scalpel operated at the resonance frequency in longitudinal mode of 278 kHz. The piezoelectric material was lead zirconate titanate (PZT) that was deposited by the hydrothermal method. The vibration velocity at the tip of the horn in longitudinal direction was 4.0 m/s with 40Vp-p driving voltage in both side electrodes. To demonstrate a beneficial effect of the scalpel, a cutting test that the transducer was stuck into pork fat was carried out.

Atomic force microscope with combined FTIR-Raman spectroscopy having a micro thermal analyzer

DOEpatents

Fink, Samuel D [Aiken, SC; Fondeur, Fernando F [North Augusta, SC

2011-10-18

An atomic force microscope is provided that includes a micro thermal analyzer with a tip. The micro thermal analyzer is configured for obtaining topographical data from a sample. A raman spectrometer is included and is configured for use in obtaining chemical data from the sample.

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.

Latching mechanism for deployable/re-stowable columns useful in satellite construction

NASA Technical Reports Server (NTRS)

Ahl, E. L., Jr. (Inventor)

1986-01-01

A column longeron latch assembly provides the securing mechanism for the deployable, telescoping column of a hoop/column antenna. The column is an open lattice structure with three longerons disposed 120 deg apart as the principle load bearing member. The column is deployed from a pair of eleven nested bays disposed on opposite sides of a center section under the influence of a motor-cable-pulley system. The longeron latch is a four bar linkage mechanism using the over-center principle for automatically locking the longeron sections into position during deployment. The latch is unlocked when the antenna is to be restowed. A spring pack disposed in the end of each longeron serves to absorb stress forces on the deployed column through the cam head piston and abutting latch from an adjacent longeron.

The role of silica colloids on facilitated cesium transport through glass bead columns and modeling

NASA Astrophysics Data System (ADS)

Noell, Alan L.; Thompson, Joseph L.; Corapcioglu, M. Yavuz; Triay, Inés R.

1998-05-01

Groundwater colloids can act as a vector which enhances the migration of contaminants. While sorbed to mobile colloids, contaminants can be held in the aqueous phase which prevents them from interacting with immobile aquifer surfaces. In this study, an idealized laboratory set-up was used to examine the influence of amorphous silica colloids on the transport of cesium. Synthetic groundwater and saturated glass bead columns were used to minimize the presence of natural colloidal material. The columns were assembled in replicate, some packed with 150-210 μm glass bead and others packed with 355-420 μm glass beads. The colloids used in these experiments were 100 nm amorphous silica colloids from Nissan Chemical Company. In the absence of these colloids, the retardation factor for cesium was 8.0 in the 150-210 μm glass bead columns and 3.6 in the 355-420 μm glass bead columns. The influence of anthropogenic colloids was tested by injecting 0.09 pore volume slugs of an equilibrated suspension of cesium and colloids into the colloid-free columns. Although there was little noticeable facilitation in the smaller glass bead columns, there was a slight reduction in the retardation of cesium in the larger glass bead columns. This was attributed to cesium having less of a retention time in the larger glass bead columns. When cesium was injected into columns with a constant flux of colloids, the retardation of cesium was reduced by 14-32% in the 150-210 μm glass bead columns and by 38-51% in the 355-420 μm glass bead columns. A model based on Corapcioglu and Jiang (1993) [Corapcioglu, M.Y., Jiang, S., 1993. Colloid-facilitated groundwater contaminant transport, Water Resour. Res., 29 (7) 2215-2226] was compared with the experimental elution data. When equilibrium sorption expressions were used and the flux of colloids through the glass bead columns was constant, the colloid facilitated transport of cesium was able to be described using an effective retardation coefficient. Fully kinetic simulations, however, more accurately described the colloid facilitated transport of cesium.

Fabrication and characterization of superporous cellulose bead for high-speed protein chromatography.

PubMed

Wang, Dong-Mei; Hao, Gang; Shi, Qing-Hong; Sun, Yan

2007-03-30

Novel superporous cellulose (SC) matrix has been fabricated by water-in-oil emulsification-thermal regeneration using granules of calcium carbonate as porogenic agents. As a control, microporous cellulose (MC) bead was fabricated in the absence of calcium carbonate. Simultaneously, double cross-linking was applied to enhance the mechanical strength of the particles. The photographs by scanning electron microscopy of the SC bead illustrated that there were more "craters" of several microns scattering on the surface of the beads. It led to a higher water content and effective porosity of the SC medium. The two beads were then modified with diethylaminoethyl (DEAE) group to prepare anion exchangers. The dynamic uptake results of bovine serum albumin (BSA) exhibited that the pore diffusivity of BSA in the DEAE-SC bead was two to three times larger than that in the DEAE-MC bead. In addition, the column packed with the DEAE-SC showed lower backpressure, higher column efficiency and dynamic binding capacity than the column packed with the DEAE-MC at a flow rate range of 150-900cm/h. Moreover, the column efficiency of the DEAE-SC column was independent of flow velocity up to a flow rate of 1200cm/h. All the results exhibited the superior characteristics of the SC bead as a potential medium for high-speed protein chromatography.

Hybrid Sargassum-sand sorbent: a novel adsorbent in packed column to treat metal-bearing wastewaters from inductively coupled plasma-optical emission spectrometry.

PubMed

Vijayaraghavan, K; Joshi, U M

2013-01-01

Laboratory batch and column experiments were carried out to examine the efficiency of algal-based treatment technique to clean-up wastewaters emanating from inductively coupled plasma-optical emission spectrometry (ICP-OES). Chemical characterization revealed the extreme complexity of the wastewater, with the presence of 14 different metals under very low pH (pH = 1.1), high conductivity (6.98 mS/cm), total dissolved solid (4.46 g/L) and salinity (3.77). Batch experiments using Sargassum biomass indicated that it was possible to attain high removal efficiencies at optimum pH of 4.0. Efforts were also made to continuously treat ICP-OES wastewater using up-flow packed column. However, swelling of Sargassum biomass leads to stoppage of column. To address the problem, Sargassum was mixed with sand at a ratio of 40: 60 on volume basis. Remarkably, the hybrid Sargassum-sand sorbent showed very high removal efficiency towards multiple metal ions with the column able to operate for 11 h at a flow rate of 10 mL/min. Metal ions such as Cu, Cd, and Pb were only under trace levels in the treated water until 11 h. The results of the treatment process were compared with trade effluent discharge standards. Further the process evaluation and cost analysis were presented.

Microfabricated thermal modulator for comprehensive two-dimensional micro gas chromatography: design, thermal modeling, and preliminary testing.

PubMed

Kim, Sung-Jin; Reidy, Shaelah M; Block, Bruce P; Wise, Kensall D; Zellers, Edward T; Kurabayashi, Katsuo

2010-07-07

In comprehensive two-dimensional gas chromatography (GC x GC), a modulator is placed at the juncture between two separation columns to focus and re-inject eluting mixture components, thereby enhancing the resolution and the selectivity of analytes. As part of an effort to develop a microGC x microGC prototype, in this report we present the design, fabrication, thermal operation, and initial testing of a two-stage microscale thermal modulator (microTM). The microTM contains two sequential serpentine Pyrex-on-Si microchannels (stages) that cryogenically trap analytes eluting from the first-dimension column and thermally inject them into the second-dimension column in a rapid, programmable manner. For each modulation cycle (typically 5 s for cooling with refrigeration work of 200 J and 100 ms for heating at 10 W), the microTM is kept approximately at -50 degrees C by a solid-state thermoelectric cooling unit placed within a few tens of micrometres of the device, and heated to 250 degrees C at 2800 degrees C s(-1) by integrated resistive microheaters and then cooled back to -50 degrees C at 250 degrees C s(-1). Thermal crosstalk between the two stages is less than 9%. A lumped heat transfer model is used to analyze the device design with respect to the rates of heating and cooling, power dissipation, and inter-stage thermal crosstalk as a function of Pyrex-membrane thickness, air-gap depth, and stage separation distance. Experimental results are in agreement with trends predicted by the model. Preliminary tests using a conventional capillary column interfaced to the microTM demonstrate the capability for enhanced sensitivity and resolution as well as the modulation of a mixture of alkanes.

Bonding with Grandparents

MedlinePlus

... to kids. Such dedicated attention only improves a child's developmental and learning skills. Tips for Staying in Touch In today's world, though, families may be scattered across the country, and jam-packed school ... often. If your child's grandparents live nearby, make an effort to save ...

Soldering tool heats workpieces and applies solder in one operation

NASA Technical Reports Server (NTRS)

Gudkese, V. W.

1966-01-01

Fountain-pen type soldering iron heats workpieces and applies solder to joints in densely packed electronics assemblies. The basic soldering tool is used with different-sized orifice tips, eliminating the need for an assortment of conventional soldering guns.

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

PubMed

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

2004-09-03

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

Fmoc-RGDS based fibrils: atomistic details of their hierarchical assembly.

PubMed

Zanuy, David; Poater, Jordi; Solà, Miquel; Hamley, Ian W; Alemán, Carlos

2016-01-14

We describe the 3D supramolecular structure of Fmoc-RGDS fibrils, where Fmoc and RGDS refer to the hydrophobic N-(fluorenyl-9-methoxycarbonyl) group and the hydrophilic Arg-Gly-Asp-Ser peptide sequence, respectively. For this purpose, we performed atomistic all-atom molecular dynamics simulations of a wide variety of packing modes derived from both parallel and antiparallel β-sheet configurations. The proposed model, which closely resembles the cross-β core structure of amyloids, is stabilized by π-π stacking interactions between hydrophobic Fmoc groups. More specifically, in this organization, the Fmoc-groups of β-strands belonging to the same β-sheet form columns of π-stacked aromatic rings arranged in a parallel fashion. Eight of such columns pack laterally forming a compact and dense hydrophobic core, in which two central columns are surrounded by three adjacent columns on each side. In addition to such Fmoc···Fmoc interactions, the hierarchical assembly of the constituent β-strands involves a rich variety of intra- and inter-strand interactions. Accordingly, hydrogen bonding, salt bridges and π-π stacking interactions coexist in the highly ordered packing network proposed for the Fmoc-RGDS amphiphile. Quantum mechanical calculations, which have been performed to quantify the above referred interactions, confirm the decisive role played by the π-π stacking interactions between the rings of the Fmoc groups, even though both inter-strand and intra-strand hydrogen bonds and salt bridges also play a non-negligible role. Overall, these results provide a solid reference to complement the available experimental data, which are not precise enough to determine the fibril structure, and reconcile previous independent observations.

Continuous adsorption and biotransformation of micropollutants by granular activated carbon-bound laccase in a packed-bed enzyme reactor.

PubMed

Nguyen, Luong N; Hai, Faisal I; Dosseto, Anthony; Richardson, Christopher; Price, William E; Nghiem, Long D

2016-06-01

Laccase was immobilized on granular activated carbon (GAC) and the resulting GAC-bound laccase was used to degrade four micropollutants in a packed-bed column. Compared to the free enzyme, the immobilized laccase showed high residual activities over a broad range of pH and temperature. The GAC-bound laccase efficiently removed four micropollutants, namely, sulfamethoxazole, carbamazepine, diclofenac and bisphenol A, commonly detected in raw wastewater and wastewater-impacted water sources. Mass balance analysis showed that these micropollutants were enzymatically degraded following adsorption onto GAC. Higher degradation efficiency of micropollutants by the immobilized compared to free laccase was possibly due to better electron transfer between laccase and substrate molecules once they have adsorbed onto the GAC surface. Results here highlight the complementary effects of adsorption and enzymatic degradation on micropollutant removal by GAC-bound laccase. Indeed laccase-immobilized GAC outperformed regular GAC during continuous operation of packed-bed columns over two months (a throughput of 12,000 bed volumes). Copyright © 2016 Elsevier Ltd. All rights reserved.

High-resolution separation of neodymium and dysprosium ions utilizing extractant-impregnated graft-type particles.

PubMed

Uchiyama, Shoichiro; Sasaki, Takaaki; Ishihara, Ryo; Fujiwara, Kunio; Sugo, Takanobu; Umeno, Daisuke; Saito, Kyoichi

2018-01-19

An efficient method for rare metal recovery from environmental water and urban mines is in high demand. Toward rapid and high-resolution rare metal ion separation, a novel bis(2-ethylhexyl) phosphate (HDEHP)-impregnated graft-type particle as a filler for a chromatography column is proposed. To achieve rapid and high-resolution separation, a convection-flow-aided elution mode is required. The combination of 35 μm non-porous particles and a polymer-brush-rich particle structure minimizes the distance from metal ion binding sites to the convection flow in the column, resulting in minimized diffusional mass transfer resistance and the convection-flow-aided elution mode. The HDEHP-impregnated graft-type non-porous-particle-packed cartridge developed in this study exhibited a higher separation performance for model rare metals, neodymium (III) and dysprosium (III) ions, and a narrower peak at a higher linear velocity, than those of previous HDEHP-impregnated fiber-packed and commercially available Lewatit ® VP OC 1026-packed cartridges. Copyright © 2017 Elsevier B.V. All rights reserved.

The effect of deformation on two-phase flow through proppant-packed fractured shale samples: A micro-scale experimental investigation

NASA Astrophysics Data System (ADS)

Arshadi, Maziar; Zolfaghari, Arsalan; Piri, Mohammad; Al-Muntasheri, Ghaithan A.; Sayed, Mohammed

2017-07-01

We present the results of an extensive micro-scale experimental investigation of two-phase flow through miniature, fractured reservoir shale samples that contained different packings of proppant grains. We investigated permeability reduction in the samples by conducting experiments under a wide range of net confining pressures. Three different proppant grain distributions in three individual fractured shale samples were studied: i) multi-layer, ii) uniform mono-layer, and iii) non-uniform mono-layer. We performed oil-displacing-brine (drainage) and brine-displacing-oil (imbibition) flow experiments in the proppant packs under net confining pressures ranging from 200 to 6000 psi. The flow experiments were performed using a state-of-the-art miniature core-flooding apparatus integrated with a high-resolution, X-ray microtomography system. We visualized fluid occupancies, proppant embedment, and shale deformation under different flow and stress conditions. We examined deformation of pore space within the proppant packs and its impact on permeability and residual trapping, proppant embedment due to changes in net confining stress, shale surface deformation, and disintegration of proppant grains at high stress conditions. In particular, geometrical deformation and two-phase flow effects within the proppant pack impacting hydraulic conductivity of the medium were probed. A significant reduction in effective oil permeability at irreducible water saturation was observed due to increase in confining pressure. We propose different mechanisms responsible for the observed permeability reduction in different fracture packings. Samples with dissimilar proppant grain distributions showed significantly different proppant embedment behavior. Thinner proppant layer increased embedment significantly and lowered the onset confining pressure of embedment. As confining stress was increased, small embedments caused the surface of the shale to fracture. The produced shale fragments were then entrained by the flow and partially blocked pore-throat connections within the proppant pack. Deformation of proppant packs resulted in significant changes in waterflood residual oil saturation. In-situ contact angles measured using micro-CT images showed that proppant grains had experienced a drastic alteration of wettability (from strong water-wet to weakly oil-wet) after the medium had been subjected to flow of oil and brine for multiple weeks. Nanometer resolution SEM images captured nano-fractures induced in the shale surfaces during the experiments with mono-layer proppant packing. These fractures improved the effective permeability of the medium and shale/fracture interactions.

Young adult smokers' perceptions of plain packs, numbered packs and pack inserts in Turkey: a focus group study.

PubMed

Mucan, Burcu; Moodie, Crawford

2017-11-09

The Turkish Government's 'National Tobacco Control Program 2015-2018' included plans to introduce plain packaging and also a ban on brand names on cigarette packs, allowing only assigned numbers on packs. We explored perceptions of these proposed measures, and also pack inserts with cessation messages, another novel way of using the packaging to communicate with consumers. Eight focus groups were conducted with 47 young adult smokers in Manisa and Kutahya (Turkey) in December 2016. Participants were shown three straight-edged plain cigarette packs, as required in Australia, and then three bevelled-edged plain packs, as permitted in the UK. They were then shown plain packs with numbers rather than brand names, and finally three pack inserts with messages encouraging quitting or offering tips on how to do so. Participants were asked about their perceptions of each. Plain packs were considered unappealing and off-putting, although the bevelled-edged packs were viewed more favourably than the straight-edged packs. Numbered packs were thought by some to diminish the appeal created by the brand name and potentially decrease interest among never smokers and newer smokers. Pack inserts were thought to have less of an impact than the on-pack warnings, but could potentially help discourage initiation and encourage cessation. That bevelled-edged plain packs were perceived more positively than straight-edged plain packs is relevant to countries planning to introduce plain packaging. The study provides a first insight into smokers' perceptions of a ban on brand names, which was perceived to reduce appeal among young people. © Article author(s) (or their employer(s) unless otherwise stated in the text of the article) 2017. All rights reserved. No commercial use is permitted unless otherwise expressly granted.

A parallel bubble column system for the cultivation of phototrophic microorganisms.

PubMed

Havel, Jan; Franco-Lara, Ezequiel; Weuster-Botz, Dirk

2008-07-01

An incubator with up to 16 parallel bubble columns was equipped with artificial light sources assuring a light supply with a homogenous light spectrum directly above the bioreactors. Cylindrical light reflecting tubes were positioned around every single bubble column to avoid light scattering effects and to redirect the light from the top onto the cylindrical outer glass surface of each bubble column. The light reflecting tubes were equipped with light intensity filters to control the total light intensity for every single photo-bioreactor. Parallel cultivations of the unicellular obligate phototrophic cyanobacterium, Synechococcus PCC7942, were studied under different constant light intensities ranging from 20 to 102 microE m(-2)s(-1) at a constant humidified air flow rate supplemented with CO(2).

[Three dimensional finite element analysis of maxillary anterior teeth retraction with micro-implant anchorage and sliding mechanics].

PubMed

Zhang, Yi; Zhang, Lei; Fan, Yu-bo; Song, Jin-lin; Deng, Feng

2009-10-01

To investigate the biomechanical effects of micro-implant anchorage technique with sliding mechanics on maxillary anterior teeth retraction under different implant insertion heights and different retraction hook heights. The three dimensional finite element model of maxillary anterior teeth retraction force system was constructed with CT scanning and MIMICS software and the relationships between brackets, teeth, wire and micro-implant were simulating the clinical factions. Then the initial tooth displacement was calculated when the insertion heights were 4 mm and 8 mm and the retraction hook heights were 1, 4, 7, 10 mm respectively. With retraction hook height added, the anterior teeth movement changed from lingual crown tipping to labial crown tipping and the intrusion movement was more apparent when the micro-implant was inserted in a higher location. The ideal teeth movement control could be achieved by different insertion heights of micro-implant and different retraction hook heights in straight wire retraction force system.

Fundamental studies of chalcogenide nanocrystals, carbonaceous nanoparticles, and chromatographic materials

NASA Astrophysics Data System (ADS)

Baker, Jared Scott

2011-12-01

The development of novel nanomaterials and the understanding of their fundamental physical and chemical properties represent an exciting area of research. These materials are continuously being sought for ever-increasing applications; finding their way into uses that influence mankind on a daily basis. Combining elements from traditional nanoparticle characterization with electrophoretic-based techniques, this dissertation presents the analysis of carbon nanoparticles (CNPs) generated from a novel source (candle soot) as well as a unique perspective on the reactivity and degradation process of magic-sized cadmium chalcogenide nanocrystals. One potential application of CNPs is their use as an alternative fluorophore in a separation-based sensor system. Laser-induced-fluorescence (LIF) is a commonly used manner of detection in this type of platform, but is limited in many cases by problems associated with the fluorophore. Carbon-based nanoparticles have the potential to improve upon traditional fluorophores in applications that make use of LIF as the detection scheme. CNPs were extracted from the carbonaceous material produced by the incomplete combustion of a candle. The soot was submitted to an oxidizing treatment and extraction/filtration procedures rendering watersoluble luminescent species. Electron microscopy was used to identify globular, amorphous structures in the nanometer size-range. An aqueous suspension of CNPs demonstrated excellent stability in terms of its electronic properties, showing little change in absorption and emission spectra upon storage under ambient conditions over a two-year period. Capitalizing on the strengths of capillary electrophoresis (CE) as a characterization technique, we have analyzed the negatively-charged CNPs in terms of charge and size by studying the influence of variable CE conditions on the resulting separation. Separations at different pH revealed a highly complex mixture of CNPs, containing species with large electrophoretic mobilities under a wide range of pH values. The mobility of these nanoparticles as a function of ionic strength was compared to classical electrokinetic theory, suggesting that the species are small, highly charged particles with appreciable zeta potentials, even at low pH. In an attempt to reduce the complexity of the CNP solution, two molecular-weight based fractionation techniques were employed and evaluated. Traditional dialysis and ultracentrifugation filtration techniques were modified to generate multiple CNPs fractions based on size. Analysis of the fractions by absorption and photoluminescence spectroscopy as well as CE revealed specific characteristics for a given sized-fraction. Namely, a strong correlation between the size of the CNPs and their luminescent emission was observed. CE was utilized to characterize each fraction and to ultimately judge the effectiveness of the fractionation techniques. The characterization of the persistence and degradation of magic-sized CdSe nanocrystals (NCs) after their removal from the original reaction mixture and dispersion into basic aqueous solutions was performed by absorption spectroscopy. NCs degraded after dilution into aqueous NaOH, resulting in red-shifted excitonic absorption bands and eventual flocculation. Dilution of NCs into basic aqueous solutions of cysteinate resulted in degradation via a different mechanism with an absence of flocculation; kinetics varied with concentration of cysteinate. The chemical fate of NCs after dilution into basic aqueous solutions containing both Cd2+ and cysteinate varied with the cysteinate-to-Cd 2+ molar ratio, which determined the relative solute mole fractions of various Cd2+-cysteinate complexes. CdSe NCs persisted on long timescales only when dispersed in solutions containing [Cd(cysteinate) 3]4-. Equilibria are presented to account for the observed spectral changes after dilution of CdSe into various basic media. Cadmium(II)-cysteinate complex-formation equilibria influenced the temporal persistence of the nanocrystals; the pathway through which CdSe NCs degraded depended on the concentration of free, uncoordinated cysteinate. These findings indicate that solution-phase chemistry can determine whether NCs remain intact upon removal from their original reaction mixtures. Departing from the analysis of nanomaterials, an additional chapter focuses on the evaluation of a new chromatographic packing material. Two chromatographic columns packed with superficially porous packing material, Kinetex(TM) 1.7 mum and 2.6 mum C18 particles were evaluated in terms of their physical properties and performance characteristics. These columns were compared to a column packed with a sub-2 mum totally porous material and to a Halo(TM) column packed with 2.7 mum C18 superficially porous packing. The columns packed with superficially porous particles displayed a comparably narrower size distribution, which is narrower than the distribution of the totally porous sub-2 mum particles. Physical characteristics of the Kinetex(TM) particles were evaluated in terms of surface area, pore diameter, and specific pore volume. Total, external, internal and shell porosities among the four different columns were evaluated and compared. The specific permeability for the Kinetex columns showed values close to those predicted by the Kozeny-Carman equation. All four columns were evaluated in terms of their chromatographic performance and compared using the Knox equation. The columns packed with the 2.6 mum and 2.7 mum superficially porous materials showed reduced plate heights below 2, while the sub-2 mum particles showed values of 2.2 and above.

Micro injector sample delivery system for charged molecules

DOEpatents

Davidson, James C.; Balch, Joseph W.

1999-11-09

A micro injector sample delivery system for charged molecules. The injector is used for collecting and delivering controlled amounts of charged molecule samples for subsequent analysis. The injector delivery system can be scaled to large numbers (>96) for sample delivery to massively parallel high throughput analysis systems. The essence of the injector system is an electric field controllable loading tip including a section of porous material. By applying the appropriate polarity bias potential to the injector tip, charged molecules will migrate into porous material, and by reversing the polarity bias potential the molecules are ejected or forced away from the tip. The invention has application for uptake of charged biological molecules (e.g. proteins, nucleic acids, polymers, etc.) for delivery to analytical systems, and can be used in automated sample delivery systems.

P39-T Analysis of Oligosaccharides by Capillary-Scale High-Performance Anion-Exchange Chromatography with Pulsed Amperometric Detection (CHPAEC-PAD) and On-Line Electrospray-Ionization Ion-Trap Mass Spectrometry (CHPAEC-ITMS)

PubMed Central

Bruggink, C.; Koeleman, C.; Barreto, V.; Lui, Y.; Pohl, C.; Ingendoh, A.; Wuhrer, M.; Hokke, C.; Deelder, A.

2007-01-01

High-pH anion-exchange chromatography with pulsed amperometric detection (HPAEC-PAD) is an established technique for selective separation and analysis of underivatized carbohydrates. The miniaturization of chromatographic techniques by means of capillary columns, and on-line coupling to mass spectrometry are critical to the further development of glycan analysis methods that are compatible with the current requirements in clinical settings. A system has been developed based on the Dionex BioLC equipped with a microbore gradient pump with PEEK flow splitter, a FAMOS micro autosampler, a modified electrochemical cell for on-line capillary PAD, and a capillary column (380 μm i.d.) packed with a new type of anion-exchange resin. This system operates with sensitivity in the low femtomol range. In addition, an on-line capillary desalter has been developed to allow direct coupling to the Bruker Esquire 3000 ion-trap mass spectrometer with electrospray ionization interface (ESI-IT-MS). Both systems have been evaluated using oligosaccharide standards as well as urine samples exhibiting various lysosomal oligosaccharide storage diseases. Initial data indicate that the robust and selective anion-exchange system, in combination with ESI-IT-MS for structure confirmation and analysis, provides a powerful platform that complements existing nano/capillary LC-MS methods for analytical determination of oligosaccharides in biological matrices.

Electrical Capacitance Volume Tomography for the Packed Bed Reactor ISS Flight Experiment

NASA Technical Reports Server (NTRS)

Marashdeh, Qussai; Motil, Brian; Wang, Aining; Liang-Shih, Fan

2013-01-01

Fixed packed bed reactors are compact, require minimum power and maintenance to operate, and are highly reliable. These features make this technology a highly desirable unit operation for long duration life support systems in space. NASA is developing an ISS experiment to address this technology with particular focus on water reclamation and air revitalization. Earlier research and development efforts funded by NASA have resulted in two hydrodynamic models which require validation with appropriate instrumentation in an extended microgravity environment. To validate these models, the instantaneous distribution of the gas and liquid phases must be measured.Electrical Capacitance Volume Tomography (ECVT) is a non-invasive imaging technology recently developed for multi-phase flow applications. It is based on distributing flexible capacitance plates on the peripheral of a flow column and collecting real-time measurements of inter-electrode capacitances. Capacitance measurements here are directly related to dielectric constant distribution, a physical property that is also related to material distribution in the imaging domain. Reconstruction algorithms are employed to map volume images of dielectric distribution in the imaging domain, which is in turn related to phase distribution. ECVT is suitable for imaging interacting materials of different dielectric constants, typical in multi-phase flow systems. ECVT is being used extensively for measuring flow variables in various gas-liquid and gas-solid flow systems. Recent application of ECVT include flows in risers and exit regions of circulating fluidized beds, gas-liquid and gas-solid bubble columns, trickle beds, and slurry bubble columns. ECVT is also used to validate flow models and CFD simulations. The technology is uniquely qualified for imaging phase concentrations in packed bed reactors for the ISS flight experiments as it exhibits favorable features of compact size, low profile sensors, high imaging speed, and flexibility to fit around columns of various shapes and sizes. ECVT is also safer than other commonly used imaging modalities as it operates in the range of low frequencies (1 MHz) and does not radiate radioactive energy. In this effort, ECVT is being used to image flow parameters in a packed bed reactor for an ISS flight experiment.

1.9 μm superficially porous packing material with radially oriented pores and tailored pore size for ultra-fast separation of small molecules and biomolecules.

PubMed

Min, Yi; Jiang, Bo; Wu, Ci; Xia, Simin; Zhang, Xiaodan; Liang, Zhen; Zhang, Lihua; Zhang, Yukui

2014-08-22

In this work, 1.9 μm reversed-phase packing materials with superficially porous structure were prepared to achieve the rapid and high efficient separation of peptides and proteins. The silica particles were synthesized via three steps, nonporous silica particle preparation by a modified seeded growth method, mesoporous shell formation by a one pot templated dissolution and redeposition strategy, and pore size expansion via acid-refluxing. By such a method, 1.9 μm superficially porous materials with 0.18 μm shell thickness and tailored pore diameter (10 nm, 15 nm) were obtained. After pore enlargement, the formerly dense arrays of mesoporous structure changed, the radially oriented pores dominated the superficially porous structure. The chromatographic performance of such particles was investigated after C18 derivatization. For packing materials with 1.9 μm diameter and 10 nm pore size, the column efficiency could reach 211,300 plates per m for naphthalene. To achieve the high resolution separation of peptides and proteins, particles with pore diameter of 15 nm were tailored, by which the baseline separation of 5 peptides and 5 intact proteins could be respectively achieved within 1 min, demonstrating the superiority in the high efficiency and high throughput analysis of biomolecules. Furthermore, BSA digests were well separated with peak capacity of 120 in 30 min on a 15 cm-long column. Finally, we compared our columns with a 1.7 μm Kinetex C18 column under the same conditions, our particles with 10nm pore size demonstrated similar performance for separation of the large intact proteins. Moreover, the particles with 15 nm pore size showed more symmetrical peaks for the separation of large proteins (BSA, OVA and IgG) and provided rapid separation of protein extracts from Escherichia coli in 5 min. All these results indicated that the synthesized 1.9 μm superficially porous silica packing materials would be promising in the ultra-fast and high-resolution separation of biomolecules. Copyright © 2014 Elsevier B.V. All rights reserved.

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

PubMed

Gritti, Fabrice; McDonald, Thomas; Gilar, Martin

2015-11-13

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

Combination fracturing/gravel-packing completion technique on the Amberjack, Mississippi Canyon 109 field

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

Hannah, R.R.; Park, E.I.; Porter, D.A.

1994-11-01

This paper describes a one-step fracturing/gravel-pack (frac-and-pack) completion procedure conducted on the BP Exploration Amberjack platform beginning in early 1992. This platform is 35 miles southwest of Venice, LA. The first four completions on this platform had an average positive skin values of 21. The goal of the frac-and-pack procedure was to reduce these skins to nearly zero. In total, 24 frac-and-pack operations were performed. Details of the fracture design, prefracture testing, fracture design and execution, and production response and a continuing optimization program are discussed. The fractures were performed with the screens in place with the gravel pack aftermore » the fracturing operation. The treatments were designed for the tip screenout technique to create wide fractures and to provide proppant loadings exceeding 8 lbm/ft. This paper presents the trend of the declining skin values, along with a discussion of time-dependent skins. The changes in fluids, breakers, and proppants are also presented. The average skin on 14 frac-and-pack completions was 5.3. The average skin on the final eight completions was 0.2.« less

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.

Development of High Precision Metal Micro-Electro-Mechanical-Systems Column for Portable Surface Acoustic Wave Gas Chromatograph

NASA Astrophysics Data System (ADS)

Iwaya, Takamitsu; Akao, Shingo; Sakamoto, Toshihiro; Tsuji, Toshihiro; Nakaso, Noritaka; Yamanaka, Kazushi

2012-07-01

In the field of environmental measurement and security, a portable gas chromatograph (GC) is required for the on-site analysis of multiple hazardous gases. Although the gas separation column has been downsized using micro-electro-mechanical-systems (MEMS) technology, an MEMS column made of silicon and glass still does not have sufficient robustness and a sufficiently low fabrication cost for a portable GC. In this study, we fabricated a robust and inexpensive high-precision metal MEMS column by combining diffusion-bonded etched stainless-steel plates with alignment evaluation using acoustic microscopy. The separation performance was evaluated using a desktop GC with a flame ionization detector and we achieved the high separation performance comparable to the best silicon MEMS column fabricated using a dynamic coating method. As an application, we fabricated a palm-size surface acoustic wave (SAW) GC combining this column with a ball SAW sensor and succeeded in separating and detecting a mixture of volatile organic compounds.

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.

A Comparative Study of Inspection Techniques for Array Packages

NASA Technical Reports Server (NTRS)

Mohammed, Jelila; Green, Christopher

2008-01-01

This viewgraph presentation reviews the inspection techniques for Column Grid Array (CGA) packages. The CGA is a method of chip scale packaging using high temperature solder columns to attach part to board. It is becoming more popular over other techniques (i.e. quad flat pack (QFP) or ball grid array (BGA)). However there are environmental stresses and workmanship challenges that require good inspection techniques for these packages.

Measuring Trace Hydrocarbons in Silanes

NASA Technical Reports Server (NTRS)

Lesser, L. A.

1984-01-01

Technique rapid and uses standard analytical equipment. Silane gas containing traces of hydrocarbons injected into carrier gas of moist nitrogen having about 0.2 percent water vapor. Carrier, water and silane pass through short column packed with powdered sodium hydroxide which combines moisture and silane to form nonvolatile sodium silicate. Carrier gas free of silane but containing nonreactive hydrocarbons, pass to silica-gel column where chromatographic separation takes place. Hydrocarbons measured by FID.

Biosorption of copper by marine algae Gelidium and algal composite material in a packed bed column.

PubMed

Vilar, Vítor J P; Botelho, Cidália M S; Loureiro, José M; Boaventura, Rui A R

2008-09-01

Marine algae Gelidium and algal composite material were investigated for the continuous removal of Cu(II) from aqueous solution in a packed bed column. The biosorption behaviour was studied during one sorption-desorption cycle of Cu(II) in the flow through column fed with 50 and 25 mg l(-1) of Cu(II) in aqueous solution, at pH 5.3, leading to a maximum uptake capacity of approximately 13 and 3 mg g(-1), respectively, for algae Gelidium and composite material. The breakthrough time decreases as the inlet copper concentration increases, for the same flow rate. The pH of the effluent decreases over the breakthrough time of copper ions, which indicates that ion exchange is one of the mechanisms involved in the biosorption process. Temperature has little influence on the metal uptake capacity and the increase of the ionic strength reduces the sorption capacity, decreasing the breakthrough time. Desorption using 0.1M HNO(3) solution was 100% effective. After two consecutive sorption-desorption cycles no changes in the uptake capacity of the composite material were observed. A mass transfer model including film and intraparticle resistances, and the equilibrium relationship, for adsorption and desorption, was successfully applied for the simulation of the biosorption column performance.

Monitoring Anaerobic TCE Degradation by Evanite Cultre in Column Packed with TCE-Contaminated Soil

NASA Astrophysics Data System (ADS)

Ko, J.; Han, K.; Ahn, G.; Park, S.; Kim, N.; Ahn, H.; Kim, Y.

2011-12-01

Trichloroethylene (TCE) is a long-term common groundwater pollutant because the compound with high density is slowly released into groundwater. Physical and chemical remediation processes have been used to clean-up the contaminant, but novel remediation technology is required to overcome a low efficiency of the traditional treatment process. Many researchers focused on biological process using an anaerobic TCE degrading culture, dehalococcoides spp., but it still needs to evaluate whether the process can be applied into field scale under aerobic condition. Therefore, in this work we examined two different types (i.e., Natural attenuation and bioaugmentation) of biological remediation process in anaerobic column packed with TCE-contaminated soil. A TCE degradation by indigenous microorganisms was confirmed by monitoring TCE and the metabolites (c-DCE, VC, ETH). However, TCE was transformed and stoichiometry amount of c-DCE was produced, and VC and ETH was not detected. To test bioaugmentation of Evanite culture containing dehalococcoides spp., Evanite culture was injected into the column and TCE degradation to c-DCE, VC, ETH was monitored. We are evaluating the transport of the Evanite culture in the column by measuring TCE and VC reductases. In the result, the TCE was completely degraded to ETH using hydrogen as electron donor generate by hydrogen-production fermentation from formate.

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.

Use of a Packed-Column Bioreactor for Isolation of Diverse Protease-Producing Bacteria from Antarctic Soil

PubMed Central

Wery, Nathalie; Gerike, Ursula; Sharman, Ajay; Chaudhuri, Julian B.; Hough, David W.; Danson, Michael J.

2003-01-01

Seventy-five aerobic heterotrophs have been isolated from a packed-column bioreactor inoculated with soil from Antarctica. The column was maintained at 10°C and continuously fed with a casein-containing medium to enrich protease producers. Twenty-eight isolates were selected for further characterization on the basis of morphology and production of clearing zones on skim milk plates. Phenotypic tests indicated that the strains were mainly psychrotrophs and presented a high morphological and metabolical diversity. The extracellular protease activities tested were optimal at neutral pH and between 30 and 45°C. 16S ribosomal DNA sequence analyses showed that the bioreactor was colonized by a wide variety of taxons, belonging to various bacterial divisions: α-, β-, and γ-Proteobacteria; the Flexibacter-Cytophaga-Bacteroides group; and high G+C gram-positive bacteria and low G+C gram-positive bacteria. Some strains represent candidates for new species of the genera Chryseobacterium and Massilia. This diversity demonstrates that the bioreactor is an efficient enrichment tool compared to traditional isolation strategies. PMID:12620829

Novel micro-extraction by packed sorbent procedure for the liquid chromatographic analysis of antiepileptic drugs in human plasma and urine.

PubMed

Rani, Susheela; Malik, Ashok K; Singh, Baldev

2012-02-01

A method for the simultaneous determination of the antiepileptic drugs, phenobarbital (PHB), phenytoin (PTN), carbamazepine (CBZ), primidone (PRM) and oxcarbazepine (OXC) in human plasma and urine samples by using micro-extraction in a packed syringe as the sample preparation method connected with LC/UV (MEPS/LC/UV) is described. Micro-extraction in a packed syringe (MEPS) is a new miniaturized, solid-phase extraction technique that can be connected online to gas or liquid chromatography without any modifications. In MEPS approximately 1 mg of the solid packing material is inserted into a syringe (100-250 μL) as a plug. Sample preparation takes place on the packed bed. The bed can be coated to provide selective and suitable sampling conditions. The new method is very promising, easy to use, fully automated, inexpensive and quick. The standard curves were obtained within the concentration range 1-500 ng/mL in both plasma and urine samples. The results showed high correlation coefficients (R(2) >0.988) for all of the analytes within the calibration range. The extraction recovery was found to be between 88.56 and 99.38%. The limit of quantification was found to be between 0.132 and 1.956 ng/mL. The precision (RSD) values of quality control samples (QC) had a maximum deviation of 4.9%. A comparison of the detection limits with similar methods indicates high sensitivity of the present method. The method is applied for the analysis of these drugs in real urine and plasma samples of epileptic patients. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Biological denitrification of high concentration nitrate waste

DOEpatents

Francis, Chester W.; Brinkley, Frank S.

1977-01-01

Biological denitrification of nitrate solutions at concentrations of greater than one kilogram nitrate per cubic meter is accomplished anaerobically in an upflow column having as a packing material a support for denitrifying bacteria.

Separation of actinides using capillary extraction chromatography-inductively coupled plasma mass spectrometry.

PubMed

Peterson, Dominic S; Montoya, Velma M

2009-08-01

Trace levels of actinides have been separated on capillary extraction chromatography columns. Detection of the actinides was achieved using an inductively coupled plasma mass spectrometer, which was coupled with the extraction chromatography system. In this study, we compare 30-cm long, 4.6 mm i.d. columns to capillary columns (750 microm i.d.) with lengths from 30 cm up to 150 cm. The columns that were tested were packed with TRU resin. We were able to separate a mixture of five actinides ((232)Th, (238)U, (237)Np, (239)Pu, and (241)Am). This work has application to rapid bioassay as well as automated separations of actinide materials.

Biofiltration of air polluted with toluene under steady-state conditions: Experimental observations

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

Kiared, K.; Fundenberger, B.; Brzezinski, R.

1997-11-01

In this study, the authors describe the removal of toluene vapors in a pilot scale biofilter. Biofiltration tests have been performed in a column fed upward with contaminated air at ambient conditions. The column was packed with a mixture of conditioned biomass and structuring agent on which a mixed microbial population of four selected strains was immobilized and then formed a biolayer. The biofilter was operated under various inlet-airstream toluene concentrations and flow rates of the contaminated airstream. Based on the present measurements, the biofilter proved effective in removing toluene at rates up to 165 g/h {center_dot} m{sup 3} ofmore » packing. The effect of some design and operation parameters (concentration of nutrients solution, presence of xylene, gas flow rate, pressure drop, temperature, etc.) are reported.« less

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

PubMed Central

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

2008-01-01

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

Reliability of simulated robustness testing in fast liquid chromatography, using state-of-the-art column technology, instrumentation and modelling software.

PubMed

Kormány, Róbert; Fekete, Jenő; Guillarme, Davy; Fekete, Szabolcs

2014-02-01

The goal of this study was to evaluate the accuracy of simulated robustness testing using commercial modelling software (DryLab) and state-of-the-art stationary phases. For this purpose, a mixture of amlodipine and its seven related impurities was analyzed on short narrow bore columns (50×2.1mm, packed with sub-2μm particles) providing short analysis times. The performance of commercial modelling software for robustness testing was systematically compared to experimental measurements and DoE based predictions. We have demonstrated that the reliability of predictions was good, since the predicted retention times and resolutions were in good agreement with the experimental ones at the edges of the design space. In average, the retention time relative errors were <1.0%, while the predicted critical resolution errors were comprised between 6.9 and 17.2%. Because the simulated robustness testing requires significantly less experimental work than the DoE based predictions, we think that robustness could now be investigated in the early stage of method development. Moreover, the column interchangeability, which is also an important part of robustness testing, was investigated considering five different C8 and C18 columns packed with sub-2μm particles. Again, thanks to modelling software, we proved that the separation was feasible on all columns within the same analysis time (less than 4min), by proper adjustments of variables. Copyright © 2013 Elsevier B.V. All rights reserved.

The Micro TIPS - Cases - Programmed Learning Course Package.

ERIC Educational Resources Information Center

Heriot-Watt Univ., Edinburgh (Scotland). Esmee Fairbairn Economics Research Centre.

Part of an economic education series, the course package is designed to teach basic concepts and principles of microeconomics and how they can be applied to various world problems. For use with college students, learning is gained through lectures, tutorials, textbooks, programmed text, cases, and TIPS (Teaching Information Processing System).…

Drill Bit Tip on Mars Rover Curiosity, Side View

NASA Image and Video Library

2013-02-04

The shape of the tip of the bit in the drill of NASA Mars rover Curiosity is apparent in this view recorded by the remote micro-imager in the rover ChemCam instrument on Mars. Jan. 29, 2012; the bit is about 0.6 inch 1.6 centimeters wide.

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.

CFD-DEM modeling the effect of column size and bed height on minimum fluidization velocity in micro fluidized beds with Geldart B particles

DOE PAGES

Xu, Yupeng; Li, Tingwen; Musser, Jordan; ...

2017-06-07

The fluidization behavior of Geldart B particles in micro fluidized beds is investigated numerically using Computational Fluid Dynamics coupled with Discrete Element Method (CFD-DEM) available in the open-source Multiphase Flow with Interphase eXchanges (MFIX) code. The effects of different bed inner diameters (D) of 8 mm, 12 mm, 16 mm and various initial static bed heights (H) were examined. It is found that both decreasing the column diameter and increasing the bed height in a micro fluidized bed increases the minimum fluidization velocity (Umf). The observed overshoot in pressure drop that occurs before the onset of fluidization decreases in magnitudemore » with increasing column diameter, however there is less sensitivity to bed height. Overall, the numerical results agree qualitatively with existing theoretical correlations and experimental studies. The simulations show that both column diameter and particle-wall friction contribute to the variation in minimum fluidization velocity. Finally, these two factors are coupled and hard to separate. The detailed influences of wall friction on minimum fluidization velocity are then investigated for a prescribed column diameter of 8 mm by varying the wall friction from 0 to 0.4.« less

CFD-DEM modeling the effect of column size and bed height on minimum fluidization velocity in micro fluidized beds with Geldart B particles

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

Xu, Yupeng; Li, Tingwen; Musser, Jordan

The fluidization behavior of Geldart B particles in micro fluidized beds is investigated numerically using Computational Fluid Dynamics coupled with Discrete Element Method (CFD-DEM) available in the open-source Multiphase Flow with Interphase eXchanges (MFIX) code. The effects of different bed inner diameters (D) of 8 mm, 12 mm, 16 mm and various initial static bed heights (H) were examined. It is found that both decreasing the column diameter and increasing the bed height in a micro fluidized bed increases the minimum fluidization velocity (Umf). The observed overshoot in pressure drop that occurs before the onset of fluidization decreases in magnitudemore » with increasing column diameter, however there is less sensitivity to bed height. Overall, the numerical results agree qualitatively with existing theoretical correlations and experimental studies. The simulations show that both column diameter and particle-wall friction contribute to the variation in minimum fluidization velocity. Finally, these two factors are coupled and hard to separate. The detailed influences of wall friction on minimum fluidization velocity are then investigated for a prescribed column diameter of 8 mm by varying the wall friction from 0 to 0.4.« less

"The Bug Investigators": Assessment of a School Teaching Resource to Improve Hygiene and Prudent Use of Antibiotics

ERIC Educational Resources Information Center

McNulty, Cliodna A. M.; Bowen, Jo; Gelb, David; Charlett, Andre

2007-01-01

Purpose: The aim of this study is to measure the effectiveness of the "Bug Investigators" pack in improving children's knowledge about micro-organisms, hygiene and antibiotics when it is used within the National Curriculum in junior schools. Design/methodology/approach: Teaching, using the "Bug Investigators" pack, was given by…

Quantitation of anticonvulsant drugs in serum by gas-chromatography on the stationary phase SP-2510.

PubMed

Godolphin, W; Thoma, J

1978-03-01

A new column packing, SP-2510 DA (Supelco, Inc., Bellefonte, Pa. 16823), is an excellent stationary phase for the determination of a wide variety of anticonvulsant drugs by gas--liquid chromatography without derivatization. However, when uncomplicated extraction procedures are used, serum cholesterol interferes with the determination of primidone. By the simple expedient of adding a short "pre-column" containing another phase (SP-2250 DA) the problem is overcome.

Determination of acetaminophen in human plasma by ion-pair reversed-phase high-performance liquid chromatography. Application to a single-dose pharmacokinetic study.

PubMed

Rustum, A M

1989-01-01

The determination of acetaminophen in biological samples of humans who have ingested normal and overdosage of the drug is necessary to understand the clinical pharmacokinetics of acetaminophen and to determine its distribution and toxicokinetic parameters. This paper describes a rapid, simple, and sensitive high-performance liquid chromatographic method for determining acetaminophen in human plasma. Acetaminophen is isolated from plasma by adding approximately 200 microL of acetonitrile and 50 mg of solid zinc sulfate to each milliliter of plasma. A short column (60 mm x 4.6 mm) slurry packed with 5.0-microns PRP-1 particles is used with an isocratic elution of 5.0 mM dibasic potassium phosphate and 5.0 mM tetrabutylammonium hydroxide/methanol, 70:30 (v/v). The flow rate is 1.0 mL/min. The acetaminophen peak is detected with a variable wavelength ultraviolet/visible detector at 250 nm and 0.50 to 0.002 AUFS. The analysis time of the assay is less than 15 min, and the limit of detection is 20 ng/mL for an 80-microL injection volume. The pharmacokinetics of acetaminophen in plasma from a subject who had orally ingested 975 mg of the drug in tablet form is conducted using this method, and various pharmacokinetic parameters are determined.

Differential expression of conserved and novel microRNAs during tail regeneration in the lizard Anolis carolinensis.

PubMed

Hutchins, Elizabeth D; Eckalbar, Walter L; Wolter, Justin M; Mangone, Marco; Kusumi, Kenro

2016-05-05

Lizards are evolutionarily the most closely related vertebrates to humans that can lose and regrow an entire appendage. Regeneration in lizards involves differential expression of hundreds of genes that regulate wound healing, musculoskeletal development, hormonal response, and embryonic morphogenesis. While microRNAs are able to regulate large groups of genes, their role in lizard regeneration has not been investigated. MicroRNA sequencing of green anole lizard (Anolis carolinensis) regenerating tail and associated tissues revealed 350 putative novel and 196 known microRNA precursors. Eleven microRNAs were differentially expressed between the regenerating tail tip and base during maximum outgrowth (25 days post autotomy), including miR-133a, miR-133b, and miR-206, which have been reported to regulate regeneration and stem cell proliferation in other model systems. Three putative novel differentially expressed microRNAs were identified in the regenerating tail tip. Differentially expressed microRNAs were identified in the regenerating lizard tail, including known regulators of stem cell proliferation. The identification of 3 putative novel microRNAs suggests that regulatory networks, either conserved in vertebrates and previously uncharacterized or specific to lizards, are involved in regeneration. These findings suggest that differential regulation of microRNAs may play a role in coordinating the timing and expression of hundreds of genes involved in regeneration.

Focus on Fruits: 10 Tips to Eat More Fruits

MedlinePlus

... lunch, pack a tangerine, banana, or grapes to eat or choose fruits from a salad bar. Individual containers of fruits like peaches or applesauce are easy to carry and convenient for lunch. 7 Enjoy fruit at dinner, too At dinner, add crushed pineapple to coleslaw ...

Hysteresis of Soil Point Water Retention Functions Determined by Neutron Radiography

NASA Astrophysics Data System (ADS)

Perfect, E.; Kang, M.; Bilheux, H.; Willis, K. J.; Horita, J.; Warren, J.; Cheng, C.

2010-12-01

Soil point water retention functions are needed for modeling flow and transport in partially-saturated porous media. Such functions are usually determined by inverse modeling of average water retention data measured experimentally on columns of finite length. However, the resulting functions are subject to the appropriateness of the chosen model, as well as the initial and boundary condition assumptions employed. Soil point water retention functions are rarely measured directly and when they are the focus is invariably on the main drying branch. Previous direct measurement methods include time domain reflectometry and gamma beam attenuation. Here we report direct measurements of the main wetting and drying branches of the point water retention function using neutron radiography. The measurements were performed on a coarse sand (Flint #13) packed into 2.6 cm diameter x 4 cm long aluminum cylinders at the NIST BT-2 (50 μm resolution) and ORNL-HFIR CG1D (70 μm resolution) imaging beamlines. The sand columns were saturated with water and then drained and rewetted under quasi-equilibrium conditions using a hanging water column setup. 2048 x 2048 pixel images of the transmitted flux of neutrons through the column were acquired at each imposed suction (~10-15 suction values per experiment). Volumetric water contents were calculated on a pixel by pixel basis using Beer-Lambert’s law in conjunction with beam hardening and geometric corrections. The pixel rows were averaged and combined with information on the known distribution of suctions within the column to give 2048 point drying and wetting functions for each experiment. The point functions exhibited pronounced hysteresis and varied with column height, possibly due to differences in porosity caused by the packing procedure employed. Predicted point functions, extracted from the hanging water column volumetric data using the TrueCell inverse modeling procedure, showed very good agreement with the range of point functions measured within the column using neutron radiography. Extension of these experiments to 3-dimensions using neutron tomography is planned.

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.

Practical Tips for the Safe Handling of Micro-organisms in Schools

ERIC Educational Resources Information Center

Holt, G.

1974-01-01

Outlines safe laboratory procedures for the handling of micro-organisms including aseptic technique, manipulation of cultures, and treatment of contaminated equipment. Identifies the principal hazard as the microbial aerosol, explains its possible effects, and describes the appropriate precautions. (GS)

Hollow Fibers Structured Packings in Olefin/Paraffin Distillation: Apparatus Scale-Up and Long-Term Stability

DOE PAGES

Yang, Dali; Le, Loan; Martinez, Ronald; ...

2013-06-21

Following the conceptual demonstration of high separation efficiency and column capacity obtained in olefin/paraffin distillation using hollow fiber structured packings (HFSPs) in a bench scale (J. Membr. Sci.2006, 2007, and 2010), we scaled-up this process with a 10-fold increase in the internal flow rate and a 3-fold increase in the module length. We confirmed that the HFSPs technology gives high separation efficiency and column capacity in iso-/n-butane distillation for 18 months. We systematically investigated the effects of packing density, concentration of light component, reflux ratio, and module age on the separation efficiency and operating stability. The comprehensive characterizations using scanningmore » electron microscopy (SEM), Brunauer–Emmett–Teller (BET), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), and dynamic mechanical analysis (DMA) were carried out to probe the changes in the morphological, thermal, and mechanical properties of polypropylene (PP) hollow fibers over the aging process. Our results suggest that after a long-term exposure to light hydrocarbon environments at ≤70 °C the morphological and mechanical properties of the PP polymer do not degrade significantly in a propane/propylene and iso-/n-butane environment.« less

Comparison of corneal collagen cross-linking (PACK-CXL) and voriconazole treatments in experimental fungal keratitis.

PubMed

Özdemir, Hüseyin Baran; Kalkancı, Ayşe; Bilgihan, Kamil; Göçün, Pınar Uyar; Öğüt, Betül; Karakurt, Funda; Erdoğan, Merve

2018-06-04

To compare the antifungal efficacy of corneal collagen cross-linking with photoactivated riboflavin (PACK-CXL) and voriconazole in experimental Fusarium solani and Candida albicans keratitis models. Sixty-four corneas of 32 New Zealand rabbits were included and divided into two main groups. Intrastromal injection of Fusarium and Candida suspensions was performed, and it was observed that keratitis was formed on the third day. Both groups were randomly separated into the following four groups: control, PACK-CXL, voriconazole and PACK-CXL combined with voriconazole. PACK-CXL was applied using 0.25% riboflavin in an accelerated Dresden protocol (total ultraviolet A dose 5.4 J/cm²). Voriconazole was applied topically as 7x1/day with a dose of 1% (10 mg/ml). Corneal buttons were excised on the tenth day, and microbiological and pathological examinations were performed. The PACK-CXL and PACK-CXL combined with voriconazole groups each had 100 colony-forming unit (CFU/ml) of reproduced micro-organisms compared with 500 CFU/ml in the voriconazole group and 1500 CFU/ml in the control group (p < 0.001) in the Fusarium keratitis model. The PACK-CXL combined with voriconazole group had 100 CFU/ml, the PACK-CXL group had 150 CFU/ml, and the voriconazole group had 200 CFU/ml of reproduced micro-organisms compared with 4000 CFU/ml in the control group (p < 0.002) in the Candida keratitis model. (p < 0.001). Fewer hyphae and non-specific stromal changes were observed in the pathological cross sections examined in subgroups that used CXL. There was less fungus reproduction and a lower keratitis score for Fusarium solani and Candida albicans in the treatment groups compared to the control groups, especially in groups that used PACK-CXL. These results suggest that it is useful to combine PACK-CXL treatment with medical treatment in the fungal keratitis algorithm at the early stage of the disease. © 2018 Acta Ophthalmologica Scandinavica Foundation. Published by John Wiley & Sons Ltd.

The rationale for the optimum efficiency of columns packed with new 1.9μm fully porous Titan-C18 particles-a detailed investigation of the intra-particle diffusivity.

PubMed

Gritti, Fabrice; Guiochon, Georges

2014-08-15

In a previous report, it was reported that columns packed with fully porous 1.9μm Titan-C18 particles provided a minimum reduced plate height as small as 1.7 for the most retained compound (n-octanophenone) under RPLC conditions. These particles are characterized by a relatively narrow size distribution with a relative standard deviation (RSD) of only 10%. A column packed with classical 5μm Symmetry-C18 particles, used as a reference RPLC column, generated a minimum reduced plate height of 2.1 for the same retained compound. This work demonstrates that this was due to an unusually low intra-particle diffusivity across these particles, which leads to a small longitudinal diffusion coefficient along the column. The demonstration is based on the combination of accurate measurements of the height equivalent to a theoretical plate (HETP), inverse size exclusion chromatography (ISEC), peak parking (PP), and minor disturbance method (MDM) experiments. The experimental results show that the reduced eddy dispersion HETP term (A=0.8 for a reduced velocity of 5), the internal particle porosity (ϵp=0.35), and the enrichment of acetonitrile in the pore volume (75% acetonitrile in the bulk, 85% inside the mesoporous volume) are identical on both the Titan-C18 and Symmetry-C18 columns. The difference between the internal structures of these two brands of RPLC-C18 fully porous particles lies in the values of the internal obstruction factor γp, which is 0.42 for the Symmetry-C18 but only 0.26 for the Titan-C18 particles. This is in part related to the diffusion hindrance due to the small average pore size of the Titan-C18 particles, around 59Å versus 77Å for Symmetry-C18 particles. A simple model of constriction along diffusion paths having the shape of a truncated cone suggests that the width of the pore size distribution (RSD of 30% and 20% for Titan-C18 and Symmetry-C18 particles) is mostly responsible for the difference in their obstruction factors. Copyright © 2014 Elsevier B.V. All rights reserved.

Simple gas chromatographic system for analysis of microbial respiratory gases

NASA Technical Reports Server (NTRS)

Carle, G. C.

1972-01-01

Dual column ambient temperature system, consisting of pair of capillary columns, microbead thermistor detector and micro gas-sampling valve, is used in remote life-detection equipment for space experiments. Performance outweighs advantage gained by utilizing single-column systems to reduce weight, conserve carrier gas and operate at lower power levels.

Chromatography modelling to describe protein adsorption at bead level.

PubMed

Gerontas, Spyridon; Shapiro, Michael S; Bracewell, Daniel G

2013-04-05

Chromatographic modelling can be used to describe and further understand the behaviour of biological species during their chromatography separation on adsorption resins. Current modelling approaches assume uniform rate parameters throughout the column. Software and hardware advances now allow us to consider what can be learnt from modelling at bead level, enabling simulation of heterogeneity in bead and packed bed structure due to design or due to changes during operation. In this paper, a model has been developed to simulate at bead level protein loading in 1.5 μl microfluidic columns. This model takes into account the heterogeneity in bead sizes and the spatial variations of the characteristics of a packed bed, such as bed void fraction and dispersion, thus offering a detailed description of the flow field and mass transfer phenomena. Simulations were shown to be in good agreement with published experimental data. Copyright © 2013 Elsevier B.V. All rights reserved.

Experimental and Numerical Investigation of Adsorption/Desorption in Packed Sorption Beds Under Ideal and Non-Ideal Flows

NASA Technical Reports Server (NTRS)

Mohamadinejad, H.; Knox, J. C.; Smith, James E.

1999-01-01

The importance of the wall effect on packed beds in the adsorption and desorption of carbon dioxide, nitrogen, and water on molecular sieve 5A of 0.127 cm in radius is examined experimentally and with one-dimensional computer simulations. Experimental results are presented for a 22.5-cm long by 4.5-cm diameter cylindrical column with concentration measurements taken at various radial locations. The set of partial differential equations are solved using finite differences and Newman's method. Comparison of test data with the axial-dispersed, non-isothermal, linear driving force model suggests that a two-dimensional model (submitted to Separation Science and Technology) is required for accurate simulation of the average column breakthrough concentration. Additional comparisons of test data with the model provided information on the interactive effects of carrier gas coadsorption with CO2, as well as CO2-H2O interactions.

Overloaded elution band profiles of ionizable compounds in reversed-phase liquid chromatography: Influence of the competition between the neutral and the ionic species

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

Gritti, Fabrice; Guiochon, Georges A

2008-01-01

The parameters that affect the shape of the band profiles of acido-basic compounds under moderately overloaded conditions (sample size less than 500 nmol for a conventional column) in RPLC are discussed. Only analytes that have a single pK{sub a} are considered. In the buffer mobile phase used for their elution, their dissociation may, under certain conditions, cause a significant pH perturbation during the passage of the band. Two consecutive injections (3.3 and 10 {micro}L) of each one of three sample solutions (0.5, 5, and 50 mM) of ten compounds were injected on five C{sub 18}-bonded packing materials, including the 5more » {micro}m Xterra-C{sub 18} (121 {angstrom}), 5 {micro}m Gemini-C{sub 18} (110 {angstrom}), 5 {micro}m Luna-C{sub 18}(2) (93 {angstrom}), 3.5 {micro}m Extend-C{sub 18} (80 {angstrom}), and 2.7 {micro}m Halo-C{sub 18} (90 {angstrom}). The mobile phase was an aqueous solution of methanol buffered at a constant {sub W}{sup W}pH of 6, with a phosphate buffer. The total concentration of the phosphate groups was constant at 50 mM. The methanol concentration was adjusted to keep all the retention factors between 1 and 10. The compounds injected were phenol, caffeine, 3-phenyl 1-propanol, 2-phenyl butyric acid, amphetamine, aniline, benzylamine, p-toluidine, procainamidium chloride, and propranololium chloride. Depending on the relative values of the analyte pK{sub a} and the buffer solution pH, these analytes elute as the neutral, the cationic, or the anionic species. The influence of structural parameters such as the charge, the size, and the hydrophobicity of the analytes on the shape of its overloaded band profile is discussed. Simple but general rules predict these shapes. An original adsorption model is proposed that accounts for the unusual peak shapes observed when the analyte is partially dissociated in the buffer solution during its elution.« less

Influence of geometry on pressure and velocity distribution in packed-bed methanol steam reforming reactor

NASA Astrophysics Data System (ADS)

Ivanović, Ivana; Sedmak, Aleksandar; Milošević, Miloš; Cvetković, Ivana; Pohar, Andrej; Likozar, Blaž

2017-07-01

The main tasks of this research is to propose several changes in the packed bed micro methanol steam reformer geometry in order to ensure its performance. The reformer is an integral part of the existing indirect internal reforming high temperature PEMFC and most of its geometry is already defined. The space for remodeling is very limited.

Efficient fabrication of carbon nanotube micro tip arrays by tailoring cross-stacked carbon nanotube sheets.

PubMed

Wei, Yang; Liu, Peng; Zhu, Feng; Jiang, Kaili; Li, Qunqing; Fan, Shoushan

2012-04-11

Carbon nanotube (CNT) micro tip arrays with hairpin structures on patterned silicon wafers were efficiently fabricated by tailoring the cross-stacked CNT sheet with laser. A blade-like structure was formed at the laser-cut edges of the CNT sheet. CNT field emitters, pulled out from the end of the hairpin by an adhesive tape, can provide 150 μA intrinsic emission currents with low beam noise. The nice field emission is ascribed to the Joule-heating-induced desorption of the emitter surface by the hairpin structure, the high temperature annealing effect, and the surface morphology. The CNT emitters with hairpin structures will greatly promote the applications of CNTs in vacuum electronic devices and hold the promises to be used as the hot tips for thermochemical nanolithography. More CNT-based structures and devices can be fabricated on a large scale by this versatile method. © 2012 American Chemical Society

Ultrahigh performance supercritical fluid chromatography of lipophilic compounds with application to synthetic and commercial biodiesel.

PubMed

Ashraf-Khorassani, M; Yang, J; Rainville, P; Jones, M D; Fountain, K J; Isaac, G; Taylor, L T

2015-03-01

Ultrahigh performance supercritical fluid chromatography (UHPSFC) in combination with sub-2μm particles and either diode array ultraviolet (UV), evaporative light scattering, (ELSD), or mass spectrometric (MS) detection has been shown to be a valuable technique for the determination of acylglycerols in soybean, corn, sesame, and tobacco seed oils. Excellent resolution on an un-endcapped single C18 column (3.0mm×150mm) with a mobile phase gradient of acetonitrile and carbon dioxide in as little as 10min served greatly as an improvement on first generation packed column SFC instrumentation. Unlike high resolution gas chromatography and high performance liquid chromatography with mass spectrometric detection, UHPSFC/MS was determined to be a superior analytical tool for both separation and detection of mono-, di-, and tri-acylglycerols as well as free glycerol itself in biodiesel without derivatization. Baseline separation of residual tri-, di-, and mono-acylglycerols alongside glycerol at 0.05% (w/w) was easily obtained employing packed column SFC. The new analytical methodology was applied to both commercial B100 biodiesel (i.e. fatty acid methyl esters) derived from vegetable oil and to an "in-house" synthetic biodiesel (i.e. fatty acid ethyl esters) derived from tobacco seed oil and ethanol both before and after purification via column chromatography on bare silica. Copyright © 2014 Elsevier B.V. All rights reserved.

Transport of bare and capped zinc oxide nanoparticles is dependent on porous medium composition

NASA Astrophysics Data System (ADS)

Kurlanda-Witek, H.; Ngwenya, B. T.; Butler, I. B.

2014-07-01

Zinc oxide (ZnO) nanoparticles are one of the most frequently used nanoparticles in industry and hence are likely to be introduced to the groundwater environment. The mobility of these nanoparticles in different aquifer materials has not been assessed. While some studies have been published on the transport of ZnO nanoparticles in individual porous media, these studies do not generally account for varying porous medium composition both within and between aquifers. As a first step towards understanding the impact of this variability, this paper compares the transport of bare ZnO nanoparticles (bZnO-NPs) and capped ZnO nanoparticles, coated with tri-aminopropyltriethoxysilane (cZnO-NPs), in saturated columns packed with glass beads, fine grained sand and fine grained calcite, at near-neutral pH and groundwater salinity levels. With the exception of cZnO-NPs in sand columns, ZnO nanoparticles are highly immobile in all three types of studied porous media, with most retention taking place near the column inlet. Results are in general agreement with DLVO theory, and the deviation in experiments with cZnO-NPs flowing through columns packed with sand is linked to variability in zeta potential of the capped nanoparticles and sand grains. Therefore, differences in surface charge of nanoparticles and porous media are demonstrated to be key drivers in nanoparticle transport.

Direct coupling of packed column supercritical fluid chromatography to continuous corona discharge ion mobility spectrometry.

PubMed

Rahmanian, A; Ghaziaskar, H S; Khayamian, T

2013-01-11

In this study, packed column supercritical fluid chromatography (SFC) was directly coupled to a continuous corona discharge (CD) ion mobility spectrometer (IMS) with several modifications. The main advantage of the developed detector is its capability to introduce full column effluent up to 2000 mL min(-1) CO(2) gas directly into the IMS cell relative to 40 mL min(-1) CO(2) gas as a maximum tolerance, reported for the previous IMS detectors. This achievement was made possible because of using corona discharge instead of (63)Ni as an ionization source and locating the inlet and outlet of the CO(2) gas in the counter electrode of the CD in opposite direction. In addition, a heated interface was placed between back pressure regulator (BPR) and the IMS cell to heat the output of the BPR for introducing sample as the gas phase into the IMS cell. Furthermore, a make-up methanol flow was introduced between the column outlet and BPR to provide a more uniform flow through the BPR and also to prevent freezing and deposition of the analytes in the BPR. The performance of the SFC-CD-IMS was evaluated by analysis of testosterone, medroxyprogesterone, caffeine, and theophylline as test compounds and figures of merit for these compounds have been calculated. Copyright © 2012 Elsevier B.V. All rights reserved.

LIQUID-LIQUID EXTRACTION COLUMNS

DOEpatents

Thornton, J.D.

1957-12-31

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

The electrical conductance growth of a metallic granular packing

NASA Astrophysics Data System (ADS)

Jakšić, Zorica M.; Cvetković, Milica; Šćepanović, Julija R.; Lončarević, Ivana; Budinski-Petković, Ljuba; Vrhovac, Slobodan B.

2017-06-01

We report on measurements of the electrical conductivity on a two-dimensional packing of metallic disks when a stable current of 1 mA flows through the system. At low applied currents, the conductance σ is found to increase by a pattern σ( t) = σ ∞ - Δσ E α [ - ( t/ τ) α ], where E α denotes the Mittag-Leffler function of order α ∈ (0,1). By changing the inclination angle θ of the granular bed from horizontal, we have studied the impact of the effective gravitational acceleration g e ff = gsin θ on the relaxation features of the conductance σ( t). The characteristic timescale τ is found to grow when effective gravity g e ff decreases. By changing both the distance between the electrodes and the number of grains in the packing, we have shown that the long term resistance decay observed in the experiment is related to local micro-contacts rearrangements at each disk. By focusing on the electro-mechanical processes that allow both creation and breakdown of micro-contacts between two disks, we present an approach to granular conduction based on subordination of stochastic processes. In order to imitate, in a very simplified way, the conduction dynamics of granular material at low currents, we impose that the micro-contacts at the interface switch stochastically between two possible states, "on" and "off", characterizing the conductivity of the micro-contact. We assume that the time intervals between the consecutive changes of state are governed by a certain waiting-time distribution. It is demonstrated how the microscopic random dynamics regarding the micro-contacts leads to the macroscopic observation of slow conductance growth, described by an exact fractional kinetic equations.

A novel AFM-based 5-axis nanoscale machine tool for fabrication of nanostructures on a micro ball

NASA Astrophysics Data System (ADS)

Geng, Yanquan; Wang, Yuzhang; Yan, Yongda; Zhao, Xuesen

2017-11-01

This paper presents a novel atomic force microscopy (AFM)-based 5-axis nanoscale machine tool developed to fabricate nanostructures on different annuli of the micro ball. Different nanostructures can be obtained by combining the scratching trajectory of the AFM tip with the movement of the high precision air-bearing spindle. The center of the micro ball is aligned to be coincided with the gyration center of the high precision to guarantee the machining process during the rotating of the air-bearing spindle. Processing on different annuli of the micro ball is achieved by controlling the distance between the center of the micro ball and the rotation center of the AFM head. Nanostructures including square cavities, circular cavities, triangular cavities, and an annular nanochannel are machined successfully on the three different circumferences of a micro ball with a diameter of 1500 μm. Moreover, the influences of the error motions of the high precision air-bearing spindle and the eccentric between the micro ball and the gyration center of the high precision air-bearing spindle on the processing position error on the micro ball are also investigated. This proposed machining method has the potential to prepare the inertial confinement fusion target with the expected dimension defects, which would advance the application of the AFM tip-based nanomachining approach.

Preparation of acryloyl β-cyclodextrin-silica hybrid monolithic column and its application in pipette tip solid-phase extraction and HPLC analysis of methyl parathion and fenthion.

PubMed

Chen, Ling; Dang, Xueping; Ai, Youhong; Chen, Huaixia

2018-05-07

An acryloyl β-cyclodextrin-silica hybrid monolithic column for pipette tip solid-phase extraction and high-performance liquid chromatography determination of methyl parathion and fenthion have been prepared through a sol-gel polymerization method. The synthesis conditions, including the volume of cross-linker and the ratio of inorganic solution to organic solution, were optimized. The prepared monolithic column was characterized by thermogravimetric analysis, scanning electron microscopy and Fourier transform infrared spectroscopy. The eluent type, volume and flow rate, sample volume, flow rate, acidity and ionic strength were optimized in detail. Under the optimized conditions, a simple and sensitive pipette tip solid-phase extraction with high-performance liquid chromatography method was developed for the determination of methyl parathion and fenthion in lettuce. The method yielded a linear calibration curve in the concentration ranges of 15-400 μg/kg for methyl parathion and 20-400 μg/kg for fenthion with correlation coefficients of above 0.9957. The limits of detection were 4.5 μg/kg for methyl parathion and 6.0 μg/kg for fenthion, respectively. The recoveries of methyl parathion and fenthion spiked in lettuce ranged from 96.0 to 104.2% with relative standard deviations less than 8.4%. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

The role of upstream distal electrodes in mitigating electrochemical degradation of ionic liquid ion sources

NASA Astrophysics Data System (ADS)

Brikner, Natalya; Lozano, Paulo C.

2012-11-01

Ionic liquid ion sources produce molecular ions from micro-tip emitters wetted with room-temperature molten salts. When a single ion polarity is extracted, counterions accumulate and generate electrochemical reactions that limit the source lifetime. The dynamics of double layer formation are reviewed and distal electrode contacts are introduced to resolve detrimental electrochemical decomposition effects at the micro-tip apex. By having the emitter follow the ionic liquid potential, operation can be achieved for an extended period of time with no apparent degradation of the material, indicating that electrochemistry can be curtailed and isolated to the upstream distal electrode.

Laser ablation and column formation in silicon under oxygen-rich atmospheres

NASA Astrophysics Data System (ADS)

Pedraza, A. J.; Fowlkes, J. D.; Lowndes, D. H.

2000-11-01

The microstructure formed at the surface of silicon by cumulative pulsed-laser irradiation in oxygen-rich atmospheres consists of an array of microcolumns surrounded by microcanyons and microholes. Formation of SiOx at the exposed surface of silicon is most likely responsible for the occurrence of etching/ablation that causes the continuous deepening of canyons and holes. The growth mechanism of columns that is supported by the experimental evidence presented here is a process in which the columns are fed at their tips by the silicon-rich ablation plasma produced during pulsed-laser irradiation.

Drying in porous media with gravity-stabilized fronts: experimental results.

PubMed

Yiotis, A G; Salin, D; Tajer, E S; Yortsos, Y C

2012-08-01

In a recent paper [Yiotis et al., Phys. Rev. E 85, 046308 (2012)] we developed a model for the drying of porous media in the presence of gravity. It incorporated effects of corner film flow, internal and external mass transfer, and the effect of gravity. Analytical results were derived when gravity opposes drying and hence leads to a stable percolation drying front. In this paper, we test the theory using laboratory experiments. A series of isothermal drying experiments in glass bead packings saturated with volatile hydrocarbons is conducted. The transparent glass cells containing the packing allow for the visual monitoring of the phase distribution patterns below the surface, including the formation of liquid films, as the gaseous phase invades the pore space, and for the control of the thickness of the diffusive mass boundary layer over the packing. The experimental results agree very well with theory, provided that the latter is generalized to account for the effects of corner roundness in the film region (which was neglected in the theoretical part). We demonstrate the existence of an early constant rate period (CRP), which lasts as long as the films saturate the surface of the packing, and of a subsequent falling rate period (FRP), which begins practically after the detachment of the film tips from the external surface. During the CRP, the process is controlled by diffusion within the stagnant gaseous phase in the upper part of the cells, yielding a Stefan tube problem solution. During the FRP, the process is controlled by diffusion within the packing, with a drying rate inversely proportional to the observed position of the film tips in the cell. Theoretical and experimental results compare favorably for a specific value of the roundness of the films, which is found to be constant and equal to 0.2 for various conditions, and verify the theoretical dependence on the capillary Ca(f), Bond Bo, and Sherwood Sh numbers.

Chromatographic performance of synthetic polycrystalline diamond as a stationary phase in normal phase high performance liquid chromatography.

PubMed

Peristyy, Anton; Paull, Brett; Nesterenko, Pavel N

2015-04-24

The chromatographic properties of high pressure high temperature synthesised diamond (HPHT) are investigated in normal phase mode of high performance liquid chromatography. Purified nonporous irregular shape particles of average particles size 1.2 μm and specific surface area 5.1 m(2) g(-1) were used for packing 100×4.6 mm ID or 50×4.6 mm ID stainless steel columns. The retention behaviour of several classes of compounds including alkyl benzenes, polyaromatic hydrocarbons (PAH), alkylphenylketones, phenols, aromatic acids and bases were studied using n-hexane-2-propanol mixtures as mobile phase. The results are compared with those observed for microdispersed sintered detonation nanodiamond (MSDN) and porous graphitic carbon (PGC). HPHT diamond revealed distinctive separation selectivity, which is orthogonal to that observed for porous graphitic carbon; while selectivities of HPHT diamond and microdispersed sintered detonation nanodiamonds are similar. Owing to non-porous particle nature, columns packed with high pressure high temperature diamond exhibited excellent mass transfer and produce separations with maximum column efficiency of 128,200 theoretical plates per meter. Copyright © 2015 Elsevier B.V. All rights reserved.

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

PubMed

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

2016-11-10

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

Critical conditions of polymer adsorption and chromatography on non-porous substrates.

PubMed

Cimino, Richard T; Rasmussen, Christopher J; Brun, Yefim; Neimark, Alexander V

2016-07-15

We present a novel thermodynamic theory and Monte Carlo simulation model for adsorption of macromolecules to solid surfaces that is applied for calculating the chain partition during separation on chromatographic columns packed with non-porous particles. We show that similarly to polymer separation on porous substrates, it is possible to attain three chromatographic modes: size exclusion chromatography at very weak or no adsorption, liquid adsorption chromatography when adsorption effects prevail, and liquid chromatography at critical conditions that occurs at the critical point of adsorption. The main attention is paid to the analysis of the critical conditions, at which the retention is chain length independent. The theoretical results are verified with specially designed experiments on isocratic separation of linear polystyrenes on a column packed with non-porous particles at various solvent compositions. Without invoking any adjustable parameters related to the column and particle geometry, we describe quantitatively the observed transition between the size exclusion and adsorption separation regimes upon the variation of solvent composition, with the intermediate mode occurring at a well-defined critical point of adsorption. A relationship is established between the experimental solvent composition and the effective adsorption potential used in model simulations. Copyright © 2016 Elsevier Inc. All rights reserved.

The zooplankton food web under East Antarctic pack ice - A stable isotope study

NASA Astrophysics Data System (ADS)

Jia, Zhongnan; Swadling, Kerrie M.; Meiners, Klaus M.; Kawaguchi, So; Virtue, Patti

2016-09-01

Understanding how sea ice serves zooplankton species during the food-limited season is crucial information to evaluate the potential responses of pelagic food webs to changes in sea-ice conditions in the Southern Ocean. Stable isotope analyses (13C/12C and 15N/14N) were used to compare the dietary preferences and trophic relationships of major zooplankton species under pack ice during two winter-spring transitions (2007 and 2012). During sampling, furcilia of Euphausia superba demonstrated dietary plasticity between years, herbivory when feeding on sea-ice biota, and with a more heterotrophic diet when feeding from both the sea ice and the water column. Carbon isotope signatures suggested that the pteropod Limacina helicina, small copepods Oithona spp., ostracods and amphipods relied heavily on sea-ice biota. Post larval E. superba and omnivorous krill Thysanoessa macrura consumed both water column and ice biota, but further investigations are needed to estimate the contribution from each source. Large copepods and chaetognaths overwintered on a water column-based diet. Our study suggests that warm and permeable sea ice is more likely to provide food for zooplankton species under the ice than the colder ice.

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

PubMed

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

2007-02-01

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

Liquid Chromatographic Determination of Nitroanilines: An Experiment for the Quantitative Analysis Laboratory.

ERIC Educational Resources Information Center

Cantwell, Frederick F.; Brown, David W.

1981-01-01

Describes a three-hour liquid chromatography experiment involving rapid separation of colored compounds in glass columns packed with a nonpolar absorbent. Includes apparatus design, sample preparation, experimental procedures, and advantages for this determination. (SK)

Hover and Wind-Tunnel Testing of Shrouded Rotors for Improved Micro Air Vehicle Design

DTIC Science & Technology

2008-01-01

and the shroud surface pressure distributions. The uniformity of the wake was improved by the presence of the shrouds and by decreasing the blade tip...213 3.35 Effect of blade tip clearance on shrouded-rotor exit-plane wake profiles215 3.36 Effects of changing blade tip clearance on induced...Wright [139] developed a vortex wake model for heavily loaded ducted fans, in which the “inner vortex sheets [shed from the blades ] move at a different

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

PubMed

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

2018-02-01

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

Characterization of Chlorinated Solvent Degradation in a Constructed Wetland

DTIC Science & Technology

2003-03-25

the flows to be different under the same pressure. A 30m Restek RTX- VRX (Model 49314) column was connected to the micro-Electron Capture Detector...min) 2.00 Gas Type: Helium Column 1 (Restek 49314 RTX- VRX ) Column 2 (J&W 113-4332 GS-GASPRO) Max Temp (deg C) 260 Max Temp (deg C

Ideal versus real automated twin column recycling chromatography process.

PubMed

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

2017-07-28

The full baseline separation of two compounds (selectivity factors α<1.03) is either impractical (too long analysis times) or even impossible when using a single column of any length given the pressure limitations of current LC instruments. The maximum efficiency is that of an infinitely long column operated at infinitely small flow rates. It is determined by the maximum allowable system pressure, the column permeability (particle size), the viscosity of the eluent, and the intensity of the effective diffusivity of the analytes along the column. Alternatively, the twin-column recycling separation process (TCRSP) can overcome the efficiency limit of the single-column approach. In the TCRSP, the sample mixture may be transferred from one to a second (twin) column until its band has spread over one column length. Basic theory of chromatography is used to confirm that the speed-resolution performance of the TCRSP is intrinsically superior to that of the single-column process. This advantage is illustrated in this work by developing an automated TCRSP for the challenging separation of two polycyclic aromatic hydrocarbon (PAH) isomers (benzo[a]anthracene and chrysene) in the reversed-phase retention mode at pressure smaller than 5000psi. The columns used are the 3.0mm×150mm column packed with 3.5μm XBridge BEH-C 18 material (α=1.010) and the 3.0mm or 4.6mm×150mm columns packed with the same 3.5μm XSelect HSST 3 material (α=1.025). The isocratic mobile phase is an acetonitrile-water mixture (80/20, v/v). Remarkably, significant differences are observed between the predicted retention times and efficiencies of the ideal TCRSP (given by the number of cycles multiplied by the retention time and efficiency of one column) and those of the real TCRSP. The fundamental explanation lies in the pressure-dependent retention of these PAHs or in the change of their partial molar volume as they are transferred from the mobile to the stationary phase. A revisited retention and efficiency model is then built to predict the actual performance of real TCRSPs. The experimental and calculated resolution data are found in very good agreement for a change, Δv m =-10cm 3 /mol, of the partial molar volume of the two PAH isomers upon transfer from the acetonitrile-water eluent mixture to the silica-C 18 stationary phase. Copyright © 2017 Elsevier B.V. All rights reserved.

Effectiveness of cigarette filter tips for reducing cadmium in relation to other mainstream smoke constituents

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

Bache, C.A.; Lisk, D.J.; Shane, B.S.

The effectiveness of filter tips for reducing cadmium, tar, nicotine, carbon monoxide and carbon dioxide in cigarettes was studied. The cigarettes were made from tobacco grown on municipal sewage sludge-amended soil and were therefore high in cadmium. When machine-smoked, filter tips did not result in a significant reduction of cadmium deposited on Cambridge filters. This may indicate that a considerable fraction of cadmium is present in the vapor phase of the smoke and therefore not reduced to the same extent as the tar by certain filters. Nicotine and carbon monoxide were reduced to a lesser extent than tar. This indicatesmore » that the filter tip has influenced the combustion of the tobacco column during smoking.« less

Gain attention, enhance memory, and improve learning with brain-based strategies.

PubMed

Restaino, Rusti

2011-05-01

Applying what we know about brain function to both traditional and online teaching is easy. This column discusses brain function and "tips" for structuring teaching based on it. Copyright 2011, SLACK Incorporated.

Simultaneous determination of creatinine, creatine, and UV-absorbing amino acids using dual-mode gradient low-capacity cation-exchange chromatography.

PubMed

Yokoyama, Yukio; Tsuji, Sachiyo; Sato, Hisakuni

2005-08-26

A simple and versatile cation-exchange chromatography technique for the simultaneous determination of urinary creatinine (Cre), creatine (Crn), methionine (Met), tyrosine (Tyr), phenylalanine (Phe), histidine (His), and tryptophan (Trp) was developed. A novel low-capacity cation-exchange column packed with a newly developed sulfoacylated hypercross-linked macroreticular polystyrene-divinylbenzene resin, referred to as TMR-A/75 (capacity: 75 microequiv/column), was successfully used with a binary dual-mode gradient eluting system. Two solvents, (A) 25 mM phosphoric acid-methanol (30:70, v/v) and (B) 25 mM disodium hydrogenphosphate-methanol (30:70, v/v) were pumped through the column by programming solvent delivery ratios as 0 to 5 min: A-B (55:45, pH 3.6); 5-21 min: A-B (49:51, pH 5.3); and 21-35 min: A-B (55:45, pH 3.6). The flow rate was simultaneously time-programmed to be 0.6 mL/min from 0 to 19 min and to be 1.0 mL/min from 19 to 35 min. This eluting system could permit the use of the UV detection at 210 nm. The analytes, Crn, Met, Tyr, His, Cre, Phe, and Trp, were well separated in this order in 27 min with minimum resolution of approximately 2, and the cycle time was about 35 min. Retention time of each analyte was very reproducible with relative standard deviations (RSDs) between 0.05 and 0.38% (n = 5). The peak area responses were also reproducible with RSDs between 0.74 and 2.24% (n = 5). Calibration lines based on area data were linear from 1 to 1000 microM with r2 values of 0.9998 (Crn), 0.9998 (Met), 0.9999 (Tyr), 0.9999 (His), 1.0000 (Cre), 1.0000 (Phe), and 0.9999 (Trp). The method was applicable to the screening and/or chemical diagnosis of inherited metabolic disorders such as phenylketonuria (PKU), tyrosinemia, and Lowe syndrome. The creatinine ratios of diagnostic markers (microM/microM Cre) were easily determined. The Phe/Cre ratios for five urines from patients with PKU ranged from 0.162 to 0.521, and the Tyr/Cre ratio for tyrosinemia was 0.147. The ratios of Tyr/Cre, Phe/Cre, and Trp/Cre for Lowe syndrome were 0.497, 0.321, and 0.495, respectively. In contrast, the creatinine ratios for healthy newborns showed one digit lower than those for patients did. The developed method is very practical and can provide useful information and results for the clinical or biomedical researches with low analytical run costs.

[High-performance liquid-liquid chromatography in beverage analysis].

PubMed

Bricout, J; Koziet, Y; de Carpentrie, B

1978-01-01

Liquid liquid chromatography was performed with columns packed with stationary phases chemically bonded to silica microparticules. These columns show a high efficiency and are used very easily. Flavouring compounds like aromatic aldehydes which have a low volatility were analyzed in brandy using a polar phase alkylnitrile. Sapid substances like amarogentin in Gentiana lutea or glyryrrhizin in Glycyrrhiza glabra were determined by reversed phase chromatography. Finally ionizable substances like synthetic dyes can be analyzed by paired ion chromatography witha non polar stationary phase.

A Feasibility Study for the Laboratory Reduction of Low Level Radioactive Wastes

DTIC Science & Technology

1988-04-01

the Los Alamos National Laboratory), pass the off-gases through a quench column, venturi scrubber , packed column. cordenser, de-mi ste-, re-heater...treatment of the off-gas. In addition to HEPA filters, all of the fully developed systems used sore type of scrubber in the exhaust system to remove...considerations shown in the table and the desired use of a muffle furnace with just a HEPA filter for the off-gas (no scrubbers ), only the slow burn ashing

[Study on preparation of composite nano-scale Fe3O4 for phosphorus control].

PubMed

Li, Lei; Pan, Gang; Chen, Hao

2010-03-01

Composite nano-scale Fe3O4 particles were prepared in sodium carboxymethyl cellulose (CMC) solution by the oxidation deposition method. The adsorptions of phosphorus by micro-scale Fe3O4 and composite nano-scale Fe3O4 were investigated in water and soil, and the role of cellulase in the adsorption of composite nano-scale Fe3O4 was studied. Kinetic tests indicated that the equilibrium adsorption capacity of phosphorous on the composite nano-scale Fe3O4 (2.1 mg/g) was less than that of micro-scale Fe3O4 (3.2 mg/g). When cellulase was added to the solution of composite nano-scale Fe3O4 to degrade CMC, the removal rate of P by the nanoparticles (86%) was enhanced to the same level as the microparticles (90%). In the column tests, when the composite nano-scale Fe3O4 suspension was introduced in the downflow mode through the soil column, 72% of Fe3O4 penetrated through the soil bed under gravity. In contrast, the micro-scale Fe3O4 failed to pass through the soil column. The retention rate of P was 45% in the soil column when treated by the CMC-stabilized nanoparticles, in comparison with only 30% for the untreated soil column, however it could be improved to 74% in the soil column when treated by both the CMC-stabilized nanoparticles and cellulase, which degraded CMC after the nanoparticles were delivered into the soil.

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

The Paraprofessional's Handbook for Effective Support in Inclusive Classrooms

ERIC Educational Resources Information Center

Causton-Theoharis, Julie

2009-01-01

"What does a great paraprofessional need to know and do?" Find out in this survival guide, equally useful for the brand-new paraprofessional or the 20-year classroom veteran. Packed with friendly guidance, practical tips, and relatable first-person stories, this book reveals the best ways to provide effective, respectful services to students in…

7 CFR 29.3046 - Oriented.

Code of Federal Regulations, 2010 CFR

2010-01-01

... Oriented. A term applied to Type 31 untied tobacco which denotes the arrangement of leaves in a straight and orderly manner. Oriented includes: (a) Any lot of baled tobacco in which the leaves are packed parallel to the length of the bale with the butts to the outside and the tips of the leaves overlapping...

7 CFR 29.3046 - Oriented.

Code of Federal Regulations, 2011 CFR

2011-01-01

... Oriented. A term applied to Type 31 untied tobacco which denotes the arrangement of leaves in a straight and orderly manner. Oriented includes: (a) Any lot of baled tobacco in which the leaves are packed parallel to the length of the bale with the butts to the outside and the tips of the leaves overlapping...

7 CFR 29.3046 - Oriented.

Code of Federal Regulations, 2014 CFR

2014-01-01

... Oriented. A term applied to Type 31 untied tobacco which denotes the arrangement of leaves in a straight and orderly manner. Oriented includes: (a) Any lot of baled tobacco in which the leaves are packed parallel to the length of the bale with the butts to the outside and the tips of the leaves overlapping...

7 CFR 29.3046 - Oriented.

Code of Federal Regulations, 2012 CFR

2012-01-01

... Oriented. A term applied to Type 31 untied tobacco which denotes the arrangement of leaves in a straight and orderly manner. Oriented includes: (a) Any lot of baled tobacco in which the leaves are packed parallel to the length of the bale with the butts to the outside and the tips of the leaves overlapping...

7 CFR 29.3046 - Oriented.

Code of Federal Regulations, 2013 CFR

2013-01-01

... Oriented. A term applied to Type 31 untied tobacco which denotes the arrangement of leaves in a straight and orderly manner. Oriented includes: (a) Any lot of baled tobacco in which the leaves are packed parallel to the length of the bale with the butts to the outside and the tips of the leaves overlapping...

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

PubMed Central

Preti, Raffaella

2016-01-01

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

Micro-Columnated Loop Heat Pipe: The Future of Electronic Substrates

NASA Astrophysics Data System (ADS)

Dhillon, Navdeep Singh

The modern world is run by semiconductor-based electronic systems. Due to continuous improvements in semiconductor device fabrication, there is a clear trend in the market towards the development of electronic devices and components that not only deliver enhanced computing power, but are also more compact. Thermal management has emerged as the primary challenge in this scenario where heat flux dissipation of electronic chips is increasing exponentially, but conventional cooling solutions such as conduction and convection are no longer feasible. To keep device junction temperatures within the safe operating limit, there is an urgent requirement for ultra-high-conductivity thermal substrates that not only absorb and transport large heat fluxes, but can also provide localized cooling to thermal hotspots. This dissertation describes the design, modeling, and fabrication of a phase change-based, planar, ultra-thin, passive thermal transport system that is inspired by the concept of loop heat pipes and capillary pumped loops. Fabricated on silicon and Pyrex wafers using microfabrication techniques, the micro-columnated loop heat pipe (muCLHP) can be integrated directly with densely packed or multiply-stacked electronic substrates, to provide localized high-heat-flux thermal management. The muCLHP employs a dual-scale coherent porous silicon(CPS)-based micro-columnated wicking structure, where the primary CPS wick provides large capillary forces for fluid transport, while a secondary surface-wick maximizes the rate of thin-film evaporation. To overcome the wick thickness limitation encountered in conventional loop heat pipes, strategies based on MEMS surface micromachining techniques were developed to reduce parasitic heat flow from the evaporator to the compensation chamber of the device. Finite element analysis was used to confirm this reduction in a planar evaporator design, thus enabling the generation of a large motive temperature head for continuous device operation. To predict the overall heat carrying capacity of the muCLHP in the capillary pumping limit, an analytical model was developed to account for a steady state pressure balance in the device flow loop. Based on this model, a design optimization study, employing monotonicity analysis and numerical optimization techniques, was undertaken. It was found that an optimized muCLHP device can absorb heat fluxes as large as 1293 W/cm2 when water is used as a working fluid. A finite volume method-based numerical model was also developed to compute the rates of thin-film evaporation from the patterned surface of the secondary wick. The numerical results indicated that, by properly optimizing the dual-scale wick topology, allowable evaporative heat fluxes can be made commensurate with the heat flux performance predicted by the capillary pumping limit. The latter part of the dissertation deals with the fabrication, packaging, and experimental testing of several in-plane-wicking micro loop heat pipe (muLHP) prototypes. These devices were fabricated on silicon and Pyrex substrates and closely resemble the muCLHP design philosophy, with the exception that the CPS wick is substituted with an easier to fabricate in-plane wick. A novel thermal-flux method was developed for the degassing and fluid charging of the muLHP prototypes. Experiments were conducted to study the process of evaporation and dynamics of the liquid and vapor phases in the device flow loop. Using these results, the overall device and individual component topologies critical to the operation of the two-phase flow loop were identified. A continuous two-phase device flow loop was demonstrated for applied evaporator heat fluxes as high as 41 W/cm2. The performance of these devices, currently found to be limited by the motive temperature head requirement, can be significantly improved by implementing the parasitic heat flow-reduction strategies developed in this work. The 3-D thin-film evaporation model, when integrated into the overall device modeling framework, will enable a design optimization of the micro-columnated wick for further device performance enhancements.

Method of filling a microchannel separation column

DOEpatents

Arnold, Don W.

2002-01-01

A method for packing a stationary phase into a small diameter fluid passageway or flow channel. Capillary action is employed to distribute a stationary phase uniformly along both the length and diameter of the flow channel. The method disclosed here: 1) eliminates the need for high pressure pumps and fittings and the safety hazards associated therewith; 2) allows the use of readily available commercial microparticles, either coated or uncoated, as the stationary phase; 3) provides for different types of particles, different particle sizes, and different particle size distributions to be packed in sequence, or simultaneously; 4) eliminates the need for plugging the flow channel prior to adding the stationary phase to retain the packing particles; and 5) many capillaries can be filled simultaneously.

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

PubMed

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

2017-01-06

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

Enamel: From brittle to ductile like tribological response.

PubMed

Guidoni, G; Swain, M; Jäger, I

2008-10-01

To identify the intrinsic nano-scale wear mechanisms of enamel by comparing it with that of highly brittle glass, and highly ductile copper and silver monocrystals. A sharp cube corner indenter tip (20-50 nm radius) was used to abrade glass, enamel as well as copper and silver monocrystals. Square abraded areas (5 microm x 5 microm, 10 microm x 10 microm) were generated with loads of 50 microN for enamel and 100 microN for the remaining materials (2D abrasion). The normal load and displacement data were utilized in a complementary manner to support the comparison. In addition normal and lateral forces were simultaneously measured along 10 microm single scratched lines (1D abrasion). Scanning electron microscopy (SEM) and atomic force microscopy (AFM) were also used to characterise the worn areas and debris. The sharp tip cuts into and ploughs the specimens creating a wedge or ridge of material ahead of itself which eventually detaches, for the ductile materials and at high loads in enamel. For glass and enamel at low loads, the indenter tip ploughs into the material and the removed material is redistributed and pressed back into the abraded area. The wear behaviour of enamel at the nano-level resembles that obtained with glass at low loads (50 microN) and that obtained with metal mono-crystals at high load (100 microN). The role of the microstructural heterogeneity in the wear behaviour of enamel is considered in the discussion. The relevance to clinical wear of enamel is also considered.

MicroPPT-Based Secondary/Backup ACS for a 160-m, 450-kg Solar Sail Spacecraft

NASA Technical Reports Server (NTRS)

Wie, Bong; Murphy, David

2005-01-01

Solar sail tip-mounted, lightweight pulsed plasma thrusters (PPTs) are proposed for a secondary (or backup) attitude control system (ACS) of a 160-m, 450-kg solar sail spacecraft of the Solar Polar Imager (SPI) mission. A propellantless primary ACS of the SPI sailcraft employs trim control masses running along mast lanyards for pitch/yaw control together with roll stabilizer bars at the mast tips for quadrant tilt (roll) control. The robustness of such a propellantless primary ACS would be further enhanced by a secondary ACS utilizing tip-mounted, lightweight PPTs. The microPPT-based ACS is intended mainly for attitude recovery maneuvers from various off-nominal conditions that cannot be reliably handled by the propellantless primary ACS. However, it can also be employed for: i) the checkout or standby mode prior to and during sail deployment, ii) the post-deployment transition mode (prior to the propellantless primary ACS mode operation), iii) the solar sailing cruise mode of a trimmed sailcraft, and iv) the spin-stabilized, sun-pointing, safe mode. Although a conventional bus ACS is required for the SPI mission as the sail is jettisoned at the start of its science mission phase, the microPPT-based ACS option promises greater redundancy and robustness for the SPI mission. For other sailing missions, where the sail is never jettisoned, this secondary ACS provides a lower-cost, lower-mass propulsion for deployment control and greater redundancy than any traditional reaction-jet control system. This paper presents an overview nf the state--of-the--art microPPT technology, the design requirements of microPPTs for solar sail attitude control, and the preliminary ACS design and simulation results.

Instrumentation: Ion Chromatography.

ERIC Educational Resources Information Center

Fritz, James S.

1987-01-01

Discusses the importance of ion chromatography in separating and measuring anions. The principles of ion exchange are presented, along with some applications of ion chromatography in industry. Ion chromatography systems are described, as well as ion pair and ion exclusion chromatography, column packings, detectors, and programming. (TW)

Specific yield - laboratory experiments showing the effect of time on column drainage

USGS Publications Warehouse

Prill, Robert C.; Johnson, A.I.; Morris, Donald Arthur

1965-01-01

The increasing use of ground water from many major aquifers in the United States has required a more thorough understanding of gravity drainage, or specific yield. This report describes one phase of specific yield research by the U.S. Geological Survey's Hydrologic Laboratory in cooperation with the California Department of Water Resources. An earlier phase of the research concentrated on the final distribution of moisture retained after drainage of saturated columns of porous media. This report presents the phase that concentrated on the distribution of moisture retained in similar columns after drainage for various periods of time. Five columns, about 4 cm in diameter by 170 cm long, were packed with homogenous sand of very fine, medium, and coarse sizes, and one column was packed with alternating layers of coarse and medium sand. The very fine materials were more uniform in size range than were the medium materials. As the saturated columns drained, tensiometers installed throughout the length recorded changes in moisture tension. The relation of tension to moisture content, determined for each of the materials, was then used to convert the tension readings to moisture content. Data were then available on the distribution of retained moisture for different periods of drainage from 1 to 148 hours. Data also are presented on the final distribution of moisture content by weight and volume and on the degree of saturation. The final zone of capillary saturation was approximately 12 cm for coarse sand, 13 cm for medium sand, and 52 cm for very fine sand. The data showed these zones were 92 to 100 percent saturated. Most of the outflow from the columns occurred in the earlier hours of drainage--90 percent in 1 hour for the coarse materials, 50 percent for the medium, and 60 percent for the very fine. Although the largest percentage of the specific yield was reached during the early hours of .drainage, this study amply demonstrates that a very long time would be required to reach drainage equilibrium. In the layered columns the middle (medium sand) layer functioned as a hanging water column accelerating the drainage of the overlying coarse-sand layer. After the middle layer started to drain, the moisture distribution as retained in all three layers showed trends similar to that obtained when the same materials were tested in homogenous columns.

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

PubMed

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

2016-10-15

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

Stability and Structure of Star-Shape Granules

NASA Astrophysics Data System (ADS)

Zhao, Yuchen; Bares, Jonathan; Zheng, Matthew; Dierichs, Karola; Menges, Achim; Behringer, Robert

2015-11-01

Columns are made of convex non-cohesive grains like sand collapse after being released from initial positions. On the other hand, various architectures built by concave grains can maintain stability. We explore why these structures are stable, and how stable they can be. We performed experiments by randomly pouring identical star-shape particles into hollow cylinders left on glass and a rough base, and observed stable granular columns after lifting the cylinders. Particles have six 9 mm arms, which extend symmetrically in the xyz directions. Both the probability of creating a stable column and mechanical stability aspects have been investigated. We define r as the weight fraction of particles that fall out of the column after removing confinement. r gradually increases as the column height increases, or the column diameter decreases. We also explored different experiment conditions such as vibration of columns with confinement, or large basal friction. We also consider different stability measures such as the maximum inclination angle or maximum weight a column can support. In order to understand structure leading to stability, 3D CT scan reconstructions of columns have been done and coordination number and packing density will be discussed. We acknowledge supports from W.M.Keck Foundation and Research Triangle MRSEC.

Novel splice techniques and micro-hole collapse effect in photonic crystal fibers

NASA Astrophysics Data System (ADS)

Xiao, Limin

Photonic crystal fibers (PCFs) represent one of the most active research areas today in the field of fiber optics. Because of the freedom they offer in their design and novel wave-guiding properties, PCFs have resulted in a number of applications that are difficult to achieve with conventional fibers. In practical applications, low-loss connection PCFs with conventional fibers is a key issue for integrating PCF devices into existing fiber optic systems. However, connecting PCFs to conventional fibers without incurring too much loss is a very challenging problem. Two novel techniques were proposed to solve this problem in the thesis. One is fusion splicing technique; the other is micro-tip technique. First, fusion splicing technique for PCFs is investigated. For fusion splicing SMFs and PCFs having similar mode field diameters, a low-loss joint with good mechanical strength can be formed by choosing a suitably weak fusion current, short fusion time, offset and overlap to minimize the collapse of air holes and well melt two fibers together. For small-core PCFs, an optimum mode field match and an adiabatic mode field variation can be achieved by repeated arc discharges. Low-loss fusion splicing of five different PCFs with SMFs are achieved, including large mode PCF, hollow-core PCF, nonlinear PCFs with low and high air-filling fraction and polarization maintaining PCF. The other novel technique is using micro-tips. The method is based on growing photopolymer micro-tips directly on the end face of SMFs. The shape and the size of the tips can be controlled, by adjusting the laser power, the exposure time and the oxygen diffusion concentration for polymerization, to match its mode field to the small-core PCFs. Micro-hole collapse effect can be used to fabricate selective injection PCFs. The suitable arc discharge energy can cause the cladding holes to collapse while leaving the central hollow core to remain open. Thus a simple method for selective filling the central hole of PCFs is developed. Hybrid PCF guides light by a novel guiding mechanism, which is a combination of index-guiding and bandgap-guiding. The properties of the hybrid PCF are systematically investigated.

The aquatic hyphomycete Heliscus lugdunensis protects its hyphae tip cells from cadmium: A micro X-ray fluorescence and X-ray absorption near edge structure spectroscopy study

NASA Astrophysics Data System (ADS)

Isaure, Marie-Pierre; Leyh, Benjamin; Salomé, Murielle; Krauss, Gerd-Joachim; Schaumlöffel, Dirk; Dobritzsch, Dirk

2017-11-01

Aquatic fungi can be used to evaluate the functioning of natural ecosystems. Heliscus lugdunensis is an early colonizer of allochthone leafs. Since this aquatic hyphomycete is able to develop in metal contaminated habitats and tolerates cadmium, it appears to be a good candidate to investigate adaptation to metal pollution. This study aimed at examining the sequestration of Cd in the hyphae of H. lugdunensis, and particularly the role of the tip cells. For that, H. lugdunensis growth was evaluated under various Cd concentrations, and a combination of synchrotron micro X-ray fluorescence and X-ray absorption near edge structure spectroscopy was carried out to determine the compartments of Cd accumulation and the Cd chemical species, respectively. Results showed that the hyphal tip cells were depleted in Cd, and that the metal was stored in older cells. Cd was mainly associated with sulfur ligands and to a lesser extent bound to phosphates and carboxyl/hydroxyl groups from cell wall and/or organic acids. Finally, the aquatic fungus was able to maintain the tip cell as a functional system, thus allowing the colonization of contaminated environments.

Surface-adaptable all-metal micro-four-point probe with unique configuration

NASA Astrophysics Data System (ADS)

Kim, J. K.; Choi, Y. S.; Lee, D. W.

2015-07-01

In this paper, we propose a surface-adaptable all-metal micro-four-point probe (μ4PP) with a unique configuration. The μ4PP consists of four independent metallic sub-cantilevers with sharp Cu tips, and an SU-8 body structure to support the sub-cantilevers. The tip height is approximately 15 μm, and the tips are fabricated by anisotropic wet-etching of silicon followed by Cu electroplating. Each metallic cantilever connected to the SU-8 body structure acts as a flexible spring, so that the conducting tip can make gentle, non-destructive contact with fragile surfaces. To enhance the adhesion between the metallic sub-cantilevers and the SU-8 body, mushroom-shaped Cu structures were fabricated using an under-baked and under-exposed photolithography process. Various μ4PPs were designed and fabricated to verify their diverse range of applications, and preliminary experiments were performed using these fabricated μ4PPs. The resultant flexibility and reliability were experimentally confirmed on several samples, such as a polymer cantilever, a graphene flake, and curved metallic surfaces. We also expect that the proposed μ4PP will be suitable for measuring the anisotropic characteristics of crystal materials or the Hall effect in semiconductors.

Interaction between a laminar starting immersed micro-jet and a parallel wall

NASA Astrophysics Data System (ADS)

Cabaleiro, Juan Martin; Laborde, Cecilia; Artana, Guillermo

2015-01-01

In the present work, we study the starting transient of an immersed micro-jet in close vicinity to a solid wall parallel to its axis. The experiments concern laminar jets (Re < 200) issuing from a 100 μm internal tip diameter glass micro-pipette. The effect of the confinement was studied placing the micro-pipette at different distances from the wall. The characterization of the jet was carried out by visualizations on which the morphology of the vortex head and trajectories was analyzed. Numerical simulations were used as a complementary tool for the analysis. The jet remains stable for very long distances away from the tip allowing for a similarity analysis. The self-similar behavior of the starting jet has been studied in terms of the frontline position with time. A symmetric and a wall dominated regime could be identified. The starting jet in the wall type regime, and in the symmetric regime as well, develops a self-similar behavior that has a relative rapid loss of memory of the preceding condition of the flow. Scaling for both regimes are those that correspond to viscous dominated flows.

Structure optimization of a micro drill bit with nonlinear constraints considering the effects of eccentricity, gyroscopic moments, lateral and torsional vibrations

NASA Astrophysics Data System (ADS)

Nguyen, Danh-Tuyen; Hoang, Tien-Dat; Lee, An-Chen

2017-10-01

A micro drill structure was optimized to give minimum lateral displacement at its drill tip, which plays an extremely important role on the quality of drilled holes. A drilling system includes a spindle, chuck and micro drill bit, which are modeled as rotating Timoshenko beam elements considering axial drilling force, torque, gyroscopic moments, eccentricity and bearing reaction force. Based on our previous work, the lateral vibration at the drill tip is evaluated. It is treated as an objective function in the optimization problem. Design variables are diameter and lengths of cylindrical and conical parts of the micro drill, along with nonlinear constraints on its mass and mass center location. Results showed that the lateral vibration was reduced by 15.83 % at a cutting speed of 70000 rpm as compared to that for a commercial UNION drill. Among the design variables, we found that the length of the conical part connecting to the drill shank plays the most important factor on the lateral vibration during cutting process.

Optical fiber micro-displacement sensor using a refractive index modulation window-assisted reflection fiber taper

NASA Astrophysics Data System (ADS)

Bao, Weijia; Qiao, Xueguang; Yin, Xunli; Rong, Qiangzhou; Wang, Ruohui; Yang, Hangzhou

2017-12-01

We demonstrate a compact fiber-optic quasi-Michelson interferometer (QMI) for micro-displacement measurement. The sensor comprises a micro-structure of a reflection taper tip containing a refractive index modification (RIM) as a coupling window over the interface between core and cladding of the fiber. Femtosecond laser-based direct inscription technique is used to achieve this window inscription and to induce large refractive index change. The RIM acts as a window for the strong coupling and recoupling of core-to-cladding modes. As the core and cladding modes are reflected at the taper tip and coupled back to lead-in fiber, a well-defined interference spectrum is achieved. The spectral intensity exhibits a high micro-bending sensitivity of 4 . 94 dB / μm because of the sensitivity to bending of recoupled intensity of cladding modes. In contrast, the spectral wavelength is insensitive to bending but linearly responds to temperature. The simultaneous measurements, including power-referenced for displacement and wavelength-referenced for temperature, were achieved by selective interference dip monitoring.

Dynamic analysis on cavitation and embolization in vascular plants under tension

NASA Astrophysics Data System (ADS)

Ryu, Jeongeun; Hwang, Bae Geun; Kim, Yangmin; Lee, Sang Joon

2014-11-01

Plants can transport sap water from the soil to the tip of their leaves using the tensile forces created by leaf transpiration without any mechanical pumps. However, the high tension adversely induces a thermodynamically metastable state in sap water with negative pressure and gas bubbles are prone to be formed in xylem vessels. Cavitation easily breaks down continuous water columns and grows into embolization, which limits water transport through xylem vessels. Meanwhile, the repair process of embolization is closely related to water management and regulation of sap flow in plants. In this study, the cavitation and embolization phenomena of liquid water in vascular plants and a physical model system are experimentally and theoretically investigated in detail under in vivo and in vitro conditions. This study will not only shed light on the understanding of these multiphase flows under tension but also provide a clue to solve cavitation problems in micro-scale conduits and microfluidic network systems. This work was supported by the National Research Foundation of Korea (NRF) grant funded by the Korea government (MSIP) (No. 2008-0061991).

Ion Chromatography-on-a-chip for Water Quality Analysis

NASA Technical Reports Server (NTRS)

Kidd, R. D.; Noell, A.; Kazarians, G.; Aubrey, A. D.; Scianmarello, N.; Tai, Y.-C.

2015-01-01

We report progress towards developing a Micro-Electro-Mechanical Systems (MEMS)- based ion chromatograph (IC) for crewed spacecraft water analysis. This IC-chip is an offshoot of a NASA-funded effort to produce a high performance liquid chromatograph (HPLC)-chip. This HPLC-chip system would require a desalting (i.e. ion chromatography) step. The complete HPLC instrument consists of the Jet Propulsion Labortory's (JPL's) quadrupole ion trap mass spectrometer integrated with a state-of-the-art MEMS liquid chromatograph (LC) system developed by the California Institute of Technology's (Caltech's) Micromachining Laboratory. The IC version of the chip consist of an electrolysis-based injector, a separation column, two electrolysis pumps for gradient generation, mixer, and a built-in conductivity detector. The HPLC version of the chip also includes a nanospray tip. The low instrument mass, coupled with its high analytical capabilities, makes the LC chip ideally suitable for wide range of applications such as trace contaminant, inorganic analytical science and, when coupled to a mass spectrometer, a macromolecular detection system for either crewed space exploration vehicles or robotic planetary missions.

Sequential injection-bead injection-lab-on-valve coupled to high-performance liquid chromatography for online renewable micro-solid-phase extraction of carbamate residues in food and environmental samples.

PubMed

Vichapong, Jitlada; Burakham, Rodjana; Srijaranai, Supalax; Grudpan, Kate

2011-07-01

A sequential injection-bead injection-lab-on-valve system was hyphenated to HPLC for online renewable micro-solid-phase extraction of carbamate insecticides. The carbamates studied were isoprocarb, methomyl, carbaryl, carbofuran, methiocarb, promecarb, and propoxur. LiChroprep(®) RP-18 beads (25-40 μm) were employed as renewable sorbent packing in a microcolumn situated inside the LOV platform mounted above the multiposition valve of the sequential injection system. The analytes sorbed by the microcolumn were eluted using 80% acetonitrile in 0.1% acetic acid before online introduction to the HPLC system. Separation was performed on an Atlantis C-18 column (4.6 × 150 mm, 5 μm) utilizing gradient elution with a flow rate of 1.0 mL/min and a detection wavelength at 270 nm. The sequential injection system offers the means of performing automated handling of sample preconcentration and matrix removal. The enrichment factors ranged between 20 and 125, leading to limits of detection (LODs) in the range of 1-20 μg/L. Good reproducibility was obtained with relative standard deviations of <0.7 and 5.4% for retention time and peak area, respectively. The developed method has been successfully applied to the determination of carbamate residues in fruit, vegetable, and water samples. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Hyphenation of ultra performance liquid chromatography (UPLC) with inductively coupled plasma mass spectrometry (ICP-MS) for fast analysis of bromine containing preservatives.

PubMed

Bendahl, Lars; Hansen, Steen Honoré; Gammelgaard, Bente; Sturup, Stefan; Nielsen, Camilla

2006-02-24

Ultra performance liquid chromatography (UPLC) was coupled to inductively coupled plasma mass spectrometry (ICP-MS) for fast analysis of three bromine-containing preservatives, monitoring the 79Br and 81Br isotopes simultaneously. Due to the efficiency of the 1.7 microm column packing material, the resolution of the test substances was only slightly affected when the linear flow velocity was increased from 0.5 to 1.9 mm s(-1). However, the sensitivity of ICP-MS detection decreased when the linear flow velocity was increased from 0.5 to 1.9 mm s(-1). Analytical figures of merit were determined at an intermediate and at a high linear velocity. The precision was better than 2.2% R.S.D. and regression analysis showed that a linear response was achieved at both flow rates (R2 > 0.9993, n = 36). The analysis time was less than 4.5 min at a flow rate of 50 microL min(-1) and limits of detection and quantification were better than 3.3 and 11 microg BrL(-1), respectively. The analysis time was reduced to 2.7 min when the flow rate was increased to 90 microL min(-1) and limits of detection and quantification were better than 20 and 65 microg BrL(-1), respectively. The method was applied for quantitative analysis of bromine-containing preservatives in commercially available cosmetic products.

Numerical investigation on the self-induced unsteadiness in tip leakage flow of a micro-axial fan rotor

NASA Astrophysics Data System (ADS)

Chen, Jinxin; Lai, Huanxin

2015-06-01

The self-induced unsteadiness in tip leakage flow (TLF) of a micro-axial fan rotor is numerically studied by solvingReynolds-averaged Navier-Stokes equations. The micro-axial fan, which is widely used in cooling systems of electronic devices, has a tip clearance of 6% of the axial chord length of the blade. At the design rotation speed, four cases near the peak efficiency point (PEP) with self-induced unsteadiness and four steady cases which have much weaker pressure fluctuations are investigated Using the "interface" separating the incoming main flow and the TLF defined by Du et al. [1], an explanation based on the propagation of the low energy spot and its multi-passing through the high gradient zone of the relativetotal pressure, is proposed to clarify the originating mechanism of the unsteadiness. At the operating points near the PEP, the main flow is weaker than the TLF and the interface moves upstream. The low energy spot which propagates along in the close behind of the interface has opportunity to circulate in the circumferential direction and passes through the sensitive interfaces several times, a slight perturbation therefore may be magnified significantlyand develops into the self-induced unsteadiness. The explanation is demonstrated by numerical results

Transport of sulfacetamide and levofloxacin in granular porous media under various conditions: Experimental observations and model simulations.

PubMed

Dong, Shunan; Gao, Bin; Sun, Yuanyuan; Shi, Xiaoqing; Xu, Hongxia; Wu, Jianfeng; Wu, Jichun

2016-12-15

Understanding the fate and transport of antibiotics in porous media can help reduce their contamination risks to soil and groundwater systems. In this work, batch and column experiments were conducted to determine the interactions between two representative antibiotics, sulfacetamide (SA) and levofloxacin (LEV), and sand porous media under various solution pH, humic acid (HA) concentration, grain size, and moisture content conditions. Batch sorption experimental results indicated that the sand had relatively strong bonding affinity to LEV, but little sorption of SA under different pH, HA concentration, grain size conditions. Results from the packed sand column experiments showed that SA had extremely high mobility in the porous media for all combinations of pH, HA concentration, grain size, and moisture content. The mass recovery of SA was higher than 98.5% in all the columns with the exception of the one packed with fine sand (97.2%). The retention of LEV in the columns was much higher and the recovery rates ranged from 0% to 71.1%. Decreases in solution pH, HA concentration, grain size, or moisture content reduced the mobility of LEV in the columns under the tested conditions. These results indicated that type of antibiotics and environmental conditions also played an important role in controlling their fate and transport in porous media. Mathematical models were applied to simulate and interpret experimental data, and model simulations described the interactions between the two antibiotics and sand porous media very well. Findings from this study elucidated the key factors and processes controlling the fate of SA and LEV in porous media, which can inform the prediction and assessment of the environmental risks of antibiotics. Copyright © 2016 Elsevier B.V. All rights reserved.

Stage-frit: A straightforward sub-2 μm nano-liquid chromatography column fabrication for proteomic analysis.

PubMed

Hsieh, Ming-Yueh; Hsiao, He-Hsuan

2015-07-30

In this work we demonstrated a facile method for the fabrication of C18 coordination polymer gel in a capillary, called stage-frit, which was efficiently applied to pack sub-2 μm C18 beads into the capillary by a high pressure bomb for the online separation of proteolytic peptides. The back pressure of the column with 10 cm × 75 μm i.d. is regularly lower than 170 bar at a flow rate of 300 nl/min, which could be operated on a common nanoLC system instead of nanoUPLC system due to the good permeability, low back pressure and high mechanical stress of the frit that will totally reduce the cost for the purchase of instrument. The stage-frit allows long-term continuous flow of the solvent and no significant beads loss or pressure instability was observed during the period. The repeatability of retention time for fifteen BSA tryptic peaks was found to be less than 1.08% (RSD) in six time nanoLC-ESI-MS/MS experiments. The average full width at half maximum (FWHM) of peptide peaks is 5.87 s. The sub-2 μm stage-frit nanoLC column showed better sensitivity than the commercial available for large scale proteomic analysis of total tissue proteins from human spleen. The number of identified peptides is approximately 0.4-fold and 0.2-fold higher than that obtained by utilizing commercial columns packed with 3 μm and 1.8 μm C18 materials, respectively. In the field of analytical chemistry, particularly the use of nanoLC systems, stage-frit nanoLC column offers a great potential for the separation of complex mixtures. Copyright © 2015 Elsevier B.V. All rights reserved.

Opening the black box: imaging nanoparticle transport with MRI

NASA Astrophysics Data System (ADS)

Phoenix, V.; Holmes, W. M.

2009-12-01

While most renown for its use in medicine, magnetic resonance imaging (MRI) has tremendous potential in the study of environmental processes. Its ability to non-invasively image inside materials that are opaque to other imaging methods (in particular light based techniques) is a particular strength. MRI has already been used, for example, to study fluid flow in rocks and image mass transport and biogeochemical processes in biofilms [1-4]. Here, we report of the use of MRI to image nanoparticle transport through porous geologic media (in this case packed gravel columns). Packed column experiments are key to understanding nanoparticulate transport in porous geologic media. Whilst highly informative, the data obtained can be a bulk average of a complex and heterogeneous array of interactions within the column. Natural environmental systems are often complex, displaying heterogeneity in geometry, hydrodynamics, geochemistry and microbiology throughout. MRI enables us to quantify better how this heterogeneity may influence nanoparticle transport and fate by enabling us to look inside the column and image the movement of nanoparticles within. To make the nanoparticle readily visible to MRI, it is labelled with a paramagnetic tag (commonly gadolinium). Indeed, a wide variety of off-the-shelf paramagnetically tagged nanoparticles and macromolecules are available, each with different properties enabling us to explore the impact of particle charge, size etc on their transport behaviour. In this preliminary study, packed columns of quartz or marble based gravels (approx 5 mm diameter) were first imaged to check their suitability for MR imaging. This was done as geologic material can contain sufficiently high concentrations of ferro- and paramagnetic ions to induce unwanted artefacts in the MR image. All gravels imaged (Rose quartz, Creswick quartz gravel and Ben Deulin white marble) produced minimal or no artefacts. A solution of the nanoparticle GadoCELLTrack (BioPAL), was prepared and connected to a 30 mm diameter flow cell containing rose quartz. GadoCELLTrack is a 30 nm diameter, neutrally charged gadolinium colloid. MR images were collected as the nanoparticle solution was pumped through the flow cell. These images were calibrated to provide fully quantitative maps of nanoparticle concentration at regular time intervals throughout the column. Such data can be used to help develop predictive models of nanoparticulate transport. [1] Holmes WM, Packer KJ (2003) Magnetic Resonance Imaging 21,389-391 [2] Seymour JD et al., (2004) Journal of Magnetic Resonance 167, 322-327 [3] McLean JS et al., (2008) ISME, 2, 121-131 [4] Phoenix et al., (2008) Applied and Environmental Microbiology, 74, 4934-4943

A non-resonant fiber scanner based on an electrothermally-actuated MEMS stage

PubMed Central

Zhang, Xiaoyang; Duan, Can; Liu, Lin; Li, Xingde; Xie, Huikai

2015-01-01

Scanning fiber tips provides the most convenient way for forward-viewing fiber-optic microendoscopy. In this paper, a distal fiber scanning method based on a large-displacement MEMS actuator is presented. A single-mode fiber is glued on the micro-platform of an electrothermal MEMS stage to realize large range non-resonantscanning. The micro-platform has a large piston scan range of up to 800 µm at only 6V. The tip deflection of the fiber can be further amplified by placing the MEMS stage at a proper location along the fiber. A quasi-static model of the fiber-MEMS assembly has been developed and validated experimentally. The frequency response has also been studied and measured. A fiber tip deflection of up to 1650 µm for the 45 mm-long movable fiber portion has been achieved when the MEMS electrothermal stage was placed 25 mm away from the free end. The electrothermally-actuated MEMS stage shows a great potential for forward viewing fiber scanning and optical applications. PMID:26347583

Elimination of PPV and PNRSV through thermotherapy and meristem-tip culture in nectarine.

PubMed

Manganaris, G A; Economou, A S; Boubourakas, I N; Katis, N I

2003-10-01

The plum pox virus (PPV) and prunus necrotic ringspot virus (PNRSV) cause serious disease problems in stone-fruit trees. In this work, the possibility of obtaining plant material free from these viruses through thermotherapy and meristem-tip culture from infected nectarine shoots (Prunus persica var. nectarina Max, cv. 'Arm King') was studied. In addition, the detection of these viruses in in vitro cultures and young acclimatized plantlets with double antibody sandwich-enzyme-linked immunosorbent assay (DAS-ELISA) and multiplex reverse transcriptase-polymerase chain reaction (RT-PCR) was studied. Meristem-tip explants (0.8-1.3 mm) derived from sprouted buds of winter wood and spring shoots from field grown plants had a 2-5% regeneration response. However, application of thermotherapy to potted nectarine trees (3 weeks at a maximum temperature of 35 degrees C) facilitated excision of longer meristem tips (1.3-2.0 mm) that resulted in a significantly higher regeneration response (38%) in woody plant medium (WPM) without plant growth regulators. Such explants formed multiple shoots with the addition of 8 microM benzylaminopurine and 0.8 microM indoleacetic acid. When they were tested for the presence of PPV and PNRSV, 86% and 81% were found to be virus-free as detected by DAS-ELISA and multiplex RT-PCR, respectively. Individual shoots excised from virus-free cultures readily rooted in vitro (half-strength WPM plus 2 microM indolebutyric acid) and grew to plantlets. The combination of an efficient protocol for virus elimination and the establishment of highly sensitive diagnostics resulted in the production of nectarine plants free from PPV and PNRSV.

Laser ablated hard coating for microtools

DOEpatents

McLean, II, William; Balooch, Mehdi; Siekhaus, Wigbert J.

1998-05-05

Wear-resistant coatings composed of laser ablated hard carbon films, are deposited by pulsed laser ablation using visible light, on instruments such as microscope tips and micro-surgical tools. Hard carbon, known as diamond-like carbon (DLC), films produced by pulsed laser ablation using visible light enhances the abrasion resistance, wear characteristics, and lifetimes of small tools or instruments, such as small, sharp silicon tips used in atomic probe microscopy without significantly affecting the sharpness or size of these devices. For example, a 10-20 nm layer of diamond-like carbon on a standard silicon atomic force microscope (AFM) tip, enables the useful operating life of the tip to be increased by at least twofold. Moreover, the low inherent friction coefficient of the DLC coating leads to higher resolution for AFM tips operating in the contact mode.

Synthesis and evaluation of sensitizer drug photorelease chemistry: Micro-optic method applied to singlet oxygen generation and drug delivery

NASA Astrophysics Data System (ADS)

Ghosh, Goutam

This thesis summarizes a new micro-optic method for singlet oxygen generation and sensitizer drug delivery, which include i) synthesis and evaluation of a first generation device for drug delivery from native and fluorinated silica probe tips, ii) synthesis of PEG conjugated sensitizers to study phototoxicity in ovarian cancer cells, and iii) synthesis and evaluation of tris-PEGylated chlorin conjugated fluorinated silica for its future integration into the device to use as a 2nd generation device. A first generation micro-optic device was developed that works by sparging O2 gas and light generating cytotoxic singlet oxygen that cleaves the covalently attached drug (sensitizer) from the probe tip at the distal end of the fiber. The aim is to develop a 1st and 2nd generation device for site specific delivery of photosensitizer and singlet oxygen to overcome the challenges involved in systemic administration of the sensitizer. Synthesis and evaluation of drug (pheophorbide-a) delivery applying micro-optic method from native and fluorinated silica probe tip was achieved. The amount of sensitizer photocleavage depends on the loading level of sensitizer onto the probe tips. We also found that photorelease efficiency depends on the nature of the solvents where sensitizer is photocleaved. For example, no photorelease was observed in an aqueous solvent where sensitizer remained adsorbed to the native silica probe-tip. But, 90% photocleavage was obtained in octanol. A significant amount of photosensitizer (formate ester of pyropheophorbide- a) diffused into the liposome when photocleavage study was carried out in liposome. Substantial increase of photorelease was observed in organic solvent when pyropheophorbide-a (PPa) sensitizer was attached to the partially fluorinated porous Vycor glass. We also explored sensitizer photorelease from the fluorinated silica surface at various temperatures and we found that autocatalytic photorelease happened at room temperature and above. No photorelease was observed at low temperature. Chlorin e6 and its one, two and three short chain methoxy triethylene glycol (PEG) conjugated derivatives were synthesized. A comparative study of photocytotoxicity and cellular uptake between each showed that 17 3,152,131- chlorin e6 methoxy triethylene glycol triester has the highest photocytotoxic activity and uptake by ovarian OVCAR-5 cancer cells. Therefore, we decided to load three short chain PEG conjugated chlorin e6 onto the silica surface through spacer alkene for delivery via a fiber-optic probe tip. In order to load chlorin e6-triPEG ester conjugate, in chapter 4, we explored different synthetic strategies. We have been successful in synthesizing spacer alkene succinate linker conjugated chlorin e6 -tri PEG ester, which was attached to the fiber-optic probe tip. Reactions were carried out in mild conditions to avoid detachment of the PEG ester from the carboxylic acid sites of chlorin. Photocleavage of the triPEG modified fluorinated probe tip system was studied in n-butanol.

Food Safety Tips for College Students

ERIC Educational Resources Information Center

US Department of Agriculture, 2005

2005-01-01

When students pack up for college, they take along the basics-- TV, laptop, MP3 player, and cell phone. Many students will arrive at school with a microwave oven, tabletop grill, mini fridge, and toaster oven in tow. Most students, however, don't know there are food safety considerations when cooking with these appliances. The USDA Meat and…

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

DOE PAGES

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

2014-09-06

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

Special Section on InterPACK 2017—Part 1

DOE PAGES

Mysore, Kaushik; Narumanchi, Sreekant; Dede, Ercan; ...

2018-03-02

InterPACK is a premier international forum for exchange of state-of-the-art knowledge in research, development, manufacturing, and applications of micro-electronics packaging. It is the flagship conference of the ASME Electronic and Photonic Packaging Division (EPPD) founded in 1992 as an ASME-JSME joint biannual conference. Rapid changes in the semiconductor landscape together with findings from InterPACK Pathfinding workshop (IPW) in 2016 led to a significant reset of InterPACK conference priorities and focus to comprehensively address needs of the InterPACK community. As a result, starting in 2017, InterPACK has become an annual conference and the scope of the conference has increased significantly togethermore » with a systems-focus to include some of the most cutting-edge topics in electronics packaging, device integration, and reliability. These topics are organized across five different tracks: (1) heterogeneous integration: microsystems with diverse functionality, (2) servers of the future, (3) structural and physical health monitoring, (4) energy conversion and storage, and (5) transportation: autonomous and electric vehicles.« less

Special Section on InterPACK 2017—Part 1

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

Mysore, Kaushik; Narumanchi, Sreekant; Dede, Ercan

InterPACK is a premier international forum for exchange of state-of-the-art knowledge in research, development, manufacturing, and applications of micro-electronics packaging. It is the flagship conference of the ASME Electronic and Photonic Packaging Division (EPPD) founded in 1992 as an ASME-JSME joint biannual conference. Rapid changes in the semiconductor landscape together with findings from InterPACK Pathfinding workshop (IPW) in 2016 led to a significant reset of InterPACK conference priorities and focus to comprehensively address needs of the InterPACK community. As a result, starting in 2017, InterPACK has become an annual conference and the scope of the conference has increased significantly togethermore » with a systems-focus to include some of the most cutting-edge topics in electronics packaging, device integration, and reliability. These topics are organized across five different tracks: (1) heterogeneous integration: microsystems with diverse functionality, (2) servers of the future, (3) structural and physical health monitoring, (4) energy conversion and storage, and (5) transportation: autonomous and electric vehicles.« less

Guest Editorial: Special Section on InterPACK 2017 - Part 2

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

Narumanchi, Sreekant V; Mysore, Kaushik; Dede, Ercan

InterPACK is a premier international forum for exchange of state-of-the-art knowledge in research, development, manufacturing, and applications of micro-electronics packaging. It is the flagship conference of the ASME Electronic and Photonic Packaging Division (EPPD) founded in 1992 as an ASME-JSME joint biannual conference. Rapid changes in the semiconductor landscape together with findings from InterPACK Pathfinding workshop (IPW) in 2016 led to a significant reset of InterPACK conference priorities and focus to comprehensively address needs of the InterPACK community. As a result, starting in 2017, InterPACK has become an annual conference and the scope of the conference has increased significantly togethermore » with a systems-focus to include some of the most cutting-edge topics in electronics packaging, device integration, and reliability. These topics are organized across five different tracks: (1) heterogeneous integration: microsystems with diverse functionality, (2) servers of the future, (3) structural and physical health monitoring, (4) energy conversion and storage, and (5) transportation: autonomous and electric vehicles.« less

GENERAL VIEW OF SHARP FREEZE ROOM ON LEVEL 2; LOOKING ...

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

GENERAL VIEW OF SHARP FREEZE ROOM ON LEVEL 2; LOOKING WEST; PIPES ON CEILING CARRIED COMPRESSED AMMONIA; NOTE NONBEARING GLAZED TILE WALLS BETWEEN COLUMNS; FLOORS ARE BRICK - Rath Packing Company, Cooler Building, Sycamore Street between Elm & Eighteenth Streets, Waterloo, Black Hawk County, IA

Optimization of denitrifying bioreactor performance with agricultural residue-based filter media

USDA-ARS?s Scientific Manuscript database

Denitrification bioreactors are a promising technology for mitigation of nitrate-nitrogen (NO3-N) losses in subsurface drainage water. Bioreactors are constructed with carbon substrates, typically wood chips, to provide a substrate for denitrifying microorganisms. Columns were packed with wood chips...

Composition and Antioxidant Activity of Water-Soluble Polysaccharides from Tuber indicum

PubMed Central

Luo, Qiang; Zhang, Jie; Yan, Liang; Tang, Yuanlin; Ding, Xiang; Yang, Zhirong

2011-01-01

Abstract Crude water-soluble Chinese truffle Tuber indicum polysaccharide (TIP) was extracted from the fruiting bodies with water and then successively purified by DEAE–cellulose 52 and Sephadex G-100 column chromatography, yielding two major polysaccharide fractions: TIP1-1 and TIP2-1. High-performance gel permeation chromatography analysis showed that the average molecular sizes of TIP1-1 and TIP2-1 were approximately 1.75×104 Da and 5.73×103 Da, respectively. Monosaccharide component analysis by gas chromatography indicated that TIP1-1 was composed of mannose, glucose, galactose, and rhamannose in the respective molar ratio of 3.93:1.24:0.75:1.26 and that TIP2-1 contained mannose, glucose, and arabinose in the respective molar ratio of 5.27:1.44:0.43. The antioxidant activity analyses revealed that TIP1-1 and TIP2-1 possessed considerable antioxidant activity. Compared with TIP1-1, which has a higher molecular weight and contains no uronic acid, TIP2-1 exhibited a protective effect on PC12 cells injured by H2O2 and a higher scavenging activity against free radicals. The relative effects of the lower molecular size, the presence of uronic acid, and the antioxidant activity of TIP2-1 appear to be significant. Accordingly, the Chinese truffle T. indicum might serve as an effective antioxidative healthcare food and source of natural antioxidants. PMID:21877953

Optimization of the microbial synthesis of dihydroxyacetone from glycerol with Gluconobacter oxydans.

PubMed

Hekmat, D; Bauer, R; Fricke, J

2003-12-01

An optimized repeated-fed-batch fermentation process for the synthesis of dihydroxyacetone (DHA) from glycerol utilizing Gluconobacter oxydans is presented. Cleaning, sterilization, and inoculation procedures could be reduced significantly compared to the conventional fed-batch process. A stringent requirement was that the product concentration was kept below a critical threshold level at all times in order to avoid irreversible product inhibition of the cells. On the basis of experimentally validated model calculations, a threshold value of about 60 kg x m(-3) DHA was obtained. The innovative bioreactor system consisted of a stirred tank reactor combined with a packed trickle-bed column. In the packed column, active cells could be retained by in situ immobilization on a hydrophilized Ralu-ring carrier material. Within 17 days, the productivity of the process could be increased by 75% to about 2.8 kg x m(-3) h(-1). However, it was observed that the maximum achievable productivity had not been reached yet.

An experimental investigation of the effect of walls on gas-liquid flows through fixed particle beds.

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

Cooper, Marcia A.; Cote, Raymond O.; Torczynski, John Robert

The effect of particle diameter on downward co-current gas-liquid flow through a fixed bed of particles confined within a cylindrical column is investigated. Several hydrodynamic regimes that depend strongly on the properties of the gas stream, the liquid stream, and the packed particle bed are known to exist within these systems. This experimental study focuses on characterizing the effect of wall confinement on these hydrodynamic regimes as the diameter d of the spherical particles becomes comparable to the column diameter D (or D/d becomes order-unity). The packed bed consists of polished, solid, spherical, monodisperse particles (beads) with mean diameter inmore » the range of 0.64-2.54 cm. These diameters yield D/d values between 15 and 3.75, so this range overlaps and extends the previously investigated range for two-phase flow, Measurements of the pressure drop across the bed and across the pulses are obtained for varying gas and liquid flow rates.« less

Performance characteristics and modeling of carbon dioxide absorption by amines in a packed column

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

Lin, S.H.; Shyu, C.T.

1999-01-01

Carbon dioxide (CO[sub 2]) is widely recognized as a major greenhouse gas contributing to global warming. To mitigate the global warming problem, removal of CO[sub 2] from the industrial flue gases is necessary. Absorption of carbon dioxide by amines in a packed column was experimentally investigated. The amines employed in the present study were the primary mono-ethanolamine (MEA) and tertiary N-methyldiethanolamine (MDEA), two very popular amines widely used in the industries for gas purification. The CO[sub 2] absorption characteristics by these two amines were experimentally examined under various operating conditions. A theoretical model was developed for describing the CO[sub 2]more » absorption behavior. Test data have revealed that the model predictions and the observed CO[sub 2] absorption breakthrough curves agree very well, validating the proposed model. Preliminary regeneration tests of exhausted amine solution were also conducted. The results indicated that the tertiary amine is easier to regenerate with less loss of absorption capacity than the primary one.« less

Silver nanoparticle-alginate composite beads for point-of-use drinking water disinfection.

PubMed

Lin, Shihong; Huang, Rixiang; Cheng, Yingwen; Liu, Jie; Lau, Boris L T; Wiesner, Mark R

2013-08-01

Silver nanoparticles (AgNPs)-alginate composite beads were synthesized using three different approaches as filler materials of packed columns for simultaneous filtration-disinfection as an alternative portable water treatment process. The prepared composite beads were packed into a column through which Escherichia coli containing water was filtered to evaluate the disinfection efficacy. Excellent disinfection performance (no detectable viable colony) was achieved with a hydraulic retention time (HRT) as short as 1 min (the shortest tested) with the SGR (Simultaneous-Gelation-Reduction) and AR (Adsorption-Reduction) beads that were prepared using in situ reduction of Ag(+). Comparatively, the SGR beads released significantly less Ag(+)/AgNPs than the AR beads did within the same HRT. From the results of this study it was identified that SGR may be the best choice among all three different synthesis approaches in that the SGR beads can achieve satisfactory bactericidal performance with a relatively low material consumption rate. Copyright © 2012 Elsevier Ltd. All rights reserved.

[Determination and analysis of toluene diisocyanate metabolites in mice using gas chromatography-mass spectrometry].

PubMed

Ji, Yu-Bin; Ji, Chen-Feng; Zou, Xiang; Liu, Hui-Xin

2007-09-01

In the present research we used gas chromatography-mass spectrometry (G C-MS) to determine metabolites of toluene diisocyanate (TDI) in mice and deduce the pathway for toluene diisocyanate metabolism in the organism. Conditions for TDI chromatography: Supelco PTETM-5 chromatographic column (30 mm x 0.25 mm x 0.25 microm); initial column temperature: 90 degrees C, which was maintained for 30 min, then the temperature was increased at a rate of 40 degrees C x min(-1) to 280 degrees C, and maintained for 5.25 min; temperature for the vaporizing chamber: 250 degrees C; carrier gas: helium flowing at 1.0 microL x min(-1). Conditions for chromatography of TDI metabolites in the organism: 94% methyl, 4% ethenyl-bonded-phase fused-silica capillary column (30 + 2 m x 0.25 + 0.02 mm); initial column temperature: 30 degrees C, which was maintained for 5 min, after and then was increased at a rate of 80 degrees C x min(-1) to 280 degrees C, and maintained for 5 min; temperature for the vaporizing chamber: 250 degrees C; carrier gas: helium flowing at 1.0 microL x min(-1). Conditions for mass spectrometry: EI for ionization; 70 eV for ionization energy; 280 degrees C for connecting tube temperature; 35-350 micro for range of scanning; and 1.0 microL for sample size. The results showed that 2 ,4-toluene diisocyanate was metabolized into 2,4-diaminotoluene. Under the conditions selected for GC-MS, TDI metabolites in the organism can be isolated and identified.

Multidose Preservative Free Eyedrops by Selective Removal of Benzalkonium Chloride from Ocular Formulations.

PubMed

Hsu, Kuan-Hui; Gupta, Karishma; Nayaka, Harish; Donthi, Aashrit; Kaul, Siddarth; Chauhan, Anuj

2017-12-01

About 70% of eye drops contain benzalkonium chloride (BAK) to maintain sterility. BAK is an effective preservative but it can cause irritation and toxicity. We propose to mitigate ocular toxicity without compromising sterility by incorporating a filter into an eye drop bottle to selectively remove BAK during the process of drop instillation. The filter is a packed bed of particles made from poly(2-hydroxyethyl methacrylate) (pHEMA), which is a common ophthalmic material. We showed that pHEMA particle prepared by using ethoxylated trimethylolpropane triacrylate as crosslinker can be incorporated into a modified eyedrop bottle tip to selectively remove the preservative as the formulation is squeezed out of the bottle. Hydraulic permeability of the plug is measured to determine the resistance to eye drop squeezing, and % removal of BAK and drugs are determined. The modified tip has a hydraulic permeability of about 2 Darcy, which allows eyedrops formulations to flow through without excessive resistance. The tip is designed such that the patients can create an eyedrop of solution of 1-10 cP viscosity in 4 s with a nominal pressure. During this short contact time, the packed particles removed nearly 100% of benzalkonium chloride (BAK) from a 15 mL, 0.012% BAK solution but have only minimal impact on the concentration of contained active components. Our novel design can eliminate the preservative induced toxicity from eye drops thereby impacting hundreds of millions of patients with chronic ophthalmic diseases like glaucoma and dry eyes.

Device-scale CFD modeling of gas-liquid multiphase flow and amine absorption for CO 2 capture: Original Research Article: Device-scale CFD modeling of gas-liquid multiphase flow and amine absorption for CO 2 capture

DOE PAGES

Pan, Wenxiao; Galvin, Janine; Huang, Wei Ling; ...

2018-03-25

In this paper we aim to develop a validated device-scale CFD model that can predict quantitatively both hydrodynamics and CO 2 capture efficiency for an amine-based solvent absorber column with random Pall ring packing. A Eulerian porous-media approach and a two-fluid model were employed, in which the momentum and mass transfer equations were closed by literature-based empirical closure models. We proposed a hierarchical approach for calibrating the parameters in the closure models to make them accurate for the packed column. Specifically, a parameter for momentum transfer in the closure was first calibrated based on data from a single experiment. Withmore » this calibrated parameter, a parameter in the closure for mass transfer was next calibrated under a single operating condition. Last, the closure of the wetting area was calibrated for each gas velocity at three different liquid flow rates. For each calibration, cross validations were pursued using the experimental data under operating conditions different from those used for calibrations. This hierarchical approach can be generally applied to develop validated device-scale CFD models for different absorption columns.« less

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

PubMed

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

2004-01-01

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

Chemotaxis Increases the Residence Time Distribution of Bacteria in Granular Media Containing Distributed Contaminant Sources

NASA Astrophysics Data System (ADS)

Adadevoh, J.; Triolo, S.; Ramsburg, C. A.; Ford, R.

2015-12-01

The use of chemotactic bacteria in bioremediation has the potential to increase access to, and biotransformation of, contaminant mass within the subsurface environment. This laboratory-scale study aimed to understand and quantify the influence of chemotaxis on residence times of pollutant-degrading bacteria within homogeneous treatment zones. Focus was placed on a continuous flow sand-packed column system in which a uniform distribution of naphthalene crystals created distributed sources of dissolved phase contaminant. A 10 mL pulse of Pseudomonas putida G7, which is chemotactic to naphthalene, and Pseudomonas putida G7 Y1, a non-chemotactic mutant strain, were simultaneously introduced into the sand-packed column at equal concentrations. Breakthrough curves obtained for the bacteria from column experiments conducted with and without naphthalene were used to quantify the effect of chemotaxis on transport parameters. In the presence of the chemoattractant, longitudinal dispersivity of PpG7 increased by a factor of 3 and percent recovery decreased from 21% to 12%. The results imply that pore-scale chemotaxis responses are evident at an interstitial fluid velocity of 1.7 m/d, which is within the range of typical groundwater flow. Within the context of bioremediation, chemotaxis may work to enhance bacterial residence times in zones of contamination thereby improving treatment.

Core-Shell in Liquid Chromatography: Application for Determining Sulphonamides in Feed and Meat Using Conventional Chromatographic Systems

PubMed Central

Armentano, Antonio; Summa, Simona; Magro, Sonia Lo; D’Antini, Pasquale; Palermo, Carmen; Muscarella, Marilena

2016-01-01

A C18 column packed with core-shell particles was used for the chromatographic separation of sulphonamides in feed and meat by a conventional high performance liquid chromatography system coupled with a diode array detector. Two analytical methods, already used in our laboratory, have been modified without any changes in the extraction and clean-up steps and in the liquid chromatography instrumentation. Chromatographic conditions applied on a traditional 5-µm column have been optimized on a column packed with 2.6 µm core-shell particles. A binary mobile phase [acetate buffer solution at pH 4.50 and a mixture of methanol acetonitrile 50: 50 (v/v)] was employed in gradient mode at the flow rate of 1.2 mL with an injection volume of 6 µL. These chromatographic conditions allow the separation of 13 sulphonamides with an entire run of 13 minutes. Preliminary studies have been carried out comparing blanks and spiked samples of feed and meat. A good resolution and the absence of interferences were achieved in chromatograms for both matrices. Since no change was made to the sample preparation, the optimized method does not require a complete revalidation and can be used to make routine analysis faster. PMID:28217560

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

PubMed

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

2016-10-21

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

Device-scale CFD modeling of gas-liquid multiphase flow and amine absorption for CO 2 capture: Original Research Article: Device-scale CFD modeling of gas-liquid multiphase flow and amine absorption for CO 2 capture

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

Pan, Wenxiao; Galvin, Janine; Huang, Wei Ling

In this paper we aim to develop a validated device-scale CFD model that can predict quantitatively both hydrodynamics and CO 2 capture efficiency for an amine-based solvent absorber column with random Pall ring packing. A Eulerian porous-media approach and a two-fluid model were employed, in which the momentum and mass transfer equations were closed by literature-based empirical closure models. We proposed a hierarchical approach for calibrating the parameters in the closure models to make them accurate for the packed column. Specifically, a parameter for momentum transfer in the closure was first calibrated based on data from a single experiment. Withmore » this calibrated parameter, a parameter in the closure for mass transfer was next calibrated under a single operating condition. Last, the closure of the wetting area was calibrated for each gas velocity at three different liquid flow rates. For each calibration, cross validations were pursued using the experimental data under operating conditions different from those used for calibrations. This hierarchical approach can be generally applied to develop validated device-scale CFD models for different absorption columns.« less

Compositional effects on the chemorheological properties and forming behavior of aqueous alumina-poly(vinyl alcohol) gelcasting suspensions

NASA Astrophysics Data System (ADS)

Morissette, Sherry L.

A new gelcasting system based on aqueous, alumina-poly(vinyl alcohol) (PVA) suspensions cross-linked by an organotitanate coupling agent has been developed. Both the chemorheological properties and forming behavior of this system exhibited a strong compositional dependence. A sol- gel phase diagram was established, which yielded the critical titanium concentration [Ti] c required for gelation at a given PVA volume fraction, as well as the minimum PVA volume fraction ( fminPVA = 0.0245) and titanium PVA concentration ([Ti]min = 9.984 x 10--4 g Ti/ml) below which gelation was not observed irrespective of solution composition. The gelation time of suspensions of constant PVA volume fraction ( fsolnPVA ) decreased with increasing cross-linking agent concentration, PVA temperature, and solids volume fraction. The steady-state viscosity and elastic modulus of polymer solutions ( fsolnPVA = 0.05) of varying [Ti] were well described by the PVA percolation model, giving scaling exponents of 0.84 and 1.79, respectively. The steady-state elastic modulus of gel casting suspensions, which provides a measure of their handling strength in the as-gelled state, increased with increasing solids volume fraction. Gelcasting suspensions were used as feedstock for solid free-form fabrication (SFF) of ceramic components. The influence of processing conditions (e.g., tip diameter, mixing rate, table speed, etc.) and suspension rheology on deposition behavior was investigated. Continuous printablity was achieved for tip diameters ranging from dt = 0.254 -- 1.370 mm for all mixing rates (Rmix 5 -- 300 rpm) and suspension compositions (i.e., fAl2O3 = 0.45, φPVA = 0.275, [Ti] 0 -- 6.30 x 10--3 g Ti/ml) probed, where the minimum tip diameter for continuous printing was 0.203 mm. Printed lines were uniform with good edge definition. Line dimensions were independent of mixing rate for the given process conditions. The as-cast alumina volume fraction ( fAl2O3 ) depended on casting conditions and cross-linking agent concentration, where fAl2O3 decreased with increasing tip diameter and increased with increasing cross-linking agent concentration. Free-fomied Al2O3 components exhibited uniform particle packing and had minimal macro-defects (e.g., slumping or stair casing) and no detectable micro-defects (e.g., bubbles or cracking).

Comparison of protocols and RNA carriers for plasma miRNA isolation. Unraveling RNA carrier influence on miRNA isolation

PubMed Central

Martos, Laura; Fernández-Pardo, Álvaro; Oto, Julia; Medina, Pilar; España, Francisco; Navarro, Silvia

2017-01-01

microRNAs are promising biomarkers in biological fluids in several diseases. Different plasma RNA isolation protocols and carriers are available, but their efficiencies have been scarcely compared. Plasma microRNAs were isolated using a phenol and column-based procedure and a column-based procedure, in the presence or absence of two RNA carriers (yeast RNA and MS2 RNA). We evaluated the presence of PCR inhibitors and the relative abundance of certain microRNAs by qRT-PCR. Furthermore, we analyzed the association between different isolation protocols, the relative abundance of the miRNAs in the sample, the GC content and the free energy of microRNAs. In all microRNAs analyzed, the addition of yeast RNA as a carrier in the different isolation protocols used gave lower raw Cq values, indicating higher microRNA recovery. Moreover, this increase in microRNAs recovery was dependent on their own relative abundance in the sample, their GC content and the free-energy of their own most stable secondary structure. Furthermore, the normalization of microRNA levels by an endogenous microRNA is more reliable than the normalization by plasma volume, as it reduced the difference in microRNA fold abundance between the different isolation protocols evaluated. Our thorough study indicates that a standardization of pre- and analytical conditions is necessary to obtain reproducible inter-laboratory results in plasma microRNA studies. PMID:29077772

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

PubMed

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

2011-10-14

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

Tuning jammed frictionless disk packings from isostatic to hyperstatic.

PubMed

Schreck, Carl F; O'Hern, Corey S; Silbert, Leonardo E

2011-07-01

We perform extensive computational studies of two-dimensional static bidisperse disk packings using two distinct packing-generation protocols. The first involves thermally quenching equilibrated liquid configurations to zero temperature over a range of thermal quench rates r and initial packing fractions followed by compression and decompression in small steps to reach packing fractions φ(J) at jamming onset. For the second, we seed the system with initial configurations that promote micro- and macrophase-separated packings followed by compression and decompression to φ(J). Using these protocols, we generate more than 10(4) static packings over a wide range of packing fraction, contact number, and compositional and positional order. We find that disordered, isostatic packings exist over a finite range of packing fractions in the large-system limit. In agreement with previous calculations, the most dilute mechanically stable packings with φ min ≈ 0.84 are obtained for r > r*, where r* is the rate above which φ(J) is insensitive to rate. We further compare the structural and mechanical properties of isostatic versus hyperstatic packings. The structural characterizations include the contact number, several order parameters, and mixing ratios of the large and small particles. We find that the isostatic packings are positionally and compositionally disordered (with only small changes in a number of order parameters), whereas bond-orientational and compositional order increase strongly with contact number for hyperstatic packings. In addition, we calculate the static shear modulus and normal mode frequencies (in the harmonic approximation) of the static packings to understand the extent to which the mechanical properties of disordered, isostatic packings differ from partially ordered packings. We find that the mechanical properties of the packings change continuously as the contact number increases from isostatic to hyperstatic.

Influence of wing tip morphology on vortex dynamics of flapping flight

NASA Astrophysics Data System (ADS)

Krishna, Swathi; Mulleners, Karen

2013-11-01

The mechanism of flapping wing flight provides insects with extraordinary flight capabilities. The uniquely shaped wing tips give insects an edge in flight performance and the interaction between the leading edge vortices and wing tip vortices enhance their propelling efficiencies and manoeuvrability. These are qualities that are sought after in current-day Micro Air Vehicles. A detailed understanding of the vortex dynamics of flapping flight and the influence of the wing tip planform is imperative for technical application. An experimental study is conducted to investigate the effects of different wing tip planforms on the formation, evolution and interaction of vortical structures. We thereby focus on the interaction between the coherent structures evolving from the leading edge and the wing tip during pitching and flapping motions.The spatial and temporal evolution of the three-dimensional flow structures are determined using Scanning (Stereo) Particle Image Velocimetry and an in-depth coherent structure analysis. By comparing the vortex dynamics, the aerodynamic performance of various wing tip planforms are evaluated.

10 CFR Appendix A to Part 725 - Categories of Restricted Data Available

Code of Federal Regulations, 2011 CFR

2011-01-01

... centrifuge or gaseous diffusion processes. b. Design, construction, and operation of any plant, facility or..., design, criticality studies and operation of reactors, reactor systems and reactor components. d... aqueous lithium hydroxide solution in packed columns. Not included is information regarding plant design...

10 CFR Appendix A to Part 725 - Categories of Restricted Data Available

Code of Federal Regulations, 2012 CFR

2012-01-01

... centrifuge or gaseous diffusion processes. b. Design, construction, and operation of any plant, facility or..., design, criticality studies and operation of reactors, reactor systems and reactor components. d... aqueous lithium hydroxide solution in packed columns. Not included is information regarding plant design...

10 CFR Appendix A to Part 725 - Categories of Restricted Data Available

Code of Federal Regulations, 2010 CFR

2010-01-01

... centrifuge or gaseous diffusion processes. b. Design, construction, and operation of any plant, facility or..., design, criticality studies and operation of reactors, reactor systems and reactor components. d... aqueous lithium hydroxide solution in packed columns. Not included is information regarding plant design...

10 CFR Appendix A to Part 725 - Categories of Restricted Data Available

Code of Federal Regulations, 2014 CFR

2014-01-01

... centrifuge or gaseous diffusion processes. b. Design, construction, and operation of any plant, facility or..., design, criticality studies and operation of reactors, reactor systems and reactor components. d... aqueous lithium hydroxide solution in packed columns. Not included is information regarding plant design...

KOVATS RETENTION INDICES OF HALOCARBONS ON A HEXAFLUOROPROPYLENE EPOXIDE-MODIFIED GRAPHITIZED CARBON BLACK

EPA Science Inventory

The article gives results of measuring Kovats retention indices of 97 halocarbons related to research on alternative refrigerants, propellants, foaming agents, and blowing agents, on a packed-column stationary phase consisting of a 5% mass coating of a low-molecular-weight polyme...

Hysteresis of Colloid Retention and Release in Saturated Porous Media During Transients in Solution Chemistry

USDA-ARS?s Scientific Manuscript database

Saturated packed column and micromodel transport studies wereconducted to gain insightonmechanismsof colloid retention and release under unfavorable attachment conditions. The initial deposition of colloids in porous media was found to be a strongly coupled process that depended on solution chemistr...

Sensitivity of the transport and retention of stabilized silver nanoparticles to physicochemical factors

USDA-ARS?s Scientific Manuscript database

Saturated sand-packed column experiments were conducted to investigate the influence of physicochemical factors on the transport and retention of surfactant stabilized silver nanoparticles (AgNPs). The normalized concentration in breakthrough curves (BTCs) of AgNPs increased with a decrease in solut...

Self-Chaperoning of the Type III Secretion System needle tip proteins IpaD and BipD

PubMed Central

Johnson, Steven; Roversi, Pietro; Espina, Marianela; Olive, Andrew; Deane, Janet E.; Birket, Susan; Field, Terry; Picking, William D.; Blocker, Ariel; Galyov, Edouard E.; Picking, Wendy L.; Lea, Susan M.

2007-01-01

Bacteria expressing type III secretion systems (T3SS) have been responsible for the deaths of millions worldwide, acting as key virulence elements in diseases ranging from plague to typhoid fever. The T3SS is composed of a basal body, which traverses both bacterial membranes, and an external needle through which effector proteins are secreted. We report multiple crystal structures of two proteins that sit at the tip of the needle and are essential for virulence; IpaD from Shigella flexneri and BipD from Burkholderia pseudomallei. The structures reveal that the N-terminal domains of the molecules are intra-molecular chaperones that prevent premature oligomerization, as well as sharing structural homology with proteins involved in eukaryotic actin rearrangement. Crystal packing has allowed us to construct a model for the tip complex that is supported by mutations designed using the structure. PMID:17077085

Self-chaperoning of the type III secretion system needle tip proteins IpaD and BipD.

PubMed

Johnson, Steven; Roversi, Pietro; Espina, Marianela; Olive, Andrew; Deane, Janet E; Birket, Susan; Field, Terry; Picking, William D; Blocker, Ariel J; Galyov, Edouard E; Picking, Wendy L; Lea, Susan M

2007-02-09

Bacteria expressing type III secretion systems (T3SS) have been responsible for the deaths of millions worldwide, acting as key virulence elements in diseases ranging from plague to typhoid fever. The T3SS is composed of a basal body, which traverses both bacterial membranes, and an external needle through which effector proteins are secreted. We report multiple crystal structures of two proteins that sit at the tip of the needle and are essential for virulence: IpaD from Shigella flexneri and BipD from Burkholderia pseudomallei. The structures reveal that the N-terminal domains of the molecules are intramolecular chaperones that prevent premature oligomerization, as well as sharing structural homology with proteins involved in eukaryotic actin rearrangement. Crystal packing has allowed us to construct a model for the tip complex that is supported by mutations designed using the structure.

Aid for the Medical Laboratory

NASA Technical Reports Server (NTRS)

1986-01-01

A process for separating chemical compounds in fluids resulted from a Jet Propulsion Laboratory (JPL)/LAPD project. The technique involves pouring a blood or urine sample into an extraction tube where packing material contained in a disposable tube called an "extraction column" absorbs water and spreads the specimen as a thin film, making it easy to identify specific components. When a solvent passes through the packing material, the desired compound dissolves and exits through the tube's bottom stem and is collected. Called AUDRI, Automated Drug Identification, it is commercially produced by Analytichem International which has successfully advanced the original technology.

[Properties and infiltration arts of machinable infiltration ceramic(MIC)].

PubMed

Yang, H; Xian, S; Liao, Y; Xue, Y; Chai, F

2000-06-01

The purpose of this study is to explore the infiltration arts of MIC and study the effects of different packing density of Al2O3 matrix on the properties of MIC. alpha-Al2O3 specimens were fabricated by pouring alpha-Al2O3 slip with different powder/liquid ratios(P/L = 3.5, 7.5, 10.5) into a mold, and subsequently pre-fired at 1160 degrees C for 6 hours to form Al2O3 matrix. The packing density of the matrices were measured. Infiltration concepts were introduced into this study by infiltrating molten mica micro-crystalline glass into the porous Al2O3 matrix at 1160 degrees C for 6 hours to form a continuous interpenetrating composite. The composite then underwent micro-crystallization by nucleating at 550 degrees C for 1 hour and crystallizing at 900 degrees C for 1 hour, which resulted in the MIC. Mechanical properties including three point flexural strength, elastic modulus, Vicker's hardness, indentation fracture toughness and Weibull's modulus of flexural strength were determined. Parameters of machinability(H/KIC)2 of MIC were calculated. XRD and SEM were employed to study its microstructure. The resulted matrices reached packing densities of 63%, 76%, 78% with P/L of 3.5, 7.5 and 10.5. The MIC attained high strength and good machinability after infiltration. Three-point flexural strength and indentation fracture toughness were 342, 431, 374 MPa and 4.05, 4.14, 5.02 MPa m1/2 for MIC with packing density of 63%, 76%, 78% separately. And parameters of machinability were 5.41, 6.84 and 7.39 respectively. Packing density of Al2O3 matrix significantly influenced the mechanical properties. Maximum properties were obtained with a matrix packing density of 75%(P/L = 7.5), with a Weibull's modulus of flexural strength of 6.8. Machinability decreased with the increase of P/L ratio. Micro-crystallizing treatment resulted in the formation of evenly distributed mica crystalline in the composite, which contributed to the high strength of this composite material. MIC is a new infiltrated ceramic with favorable strength and machinability which can satisfy the prosthodontic requirements as all ceramic crown and bridge materials, it also shows promising outlook for future developments and clinical usage.

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

PubMed

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

2010-05-23

This work presents novel approach in low-pressure chromatography flow systems--two-column Sequential Injection Chromatography (2-C SIC) and its comparison with gradient elution chromatography on the same instrument. The system was equipped with two different chromatographic columns (connected to selection valve in parallel design) for isocratic separation and determination of all components in composed anti-inflammatory pharmaceutical preparation (tablets). The sample was first injected on the first column of length 30 mm where less retained analytes were separated and then the sample was injected on the second column of length 10 mm where more retained analytes were separated. The SIC system was based on a commercial SIChrom manifold (8-port high-pressure selection valve and medium-pressure syringe pump with 4 mL reservoir) (FIAlab, USA) with two commercially available monolithic columns the "first column" Chromolith Flash RP-18e (25 mm x 4.6 mm i.d. with guard column 5 mm x 4.6 mm i.d.) and the "second column" Chromolith RP-18e (10 mm x 4.6 mm i.d.) and CCD UV-vis detector USB 4000 with micro-volume 1.0 cm Z flow cell. Two mobile phases were used for analysis (one for each column). The mobile phase 1 used for elution of paracetamol, caffeine and salicylic acid (internal standard) was acetonitrile/water (10:90, v/v, the water part of pH 3.5 adjusted with acetic acid), flow rate was 0.9 mL min(-1) (volume 3.0 mL of mobile phase per analysis). The mobile phase 2 used for elution of propyphenazone was acetonitrile/water (30:70, v/v); flow rate was 1.2 mL min(-1) (volume 1.5 mL of mobile phase per analysis). Absorbance was monitored at 210 nm. Samples were prepared by dissolving of one tablet in 30% acetonitrile and 10 microL of filtered supernatant was injected on each column (2 x 10 microL). The chromatographic resolution between all compounds was >1.45 and analysis time was 5.5 min under the optimal conditions. Limits of detection were determined at 0.4 microg mL(-1) for paracetamol, at 0.5 microg mL(-1) for caffeine and at 0.7 microg mL(-1) for propyphenazone. The new two-column chromatographic set-up developed as an alternative approach to gradient elution chromatography shows evident advantages (time and solvent reduction more than one-third) as compared with single-column gradient SIC method with Chromolith Flash RP-18 (25 mm x 4.6 mm i.d. with guard column 5 mm x 4.6 mm i.d.). Copyright 2010 Elsevier B.V. All rights reserved.

Laser ablated hard coating for microtools

DOEpatents

McLean, W. II; Balooch, M.; Siekhaus, W.J.

1998-05-05

Wear-resistant coatings composed of laser ablated hard carbon films, are deposited by pulsed laser ablation using visible light, on instruments such as microscope tips and micro-surgical tools. Hard carbon, known as diamond-like carbon (DLC), films produced by pulsed laser ablation using visible light enhances the abrasion resistance, wear characteristics, and lifetimes of small tools or instruments, such as small, sharp silicon tips used in atomic probe microscopy without significantly affecting the sharpness or size of these devices. For example, a 10--20 nm layer of diamond-like carbon on a standard silicon atomic force microscope (AFM) tip, enables the useful operating life of the tip to be increased by at least twofold. Moreover, the low inherent friction coefficient of the DLC coating leads to higher resolution for AFM tips operating in the contact mode. 12 figs.

Quantitation of pregabalin in dried blood spots and dried plasma spots by validated LC-MS/MS methods.

PubMed

Kostić, Nađa; Dotsikas, Yannis; Jović, Nebojša; Stevanović, Galina; Malenović, Anđelija; Medenica, Mirjana

2015-05-10

In this paper, novel LC-MS/MS methods for the determination of antiepileptic drug pregabalin in dried matrix spots (DMS) are presented. This attractive technique of sample collection in micro amount was utilized in the form of dried blood spots (DBS) and dried plasma spots (DPS). Following a pre-column derivatization procedure, using n-propyl chloroformate in the presence of n-propanol, and consecutive liquid-liquid extraction, derivatized pregabalin and its internal standard, 4-aminocyclohexanecarboxylic acid, were detected in positive ion mode by applying two SRM transitions per analyte. A YMC-Pack Octyl column (50mm×4.0mm, 3μm particle size) maintained at 30°C, was utilized with running mobile phase composed of acetonitrile: 0.15% formic acid (85:15, v/v). Flow rate was 550μL/min and total run time 2min. Established methods were fully validated over the concentration range of 0.200-20.0μg/mL for DBS and 0.400-40.0μg/mL for DPS, respectively, while specificity, accuracy, precision, recovery, matrix-effect, stability, dilution integrity and spot homogeneity were found within acceptance criteria. Validated methods were applied for the determination of pregabalin levels in dried blood and plasma samples obtained from patients with epilepsy, after per os administration of commercial capsules. Comparison of drug level in blood and plasma, as well as correction steps undertaken in order to overcome hematocrit issue, when analyzing DBS, are also given. Copyright © 2015 Elsevier B.V. All rights reserved.

Method for the routine quantitative gas chromatographic analysis of major free fatty acids in butter and cream.

PubMed

Woo, A H; Lindsay, R C

1980-07-01

A rapid quantiative method was developed for routine analysis of the major, even carbon-numbered free fatty acids in butter and cream. Free fatty acids were isolated directly from intact samples by a modified silicic acid-potassium hydroxide arrestant column and were separated by gas chromatography with a 1.8 m x 2 mm inner diameter glass column packed with 10% neopentyl glycol adipate on 80/100 Chromosorb W. Purified, formic acid-saturated carrier gas was required for minimal peak tailing and extended column life. The accuracy and reproducibility of the mmethod was established through quantitative recovery studies of free fatty acid mixtures, free fatty acids added to butter, and replicate analysis of butter and cream samples.

AFM-based micro/nanoscale lithography of poly(dimethylsiloxane): stick-slip on a softpolymer

NASA Astrophysics Data System (ADS)

Watson, Jolanta A.; Myhra, Sverre; Brown, Christopher L.; Watson, Gregory S.

2005-02-01

Silicone rubbers have steadily gained importance in industry since their introduction in the 1960"s. Poly(dimethylsiloxane) (PDMS) is a relatively soft and optically clear, two-part elastomer with interesting and, more importantly, useful physical and electrical properties. Some of its common applications include protective coatings (e.g., against moisture, environmental attack, mechanical and thermal shock and vibrations), and encapsulation (e.g., amplifiers, inductive coils, connectors and circuit boards). The polymer has attracted recent interest for applications in soft lithography. The polymer is now routinely used as a patterned micro-stamp for chemical modification of surfaces, in particular Au substrates. Prominent stick-slip effects, surface relaxation and elastic recovery were found to be associated with micro/nano manipulation of the polymer by an AFM-based contact mode methodology. Those effects provide the means to explore in detail the meso-scale tip-to-surface interactions between a tip and a soft surface. The dependence of scan speed, loading force, attack angle and number of scan lines have been investigated.

Spatial zonation limits magnesite dissolution in porous media

NASA Astrophysics Data System (ADS)

Li, Li; Salehikhoo, Fatemeh; Brantley, Susan L.; Heidari, Peyman

2014-02-01

We investigate how mineral spatial distribution in porous media affects their dissolution rates. Specifically, we measure the dissolution rate of magnesite interspersed in different patterns in packed columns of quartz sand where the magnesite concentration (v/v) was held constant. The largest difference was observed between a “Mixed column” containing uniformly distributed magnesite and a “One-zone column” containing magnesite packed into one cylindrical center zone aligned parallel to the main flow of acidic inlet fluid (flow-parallel One-zone column). The columns were flushed with acid water at a pH of 4.0 at flow velocities of 3.6 or 0.36 m/d. Breakthrough data show that the rate of magnesite dissolution is 1.6-2 times slower in the One-zone column compared to the Mixed column. This extent of rate limitation is much larger than what was observed in our previous work (14%) for a similar One-zone column where the magnesite was packed in a layer aligned perpendicular to flow (flow-transverse One-zone column). Two-dimensional reactive transport modeling with CrunchFlow revealed that ion activity product (IAP) and local dissolution rates at the grid block scale (0.1 cm) vary by orders of magnitude. Much of the central magnesite zone in the One-zone flow-parallel column is characterized by close or equal to equilibrium conditions with IAP/Keq > 0.1. Two important surface areas are defined to understand the observed rates: the effective surface area (Ae) reflects the magnesite that effectively dissolves under far from equilibrium conditions (IAP/Keq < 0.1), while the interface surface area (AI) reflects the effective magnesite surface that lies along the quartz-magnesite interface. Modeling results reveal that the transverse dispersivity at the interface of the quartz and magnesite zones controls mass transport and therefore the values of Ae and AI. Under the conditions examined in this work, the value of Ae varies from 2% to 67% of the total magnesite BET surface area. Column-scale bulk rates R,B (in units of mol/s) vary linearly with Ae and AI. Using Ae to normalize rates, we calculate a rate constant (10-9.56 mol/m2/s) that is very close to the value of 10-10.0 mol/m2/s under well-mixed conditions at the grid block scale. This implies that the laboratory-field rate discrepancy can potentially be caused by differences in the effective surface area. If we know the effective surface area of dissolution, we will be able to use the rate constant measured in laboratory systems to calculate field rates for some systems. In this work, approximately 60-70% of the Ae is at the magnesite-quartz interface. This implies that in some field systems where the detailed information that we have for our columns is not available, the effective mineral surface area may be approximated by the area of grains residing at the interface of reactive mineral zones. Although it has long been known that spatial heterogeneities play a significant role in determining physical processes such as flow and solute transport, our data are the first that systematically and experimentally quantifies the importance of mineral spatial distribution (chemical heterogeneity) on dissolution.

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.

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.

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

PubMed

Samuelsson, Jörgen; Fornstedt, Torgny; Shalliker, Andrew

2015-08-07

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

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

PubMed

Gritti, Fabrice; Guiochon, Georges

2014-01-31

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

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.

Axial dispersion of non-Newtonian fluids in porous media

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

Payne, L.W.; Parker, H.W.

1973-01-01

Mixing of liquids in the direction parallel to flow through porous media, usually termed axial dispersion, is a significant factor in regard to chromatography columns, packed bed reactors, and miscible displacement methods for the recovery of petroleum. For this reason, axial dispersion rates have frequently been investigated, but practically investigations have employed low viscosity Newtonian fluid such as water and light hydrocarbons. In this research, pseudoplastic fluids having a power law exponent as low as 0.6 were employed at very low flow rates to facilitate the observation of non-Newtonian effects on axial dispersion rates. The flow system used in thismore » investigation was a vertically oriented glass bead pack. Glass beads of 470 mu nominal size were packed into the flow cell while vibrating the cell. The studies were conducted by displacing an undyed solution from the bead pack with a dyed solution at a constant rate aor visa versa. Vertical, downward flow was used in all displacements. (10 refs.)« less

Microbial Degradation of Pesticides

DTIC Science & Technology

1981-11-30

with a 2-m glass, 3.2 mm I.D. column, packed with 3% Silar IOC on Gas-Chrom Q, (110-200 mesh) (Applied Science Laboratories, State College, PA) was...allowing the material to stand overnight to form trimethylsilyl (TMS) derivatives of polar compounds. All peaks recovered by GC on Silar 1OC rolumn

Transport and retention of surfactant- and polymer-stabilized engineered silver nanoparticles in silicate-dominated aquifer material

USDA-ARS?s Scientific Manuscript database

Packed column experiments were conducted to investigate the transport and blocking behavior of surfactant- and polymer-stabilized engineered silver nanoparticles (Ag-ENPs) in saturated natural aquifer material with varying silt and clay content, background solution chemistry, and flow velocity. Brea...

Evaluation of rotating-cylinder and piston-cylinder reactors for ground-based emulsion polymerization

NASA Technical Reports Server (NTRS)

Vanderhoff, J. W.; El-Aasser, M. S.

1987-01-01

The objectives of this program are to apply ground-based emulsion polymerization reactor technology to improve the production of: monodisperse latex particles for calibration standards, chromatographic separation column packing, and medical research; and commercial latexes such as those used for coatings, foams, and adhesives.

Interactions between exogenous rare earth elements and phosphorus leaching in packed soil columns

USDA-ARS?s Scientific Manuscript database

Rare earth elements (REEs) increasingly used in agriculture as an amendment for crop growth may help to lessen environmental losses of phosphorus (P) from heavily fertilized soils. The vertical transport characteristics of P and REEs, lanthanum (La), neodymium (Nd), samarium (Sm), and cerium (Ce), w...

Between the Lines. A Basic Skills Newspaper Pack.

ERIC Educational Resources Information Center

Adult Literacy and Basic Skills Unit, London (England).

This document incorporates source materials from local and regional newspapers from different parts of the United Kingdom into learning activities to develop literacy skills. The activities are organized into seven sections as follows: local newspapers (types of local newspapers, regular and special features, columns and blocks, and reading the…

Impacts of bridging complexation on the transport of surface-modified nanoparticles in saturated sand

USDA-ARS?s Scientific Manuscript database

The transport of polyacrylic acid capped cadmium telluride (CdTe) quantum dots (QDs) and carboxylate-modified latex (CML) nanoparticles (NPs) was studied in packed columns at various electrolyte concentrations and cation types. The breakthrough curves (BTCs) of QDs and CML NPs in acid-treated Accus...

A unified classification of stationary phases for packed column supercritical fluid chromatography.

PubMed

West, C; Lesellier, E

2008-05-16

The use of supercritical fluids as chromatographic mobile phases allows to obtain rapid separations with high efficiency on packed columns, which could favour the replacement of numerous HPLC methods by supercritical fluid chromatography (SFC) ones. Moreover, despite some unexpected chromatographic behaviours, general retention rules are now well understood, and mainly depend on the nature of the stationary phase. The use of polar stationary phases improves the retention of polar compounds, when C18-bonded silica favours the retention of hydrocarbonaceous compounds. In this sense, reversed-phase and normal-phase chromatography can be achieved in SFC, as in HPLC. However, these two domains are clearly separated in HPLC due to the opposite polarity of the mobile phases used for each method. In SFC, the same mobile phase can be used with both polar and non-polar stationary phases. Consequently, the need for a novel classification of stationary phases in SFC appears, allowing a unification of the classical reversed- and normal-phase domains. In this objective, the paper presents the development of a five-dimensional classification based on retention data for 94-111 solutes, using 28 commercially available columns representative of three major types of stationary phases. This classification diagram is based on a linear solvation energy relationship, on the use of solvation vectors and the calculation of similarity factors between the different chromatographic systems. This classification will be of great help in the choice of the well-suited stationary phase, either in regards of a particular separation or to improve the coupling of columns with complementary properties.

Cadmium removal in a biosorption column

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

Volesky, B.; Prasetyo, I.

New biosorbent material derived from a ubiquitous brown marine alga Ascophyllum nodosum has been examined in packed-bed flow-through sorption columns. It effectively removed 10 mg/L of cadmium down to 1.5 ppb levels in the effluent, representing 99.985% removal. The experimental methodology used was based on the early Bohart and Adams sorption model, resulting in quantitative determination of the characteristic process parameters which can be used for performance comparison and process design. An average metal loading of the biosorbent (N[sub 0]) determined was 30 mg Cd/g, corresponding closely to that observed for the batch equilibrium metal concentration of 10 mg Cd/L.more » The critical bed depth (D[sub min]) for the potable water effluent quality standard varied with the column feed flow rate from 20 to 50 cm. The sorption column mass transfer and dispersion coefficients were determined, which are also required for solving the sorption model equations.« less

Adsorption experiment of toxic micro-pollutants derived from automobiles using red soil.

PubMed

Kawai, Takahiro; Ichiki, Atsushi; Sawada, Yasunori

2015-01-01

In some countries, non-point source pollution derived from a city's economic activities tends to be a barrier to the improvement of water quality. Roadway runoff is known to contain toxic micro-pollutants such as polycyclic aromatic hydrocarbons (PAHs). Conversely, red soil is known to adsorb some organic matter. In this study, artificial roadway runoff water containing toxic micro-pollutants was made using roadway dust collected from a highway, and used for both batch-type tests and soil column tests with red soil in order to understand adsorption ability of the red soil on such toxic micro-pollutants, especially PAHs. In the batch-type tests, PAHs could be removed by approximately 40% when the contact time was 90 minutes. In the soil column tests, PAHs were removed by more than 80% while suspended solids were removed by more than 90%. Notably, PAHs with a high molecular weight were removed more readily in the tests than PAHs with a low molecular weight.

Impact of needle insertion depth on the removal of hard-tissue debris.

PubMed

Perez, R; Neves, A A; Belladonna, F G; Silva, E J N L; Souza, E M; Fidel, S; Versiani, M A; Lima, I; Carvalho, C; De-Deus, G

2017-06-01

To evaluate the effect of depth of insertion of an irrigation needle tip on the removal of hard-tissue debris using micro-computed tomographic (micro-CT) imaging. Twenty isthmus-containing mesial roots of mandibular molars were anatomically matched based on similar morphological dimensions using micro-CT evaluation and assigned to two groups (n = 10), according to the depth of the irrigation needle tip during biomechanical preparation: 1 or 5 mm short of the working length (WL). The preparation was performed with Reciproc R25 file (tip size 25, .08 taper) and 5.25% NaOCl as irrigant. The final rinse was 17% EDTA followed by bidistilled water. Then, specimens were scanned again, and the matched images of the canals, before and after preparation, were examined to quantify the amount of hard-tissue debris, expressed as the percentage volume of the initial root canal volume. Data were compared statistically using the Mann-Whitney U-test. None of the tested needle insertion depths yielded root canals completely free from hard-tissue debris. The insertion depth exerted a significant influence on debris removal, with a significant reduction in the percentage volume of hard-tissue debris when the needle was inserted 1 mm short of the WL (P < 0.05). The insertion depth of irrigation needles significantly influenced the removal of hard-tissue debris. A needle tip positioned 1 mm short of the WL resulted in percentage levels of hard-tissue debris removal almost three times higher than when positioned 5 mm from the WL. © 2016 International Endodontic Journal. Published by John Wiley & Sons Ltd.

Evaluation of Changes in Iron Interfacial Composition Using Surface Spectroscopy

NASA Astrophysics Data System (ADS)

Vikesland, P. J.; Kohn, T.; Ball, W. P.; Fairbrother, D.; Roberts, A.

2001-12-01

Although the ability of granular cast iron permeable reactive barriers to attenuate many persistent groundwater contaminants is well established, many uncertainties remain about the interactions that occur between cast iron and contaminant species. To better understand these interactions we set out to evaluate how various inorganic species and organic contaminants affect the interfacial composition of the iron over time. Column studies using granular iron enable us to observe changes in iron interfacial composition as a function of distance along the column as well as of column "age". The spectroscopic evaluations reported here are for ten columns that were fed continuously with simulated anoxic groundwaters of different chemistries. Nine of these columns were packed with untreated sieved cast iron and one was packed with a mixture of cast iron and the aluminosilicate mineral albite. Of the ten columns, seven have been continually fed chlorinated hydrocarbons (CHCs), one has been continually fed nitroaromatic compounds (NACs), and two have only periodically been fed CHCs in their influent. Six of these ten columns were operated for 1100 days and the remaining four were operated for 475 days. In an anaerobic glovebox, sample grains were extracted for surface spectroscopic characterization using solid sampling ports drilled into the columns. At each port, several iron grains were removed and immediately put into headspace free vials containing porewater obtained from the nearest aqueous sampling port. Samples were then analyzed using in-situ Raman analysis, Auger electron spectroscopy (AES), and transmission electron microscopy (TEM). Raman spectra indicate that the interfacial composition of the iron grains changes substantially between the inlet and the outlet of a given column. Near the inlet, Raman bands corresponding to the iron oxides goethite and magnetite are prevalent, whereas grains from a port near the column outlet exhibit bands at 425 and 504 cm-1, corresponding to the Fe2+-OH stretch and the Fe3+-OH stretch, respectively, of the redox-active mineral green rust. Comparisons at two different times (308 and 921 days) suggest that the interfacial composition of the iron grains also changed as the columns aged, with the longer-term downgradient compositions becoming more like those observed upgradient at earlier times. These in-situ Raman observations were supported by both AES and TEM. The observed spatial and temporal changes in the interfacial composition of the iron indicate that the iron grains become more passivated as the columns age. Initially, this passivation is most notable near the influent end of the columns, since that region receives the largest influx of reducible material. As the columns age, the passivated region slowly expands into the distal regions of the columns. This presentation will address the use of surface spectroscopy to analyze these changes in interfacial composition and will relate the observations to feed solution properties and to concurrent observations of reactivity changes. The implications of these results on the design and longevity of cast iron barriers will also be discussed.

Chip-based device for parallel sorting, amplification, detection, and identification of nucleic acid subsequences

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

Beer, Neil Reginald; Colston, Jr, Billy W.

An apparatus for chip-based sorting, amplification, detection, and identification of a sample having a planar substrate. The planar substrate is divided into cells. The cells are arranged on the planar substrate in rows and columns. Electrodes are located in the cells. A micro-reactor maker produces micro-reactors containing the sample. The micro-reactor maker is positioned to deliver the micro-reactors to the planar substrate. A microprocessor is connected to the electrodes for manipulating the micro-reactors on the planar substrate. A detector is positioned to interrogate the sample contained in the micro-reactors.

Pore-scale dynamics of salt transport in drying porous media

NASA Astrophysics Data System (ADS)

Shokri, N.

2013-12-01

Understanding the physics of water evaporation from saline porous media is important in many hydrological processes such as land-atmosphere interactions, water management, vegetation, soil salinity, and mineral-fluid interactions. We applied synchrotron x-ray micro-tomography to investigate the pore-scale dynamics of dissolved salt distribution in a three dimensional drying saline porous media using a cylindrical plastic column (15 mm in height and 8 mm in diameter) packed with sand particles saturated with CaI2 solution (5% concentration by mass) with a spatial and temporal resolution of 12 microns and 30 min, respectively. Every time the drying sand column was set to be imaged, two different images were recorded using distinct synchrotron X-rays energies immediately above (33.2690 keV) and below (33.0690 keV) the K-edge value of Iodine (33.1694 keV). Taking the difference between pixel gray values enabled us to delineate the spatial and temporal distribution of CaI2 concentration at pore scale. The experiment was continued for 12 hours. Results indicate that during early stages of evaporation, air preferentially invades large pores at the surface while finer pores remain saturated and connected to the wet zone at bottom via capillary-induced liquid flow. Consequently, the salt concentration increases preferentially in finer pores where evaporation occurs. The Peclet number (describing the competition between convection and diffusion) was greater than one in our experiment resulting in higher salt concentrations closer to the evaporation surface indicating a convection-driven process. The obtained salt profiles were used to evaluate the numerical solution of the convection-diffusion equation (CDE). Results show that the macro-scale CDE could capture the overall trend of the measured salt profiles but fail to produce the exact slope of the profiles. Our results shed new insight on the physics of salt transport and its complex dynamics in drying porous media and establish synchrotron x-ray micro-tomography as an effective tool to investigate the dynamics of dissolved salt transport in porous media with high spatial and temporal resolutions.

UltraSail - Ultra-Lightweight Solar Sail Concept

NASA Technical Reports Server (NTRS)

Burton, Rodney L.; Coverstone, Victoria L.; Hargens-Rysanek, Jennifer; Ertmer, Kevin M.; Botter, Thierry; Benavides, Gabriel; Woo, Byoungsam; Carroll, David L.; Gierow, Paul A.; Farmer, Greg

2005-01-01

UltraSail is a next-generation high-risk, high-payoff sail system for the launch, deployment, stabilization and control of very large (sq km class) solar sails enabling high payload mass fractions for high (Delta)V. Ultrasail is an innovative, non-traditional approach to propulsion technology achieved by combining propulsion and control systems developed for formation-flying micro-satellites with an innovative solar sail architecture to achieve controllable sail areas approaching 1 sq km, sail subsystem area densities approaching 1 g/sq m, and thrust levels many times those of ion thrusters used for comparable deep space missions. Ultrasail can achieve outer planetary rendezvous, a deep space capability now reserved for high-mass nuclear and chemical systems. One of the primary innovations is the near-elimination of sail supporting structures by attaching each blade tip to a formation-flying micro-satellite which deploys the sail, and then articulates the sail to provide attitude control, including spin stabilization and precession of the spin axis. These tip micro-satellites are controlled by 3-axis micro-thruster propulsion and an on-board metrology system. It is shown that an optimum spin rate exists which maximizes payload mass.

Energy Digest.

ERIC Educational Resources Information Center

Gaddy, Carol T., Ed.; Wells, Kathy, Ed.

This collection of reprints offers practical solutions, not readily available elsewhere, to everyday energy problems, such as high utility bills, insulating windows, getting more gas mileage, or buying a more efficient washer or refrigerator. The Arkansas Energy Office provides a weekly column of energy news and conservation tips to newspapers,…

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.

On-line packed magnetic in-tube solid phase microextraction of acidic drugs such as naproxen and indomethacin by using Fe3O4@SiO2@layered double hydroxide nanoparticles with high anion exchange capacity.

PubMed

Shamsayei, Maryam; Yamini, Yadollah; Asiabi, Hamid; Safari, Meysam

2018-02-22

The authors describe a 3-component nanoparticle system composed of a silica-coated magnetite (Fe 3 O 4 ) core and a layered double (Cu-Cr) hydroxide nanoplatelet shell. The sorbent has a high anion exchange capacity for extraction anionic species. A simple online system, referred to as "on-line packed magnetic-in-tube solid phase microextraction" was designed. The nanoparticles were placed in a stainless steel cartridge via dry packing. The cartridge was then applied to the preconcentration acidic drugs including naproxen and indomethacin from urine and plasma. Extraction and desorption times, pH values of the sample solution and flow rates of sample solution and eluent were optimized. Analytes were then quantified by HPLC with UV detection. Under optimal conditions, the limits of detection range from 70 to 800 ng L -1 , with linear responses from 0.1-500 μg L -1 (water samples), 0.6-500 μg L -1 (spiked urine), and 0.9-500 μg L -1 (spiked plasma). The inter- and intra-assay precisions (RSDs, for n = 5) are in the range of 2.2-5.4%, 2.8-4.9%, and 2.0-5.2% at concentration levels of 5, 25 and 50 μg L -1 , respectively. The method was applied to the analysis of the drugs in spiked human urine and plasma, and good results were achieved. Graphical abstract Fe 3 O 4 @SiO 2 @CuCr-LDH magnetic nanoparticles were synthesized and packed in to a stainless steel column. The column was applied to solid phase microextraction of acidic drugs from biological samples.

An integrated evaluation of the persistence and effects of 4-nonylphenol in an experimental littoral ecosystem

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

Liber, K.; Knuth, M.L.; Stay, F.S.

1999-03-01

A comprehensive littoral enclosure study was conducted to assess the persistence and distribution of 4-nonylphenol (NP) in a littoral ecosystem, and to evaluate the compound`s effects on resident aquatic biota. Enclosures with a mean ({+-} SD) surface area and volume of 31.4 {+-} 3.3 m{sup 2} and 32.0 {+-} 6.4 m{sup 3}, respectively, received eleven applications at 48-h intervals with one of four different rates of NP. This created a 20-d application period which was followed by a three to fourteen month observation period, depending on the endpoint measured. Mean {+-} SD NP concentrations in the water column measured 2more » h after each application averaged 5 {+-} 4, 23 {+-} 11, 76 {+-} 21, and 243 {+-} 41 {micro}g/L at nominal treatments of 3, 30, 100, and 300 {micro}g/L, respectively. Persistence in the water column was relatively short, with a dissipation half-life estimated at {le} 1.2 d. Persistence of NP in sediment and on macrophytes was substantially longer, with estimated half-lives of 28 to 104 d and 8 to 13 d, respectively. Zooplankton was the most sensitive group of organisms evaluated, with significant reductions in population abundances of some copepod taxa observed at the 23 {+-} 11-{micro}g/L treatment. Fish survival was affected at 243 {+-} 41 {micro}g/L. The most sensitive benthic macroinvertebrate taxon, Pisidium (Bivalvia) was affected at 76 {+-} 21 {micro}g/L, but most taxa were only affected at the 243 {+-} 41-{micro}g/L treatment. None of the assessed populations were affected at the 5 {+-} 4-{micro}g/L treatment. Macrophytes and periphyton were not adversely affected by any of the treatments. Overall community composition, assessed at the family level or higher, was not affected at or below the 23 {+-} 11-{micro}g/L treatment, but did exhibit substantial changes at the 243 {+-} 41-{micro}g/L treatment. Some minor changes were observed at the 76 {+-} 21-{micro}g/L treatment. The maximum acceptable toxicant concentration in the water column, based on protection of the most sensitive taxa in the test system, was estimated at {approximately} 10 {micro}g/L. Details on NP persistence and distribution within the enclosures, and detailed effects on zooplankton, benthic macroinvertebrates, and fish are described in four separate papers immediately following this overview.« less

Enantioseparation of omeprazole--effect of different packing particle size on productivity.

PubMed

Enmark, Martin; Samuelsson, Jörgen; Forssén, Patrik; Fornstedt, Torgny

2012-06-01

Enantiomeric separation of omeprazole has been extensively studied regarding both product analysis and preparation using several different chiral stationary phases. In this study, the preparative chiral separation of omeprazole is optimized for productivity using three different columns packed with amylose tris (3,5-dimethyl phenyl carbamate) coated macroporous silica (5, 10 and 25 μm) with a maximum allowed pressure drop ranging from 50 to 400 bar. This pressure range both covers low pressure process systems (50-100 bar) and investigates the potential for allowing higher pressure limits in preparative applications in a future. The process optimization clearly show that the larger 25 μm packing material show higher productivity at low pressure drops whereas with increasing pressure drops the smaller packing materials have substantially higher productivity. Interestingly, at all pressure drops, the smaller packing material result in lower solvent consumption (L solvent/kg product); the higher the accepted pressure drop, the larger the gain in reduced solvent consumption. The experimental adsorption isotherms were not identical for the different packing material sizes; therefore all calculations were recalculated and reevaluated assuming identical adsorption isotherms (with the 10 μm isotherm as reference) which confirmed the trends regarding productivity and solvent consumption. Copyright © 2012 Elsevier B.V. All rights reserved.

EEE Links, Volume 9, No. 1, January 2003 Focus on Plastic Parts

NASA Technical Reports Server (NTRS)

2003-01-01

The January 2003 issue of Electronic, Electromechanical, Electric (EEE) Links is presented. The Programmable Logic Application Notes column has been reinstated in this newsletter. Written by Rich Katz of NASA's Office of Logic Design (OLD), the application notes offer technical tips intended to prevent flight design errors and enhance research, development, and use of programmable logic and elements for space flight applications. An archive of these notes columns from previous issues of EEE Links is available at http://www.klabs.org/richcontent/eeelink s/EEE Links.htm.

Ectoenzymatic ratios in relation to particulate organic matter distribution (Ross Sea, Antarctica).

PubMed

Misic, C; Povero, P; Fabiano, M

2002-10-01

The results of a study on ectoenzymatic activity (the enzyme activity bound to particles larger than 0.2 micro m) and its relation to organic particle concentration are reported here. The sampling was carried out during the 1994 Antarctic spring, at a fixed station (Station 11) in the polynya of the Ross Sea, an area characterized by quick changes in sea ice cover. The sampling was repeated 4 times over a 20-day time period. The particulate organic matter distribution followed the physical structure of the water column, which depends on ice dynamics and is mainly determined by salinity. In the mixed-water surface layer (0-50 m) the concentrations were higher (on average 65.6 micro gC/L) than in the deeper water layer (50 m-bottom) (on average 19.1 micro gC/L). This distribution and quality, expressed by the protein:carbohydrate ratio, linked the particulate organic matter to the phytoplanktonic bloom which was in progress in the area. We determined the kinetic parameters of the glycolytic and proteolytic ectoenzymes and also the total activity for the proteolytic enzyme, in order to evaluate the contribution of the particle-bound activity. We observed higher values in the surface layer than in the deeper layer. b-Glucosidase activity ranged between 0.03 and 0.92 nmol L(-1) h(-1); b-N-acetylglucosaminidase activity was in the range of 0.04-0.58 nmol (L-1) (h-1). The total proteolytic activity (leucine aminopeptidase) ranged between 0.85 and 33.71 nmol L(-1) (h-1). The ectoproteolytic activity was about 35-60% of the total. The Km values were slightly higher for the proteolytic activity (on average 0.43 micro M for ectoproteolytic activity and 0.58 micro M for total proteolytic activity) than for the b-glucosidase (on average 0.36 micro M) and b-N-acetylglucosaminidase (on average 0.17 micro M), showing no remarkable variations in the water column. The ectoenzymatic ratios and their relationship with particulate organic substrates confirm the close link between organic substrate availability and degradation system response. The significant and positive correlations are not specific and suggest a prompt and efficient systemic response to the input of trophic resources. Nevertheless, changes in ectoenzyme activity and synthesis may act as adaptive responses to changing features of the ecosystem. In particular, variations in the proteolysis:glycolysis ratio depend on the functional features of the ecological system. In our study area this ratio is higher (about 10 or more) during production (particularly autotrophic) and lower (about 5 or less) during degradation/consumption events. The analysis of previous data, collected over a larger area characterized by different environmental conditions due to the changes of the pack ice cover, during the same cruise, confirms the existence of a significant relationship. Furthermore, the analysis of enzyme-uptake systems, expressed as Vmax:Km ratio, suggests that glycolytic ectoenzymes, although poorly expressed, may encourage microconsumers to grow rapidly on a wide range of organic substrates, including the refractory ones such as cellulose and chitin. However, low ectoenzyme potential exploitation rates of available organic substrates (on average about 5% for glycolytic and 12% for proteolytic ectoenzymes) would suggest that, during spring, zooplankton grazing or vertical and lateral transport are likely to play an important role in the removal of organic materials from the system.

Atomic force microscope based on vertical silicon probes

NASA Astrophysics Data System (ADS)

Walter, Benjamin; Mairiaux, Estelle; Faucher, Marc

2017-06-01

A family of silicon micro-sensors for Atomic Force Microscope (AFM) is presented that allows to operate with integrated transducers from medium to high frequencies together with moderate stiffness constants. The sensors are based on Micro-Electro-Mechanical-Systems technology. The vertical design specifically enables a long tip to oscillate perpendicularly to the surface to be imaged. The tip is part of a resonator including quasi-flexural composite beams, and symmetrical transducers that can be used as piezoresistive detector and/or electro-thermal actuator. Two vertical probes (Vprobes) were operated up to 4.3 MHz with stiffness constants 150 N/m to 500 N/m and the capability to oscillate from 10 pm to 90 nm. AFM images of several samples both in amplitude modulation (tapping-mode) and in frequency modulation were obtained.

Application of a novel large-volume injection method using a stomach-shaped inlet liner in capillary gas chromatographic trace analysis of dioxins in human milk and plasma.

PubMed

Saito, Koichi; Ohmura, Atsuko; Takekuma, Mikiko; Sasano, Ryoichi; Matsuki, Yasuhiko; Nakazawa, Hiroyuki

2007-06-01

A newly developed large-volume injection (LVI) technique that employs a unique stomach-shaped inlet liner (SSIL) inside of a programmable temperature vaporizer was used for the determination of trace amounts of dioxins in human milk and plasma. The initial temperature and the initial dwelling time of the inlet and the kind of solvent used were found to be critical in determining the analytical sensitivity of dioxins due to the loss of these relatively volatile compounds during solvent vaporization. Human milk and plasma were purified and fractionated by pre-packed multi-layered silica-gel chromatography and activated carbon silica-gel column chromatography. A 20-microL aliquot of the fraction collected from the chromatography with toluene was directly applied to the LVI system in high-resolution gas chromatography/high-resolution mass spectrometry. Excellent correlation (r > 0.97) between the values obtained by the LVI method using the SSIL device and those by the conventional regular-volume splitless injection method was obtained for PCDDs, PCDFs and non-ortho PCBs in human milk and plasma samples.

Micro solid phase spectrophotometry in a sequential injection lab-on-valve platform for cadmium, zinc, and copper determination in freshwaters.

PubMed

Santos, Inês C; Mesquita, Raquel B R; Rangel, António O S S

2015-09-03

This work describes the development of a solid phase spectrophotometry method in a μSI-LOV system for cadmium, zinc, and copper determination in freshwaters. NTA (Nitrilotriacetic acid) beads with 60-160 μm diameter were packed in the flow cell of the LOV for a μSPE column of 1 cm length. The spectrophotometric determination is based on the colourimetric reaction between dithizone and the target metals, previously retained on NTA resin. The absorbance of the coloured product formed is measured, at 550 nm, on the surface of the NTA resin beads in a solid phase spectrophotometry approach. The developed method presented preconcentration factors in the range of 11-21 for the metal ions. A LOD of 0.23 μg L(-1) for cadmium, 2.39 μg L(-1) for zinc, and 0.11 μg L(-1) for copper and a sampling rate of 12, 13, and 15 h(-1) for cadmium, zinc, and copper were obtained, respectively. The proposed method was successfully applied to freshwater samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Effects of pressure angle and tip relief on the life of speed increasing gearbox: a case study.

PubMed

Shanmugasundaram, Sankar; Kumaresan, Manivarma; Muthusamy, Nataraj

2014-01-01

This paper examines failure of helical gear in speed increasing gearbox used in the wind turbine generator (WTG). In addition, an attempt has been made to get suitable gear micro-geometry such as pressure angle and tip relief to minimize the gear failure in the wind turbines. As the gear trains in the wind turbine gearbox is prearranged with higher speed ratio and the gearboxes experience shock load due to atmospheric turbulence, gust wind speed, non-synchronization of pitching, frequent grid drops and failure of braking, the gear failure occurs either in the intermediate or high speed stage pinion. KISS soft gear calculation software was used to determine the gear specifications and analysis is carried out in ANSYS software version.11.0 for the existing and the proposed gear to evaluate the performance of bending stress tooth deflection and stiffness. The main objective of this research study is to propose suitable gear micro-geometry that is tip relief and pressure angle blend for increasing tooth strength of the helical gear used in the wind turbine for trouble free operation.

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.

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

Göring, Gerald; Dietrich, Philipp-Immanuel; Blaicher, Matthias

3D direct laser writing based on two-photon polymerization is considered as a tool to fabricate tailored probes for atomic force microscopy. Tips with radii of 25 nm and arbitrary shape are attached to conventionally shaped micro-machined cantilevers. Long-term scanning measurements reveal low wear rates and demonstrate the reliability of such tips. Furthermore, we show that the resonance spectrum of the probe can be tuned for multi-frequency applications by adding rebar structures to the cantilever.

Development of a dynamic pressure calibration technique

NASA Technical Reports Server (NTRS)

Vezzetti, C. F.; Hilten, J. S.; Lederer, P. S.

1975-01-01

The report deals with work continuing on the development of a method of producing sinusoidally varying pressures of at least 34 kPa zero-to-peak with amplitude variations within plus or minus 5% up to 2 kHz for the dynamic calibration of pressure transducers. Sinusoidally varying pressures of 34 kPa zero-to-peak were produced between 40 Hz and 750 Hz by vibrating a 10-cm column of a dimethyl siloxane liquid at 36gn zero-to-peak. Damping of the liquid column was accomplished by packing the fixture tube with a number of smaller diameter tubes.

Simple, specific analysis of organophosphorus and carbamate pesticides in sediments using column extraction and gas chromatography

USGS Publications Warehouse

Belisle, A.A.; Swineford, D.M.

1988-01-01

A simple, specific procedure was developed for the analysis of organophosphorus and carbamate pesticides in sediment. The wet soil was mixed with anhydrous sodium sulfate to bind water and the residues were column extracted in acetone:methylene chloride (1:l,v/v). Coextracted water was removed by additional sodium sulfate packed below the sample mixture. The eluate was concentrated and analyzed directly by capillary gas chromatography using phosphorus and nitrogen specific detectors. Recoveries averaged 93 % for sediments extracted shortly after spiking, but decreased significantly as the samples aged.

Chromatographic evaluation of self-immobilized stationary phases for reversed-phase liquid chromatography.

PubMed

Bottoli, Carla B G; Collins, Kenneth E; Collins, Carol H

2003-02-14

The preparation of stationary phases for HPLC using polymers deposited on silica usually includes an immobilization step involving cross-linking by free radicals induced by ionizing radiation or by other radical initiators. The present paper reports changes which occur at ambient temperature in the character of poly(methyloctylsiloxane) deposited on porous silica particles as a function of the time interval between particle loading and column packing. Column performance and retention factors increase with time and these changes are attributed to rearrangement (self-assembly) which result in "self-immobilization" of the polymer molecules on the silica surface.

Variable-Resistivity Material For Memory Circuits

NASA Technical Reports Server (NTRS)

Nagasubramanian, Ganesan; Distefano, Salvador; Moacanin, Jovan

1989-01-01

Nonvolatile memory elements packed densely. Electrically-erasable, programmable, read-only memory matrices made with newly-synthesized organic material of variable electrical resistivity. Material, polypyrrole doped with tetracyanoquinhydrone (TCNQ), changes reversibly between insulating or higher-resistivity state and conducting or low-resistivity state. Thin film of conductive polymer separates layer of row conductors from layer of column conductors. Resistivity of film at each intersection and, therefore, resistance of memory element defined by row and column, increased or decreased by application of suitable switching voltage. Matrix circuits made with this material useful for experiments in associative electronic memories based on models of neural networks.

Chromatographic hydrogen isotope separation

DOEpatents

Aldridge, F.T.

Intermetallic compounds with the CaCu/sub 5/ type of crystal structure, particularly LaNiCo/sub 4/ and CaNi/sub 5/, exhibit high separation factors and fast equilibrium times and therefore are useful for packing a chromatographic hydrogen isotope separation column. The addition of an inert metal to dilute the hydride improves performance of the column. A large scale multi-stage chromatographic separation process run as a secondary process off a hydrogen feedstream from an industrial plant which uses large volumes of hydrogen cn produce large quantities of heavy water at an effective cost for use in heavy water reactors.

Operation, Maintenance and Performance Evaluation of the Potomac Estuary Experimental Water Treatment Plant. Appendix. Volume 2.

DTIC Science & Technology

1983-09-01

1.2 . 7*96.69 Ŕ.40 2.43 1.16 1.7 T*100 96.40 S.45 6.22 1.4 701100049 940 .36 4.11 1.0 MKWTP Finished Water (See Table H4-20 for Results) Nu mbrs ...carbon submerged in water when loading. This provides for a uniformly packed column. c. Continue adding carbon and column sections until the desired...difficult to evaluate. Because influent to the aeration basin is submerged at an underflow baffle, it was necessary to inject the tracer at the upstream

Influence of ice and snow covers on the UV exposure of terrestrial microbial communities: dosimetric studies.

PubMed

Cockell, Charles S; Rettberg, Petra; Horneck, Gerda; Wynn-Williams, David D; Scherer, Kerstin; Gugg-Helminger, Anton

2002-08-01

Bacillus subtilis spore biological dosimeters and electronic dosimeters were used to investigate the exposure of terrestrial microbial communities in micro-habitats covered by snow and ice in Antarctica. The melting of snow covers of between 5- and 15-cm thickness, depending on age and heterogeneity, could increase B. subtilis spore inactivation by up to an order of magnitude, a relative increase twice that caused by a 50% ozone depletion. Within the snow-pack at depths of less than approximately 3 cm snow algae could receive two to three times the DNA-weighted irradiance they would receive on bare ground. At the edge of the snow-pack, warming of low albedo soils resulted in the formation of overhangs that provided transient UV protection to thawed and growing microbial communities on the soils underneath. In shallow aquatic habitats, thin layers of heterogeneous ice of a few millimetres thickness were found to reduce DNA-weighted irradiances by up to 55% compared to full-sky values with equivalent DNA-weighted diffuse attenuation coefficients (K(DNA)) of >200 m(-1). A 2-mm snow-encrusted ice cover on a pond was equivalent to 10 cm of ice on a perennially ice covered lake. Ice covers also had the effect of stabilizing the UV exposure, which was often subject to rapid variations of up to 33% of the mean value caused by wind-rippling of the water surface. These data show that changing ice and snow covers cause relative changes in microbial UV exposure at least as great as those caused by changing ozone column abundance. Copyright 2002 Elsevier Science B.V.

Learning Skills of Peace through Every Day Conflicts: Practical Activities and Resources for Families, Teachers and Other Caregivers. [Loose-Leaf Pages and Pack of Cards].

ERIC Educational Resources Information Center

Ohio Commission on Dispute Resolution and Conflict Management, Columbus.

Noting that the conflicts arising daily for young children provide an opportunity for adults to model and teach skills for handling conflict peacefully, this guide provides tips for preventing unnecessary conflict, offers "first aid" for conflict moments, and provides resources for addressing common situations that can cause conflict.…

Multiscale approach to micro/macro fatigue crack growth in 2024-T3 aluminum panel

NASA Astrophysics Data System (ADS)

Sih, G. C.

2014-01-01

When two contacting solid surfaces are tightly closed and invisible to the naked eye, the discontinuity is said to be microscopic regardless of whether its length is short or long. By this definition, it is not sufficient to distinguish the difference between a micro- and macro-crack by using the length parameter. Microcracks in high strength metal alloys have been known to be several centimeters or longer. Considered in this work is a dual scale fatigue crack growth model where the main crack can be micro or macro but there prevails an inherent microscopic tip region that is damaged depending on the irregularities of the microstructure. This region is referred to as the "micro-tip" and can be simulated by a sharp wedge with different angles in addition to mixed boundary conditions. The combination is sufficient to model microscopic entities in the form of voids, inclusions, precipitations, interfaces, in addition to subgrain imperfections, or cluster of dislocations. This is accomplished by using the method of "singularity representation" such that closed form asymptotic solutions can be obtained for the development of fatigue crack growth rate relations with three parameters. They include: (1) the crack surface tightness σ* represented by σ o/ σ ∞ = 0.3-0.5 for short cracks in region I, and 0.1-0.2 for long cracks in region II, (2) the micro/macro material properties reflected by the shear modulus ratio µ* (=µmicro/µmacro varying between 2 and 5) and (3) the most sensitive parameter d* being the micro-tip characteristic length d* (= d/ d o) whose magnitude decreases in the direction of region I→II. The existing fatigue crack growth data for 2024-T3 and 7075-T6 aluminum sheets are used to reinterpret the two-parameter d a/d N= C(Δ K) n relation where Δ K has now been re-derived for a microcrack with surfaces tightly in contact. The contact force will depend on the mean stress σm or mean stress ratio R as the primary parameter and on the stress amplitude σ a as the secondary parameter.

2,11-Dibromo-5,8-dibut­yl[4]helicene

PubMed Central

Isobe, Hiroyuki; Matsuno, Taisuke; Hitosugi, Shunpei; Nakanishi, Waka

2012-01-01

A racemic mixture of the title compound, C26H26Br2, a brominated [4]helicene, crystallizes, forming columns of stacked mol­ecules. There are two crystallographically unique mol­ecules in the asymmetric unit, both with the same helical handedness. As is typical with helicene congeners, the unique mol­ecules show short inter­atomic contacts between H atoms at the fjord region, with H⋯H distances of 1.87 and 1.94 Å. Mol­ecules with the same helical handedness segregate in the crystal packing, forming homochiral columns. The stacked mol­ecules are piled in a column with alternate orientations. The shortest C⋯C distance in the stacked mol­ecules is 3.306 (4) Å. PMID:22606172

Retention behavior of neutral solutes in pressurized flow-driven capillary electrochromatography using an ODS column.

PubMed

Nakagawa, Hiroyuki; Kitagawa, Shinya; Araki, Shuki; Ohtani, Hajime

2006-02-01

Several alkyl benzenes are separated by pressurized flow-driven capillary electrochromatography using a temperature-controlled capillary column packed with octadecyl siloxane-modified silica gel, and the effect of applied voltage on the retention is investigated. The van't Hoff plot shows good linearity at the column temperature between 305 and 330 K under applications from -6 to +6 kV. The applied voltage causes a relatively large variation in the enthalpy and the entropy of transfer of the solute from the mobile phase to the stationary phase (> 20%). However, the direction of variation in the enthalpy is almost opposite to that in the entropy, both of which might compensate each other. Therefore, the retention factor is not significantly varied (< 4%) by the application of voltage.

Gas chromatographic determination of fumigant residues in stored grains, using isooctane partitioning and dual column packings.

PubMed

Daft, J L

1983-03-01

A gas chromatographic (GC) procedure for determining fumigants in grains was developed. Fumigants were leached from grain samples with the official AOAC method using acetone-water (5 + 1). They were then partitioned from the leachate with isooctane, yielding a dry, stable extract that was analyzed by GC. Fortified sample recoveries ranged from 90 to 100%. Two GC columns were used, 20% OV-101 and 20% OV-225/20% OV-17 (2 + 1). These columns gave dissimilar retention profiles and baseline resolution for the 7 fumigants investigated: chloroform, ethylene dichloride, carbon tetrachloride, trichloroethylene, chloropicrin, ethylene dibromide, and tetrachloroethylene. Further tests showed that grain samples could be screened for fumigant residues by direct injection of the acetone-water leachates obtained using the AOAC method.

Facilitated transport of copper with hydroxyapatite nanoparticles in saturated sand

USDA-ARS?s Scientific Manuscript database

Saturated packed column experiments were conducted to investigate the facilitated transport of Cu with hydroxyapatite nanoparticles (nHAP) at different pore water velocities (0.22-2.2 cm min–1), solution pH (6.2-9.0), and fraction of Fe oxide coating on grain surfaces (', 0-0.36). The facilitated tr...

Stability and transport of graphene oxide nanoparticles in groundwater and surface water

USDA-ARS?s Scientific Manuscript database

A transport study investigating the effects of natural organic matter (NOM) in the presence of monovalent (KCl) and divalent (CaCl2) salts was performed in a packed bed column. The electrophoretic mobility (EPM) and effective diameter of the graphene oxide nanoparticles (GONPs) were measured as a fu...

Temperature dependency of virus and nanoparticle transport and retention in saturated porous media

USDA-ARS?s Scientific Manuscript database

The influence of temperature (4 and 20 °C) on virus and nanoparticle attachment in columns packed with quartz sand was studied under various physiochemical conditions. Fitted values of the attachment rate coefficient (katt) and the solid fraction that contributed to attachment (Sf) were found to be...

Use of biochar amendments for removing bacteria from simulated tile-drainage waters

USDA-ARS?s Scientific Manuscript database

The addition of biochar has been shown to increase bacterial removal rates by several orders of magnitude in sand-packed columns, suggesting that biochar may be a suitable amendment for use in end-of-tile filter systems to remove indicator and pathogenic microorganisms in tile-drainage waters. Addit...

Estimation of interfacial area in a packed cross-flow cascade with distillation of ethanol-water, methanol-water, and hexane-heptane

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

Velaga, A.

1986-01-01

Packed cross-flow internals consisting of four and ten stages including the samplers for liquid and vapor were fabricated to fit into the existing distillation column. Experiments were conducted using methanol-water, ethanol-water and hexane-heptane binary mixtures. The experimental data were collected for compositions of inlet and exist streams of cross-flow stages. The overall gas phase height transfer units (H/sub og/) were estimated using the experimental data. H/sub og/ values were compared to those of counter current conditions. The individual mass transfer coefficients in the liquid and vapor phases were estimated using the collected experimental data for degree of separation, flow ratesmore » and physical properties of the binary system used. The physical properties were estimated at an average temperature of the specific cross-flow stage. The mass transfer coefficients were evaluated using three different correlations proposed by Shulman. Onda and Hayashi respectively. The interfacial areas were estimated using the evaluated mass transfer coefficients and the experimental data at each stage of the column for different runs and compared.« less

Successive pretreatment and enzymatic saccharification of sugarcane bagasse in a packed bed flow-through column reactor aiming to support biorefineries.

PubMed

Terán-Hilares, R; Reséndiz, A L; Martínez, R T; Silva, S S; Santos, J C

2016-03-01

A packed bed flow-through column reactor (PBFTCR) was used for pretreatment and subsequent enzymatic hydrolysis of sugarcane bagasse (SCB). Alkaline pretreatment was performed at 70 °C for 4h with fresh 0.3M NaOH solution or with liquor recycled from a previous pretreatment batch. Scheffersomyces stipitis NRRL-Y7124 was used for fermentation of sugars released after enzymatic hydrolysis (20 FPU g(-1) of dry SCB). The highest results for lignin removal were 61% and 52%, respectively, observed when using fresh NaOH or the first reuse of the liquor. About 50% of cellulosic and 57% of hemicellulosic fractions of pretreated SCBs were enzymatically hydrolyzed and the maximum ethanol production was 23.4 g L(-1) (ethanol yield of 0.4 gp gs(-1)), with near complete consumption of both pentoses and hexoses present in the hydrolysate during the fermentation. PBFTCR as a new alternative for SCB-biorefineries is presented, mainly considering its simple configuration and efficiency for operating with a high solid:liquid ratio. Copyright © 2015 Elsevier Ltd. All rights reserved.

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

PubMed

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

2010-07-16

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

Shape memory alloy/shape memory polymer tools

DOEpatents

Seward, Kirk P.; Krulevitch, Peter A.

2005-03-29

Micro-electromechanical tools for minimally invasive techniques including microsurgery. These tools utilize composite shape memory alloy (SMA), shape memory polymer (SMP) and combinations of SMA and SMP to produce catheter distal tips, actuators, etc., which are bistable. Applications for these structures include: 1) a method for reversible fine positioning of a catheter tip, 2) a method for reversible fine positioning of tools or therapeutic catheters by a guide catheter, 3) a method for bending articulation through the body's vasculature, 4) methods for controlled stent delivery, deployment, and repositioning, and 5) catheters with variable modulus, with vibration mode, with inchworm capability, and with articulated tips. These actuators and catheter tips are bistable and are opportune for in vivo usage because the materials are biocompatible and convenient for intravascular use as well as other minimal by invasive techniques.

Dynamic response of tapered optical multimode fiber coated with carbon nanotubes for ethanol sensing application.

PubMed

Shabaneh, Arafat; Girei, Saad; Arasu, Punitha; Mahdi, Mohd; Rashid, Suraya; Paiman, Suriati; Yaacob, Mohd

2015-05-04

Ethanol is a highly combustible chemical universally designed for biomedical applications. In this paper, optical sensing performance of tapered multimode fiber tip coated with carbon nanotube (CNT) thin film towards aqueous ethanol with different concentrations is investigated. The tapered optical multimode fiber tip is coated with CNT using drop-casting technique and is annealed at 70 °C to enhance the binding of the nanomaterial to the silica fiber tip. The optical fiber tip and the CNT sensing layer are micro-characterized using FESEM and Raman spectroscopy techniques. When the developed sensor was exposed to different concentrations of ethanol (5% to 80%), the sensor reflectance reduced proportionally. The developed sensors showed high sensitivity, repeatability and fast responses (<55 s) towards ethanol.