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

DOEpatents

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

1994-01-04

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

Design procedures for fiber composite structural components - Rods, beams, and beam columns

NASA Technical Reports Server (NTRS)

Chamis, C. C.

1984-01-01

Step by step procedures are described which are used to design structural components (rods, columns, and beam columns) subjected to steady state mechanical loads and hydrothermal environments. Illustrative examples are presented for structural components designed for static tensile and compressive loads, and fatigue as well as for moisture and temperature effects. Each example is set up as a sample design illustrating the detailed steps that are used to design similar components.

The effect of column purification on cDNA indirect labelling for microarrays

PubMed Central

Molas, M Lia; Kiss, John Z

2007-01-01

Background The success of the microarray reproducibility is dependent upon the performance of standardized procedures. Since the introduction of microarray technology for the analysis of global gene expression, reproducibility of results among different laboratories has been a major problem. Two of the main contributors to this variability are the use of different microarray platforms and different laboratory practices. In this paper, we address the latter question in terms of how variation in one of the steps of a labelling procedure affects the cDNA product prior to microarray hybridization. Results We used a standard procedure to label cDNA for microarray hybridization and employed different types of column chromatography for cDNA purification. After purifying labelled cDNA, we used the Agilent 2100 Bioanalyzer and agarose gel electrophoresis to assess the quality of the labelled cDNA before its hybridization onto a microarray platform. There were major differences in the cDNA profile (i.e. cDNA fragment lengths and abundance) as a result of using four different columns for purification. In addition, different columns have different efficiencies to remove rRNA contamination. This study indicates that the appropriate column to use in this type of protocol has to be experimentally determined. Finally, we present new evidence establishing the importance of testing the method of purification used during an indirect labelling procedure. Our results confirm the importance of assessing the quality of the sample in the labelling procedure prior to hybridization onto a microarray platform. Conclusion Standardization of column purification systems to be used in labelling procedures will improve the reproducibility of microarray results among different laboratories. In addition, implementation of a quality control check point of the labelled samples prior to microarray hybridization will prevent hybridizing a poor quality sample to expensive micorarrays. PMID:17597522

The effect of column purification on cDNA indirect labelling for microarrays.

PubMed

Molas, M Lia; Kiss, John Z

2007-06-27

The success of the microarray reproducibility is dependent upon the performance of standardized procedures. Since the introduction of microarray technology for the analysis of global gene expression, reproducibility of results among different laboratories has been a major problem. Two of the main contributors to this variability are the use of different microarray platforms and different laboratory practices. In this paper, we address the latter question in terms of how variation in one of the steps of a labelling procedure affects the cDNA product prior to microarray hybridization. We used a standard procedure to label cDNA for microarray hybridization and employed different types of column chromatography for cDNA purification. After purifying labelled cDNA, we used the Agilent 2100 Bioanalyzer and agarose gel electrophoresis to assess the quality of the labelled cDNA before its hybridization onto a microarray platform. There were major differences in the cDNA profile (i.e. cDNA fragment lengths and abundance) as a result of using four different columns for purification. In addition, different columns have different efficiencies to remove rRNA contamination. This study indicates that the appropriate column to use in this type of protocol has to be experimentally determined. Finally, we present new evidence establishing the importance of testing the method of purification used during an indirect labelling procedure. Our results confirm the importance of assessing the quality of the sample in the labelling procedure prior to hybridization onto a microarray platform. Standardization of column purification systems to be used in labelling procedures will improve the reproducibility of microarray results among different laboratories. In addition, implementation of a quality control check point of the labelled samples prior to microarray hybridization will prevent hybridizing a poor quality sample to expensive micorarrays.

Contents of Structures to Resist the Effects of Accidental Explosions (TM 5-1300, NAVFAC P-397, AFM 22)

DTIC Science & Technology

1986-08-01

walls of various support conditions, as well as design procedures and deflection criteria for beams and both interior and exterior columns . The... columns of shear wall type structures are generally designed as beams . 159 The structural design for brittle mode response contains most of the data...flat slabs, beams , columns and foundations. 1OUNE V - STUCTRMAL STEEL DESIME This volume covers detailed procedures and design techniques for the blast

Virus elimination during the recycling of chromatographic columns used during the manufacture of coagulation factors.

PubMed

Roberts, Peter L

2014-07-01

Various chromatographic procedures are used during the purification and manufacture of plasma products such as coagulation factors. These steps contribute to the overall safety of such products by removing potential virus contamination. Virus removal by two affinity chromatography procedures, i.e. monoclonal antibody chromatography and metal chelate chromatography (immobilised metal ion affinity chromatography), used during the manufacture of the high purity factor VIII (Replenate®) and factor IX (Replenine®-VF), respectively, has been investigated. In addition, as these columns are recycled after use, the effectiveness of the sanitisation procedures for preventing possible cross-contamination, has also been investigated. Both chromatographic steps proved effective for eliminating a range of model enveloped and non-enveloped viruses by 4 to >6 and 5 to >8 log for the monoclonal and metal chelate columns, respectively. The effectiveness of the relatively mild column sanitisation conditions used, i.e. ethanol for factor IX and acetic acid for factor VIII, was confirmed using non-spiked column runs. The chemicals used contributed to virus elimination by inactivation and/or by physical removal of the virus. In summary, these studies demonstrate that potential virus contamination between chromatographic runs can be prevented when an effective column recycling and sanitisation procedure is included. Copyright © 2014 The International Alliance for Biological Standardization. Published by Elsevier Ltd. All rights reserved.

Forward marching procedure for separated boundary-layer flows

NASA Technical Reports Server (NTRS)

Carter, J. E.; Wornom, S. F.

1975-01-01

A forward-marching procedure for separated boundary-layer flows which permits the rapid and accurate solution of flows of limited extent is presented. The streamwise convection of vorticity in the reversed flow region is neglected, and this approximation is incorporated into a previously developed (Carter, 1974) inverse boundary-layer procedure. The equations are solved by the Crank-Nicolson finite-difference scheme in which column iteration is carried out at each streamwise station. Instabilities encountered in the column iterations are removed by introducing timelike terms in the finite-difference equations. This provides both unconditional diagonal dominance and a column iterative scheme, found to be stable using the von Neumann stability analysis.

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

PubMed

Hayes, J D; Malik, A

1997-07-18

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

Decision making regarding Smith-Petersen vs. pedicle subtraction osteotomy vs. vertebral column resection for spinal deformity.

PubMed

Bridwell, Keith H

2006-09-01

Author experience and literature review. To investigate and discuss decision-making on when to perform a Smith-Petersen osteotomy as opposed to a pedicle subtraction procedure and/or a vertebral column resection. Articles have been published regarding Smith-Petersen osteotomies, pedicle subtraction procedures, and vertebral column resections. Expectations and complications have been reviewed. However, decision-making regarding which of the 3 procedures is most useful for a particular spinal deformity case is not clearly investigated. Discussed in this manuscript is the author's experience and the literature regarding the operative options for a fixed coronal or sagittal deformity. There are roles for Smith-Petersen osteotomy, pedicle subtraction, and vertebral column resection. Each has specific applications and potential complications. As the magnitude of resection increases, the ability to correct deformity improves, but also the risk of complication increases. Therein, an understanding of potential applications and complications is helpful.

Soil Overconsolidation Changes Caused by Dynamic Replacement

NASA Astrophysics Data System (ADS)

Piotr, Kanty; Sławomir, Kwiecień; Jerzy, Sękowski

2017-10-01

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

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

EPA Science Inventory

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

Concentration of perrhenate and pertechnetate solutions

DOEpatents

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

1998-03-17

A method is described for preparing a concentrated solution of a carrier-free radioisotope which includes the steps of: (a) providing a generator column loaded with a composition containing a parent radioisotope; (b) eluting the generator column with an eluent solution which includes a salt of a weak acid to elute a target daughter radioisotope from the generator column in a first eluate; (c) eluting a cation-exchange column with the first eluate to exchange cations of the salt for hydrogen ions and to elute the target daughter radioisotope and a weak acid in a second eluate; (d) eluting an anion-exchange column with the second eluate to trap and concentrate the target daughter radioisotope and to elute the weak acid solution therefrom; and (e) eluting the concentrated target daughter radioisotope from the anion-exchange column with a saline solution. 1 fig.

Concentration of perrhenate and pertechnetate solutions

DOEpatents

Knapp, Furn F.; Beets, Arnold L.; Mirzadeh, Saed; Guhlke, Stefan

1998-01-01

A method of preparing a concentrated solution of a carrier-free radioisotope which includes the steps of: a. providing a generator column loaded with a composition containing a parent radioisotope; b. eluting the generator column with an eluent solution which includes a salt of a weak acid to elute a target daughter radioisotope from the generator column in a first eluate. c. eluting a cation-exchange column with the first eluate to exchange cations of the salt for hydrogen ions and to elute the target daughter radioisotope and a weak acid in a second eluate; d. eluting an anion-exchange column with the second eluate to trap and concentrate the target daughter radioisotope and to elute the weak acid solution therefrom; and e. eluting the concentrated target daughter radioisotope from the anion-exchange column with a saline solution.

Comparison between Procedures using Sodium Dodecyl Sulfate for Shotgun Proteomic Analyses of Complex Samples

PubMed Central

Bereman, Michael S.; Egertson, Jarrett D.; MacCoss, Michael J.

2012-01-01

Filter aided sample preparation (FASP) and a new sample preparation method using a modified commercial SDS removal spin column are quantitatively compared in terms of their performance for shotgun proteomic experiments in three complex proteomic samples: a Saccharomyces cerevisiae lysate (insoluble fraction), a Caenorhabditis elegans lysate (soluble fraction), and a human embryonic kidney cell line (HEK293T). The characteristics and total number of peptides and proteins identified are compared between the two procedures. The SDS spin column procedure affords a conservative 4-fold improvement in throughput, is more reproducible, less expensive (i.e., requires less materials), and identifies between 30–107% more peptides at a q≤0.01, than the FASP procedure. The peptides identified by SDS spin column are more hydrophobic than species identified by the FASP procedure as indicated by the distribution of GRAVY scores. Ultimately, these improvements correlate to as great as a 50% increase in protein identifications with 2 or more peptides. PMID:21656683

Technetium-99m generator system

DOEpatents

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

1998-01-01

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

Technetium-99m generator system

DOEpatents

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

1998-06-30

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

Evaluation of environmental compatibility of EAFD using different leaching standards.

PubMed

Sebag, M G; Korzenowski, C; Bernardes, A M; Vilela, A C

2009-07-30

A study on laboratory scale to evaluate the environmental compatibility of electric arc furnace dust (EAFD) is reported in this article. EAFD, a waste by-product of the steel-making process, was generated on a steel plant located in Brazil. Different leaching tests, NBR10005 (Brazilian), AFNORX31-210 (French), JST-13 (Japanese), DIN38414-S4 (German), TCLP (American), and NEN 7343 (Netherland) were conducted. These leaching procedures are batch tests and are columns conducted in a way that an equilibrium condition should be achieved. The pH of the medium showed a crucial parameter governing the release of metals from the solid phase into solution. As the pH of the medium varies with the leachant used, this determines the dissolution of the elements. Zn, Pb, Mn, Cd, and Cu presented high leachability at NBR10005 procedures (acid pH). Except Pb and Cr, the leachability of all others metals in leaching tests with alkaline pH decreases with the increase of the pH. NBR10005 classifies the EAFD as a hazardous waste due to high concentration of Pb and Cd in leachate. The column tests are presented in the following order of leaching: Pb>Cr>Zn>Mn>Cu>Cd.

Stability of the neurotensin receptor NTS1 free in detergent solution and immobilized to affinity resin.

PubMed

White, Jim F; Grisshammer, Reinhard

2010-09-07

Purification of recombinant membrane receptors is commonly achieved by use of an affinity tag followed by an additional chromatography step if required. This second step may exploit specific receptor properties such as ligand binding. However, the effects of multiple purification steps on protein yield and integrity are often poorly documented. We have previously reported a robust two-step purification procedure for the recombinant rat neurotensin receptor NTS1 to give milligram quantities of functional receptor protein. First, histidine-tagged receptors are enriched by immobilized metal affinity chromatography using Ni-NTA resin. Second, remaining contaminants in the Ni-NTA column eluate are removed by use of a subsequent neurotensin column yielding pure NTS1. Whilst the neurotensin column eluate contained functional receptor protein, we observed in the neurotensin column flow-through misfolded NTS1. To investigate the origin of the misfolded receptors, we estimated the amount of functional and misfolded NTS1 at each purification step by radio-ligand binding, densitometry of Coomassie stained SDS-gels, and protein content determination. First, we observed that correctly folded NTS1 suffers damage by exposure to detergent and various buffer compositions as seen by the loss of [(3)H]neurotensin binding over time. Second, exposure to the neurotensin affinity resin generated additional misfolded receptor protein. Our data point towards two ways by which misfolded NTS1 may be generated: Damage by exposure to buffer components and by close contact of the receptor to the neurotensin affinity resin. Because NTS1 in detergent solution is stabilized by neurotensin, we speculate that the occurrence of aggregated receptor after contact with the neurotensin resin is the consequence of perturbations in the detergent belt surrounding the NTS1 transmembrane core. Both effects reduce the yield of functional receptor protein.

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.

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

PubMed

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

2017-08-01

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

Colorful Column Chromatography: A Classroom Demonstration of a Three-Component Separation

ERIC Educational Resources Information Center

Heumann, Lars V.

2008-01-01

A classroom demonstration detailing the procedure for the separation of a ternary mixture consisting of intensely colored compounds using silica gel column chromatography is described. The audience can follow the compounds during their passage through the column as individual, colored bands while learning about different tools and techniques used…

Isotopic generator for bismuth-212 and lead-212 based on radium

DOEpatents

Hines, J.J.; Atcher, R.W.; Friedman, A.M.

1985-01-30

Disclosed are method and apparatus for providing radionuclides of bismuth-212 and lead-212. Thorium-228 and carrier solution starting material is input to a radiologically contained portion of an isotopic generator system, and radium-224 is separated from thorium-228 which is retained by a strongly basic anion exchange column. The separated radium-224 is transferred to an accessible, strongly acidic cationic exchange column. The cationic column retains the radium-224, and natural radioactive decay generates bismuth-212 and lead-212. The cationic exchange column can also be separated from the contained portion of the system and utilized without the extraordinary safety measures necessary in the contained portion. Furthermore, the cationic exchange column provides over a relatively long time period the short lived lead-212 and bismuth-212 radionuclides which are useful for a variety of medical therapies.

Isotopic generator for bismuth-212 and lead-212 from radium

DOEpatents

Atcher, Robert W.; Friedman, Arnold M.; Hines, John

1987-01-01

A method and apparatus for providing radionuclides of bismuth-212 and lead-212. Thorium-228 and carrier solution starting material is input to a radiologically contained portion of an isotopic generator system, and radium-224 is separated from thorium-228 which is retained by a strongly basic anion exchange column. The separated radium-224 is transferred to an accessible, strongly acidic cationic exchange column. The cationic column retains the radium-224, and natural radioactive decay generates bismuth-212 and lead-212. The cationic exchange column can also be separated from the contained portion of the system and utilized without the extraordinary safety measures necessary in the contained portion. Furthermore, the cationic exchange column provides over a relatively long time period the short lived lead-212 and bismuth-212 radionuclides which are useful for a variety of medical therapies.

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

PubMed Central

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

2017-01-01

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

Simultaneous determination of quinolones in fish by liquid chromatography coupled with fluorescence detection: comparison of sub-2 microm particles and conventional C18 columns.

PubMed

Zhang, Hong; Chen, Si; Lu, Yanbin; Dai, Zhiyuan

2010-07-01

A simple and effective multi-residue analysis method is presented for the extraction and determination of eleven quinolones (pipemidic acid, enoxacin, norfloxacin, ciprofloxacin, lomefloxacin, enrofloxacin, gatifloxacin, difloxacin, oxolinic acid, nalidixic acid and flumequine) in fish tissues. In this study, multi-residue separations on four columns packed with 5 microm or sub-2 microm particles were simultaneously developed for the purpose of comparison. Various gradients were optimized and best resolutions were achieved on each column. A short and sub-2 microm particle-sized HPLC column was chosen for its advantages in analysis time and column performance. Additionally, considering the matrix effect of the complex crude fish tissue, an effective extraction protocol was also established for sample pre-treatment procedure. Good recoveries (71-98%) were obtained from samples fortified with a mix of eleven quinolones at three levels, with satisfactory relative standard deviations and limits of detection. As a result, the sub-2 microm HPLC column and proposed analytical procedures have been evaluated and applied to the analysis of different fish tissues. Detectable residues were observed in 8 of 30 samples, at concentrations ranging from 4.74 to 23.27 microg/kg.

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

PubMed

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

1999-10-08

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

Solution methods for one-dimensional viscoelastic problems

NASA Technical Reports Server (NTRS)

Stubstad, John M.; Simitses, George J.

1987-01-01

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

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

NASA Astrophysics Data System (ADS)

Jivkov, Venelin S.; Zahariev, Evtim V.

2016-12-01

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

Modeling molecular hydrogen emission in M dwarf exoplanetary systems

NASA Astrophysics Data System (ADS)

Evonosky, William; France, Kevin; Kruczek, Nick E.; Youngblood, Allison; Measurements of the Ultraviolet Spectral Characteristics of Low-mass Exoplanet host Stars (MUSCLES)

2017-01-01

Exoplanets orbiting low-mass stars are prime candidates for atmospheric characterization due to their astronomical abundance and short orbital periods. These planets orbit stars that are often more active than main sequence solar-type stars. They are exposed to differing levels of ultraviolet radiation which can cause traditional “biosignature” gases to be generated abiotically, potentially causing false-positive identifications of life. We modeled the recently discovered molecular hydrogen emission in the ultraviolet spectra (1350 - 1650 Å) as arising from the stellar surface, excited by radiation generated in the upper chromosphere. The model was compared with observed hydrogen emission from the “Measurements of the Ultraviolet Spectral Characteristics of Low-mass Exoplanet host Stars” (MUSCLES) survey by conducting a grid search and implementing a chi-squared minimization routine. We considered only progressions from the [1, 4] and [1, 7] first excited electronic levels. Our modeling procedure varied the atomic hydrogen column density (in the chromosphere) as well as the photospheric molecular hydrogen column density and temperature. The model required as an input a reconstructed intrinsic Lyman α profile which served as the pumping radiation for the molecular hydrogen. We found that an atomic hydrogen column density of log10N(H I) = 14.13 ± 0.16 cm-2 represents a breaking point above which there is not enough Lyman α flux available to excite a significant molecular hydrogen population into the [1, 7] state. We also present H2 temperatures which may suggest that star spots on low mass stars persist longer, and encompass more area than star spots on solar-type stars.

Modeling Molecular Hydrogen Emission in M-Dwarf Exoplanetary Systems

NASA Astrophysics Data System (ADS)

Evonosky, W. R.; France, K.; Kruczek, N.; Youngblood, A.

2016-12-01

Exoplanets orbiting low-mass stars are prime candidates for atmospheric characterization due to their astronomical abundance and short orbital periods. These planets orbit stars that are often more active than main sequence solar-type stars. They are exposed to differing levels of ultraviolet radiation which can cause traditional "biosignature" gases to be generated abiotically, potentially causing false-positive identifications of life. We modeled the recently discovered molecular hydrogen emission in the ultraviolet spectra (1350 - 1650 Å) as arising from the stellar surface, excited by radiation generated in the upper chromosphere. The model was compared with observed hydrogen emission from the "Measurements of the Ultraviolet Spectral Characteristics of Low-mass Exoplanet host Stars" (MUSCLES) survey by conducting a grid search and implementing a chi-squared minimization routine. We considered only progressions from the [1, 4] and [1, 7] first excited electronic levels. Our modeling procedure varied the atomic hydrogen column density (in the chromosphere) as well as the photospheric molecular hydrogen column density and temperature. The model required as an input a reconstructed intrinsic Lyman α profile which served as the pumping radiation for the molecular hydrogen. We found that an atomic hydrogen column density of log10N(H I) = 14.13 ± 0.16 cm-2 represents a breaking point above which there is not enough Lyman α flux available to excite a significant molecular hydrogen population into the [1, 7] state. We also present H2 temperatures which may suggest that star spots on low mass stars persist longer, and encompass more area than star spots on solar-type stars.

Randomized prospective study comparing tri-cortical iliac crest autograft to allograft in the lateral column lengthening component for operative correction of adult acquired flatfoot deformity.

PubMed

Dolan, Christopher M; Henning, Jeffrey A; Anderson, John G; Bohay, Donald R; Kornmesser, Marc J; Endres, Terrence J

2007-01-01

Operative treatment of stage II posterior tibial tendon insufficiency (PTTI) is controversial. Many soft-tissue and bony procedures and various combinations of the two have been reported for treatment of stage II PTTI. Orthopaedists recognize the lateral column lengthening component of the procedure as a successful reconstructive technique. The use of cortical allograft for lateral column lengthening in the correction of pes planus in the pediatric patient population has been routine. In the adult population, however, tricortical iliac crest autograft has been the bone graft of choice. Harvest of this autograft can precipitate significant morbidity and cost. Therefore, we undertook this randomized controlled trial to compare graft incorporation and healing of allograft and autograft in the lateral column lengthening component of adult flatfoot reconstruction. Lateral column lengthening was done as a component of operative correction for stage II PTTI in adult patients (older than 18 years) by two surgeons using similar procedures. The patients were randomized to either the allograft or autograft procedures. The primary endpoint was graft incorporation and healing as assessed by radiographs. The study included 33 randomized feet in 31 patients. We followed 18 feet in the allograft group and 15 in the autograft group to the point of union. There were 21 women and 10 men. There were no delayed unions, nonunions, or hardware failures. All patients in both groups achieved bony union by the 12-week followup evaluation. Two superficial foot infections were successfully treated with oral antibiotics. Two patients in the autograft group continued to have hip donor site pain at 3 months. This study suggests that union rates of allograft and autograft (iliac crest bone graft) are equal. The use of allograft in the lateral column lengthening component of operative correction of adult stage II PTTI appears to be a viable alternative to the use of iliac crest autograft and eliminates the morbidity and increased cost associated with autograft harvest.

Density Gradient Columns for Chemical Displays.

ERIC Educational Resources Information Center

Guenther, William B.

1986-01-01

Procedures for preparing density gradient columns for chemical displays are presented. They include displays illustrating acid-base reactions, metal ion equilibria, and liquid density. The lifetime of these metastable displays is surprising, some lasting for months in display cabinets. (JN)

Combined extraction-cleanup column chromatographic procedure for determination of dicofol in avian eggs

USGS Publications Warehouse

Krynitsky, A.J.; Stafford, C.J.; Wiemeyer, Stanley N.

1988-01-01

Dicofol in avian eggs was completely oxidized to dichlorobenzophenone (DCBP) when a hexane Soxhlet extraction procedure was used. This degradation did not occur with other avian tissues (muscle and liver). For this reason, a combined extraction-cleanup column chromatographic procedure, without added heat, was developed for the determination of dicofol in avian eggs. Homogenized subsamples of eggs were mixed with sodium sulfate, and the mixture was added as the top layer on a column prepacked with Florisil. The dicofol and other compounds of interest were then eluted with ethyl ether-hexane. The extracts, relatively free from lipids, were quantitated on a gas chromatograph equipped with a 63Ni electron-capture detector and a methyl silicone capillary column. Recoveries from chicken eggs, fortified with dicofol and other DDT-related compounds, averaged 96%. Analysis of eggs of eastern screech-owls, fed a meat diet containing 10 ppm technical Kelthane, showed that both dicofol and DCBP were present. Results were confirmed by gas chromatography/mass spectrometry. This method is rapid and reliable, involves a minimum of sample handling, and is well suited for high volume determination of dicofol in eggs and other avian tissues.

Combination of COFRADIC and high temperature-extended column length conventional liquid chromatography: a very efficient way to tackle complex protein samples, such as serum.

PubMed

Sandra, Koen; Verleysen, Katleen; Labeur, Christine; Vanneste, Lies; D'Hondt, Filip; Thomas, Grégoire; Kas, Koen; Gevaert, Kris; Vandekerckhove, Joël; Sandra, Pat

2007-03-01

The previously reported COmbined FRActional DIagonal Chromatography (COFRA-DIC) methodology, in which a subset of peptides representative for their parent proteins are sorted, is particularly powerful for whole proteome analysis. This peptide-centric technology is built around diagonal chromatography, where peptide separations are crucial. This paper presents high efficiency peptide separations, in which four 250 x 2.1 mm, 5 microm Zorbax 300SB-C18 columns (total length 1 m) were coupled at operating temperatures of 60'C using a dedicated LC oven and conventional LC equipment. The high efficiency separations were combined with the COFRADIC procedure. This extremely powerful combination resulted, for the analysis of serum, in an increase in the uniquely identified peptide sequences by a factor of 2.6, compared to the COFRADIC procedure on a 25 cm column. This is a reflection of the increased peak capacity obtained on the 1 m column, which was calculated to be a factor 2.7 higher than on the 25 cm column. Besides more efficient sorting, less ion suppression was noticed.

Generator for ionic gallium-68 based on column chromatography

DOEpatents

Neirinckx, Rudi D.; Davis, Michael A.

1981-01-01

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

Infill Walls Contribution on the Progressive Collapse Resistance of a Typical Mid-rise RC Framed Building

NASA Astrophysics Data System (ADS)

Besoiu, Teodora; Popa, Anca

2017-10-01

This study investigates the effect of the autoclaved aerated concrete infill walls on the progressive collapse resistance of a typical RC framed structure. The 13-storey building located in Brăila (a zone with high seismic risk in Romania) was designed according to the former Romanian seismic code P13-70 (1970). Two models of the structure are generated in the Extreme Loading® for Structures computer software: a model with infill walls and a model without infill walls. Following GSA (2003) Guidelines, a nonlinear dynamic procedure is used to determine the progressive collapse risk of the building when a first-storey corner column is suddenly removed. It was found that, the structure is not expected to fail under the standard GSA loading: DL+0.25LL. Moreover, if the infill walls are introduced in the model, the maximum vertical displacement of the node above the removed column is reduced by about 48%.

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

Suspension of Drops of a Liquid in a Column of Water.

ERIC Educational Resources Information Center

Ahmad, Jamil

1995-01-01

Describes a demonstration which creates the illusion of violating Archimedes Principle. The procedure involves two liquids with identical densities and produces drops of one liquid suspended in the middle of a column of the second liquid. (DDR)

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

PubMed

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

2017-04-28

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

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

NASA Astrophysics Data System (ADS)

Rahai, A. R.; Kazemi, S.

2008-10-01

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

Neutron camera employing row and column summations

DOEpatents

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

2016-06-14

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

Automated Design of Restraint Layer of an Inflatable Vessel

NASA Technical Reports Server (NTRS)

Spexarth, Gary

2007-01-01

A Mathcad computer program largely automates the design and analysis of the restraint layer (the primary load-bearing layer) of an inflatable vessel that consists of one or more sections having cylindrical, toroidal, and/or spherical shape(s). A restraint layer typically comprises webbing in the form of multiple straps. The design task includes choosing indexing locations along the straps, computing the load at every location in each strap, computing the resulting stretch at each location, and computing the amount of undersizing required of each strap so that, once the vessel is inflated and the straps thus stretched, the vessel can be expected to assume the desired shape. Prior to the development of this program, the design task was performed by use of a difficult-to-use spreadsheet program that required manual addition of rows and columns depending on the numbers of strap rows and columns of a given design. In contrast, this program is completely parametric and includes logic that automatically adds or deletes rows and columns as needed. With minimal input from the user, this program automatically computes indexing locations, strap lengths, undersizing requirements, and all design data required to produce detailed drawings and assembly procedures. It also generates textual comments that help the user understand the calculations.

Chromato-panning: an efficient new mode of identifying suitable ligands from phage display libraries

PubMed Central

Noppe, Wim; Plieva, Fatima; Galaev, Igor Yu; Pottel, Hans; Deckmyn, Hans; Mattiasson, Bo

2009-01-01

Background Phage Display technology is a well established technique for high throughput screening of affinity ligands. Here we describe a new compact chromato-panning procedure for selection of suitable binders from a phage peptide display library. Results Both phages and E. coli cells pass non-hindered through the interconnected pores of macroporous gel, so called cryogel. After coupling a ligand to a monolithic cryogel column, the phage library was applied on the column and non-bound phages were washed out. The selection of strong phage-binders was achieved already after the first panning cycle due to the efficient separation of phage-binders from phage-non-binders in chromatographic mode rather than in batch mode as in traditional biopanning procedures. E. coli cells were applied on the column for infection with the specifically bound phages. Conclusion Chromato-panning allows combining several steps of the panning procedure resulting in 4–8 fold decrease of total time needed for phage selection. PMID:19292898

Smart-aggregate-based damage detection of fiber-reinforced-polymer-strengthened columns under reversed cyclic loading

NASA Astrophysics Data System (ADS)

Howser, Rachel; Moslehy, Yashar; Gu, Haichang; Dhonde, Hemant; Mo, Y. L.; Ayoub, Ashraf; Song, Gangbing

2011-07-01

Structural health monitoring is an important aspect of the maintenance of large civil infrastructures, especially for bridge columns in areas of high seismic activity. In this project, recently developed innovative piezoceramic-based sensors were utilized to perform the health monitoring of a shear-critical reinforced concrete (RC) bridge column subjected to reversed cyclic loading. After the column failed, it was wrapped with fiber reinforced polymer (FRP) sheets, commonly used to retrofit seismically damaged structures. The FRP-strengthened column was retested under the same reversed cyclic loading pattern. Innovative piezoceramic-based sensors, called 'smart aggregates', were utilized as transducers for health monitoring purposes. On the basis of the smart aggregates developed, an active-sensing approach and an impact-hammer-based approach were used to evaluate the health status of the RC column during the loading procedure. Wave transmission energy is attenuated by the existence of cracks during the loading procedure, and this attenuation phenomenon alters the curve of the transfer function between the actuator and sensor. To detect the damage occurrence and evaluate the damage severity, transfer function curves were compared with those obtained during the period of healthy status. A transfer-function-based damage index matrix was developed to demonstrate the damage severity at different locations. Experimental results verified the effectiveness of the smart aggregates in health monitoring of the FRP-strengthened column as well as the unstrengthened column. The experimental results show that the proposed smart-aggregate-based approach can successfully detect damage occurrence and evaluate its severity.

Minesweeping for Pressure Actuated Mines by Air Injection into a Water Column

DTIC Science & Technology

2011-09-01

19 B. PROTOTYPE DESIGN USED............................................................ 20 C. PROCEDURES ...Supply Considerations.................................................... 34 C. PROCEDURES ...Chapter III. Chapter IV covers the details of the NPS tow tank facility, testing procedures and results from testing completed in March 2010. Chapter V

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.

Multi-capillary column-ion mobility spectrometry: a potential screening system to differentiate virgin olive oils.

PubMed

Garrido-Delgado, Rocío; Arce, Lourdes; Valcárcel, Miguel

2012-01-01

The potential of a headspace device coupled to multi-capillary column-ion mobility spectrometry has been studied as a screening system to differentiate virgin olive oils ("lampante," "virgin," and "extra virgin" olive oil). The last two types are virgin olive oil samples of very similar characteristics, which were very difficult to distinguish with the existing analytical method. The procedure involves the direct introduction of the virgin olive oil sample into a vial, headspace generation, and automatic injection of the volatiles into a gas chromatograph-ion mobility spectrometer. The data obtained after the analysis by duplicate of 98 samples of three different categories of virgin olive oils, were preprocessed and submitted to a detailed chemometric treatment to classify the virgin olive oil samples according to their sensory quality. The same virgin olive oil samples were also analyzed by an expert's panel to establish their category and use these data as reference values to check the potential of this new screening system. This comparison confirms the potential of the results presented here. The model was able to classify 97% of virgin olive oil samples in their corresponding group. Finally, the chemometric method was validated obtaining a percentage of prediction of 87%. These results provide promising perspectives for the use of ion mobility spectrometry to differentiate virgin olive oil samples according to their quality instead of using the classical analytical procedure.

A Hands-On Approach to Teaching the Terrane Concept in Historical Geology.

ERIC Educational Resources Information Center

Bykerk-Kauffman, Ann

1989-01-01

Describes an exercise in which students convert lithostratigraphic columns into chronostratigraphic columns, infer paleolatitude using paleomagnetic data, interpret depositional environments, determine the timing of deformation and terrane collision, construct models, and synthesize the results into a geologic history. Background data, procedures,…

40 CFR 1065.275 - N2O measurement devices.

Code of Federal Regulations, 2014 CFR

2014-07-01

... procedures for interpretation of infrared spectra. For example, EPA Test Method 320 is considered a valid... infrared analyzer. Examples of laser infrared analyzers are pulsed-mode high-resolution narrow band mid... for analysis. Examples of acceptable columns are a PLOT column consisting of bonded polystyrene...

Cross flow cyclonic flotation column for coal and minerals beneficiation

DOEpatents

Lai, Ralph W.; Patton, Robert A.

2000-01-01

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

Separation of Albumin, Ceruloplasmin, and Transferrin from Human Plasma.

ERIC Educational Resources Information Center

Barnes, Grady; Frieden, Earl

1982-01-01

Procedures are provided for separating the principal metalloproteins (albumin, ceruloplasmin, and transferrin) from plasma using column chromatographic techniques. The experiment can be completed in two separate three-hour laboratory periods during which column chromatography is illustrated and the effect of pH on charge and affinity of a protein…

40 CFR 86.516-90 - Calibrations, frequency and overview.

Code of Federal Regulations, 2011 CFR

2011-07-01

... be checked at a frequency consistent with observed column life or when the indicator of the column... Regulations for 1978 and Later New Motorcycles; Test Procedures § 86.516-90 Calibrations, frequency and...) At least monthly or after any maintenance which could alter calibration, the following calibrations...

40 CFR 86.516-90 - Calibrations, frequency and overview.

Code of Federal Regulations, 2010 CFR

2010-07-01

... be checked at a frequency consistent with observed column life or when the indicator of the column... Regulations for 1978 and Later New Motorcycles; Test Procedures § 86.516-90 Calibrations, frequency and...) At least monthly or after any maintenance which could alter calibration, the following calibrations...

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

DTIC Science & Technology

2013-08-01

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

Comparison of methods for hydrocarbon analysis of marine biota

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

Gritz, R.L.; Shaw, D.G.

1977-04-01

A comparison was made of several procedures for the isolation of hydrocarbons from other matter and for the fractionation of hydrocarbons according to chemical type. The efficiency of Soxhlet extraction followed by saponification with extraction by alkaline digestion (direct saponification) was compared using two hour and 24 hour reaction times. All procedures were performed on approximately 60 g of soft parts of Saxidomus gigantea (butter clam). The 24 hour saponification and column chromatography on partially deactivated columns constituted the best procedure tested. Soxhlet extraction followed by two hour saponification did not completely remove methyl esters and was the most laboriousmore » technique. Direct two hour saponification was also questionable in the removal of esters and led to severe emulsion problems. The recoveries of hydrocarbons by the three procedures was substantially the same.« less

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

PubMed

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

2016-06-10

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

Removal of uranium from soil sample digests for ICP-OES analysis of trace metals

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

Foust, R.D. Jr.; Bidabad, M.

1996-10-01

An analytical procedure has been developed to quantitatively remove uranium from soil sample digests, permitting ICP-OES analysis of trace metals. The procedure involves digesting a soil sample with standard procedures (EPA SW-846, Method 3050), and passing the sample digestate through commercially available resin (U/TEVA{sm_bullet}Spec, Eichrom Industries, Inc.) containing diarryl amylphosphonate as the stationary phase. Quantitative removal of uranium was achieved with soil samples containing up to 60% uranium, and percent recoveries averaged better than 85% for 9 of the 10 metals evaluated (Ag, As, Cd. Cr, Cu, Ni, Pb, Se and Tl). The U/TEVA{sm_bullet}Spec column was regenerated by washing withmore » 200 mL of a 0.01 M oxalic acid/0.02 M nitric acid solution, permitting re-use of the column. GFAAS analysis of a sample spiked with 56.5% uranium, after treatment of the digestate with a U/TEVA{sm_bullet}Spec resin column, resulted in percent recoveries of 97% or better for all target metals.« less

The total carbon column observing network.

PubMed

Wunch, Debra; Toon, Geoffrey C; Blavier, Jean-François L; Washenfelder, Rebecca A; Notholt, Justus; Connor, Brian J; Griffith, David W T; Sherlock, Vanessa; Wennberg, Paul O

2011-05-28

A global network of ground-based Fourier transform spectrometers has been founded to remotely measure column abundances of CO(2), CO, CH(4), N(2)O and other molecules that absorb in the near-infrared. These measurements are directly comparable with the near-infrared total column measurements from space-based instruments. With stringent requirements on the instrumentation, acquisition procedures, data processing and calibration, the Total Carbon Column Observing Network (TCCON) achieves an accuracy and precision in total column measurements that is unprecedented for remote-sensing observations (better than 0.25% for CO(2)). This has enabled carbon-cycle science investigations using the TCCON dataset, and allows the TCCON to provide a link between satellite measurements and the extensive ground-based in situ network. © 2011 The Royal Society

[Complex program for the recovery of the vertebral column motor function].

PubMed

Kukareko, V P; Furmanov, A G

2011-01-01

This paper addresses the problems pertinent to the improvement of the efficacy of restoration of the vertebral column motor function based on the implementation of a comprehensive therapeutic program including massage, thermal procedures, and physical exercises. The program was realized in three phases, viz. preparatory, basic, and consolidating. The results of integral estimation of the whole body and vertebral column condition were taken into consideration. The experiment lasted 6 months and confirmed high efficiency of the comprehensive program.

Approach for ochratoxin A fast screening in spices using clean-up tandem immunoassay columns with confirmation by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS).

PubMed

Goryacheva, I Yu; De Saeger, S; Lobeau, M; Eremin, S A; Barna-Vetró, I; Van Peteghem, C

2006-09-01

An approach for ochratoxin A (OTA) fast cost-effective screening based on clean-up tandem immunoassay columns was developed and optimized for OTA detection with a cut-off level of 10 microg kg(-1) in spices. Two procedures were tested and applied for OTA detection. Column with bottom detection immunolayer was optimized for OTA determination in Capsicum ssp. spices. A modified clean-up tandem immunoassay procedure with top detection immunolayer was successfully applied for all tested spices. Its main advantages were decreasing of the number of analysis steps and quantity of antibody and also minimizing of matrix effects. The total duration of the extraction and analysis was about 40 min for six samples. Chilli, red pepper, pili-pili, cayenne, paprika, nutmeg, ginger, white pepper and black pepper samples were analyzed for OTA contamination by the proposed clean-up tandem immunoassay procedures. Clean-up tandem immunoassay results were confirmed by HPLC-MS/MS with immunoaffinity column clean-up. Among 17 tested Capsicum ssp. spices, 6 samples (35%) contained OTA in a concentration exceeding the 10 microg kg(-1) limit discussed by the European Commission. All tested nutmeg (n=8), ginger (n=5), white pepper (n=7) and black pepper (n=6) samples did not contain OTA above this action level.

Developing and Validating a Rapid Small-Scale Column Test Procedure for GAC Selection using Reconstituted Lyophilized NOM

EPA Science Inventory

Cost effective design and operation of Granular Activated Carbon (GAC) facilities requires the selection of GAC that is optimal for a specific site. Rapid small-scale column tests (RSSCTs) are widely used for GAC assessment due to several advantages, including the ability to simu...

A Hierarchical Bayesian Procedure for Two-Mode Cluster Analysis

ERIC Educational Resources Information Center

DeSarbo, Wayne S.; Fong, Duncan K. H.; Liechty, John; Saxton, M. Kim

2004-01-01

This manuscript introduces a new Bayesian finite mixture methodology for the joint clustering of row and column stimuli/objects associated with two-mode asymmetric proximity, dominance, or profile data. That is, common clusters are derived which partition both the row and column stimuli/objects simultaneously into the same derived set of clusters.…

Developing and Validating a Rapid Small-Scale Column Test Procedure for GAC Selection using Reconstituted Lyophilized NOM - Portland, OR

EPA Science Inventory

Cost effective design and operation of Granular Activated Carbon (GAC) facilities requires the selection of GAC that is optimal for a specific site. Rapid small-scale column tests (RSSCTs) are widely used for GAC assessment due to several advantages, including the ability to simu...

Accuracy of three-dimensional seismic ground response analysis in time domain using nonlinear numerical simulations

NASA Astrophysics Data System (ADS)

Liang, Fayun; Chen, Haibing; Huang, Maosong

2017-07-01

To provide appropriate uses of nonlinear ground response analysis for engineering practice, a three-dimensional soil column with a distributed mass system and a time domain numerical analysis were implemented on the OpenSees simulation platform. The standard mesh of a three-dimensional soil column was suggested to be satisfied with the specified maximum frequency. The layered soil column was divided into multiple sub-soils with a different viscous damping matrix according to the shear velocities as the soil properties were significantly different. It was necessary to use a combination of other one-dimensional or three-dimensional nonlinear seismic ground analysis programs to confirm the applicability of nonlinear seismic ground motion response analysis procedures in soft soil or for strong earthquakes. The accuracy of the three-dimensional soil column finite element method was verified by dynamic centrifuge model testing under different peak accelerations of the earthquake. As a result, nonlinear seismic ground motion response analysis procedures were improved in this study. The accuracy and efficiency of the three-dimensional seismic ground response analysis can be adapted to the requirements of engineering practice.

Analytic H I-to-H2 Photodissociation Transition Profiles

NASA Astrophysics Data System (ADS)

Bialy, Shmuel; Sternberg, Amiel

2016-05-01

We present a simple analytic procedure for generating atomic (H I) to molecular ({{{H}}}2) density profiles for optically thick hydrogen gas clouds illuminated by far-ultraviolet radiation fields. Our procedure is based on the analytic theory for the structure of one-dimensional H I/{{{H}}}2 photon-dominated regions, presented by Sternberg et al. Depth-dependent atomic and molecular density fractions may be computed for arbitrary gas density, far-ultraviolet field intensity, and the metallicity-dependent H2 formation rate coefficient, and dust absorption cross section in the Lyman-Werner photodissociation band. We use our procedure to generate a set of {{H}} {{I}}{-}{to}{-}{{{H}}}2 transition profiles for a wide range of conditions, from the weak- to strong-field limits, and from super-solar down to low metallicities. We show that if presented as functions of dust optical depth, the {{H}} {{I}} and {{{H}}}2 density profiles depend primarily on the Sternberg “α G parameter” (dimensionless) that determines the dust optical depth associated with the total photodissociated {{H}} {{I}} column. We derive a universal analytic formula for the {{H}} {{I}}{-}{to}{-}{{{H}}}2 transition points as a function of just α G. Our formula will be useful for interpreting emission-line observations of H I/{{{H}}}2 interfaces, for estimating star formation thresholds, and for sub-grid components in hydrodynamics simulations.

Identification and Correction of Additive and Multiplicative Spatial Biases in Experimental High-Throughput Screening.

PubMed

Mazoure, Bogdan; Caraus, Iurie; Nadon, Robert; Makarenkov, Vladimir

2018-06-01

Data generated by high-throughput screening (HTS) technologies are prone to spatial bias. Traditionally, bias correction methods used in HTS assume either a simple additive or, more recently, a simple multiplicative spatial bias model. These models do not, however, always provide an accurate correction of measurements in wells located at the intersection of rows and columns affected by spatial bias. The measurements in these wells depend on the nature of interaction between the involved biases. Here, we propose two novel additive and two novel multiplicative spatial bias models accounting for different types of bias interactions. We describe a statistical procedure that allows for detecting and removing different types of additive and multiplicative spatial biases from multiwell plates. We show how this procedure can be applied by analyzing data generated by the four HTS technologies (homogeneous, microorganism, cell-based, and gene expression HTS), the three high-content screening (HCS) technologies (area, intensity, and cell-count HCS), and the only small-molecule microarray technology available in the ChemBank small-molecule screening database. The proposed methods are included in the AssayCorrector program, implemented in R, and available on CRAN.

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

PubMed

Megalla, S E

1983-12-01

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

Short-range precipitation forecasts using assimilation of simulated satellite water vapor profiles and column cloud liquid water amounts

NASA Technical Reports Server (NTRS)

Wu, Xiaohua; Diak, George R.; Hayden, Cristopher M.; Young, John A.

1995-01-01

These observing system simulation experiments investigate the assimilation of satellite-observed water vapor and cloud liquid water data in the initialization of a limited-area primitive equations model with the goal of improving short-range precipitation forecasts. The assimilation procedure presented includes two aspects: specification of an initial cloud liquid water vertical distribution and diabatic initialization. The satellite data is simulated for the next generation of polar-orbiting satellite instruments, the Advanced Microwave Sounding Unit (AMSU) and the High-Resolution Infrared Sounder (HIRS), which are scheduled to be launched on the NOAA-K satellite in the mid-1990s. Based on cloud-top height and total column cloud liquid water amounts simulated for satellite data a diagnostic method is used to specify an initial cloud water vertical distribution and to modify the initial moisture distribution in cloudy areas. Using a diabatic initialization procedure, the associated latent heating profiles are directly assimilated into the numerical model. The initial heating is estimated by time averaging the latent heat release from convective and large-scale condensation during the early forecast stage after insertion of satellite-observed temperature, water vapor, and cloud water formation. The assimilation of satellite-observed moisture and cloud water, together withy three-mode diabatic initialization, significantly alleviates the model precipitation spinup problem, especially in the first 3 h of the forecast. Experimental forecasts indicate that the impact of satellite-observed temperature and water vapor profiles and cloud water alone in the initialization procedure shortens the spinup time for precipitation rates by 1-2 h and for regeneration of the areal coverage by 3 h. The diabatic initialization further reduces the precipitation spinup time (compared to adiabatic initialization) by 1 h.

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

PubMed

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

2012-12-01

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

Sub-micron resolution selected area electron channeling patterns.

PubMed

Guyon, J; Mansour, H; Gey, N; Crimp, M A; Chalal, S; Maloufi, N

2015-02-01

Collection of selected area channeling patterns (SACPs) on a high resolution FEG-SEM is essential to carry out quantitative electron channeling contrast imaging (ECCI) studies, as it facilitates accurate determination of the crystal plane normal with respect to the incident beam direction and thus allows control the electron channeling conditions. Unfortunately commercial SACP modes developed in the past were limited in spatial resolution and are often no longer offered. In this contribution we present a novel approach for collecting high resolution SACPs (HR-SACPs) developed on a Gemini column. This HR-SACP technique combines the first demonstrated sub-micron spatial resolution with high angular accuracy of about 0.1°, at a convenient working distance of 10mm. This innovative approach integrates the use of aperture alignment coils to rock the beam with a digitally calibrated beam shift procedure to ensure the rocking beam is maintained on a point of interest. Moreover a new methodology to accurately measure SACP spatial resolution is proposed. While column considerations limit the rocking angle to 4°, this range is adequate to index the HR-SACP in conjunction with the pattern simulated from the approximate orientation deduced by EBSD. This new technique facilitates Accurate ECCI (A-ECCI) studies from very fine grained and/or highly strained materials. It offers also new insights for developing HR-SACP modes on new generation high-resolution electron columns. Copyright © 2014 Elsevier B.V. All rights reserved.

Evaluation of SLAR and thematic mapper MSS data for forest cover mapping using computer-aided analysis techniques

NASA Technical Reports Server (NTRS)

Hoffer, R. M. (Principal Investigator); Knowlton, D. J.; Dean, M. E.

1981-01-01

A set of training statistics for the 30 meter resolution simulated thematic mapper MSS data was generated based on land use/land cover classes. In addition to this supervised data set, a nonsupervised multicluster block of training statistics is being defined in order to compare the classification results and evaluate the effect of the different training selection methods on classification performance. Two test data sets, defined using a stratified sampling procedure incorporating a grid system with dimensions of 50 lines by 50 columns, and another set based on an analyst supervised set of test fields were used to evaluate the classifications of the TMS data. The supervised training data set generated training statistics, and a per point Gaussian maximum likelihood classification of the 1979 TMS data was obtained. The August 1980 MSS data was radiometrically adjusted. The SAR data was redigitized and the SAR imagery was qualitatively analyzed.

Taming tosyl azide: the development of a scalable continuous diazo transfer process.

PubMed

Deadman, Benjamin J; O'Mahony, Rosella M; Lynch, Denis; Crowley, Daniel C; Collins, Stuart G; Maguire, Anita R

2016-04-07

Heat and shock sensitive tosyl azide was generated and used on demand in a telescoped diazo transfer process. Small quantities of tosyl azide were accessed in a 'one pot' batch procedure using shelf stable, readily available reagents. For large scale diazo transfer reactions tosyl azide was generated and used in a telescoped flow process, to mitigate the risks associated with handling potentially explosive reagents on scale. The in situ formed tosyl azide was used to rapidly perform diazo transfer to a range of acceptors, including β-ketoesters, β-ketoamides, malonate esters and β-ketosulfones. An effective in-line quench of sulfonyl azides was also developed, whereby a sacrificial acceptor molecule ensured complete consumption of any residual hazardous diazo transfer reagent. The telescoped diazo transfer process with in-line quenching was used to safely prepare over 21 g of an α-diazocarbonyl in >98% purity without any column chromatography.

Consensus generation and variant detection by Celera Assembler.

PubMed

Denisov, Gennady; Walenz, Brian; Halpern, Aaron L; Miller, Jason; Axelrod, Nelson; Levy, Samuel; Sutton, Granger

2008-04-15

We present an algorithm to identify allelic variation given a Whole Genome Shotgun (WGS) assembly of haploid sequences, and to produce a set of haploid consensus sequences rather than a single consensus sequence. Existing WGS assemblers take a column-by-column approach to consensus generation, and produce a single consensus sequence which can be inconsistent with the underlying haploid alleles, and inconsistent with any of the aligned sequence reads. Our new algorithm uses a dynamic windowing approach. It detects alleles by simultaneously processing the portions of aligned reads spanning a region of sequence variation, assigns reads to their respective alleles, phases adjacent variant alleles and generates a consensus sequence corresponding to each confirmed allele. This algorithm was used to produce the first diploid genome sequence of an individual human. It can also be applied to assemblies of multiple diploid individuals and hybrid assemblies of multiple haploid organisms. Being applied to the individual human genome assembly, the new algorithm detects exactly two confirmed alleles and reports two consensus sequences in 98.98% of the total number 2,033311 detected regions of sequence variation. In 33,269 out of 460,373 detected regions of size >1 bp, it fixes the constructed errors of a mosaic haploid representation of a diploid locus as produced by the original Celera Assembler consensus algorithm. Using an optimized procedure calibrated against 1 506 344 known SNPs, it detects 438 814 new heterozygous SNPs with false positive rate 12%. The open source code is available at: http://wgs-assembler.cvs.sourceforge.net/wgs-assembler/

Dogs lap using acceleration-driven open pumping

PubMed Central

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

2015-01-01

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

Rapid Two-Step Procedure for Large-Scale Purification of Pediocin-Like Bacteriocins and Other Cationic Antimicrobial Peptides from Complex Culture Medium

PubMed Central

Uteng, Marianne; Hauge, Håvard Hildeng; Brondz, Ilia; Nissen-Meyer, Jon; Fimland, Gunnar

2002-01-01

A rapid and simple two-step procedure suitable for both small- and large-scale purification of pediocin-like bacteriocins and other cationic peptides has been developed. In the first step, the bacterial culture was applied directly on a cation-exchange column (1-ml cation exchanger per 100-ml cell culture). Bacteria and anionic compounds passed through the column, and cationic bacteriocins were subsequently eluted with 1 M NaCl. In the second step, the bacteriocin fraction was applied on a low-pressure, reverse-phase column and the bacteriocins were detected as major optical density peaks upon elution with propanol. More than 80% of the activity that was initially in the culture supernatant was recovered in both purification steps, and the final bacteriocin preparation was more than 90% pure as judged by analytical reverse-phase chromatography and capillary electrophoresis. PMID:11823243

Basic Aspects of Deep Soil Mixing Technology Control

NASA Astrophysics Data System (ADS)

Egorova, Alexandra A.; Rybak, Jarosław; Stefaniuk, Damian; Zajączkowski, Przemysław

2017-10-01

Improving a soil is a process of increasing its physical/mechanical properties without changing its natural structure. Improvement of soil subbase is reached by means of the knitted materials, or other methods when strong connection between soil particles is established. The method of DSM (Deep Soil Mixing) columns has been invented in Japan in 1970s. The main reason of designing cement-soil columns is to improve properties of local soils (such as strength and stiffness) by mixing them with various cementing materials. Cement and calcium are the most commonly used binders. However new research undertaken worldwide proves that apart from these materials, also gypsum or fly ashes can also be successfully implemented. As the Deep Soil Mixing is still being under development, anticipating mechanical properties of columns in particular soils and the usage of cementing materials in formed columns is very difficult and often inappropriate to predict. That is why a research is carried out in order to find out what binders and mixing technology should be used. The paper presents several remarks on the testing procedures related to quality and capacity control of Deep Soil Mixing columns. Soil improvement methods, their advantages and limitations are briefly described. The authors analyse the suitability of selected testing methods on subsequent stages of design and execution of special foundations works. Chosen examples from engineering practice form the basis for recommendations for the control procedures. Presented case studies concerning testing the on capacity field samples and laboratory procedures on various categories of soil-cement samples were picked from R&D and consulting works offered by Wroclaw University of Science and Technology. Special emphasis is paid to climate conditions which may affect the availability of performing and controlling of DSM techniques in polar zones, with a special regard to sample curing.

Cellular Targets of Dietary Polyphenol Resveratrol

DTIC Science & Technology

2005-03-01

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

Design of hat-stiffened composite panels loaded in axial compression

NASA Astrophysics Data System (ADS)

Paul, T. K.; Sinha, P. K.

An integrated step-by-step analysis procedure for the design of axially compressed stiffened composite panels is outlined. The analysis makes use of the effective width concept. A computer code, BUSTCOP, is developed incorporating various aspects of buckling such as skin buckling, stiffener crippling and column buckling. Other salient features of the computer code include capabilities for generation of data based on micromechanics theories and hygrothermal analysis, and for prediction of strength failure. Parametric studies carried out on a hat-stiffened structural element indicate that, for all practical purposes, composite panels exhibit higher structural efficiency. Some hybrid laminates with outer layers made of aluminum alloy also show great promise for flight vehicle structural applications.

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.

Fatigue and stress studies : an improved semi-automated procedure for flurometric determination of plasma catecholamines.

DOT National Transportation Integrated Search

1966-04-01

A semiautomated technique is described for the estimation of total catecholamines in plasma by the trihydroxyindole procedure. The method utilizes conventional alumina-column chromatography for isolation of the amines. Catecholamine oxidation, tautom...

Separation of Be and Al for AMS using single-step column chromatography

NASA Astrophysics Data System (ADS)

Binnie, Steven A.; Dunai, Tibor J.; Voronina, Elena; Goral, Tomasz; Heinze, Stefan; Dewald, Alfred

2015-10-01

With the aim of simplifying AMS target preparation procedures for TCN measurements we tested a new extraction chromatography approach which couples an anion exchange resin (WBEC) to a chelating resin (Beryllium resin) to separate Be and Al from dissolved quartz samples. Results show that WBEC-Beryllium resin stacks can be used to provide high purity Be and Al separations using a combination of hydrochloric/oxalic and nitric acid elutions. 10Be and 26Al concentrations from quartz samples prepared using more standard procedures are compared with results from replicate samples prepared using the coupled WBEC-Beryllium resin approach and show good agreement. The new column procedure is performed in a single step, reducing sample preparation times relative to more traditional methods of TCN target production.

The Deformity Angular Ratio: Does It Correlate With High-Risk Cases for Potential Spinal Cord Monitoring Alerts in Pediatric 3-Column Thoracic Spinal Deformity Corrective Surgery?

PubMed

Lewis, Noah D H; Keshen, Sam G N; Lenke, Lawrence G; Zywiel, Michael G; Skaggs, David L; Dear, Taylor E; Strantzas, Samuel; Lewis, Stephen J

2015-08-01

A retrospective analysis. The purpose of this study was to determine whether the deformity angular ratio (DAR) can reliably assess the neurological risks of patients undergoing deformity correction. Identifying high-risk patients and procedures can help ensure that appropriate measures are taken to minimize neurological complications during spinal deformity corrections. Subjectively, surgeons look at radiographs and evaluate the riskiness of the procedure. However, 2 curves of similar magnitude and location can have significantly different risks of neurological deficit during surgery. Whether the curve spans many levels or just a few can significantly influence surgical strategies. Lenke et al have proposed the DAR, which is a measure of curve magnitude per level of deformity. The data from 35 pediatric spinal deformity correction procedures with thoracic 3-column osteotomies were reviewed. Measurements from preoperative radiographs were used to calculate the DAR. Binary logistic regression was used to model the relationship between DARs (independent variables) and presence or absence of an intraoperative alert (dependent variable). In patients undergoing 3-column osteotomies, sagittal curve magnitude and total curve magnitude were associated with increased incidence of transcranial motor evoked potential changes. Total DAR greater than 45° per level and sagittal DAR greater than 22° per level were associated with a 75% incidence of a motor evoked potential alert, with the incidence increasing to 90% with sagittal DAR of 28° per level. In patients undergoing 3-column osteotomies for severe spinal deformities, the DAR was predictive of patients developing intraoperative motor evoked potential alerts. Identifying accurate radiographical, patient, and procedural risk factors in the correction of severe deformities can help prepare the surgical team to improve safety and outcomes when carrying out complex spinal corrections. 3.

Vessel structural support system

DOEpatents

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

1992-01-01

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

Ranking of predictor variables based on effect size criterion provides an accurate means of automatically classifying opinion column articles

NASA Astrophysics Data System (ADS)

Legara, Erika Fille; Monterola, Christopher; Abundo, Cheryl

2011-01-01

We demonstrate an accurate procedure based on linear discriminant analysis that allows automatic authorship classification of opinion column articles. First, we extract the following stylometric features of 157 column articles from four authors: statistics on high frequency words, number of words per sentence, and number of sentences per paragraph. Then, by systematically ranking these features based on an effect size criterion, we show that we can achieve an average classification accuracy of 93% for the test set. In comparison, frequency size based ranking has an average accuracy of 80%. The highest possible average classification accuracy of our data merely relying on chance is ∼31%. By carrying out sensitivity analysis, we show that the effect size criterion is superior than frequency ranking because there exist low frequency words that significantly contribute to successful author discrimination. Consistent results are seen when the procedure is applied in classifying the undisputed Federalist papers of Alexander Hamilton and James Madison. To the best of our knowledge, the work is the first attempt in classifying opinion column articles, that by virtue of being shorter in length (as compared to novels or short stories), are more prone to over-fitting issues. The near perfect classification for the longer papers supports this claim. Our results provide an important insight on authorship attribution that has been overlooked in previous studies: that ranking discriminant variables based on word frequency counts is not necessarily an optimal procedure.

Effects of porous media preparation on bacteria transport through laboratory columns.

PubMed

Brown, Derick G; Stencel, Joseph R; Jaffé, Peter R

2002-01-01

Bacterial and colloid transport experiments related to environmental systems are typically performed in the laboratory, with sand often used as the porous media. In order to prepare the sand, mechanical sieving is frequently used to tighten the sand grain size distribution. However, mechanical sieving has been reported to provide insufficient repeatability between identical colloidal transport experiments. This work examined the deficiencies of mechanical sieving with respect to bacterial transport through sand columns. It was found that sieving with standard brass sieves (1) contaminates the sand with copper and zinc as a linear function of sieving time and (2) inefficiently sizes sand grains below 300 microm (the largest size examined in this study) due to rapid clogging of the sieves. A procedure was developed that allows utilization of brass sieves for sizing the sand grains and removes the metal contamination introduced from the sieves. Bacterial transport experiments utilizing this column preparation procedure gave repeatable breakthrough curves. Further examination of the effects of these treatments on bacterial transport showed interesting results. First, it was found that the metal contamination did not affect the clean-bed bacterial transport. Second. it was found that variations of the column flushing procedure did not alter the clean-bed breakthrough of the bacteria, but did alter the inter-particle blocking. Finally, it was found that the shape of the sand grains (oblong vs. rounded) significantly alters the bacterial transport. with the transport being dominated by the smallest dimension of the oblong grains.

Microscale speciation of arsenic and iron in ferric-based sorbents subjected to simulated landfill conditions

PubMed Central

Root, Robert A.; Fathordoobadi, Sahar; Alday, Fernando; Ela, Wendell; Chorover, Jon

2013-01-01

During treatment for potable use, water utilities generate arsenic-bearing ferric wastes that are subsequently dispatched to landfills. The biogeochemical weathering of these residuals in mature landfills affects the potential mobilization of sorbed arsenic species via desorption from solids subjected to phase transformations driven by abundant organic matter and bacterial activity. Such processes are not simulated with the Toxicity Characteristic Leaching Procedure (TCLP) currently used to characterize hazard. To examine the effect of sulfate on As retention in landfill leachate, columns of As(V) loaded amorphous ferric hydroxide were reacted biotically at two leachate sulfate concentrations (0.064 mM and 2.1 mM). After 300 d, ferric sorbents were reductively dissolved. Arsenic released to porewaters was partially co-precipitated in mixed-valent secondary iron phases whose speciation was dependent on sulfate concentration. As and Fe XAS showed that, in the low sulfate column, 75–81% of As(V) was reduced to As(III), and 53–68% of the Fe(III) sorbent was transformed, dominantly to siderite and green rust. In the high sulfate column, Fe(III) solids were reduced principally to FeS(am), whereas As(V) was reduced to a polymeric sulfide with local atomic structure of realgar. Multi-energy micro-X-ray fluorescence (ME-μXRF) imaging at Fe and As K-edges showed that As formed surface complexes with ferrihydrite > siderite > green rust in the low sulfate column; while discrete realgar-like phases formed in the high sulfate systems. Results indicate that landfill sulfur chemistry exerts strong control over the potential mobilization of As from ferric sorbent residuals by controlling secondary As and Fe sulfide co-precipitate formation. PMID:24102155

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

PubMed

Berger, Terry A

2016-12-02

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

Analysis of programming properties and the row-column generation method for 1-norm support vector machines.

PubMed

Zhang, Li; Zhou, WeiDa

2013-12-01

This paper deals with fast methods for training a 1-norm support vector machine (SVM). First, we define a specific class of linear programming with many sparse constraints, i.e., row-column sparse constraint linear programming (RCSC-LP). In nature, the 1-norm SVM is a sort of RCSC-LP. In order to construct subproblems for RCSC-LP and solve them, a family of row-column generation (RCG) methods is introduced. RCG methods belong to a category of decomposition techniques, and perform row and column generations in a parallel fashion. Specially, for the 1-norm SVM, the maximum size of subproblems of RCG is identical with the number of Support Vectors (SVs). We also introduce a semi-deleting rule for RCG methods and prove the convergence of RCG methods when using the semi-deleting rule. Experimental results on toy data and real-world datasets illustrate that it is efficient to use RCG to train the 1-norm SVM, especially in the case of small SVs. Copyright © 2013 Elsevier Ltd. All rights reserved.

76 FR 45811 - Animal Drug User Fee Rates and Payment Procedures for Fiscal Year 2012

Federal Register 2010, 2011, 2012, 2013, 2014

2011-08-01

... Lisa Kable, Center for Veterinary Medicine (HFV-10), Food and Drug Administration, 7529 Standish Pl... Medicine (CVM) at: [email protected] . SUPPLEMENTARY INFORMATION: I. Background Section 740 of the FD&C... from the base years in column 3. At the bottom right of the table the sum of the values in column 5 is...

24 CFR 3285.605 - Fuel supply system.

Code of Federal Regulations, 2010 CFR

2010-04-01

... designed for a pressure that is at least 7 inches of water column [4oz./in.2 or 0.25 psi] and not more than 14 inches of water column [8 oz./in.2 or 0.5 psi]. If gas from any supply source exceeds, or could... connector quick-disconnect. (c) Testing procedures. The gas system must be inspected and tested for leaks...

The Extended Direct Anterior Approach for Column Augmentation in the Deficient Pelvis: A Novel Surgical Technique, and Case Series Report.

PubMed

Spanyer, Jonathon M; Beaumont, Christopher M; Yerasimides, Jonathan G

2017-02-01

Anterior column deficiency of the pelvis may pose a serious threat to the stability of the acetabular component after total hip arthroplasty and, thus, jeopardize the overall success of the procedure. After Institutional Review Board approval, a retrospective review was undertaken to identify all patients undergoing revision total hip arthroplasty with anterior column augmentation through an extended direct anterior approach. Demographics and surgical details were collected, and subjects were followed for a 2-year minimum period to measure patient outcomes and to evaluate for the stability of construct fixation. A novel surgical procedure description was provided and supplemented with an illustrative case example. At 2 years post augmentation, patients had favorable functional outcomes with radiologic evidence of stable fixation. Proximal extension of the direct anterior approach to the hip can facilitate anterior column access and augmentation to improve stability of the hip reconstruction. This treatment may be an alternative to spanning constructs such as cup-cage constructs and custom implants, affording the potential for long-term biologic fixation. Further investigation into this technique is warranted. Copyright © 2016 Elsevier Inc. All rights reserved.

An alternative procedure for uranium analysis in drinking water using AQUALIX columns: application to varied French bottled waters.

PubMed

Bouvier-Capely, C; Bonthonneau, J P; Dadache, E; Rebière, F

2014-01-01

The general population is chronically exposed to uranium ((234)U, (235)U, and (238)U) and polonium ((210)Po) mainly through day-to-day food and beverage intake. The measurement of these naturally-occurring radionuclides in drinking water is important to assess their health impact. In this work the applicability of calix[6]arene-derivatives columns for uranium analysis in drinking water was investigated. A simple and effective method was proposed on a specific column called AQUALIX, for the separation and preconcentration of U from drinking water. This procedure is suitable for routine analysis and the analysis time is considerably shortened (around 4h) by combining the separation on AQUALIX with fast ICP-MS measurement. This new method was tested on different French bottled waters (still mineral water, sparkling mineral water, and spring water). Then, the case of simultaneous presence of uranium and polonium in water was considered due to interferences in alpha spectrometry measurement. A protocol was proposed using a first usual step of spontaneous deposition of polonium on silver disc in order to separate Po, followed by the uranium extraction on AQUALIX column before alpha spectrometry counting. © 2013 Published by Elsevier B.V.

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.

Generating moment matching scenarios using optimization techniques

DOE PAGES

Mehrotra, Sanjay; Papp, Dávid

2013-05-16

An optimization based method is proposed to generate moment matching scenarios for numerical integration and its use in stochastic programming. The main advantage of the method is its flexibility: it can generate scenarios matching any prescribed set of moments of the underlying distribution rather than matching all moments up to a certain order, and the distribution can be defined over an arbitrary set. This allows for a reduction in the number of scenarios and allows the scenarios to be better tailored to the problem at hand. The method is based on a semi-infinite linear programming formulation of the problem thatmore » is shown to be solvable with polynomial iteration complexity. A practical column generation method is implemented. The column generation subproblems are polynomial optimization problems; however, they need not be solved to optimality. It is found that the columns in the column generation approach can be efficiently generated by random sampling. The number of scenarios generated matches a lower bound of Tchakaloff's. The rate of convergence of the approximation error is established for continuous integrands, and an improved bound is given for smooth integrands. Extensive numerical experiments are presented in which variants of the proposed method are compared to Monte Carlo and quasi-Monte Carlo methods on both numerical integration problems and stochastic optimization problems. The benefits of being able to match any prescribed set of moments, rather than all moments up to a certain order, is also demonstrated using optimization problems with 100-dimensional random vectors. Here, empirical results show that the proposed approach outperforms Monte Carlo and quasi-Monte Carlo based approaches on the tested problems.« less

Steel-reinforced concrete-filled steel tubular columns under axial and lateral cyclic loading

NASA Astrophysics Data System (ADS)

Farajpourbonab, Ebrahim; Kute, Sunil Y.; Inamdar, Vilas M.

2018-03-01

SRCFT columns are formed by inserting a steel section into a concrete-filled steel tube. These types of columns are named steel-reinforced concrete-filled steel tubular (SRCFT) columns. The current study aims at investigating the various types of reinforcing steel section to improve the strength and hysteresis behavior of SRCFT columns under axial and lateral cyclic loading. To attain this objective, a numerical study has been conducted on a series of composite columns. First, FEM procedure has been verified by the use of available experimental studies. Next, eight composite columns having different types of cross sections were analyzed. For comparison purpose, the base model was a CFT column used as a benchmark specimen. Nevertheless, the other specimens were SRCFT types. The results indicate that reinforcement of a CFT column through this method leads to enhancement in load-carrying capacity, enhancement in lateral drift ratio, ductility, preventing of local buckling in steel shell, and enhancement in energy absorption capacity. Under cyclic displacement history, it was observed that the use of cross-shaped reinforcing steel section causes a higher level of energy dissipation and the moment of inertia of the reinforcing steel sections was found to be the most significant parameter affecting the hysteresis behavior of SRCFT columns.

Reversed-phase liquid chromatography column testing: robustness study of the test.

PubMed

Le Mapihan, K; Vial, J; Jardy, A

2004-12-24

Choosing the right RPLC column for an actual separation among the more than 600 commercially available ones still represents a real challenge for the analyst particularly when basic solutes are involved. Many tests dedicated to the characterization and the classification of stationary phases have been proposed in the literature and some of them highlighted the need of a better understanding of retention properties to lead to a rational choice of columns. However, unlike classical chromatographic methods, the problem of their robustness evaluation has often been left unaddressed. In the present study, we present a robustness study that was applied to the chromatographic testing procedure we had developed and optimized previously. A design of experiment (DoE) approach was implemented. Four factors, previously identified as potentially influent, were selected and subjected to small controlled variations: solvent fraction, temperature, pH and buffer concentration. As our model comprised quadratic terms instead of a simple linear model, we chose a D-optimal design in order to minimize the experiment number. As a previous batch-to-batch study [K. Le Mapihan, Caractérisation et classification des phases stationnaires utilisées pour l'analyse CPL de produits pharmaceutiques, Ph.D. Thesis, Pierre and Marie Curie University, 2004] had shown a low variability on the selected stationary phase, it was then possible to split the design into two parts, according to the solvent nature, each using one column. Actually, our testing procedure involving assays both with methanol and with acetonitrile as organic modifier, such an approach enabled to avoid a possible bias due to the column ageing considering the number of experiments required (16 + 6 center points). Experimental results were computed thanks to a Partial Least Squares regression procedure, more adapted than the classical regression to handle factors and responses not completely independent. The results showed the behavior of the solutes in relation to their physico-chemical properties and the relevance of the second term degree of our model. Finally, the robust domain of the test has been fairly identified, so that any potential user precisely knows to which extend each experimental parameter must be controlled when our testing procedure is to be implemented.

CRISM Hyperspectral Data Filtering with Application to MSL Landing Site Selection

NASA Astrophysics Data System (ADS)

Seelos, F. P.; Parente, M.; Clark, T.; Morgan, F.; Barnouin-Jha, O. S.; McGovern, A.; Murchie, S. L.; Taylor, H.

2009-12-01

We report on the development and implementation of a custom filtering procedure for Compact Reconnaissance Imaging Spectrometer for Mars (CRISM) IR hyperspectral data that is suitable for incorporation into the CRISM Reduced Data Record (RDR) calibration pipeline. Over the course of the Mars Reconnaissance Orbiter (MRO) Primary Science Phase (PSP) and the ongoing Extended Science Phase (ESP) CRISM has operated with an IR detector temperature between ~107 K and ~127 K. This ~20 K range in operational temperature has resulted in variable data quality, with observations acquired at higher detector temperatures exhibiting a marked increase in both systematic and stochastic noise. The CRISM filtering procedure consists of two main data processing capabilities. The primary systematic noise component in CRISM IR data appears as along track or column oriented striping. This is addressed by the robust derivation and application of an inter-column ratio correction frame. The correction frame is developed through the serial evaluation of band specific column ratio statistics and so does not compromise the spectral fidelity of the image cube. The dominant CRISM IR stochastic noise components appear as isolated data spikes or column oriented segments of variable length with erroneous data values. The non-systematic noise is identified and corrected through the application of an iterative-recursive kernel modeling procedure which employs a formal statistical outlier test as the iteration control and recursion termination criterion. This allows the filtering procedure to make a statistically supported determination between high frequency (spatial/spectral) signal and high frequency noise based on the information content of a given multidimensional data kernel. The governing statistical test also allows the kernel filtering procedure to be self regulating and adaptive to the intrinsic noise level in the data. The CRISM IR filtering procedure is scheduled to be incorporated into the next augmentation of the CRISM IR calibration (version 3). The filtering algorithm will be applied to the I/F data (IF) delivered to the Planetary Data System (PDS), but the radiance on sensor data (RA) will remain unfiltered. The development of CRISM hyperspectral analysis products in support of the Mars Science Laboratory (MSL) landing site selection process has motivated the advance of CRISM-specific data processing techniques. The quantitative results of the CRISM IR filtering procedure as applied to CRISM observations acquired in support of MSL landing site selection will be presented.

CT measurement of range of motion of ankle and subtalar joints following two lateral column lengthening procedures.

PubMed

Beimers, Lijkele; Louwerens, Jan W K; Tuijthof, Gabrielle Josephine Maria; Jonges, Remmet; van Dijk, C N Niek; Blankevoort, Leendert

2012-05-01

Lateral column lengthening (LCL) has become an accepted procedure for the operative treatment of the flexible flatfoot deformity. Hindfoot arthrodesis via a calcaneocuboid distraction arthrodesis (CCDA) has been considered a less favourable surgical option than the anterior open wedge calcaneal distraction osteotomy (ACDO), as CCDA has been associated with reduced hindfoot joint motion postoperatively. The ankle and subtalar joint ranges of motion were measured in patients who underwent an ACDO or CCDA procedure for flatfoot deformity. CT scanning was performed with the foot in extreme positions in five ACDO and five CCDA patients. A bone segmentation and registration technique for the tibia, talus and calcaneus was applied to the CT images. Finite helical axis (FHA) rotations representing the range of motion of the joints were calculated for the motion between opposite extreme foot positions of the tibia and the calcaneus relative to the talus. The maximum mean FHA rotation of the ankle joint (for extreme dorsiflexion to extreme plantarflexion) after ACDO was 52.2 degrees ± 12.4 degrees and after CCDA 49.0 degrees ± 12.0 degrees. Subtalar joint maximum mean FHA rotation (for extreme eversion to extreme inversion) following ACDO was 22.8 degrees ± 8.6 degrees, and following CCDA 24.4 degrees ± 7.6 degrees. An accurate CT-based technique was used to assess the range of motion of the ankle and subtalar joints following two lateral column lengthening procedures for flatfoot deformity. Comparable results with a considerable amount of variance were found for the range of motion following the ACDO and CCDA procedures.

Determination of strontium-90 in deer bones by liquid scintillation spectrometry after separation on Sr-specific ion exchange columns.

PubMed

Landstetter, Claudia; Wallner, Gabriele

2006-01-01

The activity concentration of (90)Sr was determined in several deer bones from Austria. Strontium specific ion exchange columns with 4',4''(5'')-di-t-butylcyclohexane-18-crown-6 from Eichrom Industries, Inc. were used for separation. The yield of the chemical procedure was quantified with AAS. Directly after column separation, the solution containing (90)Sr was mixed with the scintillation cocktail HiSafe III and measured by liquid scintillation counting. Prevention of (210)Pb contamination and reusability of the separation columns was investigated as well as the activity distribution within the bones. Results were compared with pre-Chernobyl measurements in Austria; a correlation between activity concentration of (90)Sr and site altitude was found.

Implied alignment: a synapomorphy-based multiple-sequence alignment method and its use in cladogram search

NASA Technical Reports Server (NTRS)

Wheeler, Ward C.

2003-01-01

A method to align sequence data based on parsimonious synapomorphy schemes generated by direct optimization (DO; earlier termed optimization alignment) is proposed. DO directly diagnoses sequence data on cladograms without an intervening multiple-alignment step, thereby creating topology-specific, dynamic homology statements. Hence, no multiple-alignment is required to generate cladograms. Unlike general and globally optimal multiple-alignment procedures, the method described here, implied alignment (IA), takes these dynamic homologies and traces them back through a single cladogram, linking the unaligned sequence positions in the terminal taxa via DO transformation series. These "lines of correspondence" link ancestor-descendent states and, when displayed as linearly arrayed columns without hypothetical ancestors, are largely indistinguishable from standard multiple alignment. Since this method is based on synapomorphy, the treatment of certain classes of insertion-deletion (indel) events may be different from that of other alignment procedures. As with all alignment methods, results are dependent on parameter assumptions such as indel cost and transversion:transition ratios. Such an IA could be used as a basis for phylogenetic search, but this would be questionable since the homologies derived from the implied alignment depend on its natal cladogram and any variance, between DO and IA + Search, due to heuristic approach. The utility of this procedure in heuristic cladogram searches using DO and the improvement of heuristic cladogram cost calculations are discussed. c2003 The Willi Hennig Society. Published by Elsevier Science (USA). All rights reserved.

Avoid problems during distillation column startups

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

Sloley, A.W.

1996-07-01

The startup of a distillation column is the end product of the design process. Indeed, startup is the culmination of the theory and practice of designing the column to meet the process objectives. The author will direct most of this discussion towards column revamps due to their inherent complexity; however, the points apply equally to new columns, as well. The most important question that must be answered prior to a startup is how will the distillation system changes affect initial startup, process control of the system, and normal day-to-day operations? How will the operators run the system? Steady-state distillation-column simulationsmore » alone cannot provide an authoritative answer and, indeed, engineers` over-reliance on software too often has led them to ignore many practical aspects. Computer modeling, while an important engineering tool, is not reality. Distillation columns are real functioning pieces of equipment that require practical skills to successfully modify. They are not steady-state solutions that result from converged computer simulations. Early planning, coupled with thorough inspections and comprehensive reviews of instrumentation and procedures, can play a key role in assuring smooth startups.« less

Development of double chain phosphatidylcholine functionalized polymeric monoliths for immobilized artificial membrane chromatography.

PubMed

Wang, Qiqin; Peng, Kun; Chen, Weijia; Cao, Zhen; Zhu, Peijie; Zhao, Yumei; Wang, Yuqiang; Zhou, Haibo; Jiang, Zhengjin

2017-01-06

This study described a simple synthetic methodology for preparing biomembrane mimicking monolithic column. The suggested approach not only simplifies the preparation procedure but also improves the stability of double chain phosphatidylcholine (PC) functionalized monolithic column. The physicochemical properties of the optimized monolithic column were characterized by scanning electron microscopy, energy-dispersive X-ray spectrometry, and nano-LC. Satisfactory column permeability, efficiency, stability and reproducibility were obtained on this double chain PC functionalized monolithic column. It is worth noting that the resulting polymeric monolith exhibits great potential as a useful alternative of commercial immobilized artificial membrane (IAM) columns for in vitro predication of drug-membrane interactions. Furthermore, the comparative study of both double chain and single chain PC functionalized monoliths indicates that the presence or absence of glycerol backbone and the number of acyl chains are not decisive for the predictive ability of IAM monoliths on drug-membrane interactions. This novel PC functionalized monolithic column also exhibited good selectivity for a protein mixture and a set of pharmaceutical compounds. Copyright © 2016 Elsevier B.V. All rights reserved.

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.

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

PubMed

Abdollahpour, Assem; Heydari, Rouhollah; Shamsipur, Mojtaba

2017-07-01

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

Generation of accurate peptide retention data for targeted and data independent quantitative LC-MS analysis: Chromatographic lessons in proteomics.

PubMed

Krokhin, Oleg V; Spicer, Vic

2016-12-01

The emergence of data-independent quantitative LC-MS/MS analysis protocols further highlights the importance of high-quality reproducible chromatographic procedures. Knowing, controlling and being able to predict the effect of multiple factors that alter peptide RP-HPLC separation selectivity is critical for successful data collection for the construction of ion libraries. Proteomic researchers have often regarded RP-HPLC as a "black box", while vast amount of research on peptide separation is readily available. In addition to obvious parameters, such as the type of ion-pairing modifier, stationary phase and column temperature, we describe the "mysterious" effects of gradient slope, column size and flow rate on peptide separation selectivity. Retention time variations due to these parameters are governed by the linear solvent strength (LSS) theory on a peptide level by the value of its slope S in the basic LSS equation-a parameter that can be accurately predicted. Thus, the application of shallower gradients, higher flow rates, or smaller columns will each increases the relative retention of peptides with higher S-values (long species with multiple positively charged groups). Simultaneous changes to these parameters that each drive shifts in separation selectivity in the same direction should be avoided. The unification of terminology represents another pressing issue in this field of applied proteomics that should be addressed to facilitate further progress. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Local connections between the columns of the periaqueductal gray matter: a case for intrinsic neuromodulation.

PubMed

Jansen, A S; Farkas, E; Mac Sams, J; Loewy, A D

1998-02-16

Chemical stimulation of the lateral or ventrolateral columns of the midbrain periaqueductal gray matter (PAG) in conscious animals produces opposite responses (viz., defensive behavior and pressor responses from the lateral column vs. quiescence and depressor responses from the ventrolateral column), raising the possibility that the two columns are interconnected. To test this hypothesis, two types of anatomical experiments were performed in rats. First, the anterograde axonal marker Phaseolus vulgaris leuco-agglutinin (PHA-L) was injected into individual PAG columns or adjoining regions which included the Edinger-Westphal, dorsal raphe, and precommissural nuclei. The results shows that each column projects bilaterally to all of the other PAG columns, and also provides local connections within its own column. Furthermore, the Edinger-Westphal and precommissural nuclei project to all four PAG columns, while the dorsal raphe nucleus projects only to the ventrolateral and lateral columns. In a second experiment, we found that cardiovascular-related PAG projection neurons of both the lateral and ventrolateral columns receive an input from the reciprocal PAG column. This was demonstrated by a double tracer neuroanatomical study in which PHA-L was first iontophoretically ejected into either the lateral or ventrolateral PAG columns and then, several days later the retrograde transneuronal viral tracer, pseudorabies virus, was injected into the stellate sympathetic ganglion. Intra-PAG circuits were visualized by a dual immunohistochemical procedure. These results suggest that during the fight-or-flight response when the 'fight' program is activated, inhibition of the 'flight' PAG network may occur and the converse situation may occur during the flight response. Copyright 1997 Elsevier Science B.V.

Development of a screening method for the determination of forty-nine priority pollutants in soil

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

Kiang, P.H.T.

1985-01-01

An extraction procedure followed by capillary GC-MS analysis was used to determine soil pollutants. Dual pH solutions with methylene chloride were used as extraction solvent system. Both base/neutral and acidic fractions were analyzed on the same fused silica 30 meter SPB-1 (SE-30) column. A GC-FID with a 60 meter wide-bore SPB-1 glass capillary column was used for quantitative analysis due to its larger sample capacity and higher sensitivity. The precision and accuracy for 5.1 ppm (51 ..mu..g/10 g) concentration in zero soil was less than 25% RSD. A headspace technique was also developed for the determination of volatile compounds. Themore » same instrumental conditions and columns were used as in the extraction procedure. The precision and accuracy for 3 grams soil sample spiked with 5.1 ppm (52 ..mu..g/10 mL) pollutant mixture in a 20 mL vial was less than 3% RSD.« less

Bonded-phase extraction column isolation of organic compounds in groundwater at a hazardous waste site

USGS Publications Warehouse

Rostad, C.E.; Pereira, W.E.; Ratcliff, S.M.

1984-01-01

A procedure for isolation of hazardous organic compounds from water for gas chromatography/mass spectrometry analysis Is presented and applied to creosote- and pentachlorophenol-contaminated groundwater resulting from wood-treatment processes. This simple procedure involved passing a 50-100-mL sample through a bonded-phase extraction column, eluting the trapped organic compounds from the column with 2-4 mL of solvent, and evaporating the sample to 100 ??L with a stream of dry nitrogen, after which the sample was ready for gas chromatography/mass spectrometry analysis. Representative compounds indicative of creosote contamination were used for recovery and precision studies from the cyclohexyl-bonded phase. Recovery of these compounds from n-octyl-, n-octadecyl-, cyclohexyl-, and phenyl-bonded phases was compared. The bonded phase that exhibited the best recovery and least bias toward acidic or basic cmpounds was the n-octadecyl phase. Detailed compound Identification Is given for compounds Isolated from creosote- and pentachlorophenol-contaminated groundwater using the cyclohexyl-bonded phase.

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

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

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

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

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

PubMed

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

2003-10-25

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

Preparation and characterization of fluorophenylboronic acid-functionalized affinity monolithic columns for the selective enrichment of cis-diol-containing biomolecules.

PubMed

Li, Qianjin; Liu, Zhen

2015-01-01

Boronate affinity monolithic columns have been developed into an important means for the selective recognition and capture of cis-diol-containing biomolecules, such as glycoproteins, nucleosides and saccharides. The ligands of boronic acids are playing an important role in boronate affinity monolithic columns. Although several boronate affinity monoliths with high affinity toward cis-diol-containing biomolecules have been reported, only few publications are focused on their detailed procedures for preparation and characterization. This chapter describes in detail the preparation and characterization of a boronate affinity monolithic column applying 2,4-difluoro-3-formyl-phenylboronic acid (DFFPBA) as a ligand. The DFFPBA-functionalized monolithic column not only exhibited an ultrahigh boronate affinity toward cis-diol-containing biomolecules, but also showed great potential for the selective enrichment of cis-diol-containing biomolecules in real samples.

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

PubMed

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

2016-05-06

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

Improved synthesis of carbon-clad silica stationary phases.

PubMed

Haidar Ahmad, Imad A; Carr, Peter W

2013-12-17

Previously, we described a novel method for cladding elemental carbon onto the surface of catalytically activated silica by a chemical vapor deposition (CVD) method using hexane as the carbon source and its use as a substitute for carbon-clad zirconia.1,2 In that method, we showed that very close to exactly one uniform monolayer of Al (III) was deposited on the silica by a process analogous to precipitation from homogeneous solution in order to preclude pore blockage. The purpose of the Al(III) monolayer is to activate the surface for subsequent CVD of carbon. In this work, we present an improved procedure for preparing the carbon-clad silica (denoted CCSi) phases along with a new column packing process. The new method yields CCSi phases having better efficiency, peak symmetry, and higher retentivity compared to carbon-clad zirconia. The enhancements were achieved by modifying the original procedure in three ways: First, the kinetics of the deposition of Al(III) were more stringently controlled. Second, the CVD chamber was flushed with a mixture of hydrogen and nitrogen gas during the carbon cladding process to minimize generation of polar sites by oxygen incorporation. Third, the fine particles generated during the CVD process were exhaustively removed by flotation in an appropriate solvent.

Development of a purification procedure for the isolation of nucleosides from urine prior to mass spectrometric analysis.

PubMed

Dudley, E; El-Shakawi, S; Games, D E; Newton, R P

2000-03-01

A chromatographic separation of nucleosides from urine has been developed in order to facilitate their mass spectrometric analysis for clinical diagnosis. A number of chromatographic resins were studied in order to develop an effective and efficient purification procedure. The optimized sequential protocol comprises a centrifugation, acidification and neutralization step, followed by application of an affinity chromatographic column and finally further separation on an acidic cation exchange column and a basic anion exchanger. This scheme shows effective clean-up of a standard radiolabelled nucleoside with a recovery of 92.5%, and recovery of nucleosides added to urine samples before extraction showed recoveries of 72-82%.

IT-CARES: an interactive tool for case-crossover analyses of electronic medical records for patient safety.

PubMed

Caron, Alexandre; Chazard, Emmanuel; Muller, Joris; Perichon, Renaud; Ferret, Laurie; Koutkias, Vassilis; Beuscart, Régis; Beuscart, Jean-Baptiste; Ficheur, Grégoire

2017-03-01

The significant risk of adverse events following medical procedures supports a clinical epidemiological approach based on the analyses of collections of electronic medical records. Data analytical tools might help clinical epidemiologists develop more appropriate case-crossover designs for monitoring patient safety. To develop and assess the methodological quality of an interactive tool for use by clinical epidemiologists to systematically design case-crossover analyses of large electronic medical records databases. We developed IT-CARES, an analytical tool implementing case-crossover design, to explore the association between exposures and outcomes. The exposures and outcomes are defined by clinical epidemiologists via lists of codes entered via a user interface screen. We tested IT-CARES on data from the French national inpatient stay database, which documents diagnoses and medical procedures for 170 million inpatient stays between 2007 and 2013. We compared the results of our analysis with reference data from the literature on thromboembolic risk after delivery and bleeding risk after total hip replacement. IT-CARES provides a user interface with 3 columns: (i) the outcome criteria in the left-hand column, (ii) the exposure criteria in the right-hand column, and (iii) the estimated risk (odds ratios, presented in both graphical and tabular formats) in the middle column. The estimated odds ratios were consistent with the reference literature data. IT-CARES may enhance patient safety by facilitating clinical epidemiological studies of adverse events following medical procedures. The tool's usability must be evaluated and improved in further research. © The Author 2016. Published by Oxford University Press on behalf of the American Medical Informatics Association.

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.

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.

Simultaneous double-rod rotation technique in posterior instrumentation surgery for correction of adolescent idiopathic scoliosis.

PubMed

Ito, Manabu; Abumi, Kuniyoshi; Kotani, Yoshihisa; Takahata, Masahiko; Sudo, Hideki; Hojo, Yoshihiro; Minami, Akio

2010-03-01

The authors present a new posterior correction technique consisting of simultaneous double-rod rotation using 2 contoured rods and polyaxial pedicle screws with or without Nesplon tapes. The purpose of this study is to introduce the basic principles and surgical procedures of this new posterior surgery for correction of adolescent idiopathic scoliosis. Through gradual rotation of the concave-side rod by 2 rod holders, the convex-side rod simultaneously rotates with the the concave-side rod. This procedure does not involve any force pushing down the spinal column around the apex. Since this procedure consists of upward pushing and lateral translation of the spinal column with simultaneous double-rod rotation maneuvers, it is simple and can obtain thoracic kyphosis as well as favorable scoliosis correction. This technique is applicable not only to a thoracic single curve but also to double major curves in cases of adolescent idiopathic scoliosis.

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

PubMed

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

2016-05-15

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

A novel experimental procedure to investigate the biodegradation of NAPL under unsaturated conditions

NASA Astrophysics Data System (ADS)

Andre, Laurent; Kedziorek, Monika A. M.; Bourg, Alain C. M.; Haeseler, Frank; Blanchet, Denis

2009-05-01

SummarySoils need to be thoroughly investigated regarding their potential for the natural attenuation of non-aqueous phase liquids (NAPL). Laboratory investigations truly representative of degradation processes in field conditions are difficult to implement for porous media partially saturated with water, NAPL and air. We propose an innovative protocol to investigate degradation processes under steady-state vadose zone conditions. Experiments are carried out in glass columns filled with a sand and, as bacteria source, a soil from a diesel-fuel-polluted site. Water and NAPL ( n-hexadecane diluted in heptamethylnonane (HMN)) are added to the porous medium in a two-step procedure using ceramic membranes placed at the bottom of the column. This procedure results, for appropriate experimental conditions, in a uniform distribution of the two fluids (water and NAPL) throughout the column. In a biodegradation experiment non-biodegradable HMN is used to provide NAPL mass, while keeping biodegradable n-hexadecane small enough to monitor its rapid degradation. Biodegradation is followed as a function of time by measuring oxygen consumption, using a respirometer. Degradative activity is controlled by diffusive transfers in the porous network, of oxygen from the gas phase to the water phase and of n-hexadecane from the NAPL phase to the water phase.

30 CFR 735.18 - Grant application procedures.

Code of Federal Regulations, 2010 CFR

2010-07-01

... Column 5A of Forms OSM-51A and OSM-51B which reports the quantitative Program Management information of... of Form OSM-51C which reports the quantitative Program Management information of the Small Operator... use the application forms and procedures specified by OSM in accordance with Office of Management and...

Liquid chromatographic extraction medium

DOEpatents

Horwitz, E. Philip; Dietz, Mark L.

1994-01-01

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

Volatile Transport by Volcanic Plumes on Earth, Venus and Mars

NASA Technical Reports Server (NTRS)

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

2012-01-01

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

Transferring research data to producers

USDA-ARS?s Scientific Manuscript database

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

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

PubMed

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

2016-02-26

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

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

DOEpatents

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

1992-01-01

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

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

DOEpatents

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

1995-01-01

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

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

DOEpatents

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

1995-03-14

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

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

DOEpatents

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

1998-01-01

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

Processes and catalysts for conducting fischer-tropsch synthesis in a slurry bubble column reactor

DOEpatents

Singleton, Alan H.; Oukaci, Rachid; Goodwin, James G.

1999-01-01

Processes and catalysts for conducting Fischer-Tropsch synthesis in a slurry bubble column reactor (SBCR). One aspect of the invention involves the use of cobalt catalysts without noble metal promotion in an SBCR. Another aspect involves using palladium promoted cobalt catalysts in an SBCR. Methods for preparing noble metal promoted catalysts via totally aqueous impregnation and procedures for producing attrition resistant catalysts are also provided.

Comparative evaluation of seven commercial products for human serum enrichment/depletion by shotgun proteomics.

PubMed

Pisanu, Salvatore; Biosa, Grazia; Carcangiu, Laura; Uzzau, Sergio; Pagnozzi, Daniela

2018-08-01

Seven commercial products for human serum depletion/enrichment were tested and compared by shotgun proteomics. Methods were based on four different capturing agents: antibodies (Qproteome Albumin/IgG Depletion kit, ProteoPrep Immunoaffinity Albumin and IgG Depletion Kit, Top 2 Abundant Protein Depletion Spin Columns, and Top 12 Abundant Protein Depletion Spin Columns), specific ligands (Albumin/IgG Removal), mixture of antibodies and ligands (Albumin and IgG Depletion SpinTrap), and combinatorial peptide ligand libraries (ProteoMiner beads), respectively. All procedures, to a greater or lesser extent, allowed an increase of identified proteins. ProteoMiner beads provided the highest number of proteins; Albumin and IgG Depletion SpinTrap and ProteoPrep Immunoaffinity Albumin and IgG Depletion Kit resulted the most efficient in albumin removal; Top 2 and Top 12 Abundant Protein Depletion Spin Columns decreased the overall immunoglobulin levels more than other procedures, whereas specifically gamma immunoglobulins were mostly removed by Albumin and IgG Depletion SpinTrap, ProteoPrep Immunoaffinity Albumin and IgG Depletion Kit, and Top 2 Abundant Protein Depletion Spin Columns. Albumin/IgG Removal, a resin bound to a mixture of protein A and Cibacron Blue, behaved less efficiently than the other products. Copyright © 2018 Elsevier B.V. All rights reserved.

Development of a multiple immunoaffinity column for simultaneous determination of multiple mycotoxins in feeds using UPLC-MS/MS.

PubMed

Hu, Xiaofeng; Hu, Rui; Zhang, Zhaowei; Li, Peiwu; Zhang, Qi; Wang, Min

2016-09-01

A sensitive and specific immunoaffinity column to clean up and isolate multiple mycotoxins was developed along with a rapid one-step sample preparation procedure for ultra-performance liquid chromatography-tandem mass spectrometry analysis. Monoclonal antibodies against aflatoxin B1, aflatoxin B2, aflatoxin G1, aflatoxin G2, zearalenone, ochratoxin A, sterigmatocystin, and T-2 toxin were coupled to microbeads for mycotoxin purification. We optimized a homogenization and extraction procedure as well as column loading and elution conditions to maximize recoveries from complex feed matrices. This method allowed rapid, simple, and simultaneous determination of mycotoxins in feeds with a single chromatographic run. Detection limits for these toxins ranged from 0.006 to 0.12 ng mL(-1), and quantitation limits ranged from 0.06 to 0.75 ng mL(-1). Concentration curves were linear from 0.12 to 40 μg kg(-1) with correlation coefficients of R (2) > 0.99. Intra-assay and inter-assay comparisons indicated excellent repeatability and reproducibility of the multiple immunoaffinity columns. As a proof of principle, 80 feed samples were tested and several contained multiple mycotoxins. This method is sensitive, rapid, and durable enough for multiple mycotoxin determinations that fulfill European Union and Chinese testing criteria.

Improved quality-by-design compliant methodology for method development in reversed-phase liquid chromatography.

PubMed

Debrus, Benjamin; Guillarme, Davy; Rudaz, Serge

2013-10-01

A complete strategy dedicated to quality-by-design (QbD) compliant method development using design of experiments (DOE), multiple linear regressions responses modelling and Monte Carlo simulations for error propagation was evaluated for liquid chromatography (LC). The proposed approach includes four main steps: (i) the initial screening of column chemistry, mobile phase pH and organic modifier, (ii) the selectivity optimization through changes in gradient time and mobile phase temperature, (iii) the adaptation of column geometry to reach sufficient resolution, and (iv) the robust resolution optimization and identification of the method design space. This procedure was employed to obtain a complex chromatographic separation of 15 antipsychotic basic drugs, widely prescribed. To fully automate and expedite the QbD method development procedure, short columns packed with sub-2 μm particles were employed, together with a UHPLC system possessing columns and solvents selection valves. Through this example, the possibilities of the proposed QbD method development workflow were exposed and the different steps of the automated strategy were critically discussed. A baseline separation of the mixture of antipsychotic drugs was achieved with an analysis time of less than 15 min and the robustness of the method was demonstrated simultaneously with the method development phase. Copyright © 2013 Elsevier B.V. All rights reserved.

Experimental design of a twin-column countercurrent gradient purification process.

PubMed

Steinebach, Fabian; Ulmer, Nicole; Decker, Lara; Aumann, Lars; Morbidelli, Massimo

2017-04-07

As typical for separation processes, single unit batch chromatography exhibits a trade-off between purity and yield. The twin-column MCSGP (multi-column countercurrent solvent gradient purification) process allows alleviating such trade-offs, particularly in the case of difficult separations. In this work an efficient and reliable procedure for the design of the twin-column MCSGP process is developed. This is based on a single batch chromatogram, which is selected as the design chromatogram. The derived MCSGP operation is not intended to provide optimal performance, but it provides the target product in the selected fraction of the batch chromatogram, but with higher yield. The design procedure is illustrated for the isolation of the main charge isoform of a monoclonal antibody from Protein A eluate with ion-exchange chromatography. The main charge isoform was obtained at a purity and yield larger than 90%. At the same time process related impurities such as HCP and leached Protein A as well as aggregates were at least equally well removed. Additionally, the impact of several design parameters on the process performance in terms of purity, yield, productivity and buffer consumption is discussed. The obtained results can be used for further fine-tuning of the process parameters so as to improve its performance. Copyright © 2017 Elsevier B.V. All rights reserved.

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

PubMed

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

2017-01-01

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

Semiconductor radiation detector

DOEpatents

Bell, Zane W.; Burger, Arnold

2010-03-30

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

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

DOEpatents

Fitzsimmons, Jonathan M.; Atcher, Robert W.

2010-06-01

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

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

NASA Technical Reports Server (NTRS)

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

1971-01-01

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

Comparing monolithic and fused core HPLC columns for fast chromatographic analysis of fat-soluble vitamins.

PubMed

Kurdi, Said El; Muaileq, Dina Abu; Alhazmi, Hassan A; Bratty, Mohammed Al; Deeb, Sami El

2017-06-27

HPLC stationary phases of monolithic and fused core type can be used to achieve fast chromatographic separation as an alternative to UPLC. In this study, monolithic and fused core stationary phases are compared for fast separation of four fat-soluble vitamins. Three new methods on the first and second generation monolithic silica RP-18e columns and a fused core pentafluoro-phenyl propyl column were developed. Application of three fused core columns offered comparable separations of retinyl palmitate, DL-α-tocopheryl acetate, cholecalciferol and menadione in terms of elution speed and separation efficiency. Separation was achieved in approx. 5 min with good resolution (Rs > 5) and precision (RSD ≤ 0.6 %). Monolithic columns showed, however, a higher number of theoretical plates, better precision and lower column backpressure than the fused core column. The three developed methods were successfully applied to separate and quantitate fat-soluble vitamins in commercial products.

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.

QSPR models for predicting generator-column-derived octanol/water and octanol/air partition coefficients of polychlorinated biphenyls.

PubMed

Yuan, Jintao; Yu, Shuling; Zhang, Ting; Yuan, Xuejie; Cao, Yunyuan; Yu, Xingchen; Yang, Xuan; Yao, Wu

2016-06-01

Octanol/water (K(OW)) and octanol/air (K(OA)) partition coefficients are two important physicochemical properties of organic substances. In current practice, K(OW) and K(OA) values of some polychlorinated biphenyls (PCBs) are measured using generator column method. Quantitative structure-property relationship (QSPR) models can serve as a valuable alternative method of replacing or reducing experimental steps in the determination of K(OW) and K(OA). In this paper, two different methods, i.e., multiple linear regression based on dragon descriptors and hologram quantitative structure-activity relationship, were used to predict generator-column-derived log K(OW) and log K(OA) values of PCBs. The predictive ability of the developed models was validated using a test set, and the performances of all generated models were compared with those of three previously reported models. All results indicated that the proposed models were robust and satisfactory and can thus be used as alternative models for the rapid assessment of the K(OW) and K(OA) of PCBs. Copyright © 2016 Elsevier Inc. All rights reserved.

TEFLON BELLOWS PULSE GENERATORS FOR SOLVENT EXTRACTION PULSE COLUMNS

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

McCarthy, P.B.

1954-01-01

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

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

PubMed

Vasdev, Neil; Collier, Thomas Lee

2016-08-17

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

Liquid chromatographic extraction medium

DOEpatents

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

1994-09-13

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

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

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

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

2013-08-15

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

Dynamic Pressure Calibration Standard

NASA Technical Reports Server (NTRS)

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

1986-01-01

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

Internal waves interacting with particles in suspension

NASA Astrophysics Data System (ADS)

Micard, Diane

2016-04-01

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

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

PubMed

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

2017-10-10

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

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

PubMed Central

Li, Yuwei; Li, Ang; Junge, Jason

2017-01-01

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

76 FR 61999 - Energy Conservation Program for Consumer Products: Test Procedures for Residential Furnaces and...

Federal Register 2010, 2011, 2012, 2013, 2014

2011-10-06

... for Residential Furnaces and Boilers (Standby Mode and Off Mode); Correction AGENCY: Office of Energy... Consumer Products: Test Procedures for Residential Furnaces and Boilers. This correction provides the... page 56339, in the third column after ``2. E- mail:'' the e-mail address should read `` FurnaceBoiler...

Validated Test Method 1314: Liquid-Solid Partitioning as a Function of Liquid-Solid Ratio for Constituents in Solid Materials Using An Up-Flow Percolation Column Procedure

EPA Pesticide Factsheets

Describes procedures written based on the assumption that they will be performed by analysts who are formally trained in at least the basic principles of chemical analysis and in the use of the subject technology.

Rapid analytical procedure for determination of mineral oils in edible oil by GC-FID.

PubMed

Wrona, Magdalena; Pezo, Davinson; Nerin, Cristina

2013-12-15

A procedure for the determination of mineral oils in edible oil has been fully developed. The procedure consists of using a sulphuric acid-impregnated silica gel (SAISG) glass column to eliminate the fat matter. A chemical combustion of the fatty acids takes place, while the mineral oils are not affected by the sulphuric acid. The column is eluted with hexane using a vacuum pump and the final extract is concentrated and analysed by gas chromatography (GC) with flame ionisation detector (FID). The detection limit (LOD) and the quantification limit (LOQ) in hexane were 0.07 and 0.21 μg g(-1) respectively and the LOQ in vegetable oil was 1 μg g(-1). Only a few minutes were necessary for sample treatment to have a clean extract. The efficiency of the process, measured through the recoveries from spiked samples of edible oil was higher than 95%. The procedure has been applied to determine mineral oil in olive oil from the retailed market. Copyright © 2013 Elsevier Ltd. All rights reserved.

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

NASA Astrophysics Data System (ADS)

Gao, Yanjiao; Liu, Rui

2017-11-01

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

Cryogenic focussing, ohmically heated on-column trap

NASA Technical Reports Server (NTRS)

Springston, Stephen R.

1991-01-01

A procedure is described for depositing a conductive layer of gold on the exterior of a fused-silica capillary used in gas chromatography. By subjecting a section of the column near the inlet to a thermal cycle of cryogenic cooling and ohmic heating, volatile samples are concentrated and subsequently injected. The performance of this trap as a chromatographic injector is demonstrated. Several additional applications are suggested and the unique properties of this device are discussed.

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.

Processes and catalysts for conducting Fischer-Tropsch synthesis in a slurry bubble column reactor

DOEpatents

Singleton, A.H.; Oukaci, R.; Goodwin, J.G.

1999-08-17

Processes and catalysts are disclosed for conducting Fischer-Tropsch synthesis in a slurry bubble column reactor (SBCR). One aspect of the invention involves the use of cobalt catalysts without noble metal promotion in an SBCR. Another aspect involves using palladium promoted cobalt catalysts in an SBCR. Methods for preparing noble metal promoted catalysts via totally aqueous impregnation and procedures for producing attrition resistant catalysts are also provided. 1 fig.

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

DOEpatents

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

1992-12-01

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

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

DOEpatents

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

1998-09-29

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

Spermatozoa with numerical chromosomal abnormalities are more prone to be retained by Annexin V-MACS columns.

PubMed

Esbert, M; Godo, A; Soares, S R; Florensa, M; Amorós, D; Ballesteros, A; Vidal, F

2017-07-01

Colloidal super-paramagnetic microbeads conjugated with annexin V are effective for separating apoptotic spermatozoa by MACS as a result of the high affinity of annexin V for externalized PS molecules. The effectiveness of the procedure in reducing the percentage of sperm with fragmented DNA and abnormal morphology has also been reported. However, it is still unknown if it could decrease the percentage of aneuploid spermatozoa. The objective of our prospective study, performed on 16 males with abnormal FISH on spermatozoa, was to assess if MACS columns were useful tools to retain spermatozoa carrying chromosomal abnormalities in semen samples processed after density gradient centrifugation (DGC). The pellet obtained after DGC was subjected to MACS, and sperm FISH analyses were performed both in the eluded fraction and in the fraction retained in the column. The observed frequencies of disomy and nullisomy 13, 18, and 21, X and Y, as well as the diploidy rates in the MACS eluded fraction and the fraction retained in the MACS column were recorded. We observed that the frequencies of aneuploidies in the eluded fraction were lower than in the fraction retained in the MACS column (0.59% vs. 0.75%; p = 0.010). DGC determined a significant reduction in sperm concentration (z-ratio = 2.83; p = 0.005) and a significant increase in sperm progressive motility (z-ratio = -3.5; p < 0.001). MACS also led to a significant reduction in sperm concentration (z-ratio = 3.14; p = 0.002) and a significant increase in progressive motility (z-ratio = -2.59; p = 0.01) when compared with the post-DGC sample. Sperm concentration was similar in the two fractions generated by MACS (z-ratio = 0.63; p = 0.52), while progressive motility was significantly higher in the MACS eluded fraction (z-ratio = 2.42; p = 0.02). According to our results, MACS columns are able to selectively retain spermatozoa carrying chromosomal abnormalities. Furthermore, the performance of DGC and MACS on semen samples leads to an enrichment of progressive motility. © 2017 American Society of Andrology and European Academy of Andrology.

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

PubMed

Nagatsu, T; Oka, K; Kato, T

1979-07-21

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

Method for liquid chromatographic extraction of strontium from acid solutions

DOEpatents

Horwitz, E. Philip; Dietz, Mark L.

1992-01-01

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

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.

Spine segmentation from C-arm CT data sets: application to region-of-interest volumes for spinal interventions

NASA Astrophysics Data System (ADS)

Buerger, C.; Lorenz, C.; Babic, D.; Hoppenbrouwers, J.; Homan, R.; Nachabe, R.; Racadio, J. M.; Grass, M.

2017-03-01

Spinal fusion is a common procedure to stabilize the spinal column by fixating parts of the spine. In such procedures, metal screws are inserted through the patients back into a vertebra, and the screws of adjacent vertebrae are connected by metal rods to generate a fixed bridge. In these procedures, 3D image guidance for intervention planning and outcome control is required. Here, for anatomical guidance, an automated approach for vertebra segmentation from C-arm CT images of the spine is introduced and evaluated. As a prerequisite, 3D C-arm CT images are acquired covering the vertebrae of interest. An automatic model-based segmentation approach is applied to delineate the outline of the vertebrae of interest. The segmentation approach is based on 24 partial models of the cervical, thoracic and lumbar vertebrae which aggregate information about (i) the basic shape itself, (ii) trained features for image based adaptation, and (iii) potential shape variations. Since the volume data sets generated by the C-arm system are limited to a certain region of the spine the target vertebra and hence initial model position is assigned interactively. The approach was trained and tested on 21 human cadaver scans. A 3-fold cross validation to ground truth annotations yields overall mean segmentation errors of 0.5 mm for T1 to 1.1 mm for C6. The results are promising and show potential to support the clinician in pedicle screw path and rod planning to allow accurate and reproducible insertions.

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

PubMed

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

2006-08-01

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

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

PubMed

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

2013-11-01

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

Significance of fixation of the vertebral column for spinal cord injury experiments.

PubMed

Liu, Fei; Luo, Zhuo-Jin; You, Si-Wei; Jiao, Xi-Ying; Meng, Xiao-Mei; Shi, Ming; Wang, Chun-Ting; Ju, Gong

2003-08-01

Thoracic spinal cord transections were performed in adult rats. The animals were divided into two groups, with or without internal fixation of the involved vertebral column. Histologic and immunohistochemical studies were performed to compare the effect of internal fixation of the vertebral column. To find out the aspects and extent of beneficial effects of vertebral column fixation for spinal cord repair. Vertebral column fixation is a routine procedure in clinical spinal cord surgery. Paradoxically, most, if not all, animal spinal cord experiments seem to have ignored the importance of vertebral column fixation. During trunk movements, the vertebral column flexes to different directions, accompanied by bending of the spinal cord. Following spinal cord lesions, with frequent bending of the cord there will be repeated bleeding, inflammation, and other pathologic processes at the lesion site. Thus, the healing process will be hampered. The severity of the damages that will be brought about by bending of the cord is, to a certain degree, unpredictable. There will be rather big individual variations in injury and repair among the same type of experiments, rendering quantification and conclusion difficult. Adult Sprague-Dawley rats were used. The thoracic spinal cord was transected. Strong stainless steel wires were used for internal fixation of the vertebral column. The histology of the horizontal sections of the spinal cord segment, which included the lesion site, was examined at the 14th postoperative day. The volumes of the secondary degeneration and meningeal scar, the gap between the borders of the proximal and distal stumps of the transected spinal cord, the thickness of the meningeal scar, the astrocytic reaction, and the abundance of regenerating nerve fibers at the lesion site were compared between the vertebral column fixed and nonfixed groups. Whenever possible, the results were evaluated quantitatively. In all these aspects, the internally fixed group was consistently far better than the unfixed group. The quantitative analyses were as follows (fixed/unfixed): 1)volume of secondary degeneration: 1.07 +/- 0.20/1.81 +/- 0.43 mm3 (P < 0.01); 2) volume of meningeal scar: 2.38 +/- 0.55/4.34 +/- 1.40 mm3 (P < 0.05); 3) distance between cord stumps: 1.38 +/- 0.34/2.35 +/- 0.79 mm (P < 0.05); 4) the mean thinnest dimension of the meningeal scar: 0.90 +/- 0.43/1.98 +/- 0.85 mm (P < 0.05). Vertebral column fixation is a crucial procedure for spinal cord animal experiments.

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

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

Jeong, J M; Knapp Jr, Russ F

2008-01-01

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

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

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

Knapp Jr, Russ F; Jeong, J M

2008-01-01

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

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

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

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

2009-07-15

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

Investigation of Pinus mugo essential oil oxygenated fraction by combined use of gas chromatography and dry column chromatography.

PubMed

A, M B; Coran, S A; Giannellini, V; Vincieri, F F; Moneti, G

1981-09-01

The oxygenated compounds of Pinus mugo Turra essential oil were investigated by a combination of GC and dry column chromatography (DCC) coordinated by GC data processing. The collected data resulted in a bar graph ("normalized" gas chromatogram) giving the RRT's and relative amounts of 68 components; 38 of them were identified by MS and IR. The described procedure may be used for essential oil analysis in general.

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

NASA Astrophysics Data System (ADS)

Kvaltin, J.

1990-06-01

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

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

PubMed

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

2014-01-01

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

Purification of NAD glycohydrolase from Agkistrodon acutus venom.

PubMed

Wu, Shuang Ding; Liu, Yanli; Xu, Xiaolong; Zhu, Zhengang

2002-07-01

NAD glycohydrolase (NADase) from Agkistrodon acutus venom was purified to electrophoretic homogeneity by a fast, reproducible 3-step procedure including Q Sepharose Fast Flow, Superdex 75, and Mono S column chromatography. This new procedure gave a 15.6-fold purification with a recovery yield of 7.9% and a specific activity of 12.8 units/mg.

75 FR 81474 - Approval and Promulgation of Air Quality Implementation Plans; West Virginia; Update to Materials...

Federal Register 2010, 2011, 2012, 2013, 2014

2010-12-28

... revised the procedures for incorporating by reference Federally-approved SIPs as a result of consultations... procedures and ``Identification of plan'' format are discussed in further detail in the May 22, 1997 Federal... column so that the date format is consistent with that found throughout the paragraph. c. 45 CSR 21...

Microdynamics of the piezo-driven pipettes in ICSI.

PubMed

Ediz, Kerem; Olgac, Nejat

2004-07-01

Undesirably low success rates have been reported in the intracytoplasmic sperm injection procedure. Recently a method using piezo-driven pipettes with a very small mercury column contributed substantial improvements in this process. Despite the toxicity of mercury, this new procedure is commonly utilized in many laboratories. However, there is no study available to date on the micromechanics of this procedure. The underlying principles of piercing are not clear for both cases, with and without the mercury. Presently, the pressure burst, which is caused by the abrupt axial motion of the mercury column, is attributed to this effect. Here, we take the mercury-filled pipettes and try to understand the governing physics. The findings point out the occurrence of considerable lateral tip oscillations of the injection pipette as the piezoelectric pulse train is introduced. We claim that the lateral dynamics play an important role in the piercing and should be considered to enlighten the process and the effects of the mercury. These claims are analytically studied and experimentally verified.

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

PubMed Central

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

2011-01-01

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

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

NASA Astrophysics Data System (ADS)

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

2014-03-01

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

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

NASA Technical Reports Server (NTRS)

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

1971-01-01

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

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

NASA Technical Reports Server (NTRS)

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

1992-01-01

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

Simple interface of high-performance liquid chromatography-atomic fluorescence spectrometry hyphenated system for speciation of mercury based on photo-induced chemical vapour generation with formic acid in mobile phase as reaction reagent.

PubMed

Yin, Yongguang; Liu, Jingfu; He, Bin; Shi, Jianbo; Jiang, Guibin

2008-02-15

Photo-induced chemical vapour generation (CVG) with formic acid in mobile phase as reaction reagent was developed as interface to on-line couple HPLC with atomic fluorescence spectrometry for the separation and determination of inorganic mercury, methylmercury (MeHg), ethylmercury (EtHg) and phenylmercury (PhHg). In the developed procedure, formic acid in mobile phase was used to decompose organomercuries and reduce Hg(2+) to mercury cold vapour under UV irradiation. Therefore, no post-column reagent was used and the flow injection system in traditional procedure is omitted. A number of operating parameters including pH of mobile phase, concentration of formate, flow rate of mobile phase, length of PTFE reaction coil, flow rate of carrier gas and Na(2)S(2)O(3) in sample matrix were optimized. The limits of detection at the optimized conditions were 0.085, 0.033, 0.029 and 0.038 microg L(-1) for inorganic mercury, MeHg, EtHg and PhHg, respectively. The developed method was validated by determination of certified reference material DORM-2 and was further applied in analyses of seafood samples from Yantai port, China. The UV-CVG with formic acid simplifies the instrumentation and reduces the analytical cost significantly.

Robust alignment of chromatograms by statistically analyzing the shifts matrix generated by moving window fast Fourier transform cross-correlation.

PubMed

Zhang, Mingjing; Wen, Ming; Zhang, Zhi-Min; Lu, Hongmei; Liang, Yizeng; Zhan, Dejian

2015-03-01

Retention time shift is one of the most challenging problems during the preprocessing of massive chromatographic datasets. Here, an improved version of the moving window fast Fourier transform cross-correlation algorithm is presented to perform nonlinear and robust alignment of chromatograms by analyzing the shifts matrix generated by moving window procedure. The shifts matrix in retention time can be estimated by fast Fourier transform cross-correlation with a moving window procedure. The refined shift of each scan point can be obtained by calculating the mode of corresponding column of the shifts matrix. This version is simple, but more effective and robust than the previously published moving window fast Fourier transform cross-correlation method. It can handle nonlinear retention time shift robustly if proper window size has been selected. The window size is the only one parameter needed to adjust and optimize. The properties of the proposed method are investigated by comparison with the previous moving window fast Fourier transform cross-correlation and recursive alignment by fast Fourier transform using chromatographic datasets. The pattern recognition results of a gas chromatography mass spectrometry dataset of metabolic syndrome can be improved significantly after preprocessing by this method. Furthermore, the proposed method is available as an open source package at https://github.com/zmzhang/MWFFT2. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

NASA Astrophysics Data System (ADS)

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

2018-01-01

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

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

PubMed

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

1986-07-01

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

Rapid sequential determination of Pu, 90Sr and 241Am nuclides in environmental samples using an anion exchange and Sr-Spec resins.

PubMed

Lee, M H; Ahn, H J; Park, J H; Park, Y J; Song, K

2011-02-01

This paper presents a quantitative and rapid method of sequential separation of Pu, (90)Sr and (241)Am nuclides in environmental soil samples with an anion exchange resin and Sr Spec resin. After the sample solution was passed through an anion exchange column connected to a Sr Spec column, Pu isotopes were purified from the anion exchange column. Strontium-90 was separated from other interfering elements by the Sr Spec column. Americium-241 was purified from lanthanides by the anion exchange resin after oxalate co-precipitation. Measurement of Pu and Am isotopes was carried out using an α-spectrometer. Strontium-90 was measured by a low-level liquid scintillation counter. The radiochemical procedure of Pu, (90)Sr and (241)Am nuclides investigated in this study validated by application to IAEA reference materials and environmental soil samples. Copyright © 2010 Elsevier Ltd. All rights reserved.

Development of procedures for programmable proximity aperture lithography

NASA Astrophysics Data System (ADS)

Whitlow, H. J.; Gorelick, S.; Puttaraksa, N.; Napari, M.; Hokkanen, M. J.; Norarat, R.

2013-07-01

Programmable proximity aperture lithography (PPAL) with MeV ions has been used in Jyväskylä and Chiang Mai universities for a number of years. Here we describe a number of innovations and procedures that have been incorporated into the LabView-based software. The basic operation involves the coordination of the beam blanker and five motor-actuated translators with high accuracy, close to the minimum step size with proper anti-collision algorithms. By using special approaches, such writing calibration patterns, linearisation of position and careful backlash correction the absolute accuracy of the aperture size and position, can be improved beyond the standard afforded by the repeatability of the translator end-point switches. Another area of consideration has been the fluence control procedures. These involve control of the uniformity of the beam where different approaches for fluence measurement such as simultaneous aperture current and the ion current passing through the aperture using a Faraday cup are used. Microfluidic patterns may contain many elements that make-up mixing sections, reaction chambers, separation columns and fluid reservoirs. To facilitate conception and planning we have implemented a .svg file interpreter, that allows the use of scalable vector graphics files produced by standard drawing software for generation of patterns made up of rectangular elements.

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

NASA Astrophysics Data System (ADS)

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

2017-07-01

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

The Measurement of Human Body-Fluid Volumes: Resting Fluid Volumes Before and After Heat Acclimation

DTIC Science & Technology

2001-01-01

equilibration period. Erythrocytes aliquots were haemolysed before counting with saponin . Both counts were used to correct the derived ECFV, which was...was largely in accordance with the procedures of Greenleaf et al. (1980). This technique used an extraction procedure in which the dye was first...collection. Therefore, the above extraction procedure was not used. A major limitation of using a cellulose column is the possibility of not collecting all

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

PubMed

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

2015-08-01

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

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

NASA Technical Reports Server (NTRS)

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

1974-01-01

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

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

DTIC Science & Technology

2005-02-01

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

Molecular Analysis Research at Community College of Philadelphia

DTIC Science & Technology

2015-09-21

projects presented below fall under the category of "molecular genetics ", as presented in ARO Solicitation Number W911NF-12-R-0012-01. These projects...role of the GADD45 family of genes in innate immunity and sepsis. In addition to studying genetic components of the molecular response of myeloid...Equipment in left  column, procedure in right column.  kinetics of these molecular signaling pathways in genetic variants (gene KO models) has yet to

TH-EF-BRB-05: 4pi Non-Coplanar IMRT Beam Angle Selection by Convex Optimization with Group Sparsity Penalty

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

O’Connor, D; Nguyen, D; Voronenko, Y

Purpose: Integrated beam orientation and fluence map optimization is expected to be the foundation of robust automated planning but existing heuristic methods do not promise global optimality. We aim to develop a new method for beam angle selection in 4π non-coplanar IMRT systems based on solving (globally) a single convex optimization problem, and to demonstrate the effectiveness of the method by comparison with a state of the art column generation method for 4π beam angle selection. Methods: The beam angle selection problem is formulated as a large scale convex fluence map optimization problem with an additional group sparsity term thatmore » encourages most candidate beams to be inactive. The optimization problem is solved using an accelerated first-order method, the Fast Iterative Shrinkage-Thresholding Algorithm (FISTA). The beam angle selection and fluence map optimization algorithm is used to create non-coplanar 4π treatment plans for several cases (including head and neck, lung, and prostate cases) and the resulting treatment plans are compared with 4π treatment plans created using the column generation algorithm. Results: In our experiments the treatment plans created using the group sparsity method meet or exceed the dosimetric quality of plans created using the column generation algorithm, which was shown superior to clinical plans. Moreover, the group sparsity approach converges in about 3 minutes in these cases, as compared with runtimes of a few hours for the column generation method. Conclusion: This work demonstrates the first non-greedy approach to non-coplanar beam angle selection, based on convex optimization, for 4π IMRT systems. The method given here improves both treatment plan quality and runtime as compared with a state of the art column generation algorithm. When the group sparsity term is set to zero, we obtain an excellent method for fluence map optimization, useful when beam angles have already been selected. NIH R43CA183390, NIH R01CA188300, Varian Medical Systems; Part of this research took place while D. O’Connor was a summer intern at RefleXion Medical.« less

Potential of capillary-column-switching liquid chromatography-tandem mass spectrometry for the quantitative trace analysis of small molecules. Application to the on-line screening of drugs in water.

PubMed

Pitarch, Elena; Hernandez, Felix; ten Hove, Jan; Meiring, Hugo; Niesing, Willem; Dijkman, Ellen; Stolker, Linda; Hogendoorn, Elbert

2004-03-26

We have investigated the potential of capillary-column-switching liquid chromatography coupled to tandem mass spectrometry (cLC-MS-MS) for the quantitative on-line trace analysis of target compounds in aqueous solutions. The technical design of the nano-scale cLC system developed at our Institute for peptide and protein identification has been tested and evaluated for the direct trace analysis of drugs in water samples. Sulphametoxazole, bezafibrate, metoprolol, carbamazepine and bisoprolol occurring frequently in Dutch waters, were selected as test compounds. Adequate conditions for trapping, elution and MS-MS detection were investigated by employing laboratory made 200 microm i.d. capillary columns packed with 5 microm aqua C18 material. In the final cLC-MS-MS conditions, a 1 cm length trapping column and a 4 cm length analytical column were selected. Under these conditions, the target compounds could be directly determined in water down to a level of around 50 ng/l employing only 25 microl of water sample. Validation was done by recovery experiments in ground-, surface- and drinking-water matrices as well as by the analysis of water samples with incurred residues and previously analyzed with a conventional procedure involving off-line solid-phase extraction and narrow-bore LC with MS-MS detection. The new methodology provided recoveries (50-500 ng/l level) between 50 and 114% with RSDs (n = 3, each level) below 20% for most of the compounds. Despite the somewhat less analytical performance in comparison to the conventional procedure, the on-line approach of the new methodology is very suitable for screening of drugs in aqueous samples.

40 CFR Appendix E to Part 63 - Monitoring Procedure for Nonthoroughly Mixed Open Biological Treatment Systems at Kraft Pulp...

Code of Federal Regulations, 2014 CFR

2014-07-01

... for each data set that is collected during the initial performance test. A single composite value of... Multiple Zone Concentrations Calculations Procedure based on inlet and outlet concentrations (Column A of... composite value of Ks discussed in section III.C of this appendix. This value of Ks is calculated during the...

Rapid non-enzymatic extraction method for isolating PCR-quality camelpox virus DNA from skin.

PubMed

Yousif, A Ausama; Al-Naeem, A Abdelmohsen; Al-Ali, M Ahmad

2010-10-01

Molecular diagnostic investigations of orthopoxvirus (OPV) infections are performed using a variety of clinical samples including skin lesions, tissues from internal organs, blood and secretions. Skin samples are particularly convenient for rapid diagnosis and molecular epidemiological investigations of camelpox virus (CMLV). Classical extraction procedures and commercial spin-column-based kits are time consuming, relatively expensive, and require multiple extraction and purification steps in addition to proteinase K digestion. A rapid non-enzymatic procedure for extracting CMLV DNA from dried scabs or pox lesions was developed to overcome some of the limitations of the available DNA extraction techniques. The procedure requires as little as 10mg of tissue and produces highly purified DNA [OD(260)/OD(280) ratios between 1.47 and 1.79] with concentrations ranging from 6.5 to 16 microg/ml. The extracted CMLV DNA was proven suitable for virus-specific qualitative and, semi-quantitative PCR applications. Compared to spin-column and conventional viral DNA extraction techniques, the two-step extraction procedure saves money and time, and retains the potential for automation without compromising CMLV PCR sensitivity. Copyright (c) 2010 Elsevier B.V. All rights reserved.

Determination of available phosphorus in soils by using a new extraction procedure and a flow injection amperometric system.

PubMed

Jakmunee, Jaroon; Junsomboon, Jaroon

2009-09-15

A new extraction procedure based on an off-line extraction column was proposed for extracting of available phosphorus from soils. The column was fabricated from a plastic syringe fitted at the bottom with a cotton wool and a piece of filter paper to support a soil sample. An aliquot (50 mL) of extracting solution (0.05 M HCl+0.0125 M H(2)SO(4)) was used to extract the sample under gravity flow and the eluate was collected in a polyethylene bottle. The extract was then analyzed for phosphorus contents by a simple flow injection amperometric system, employing a set of three-way solenoid valves as an injection valve. The method is based on the electrochemical reduction of 12-molybdophosphate which is produced on-line by the reaction of orthophosphate with acidic molybdate and the electrical current produced was directly proportional to the concentration of phosphate in range of 0.1-10.0 mg L(-1) PO(4)-P, with a detection limit of 0.02 mg L(-1). Relative standard for 11 replicate injections of 5 mg L(-1) PO(4)-P was 0.5%. A sample through put of 35 h(-1) was achieved, with consumption of 14 mg KCl, 10mg ammonium molybdate and 0.05 mL H(2)SO(4) per analysis. The detection system does not suffer from the interferences that are encountered in the photometric method such as colored substances, colloids, metal ions, silicate and refractive index effect (Schlieren effect). The results obtained by the column extraction procedure were well correlated with those obtained by the steady-state extraction procedure, but showed slightly higher extraction efficiency.

Variable surgical outcomes after hospital consolidation: Implications for local health care delivery.

PubMed

Chang, Victor; Blackwell, Robert H; Yau, Ryan M; Besser, Stephanie; Albright, Joslyn M; Gupta, Gopal N; Kuo, Paul C; Kothari, Anai N

2016-11-01

With more hospital consolidations as an inevitable part of our future health care ecosystem, we investigated the relationship between hospital consolidations and operative outcomes. Using the Health Care Cost and Utilization Project State Inpatient Database (Florida and California), the American Hospital Association Annual Survey Database, and Medicare's Case Mix Index data, we identified 19 hospitals that consolidated between 2007 and 2013 and propensity matched them with 19 independent hospitals, using patient and hospital characteristics. One year before consolidation and again 1 year after, we used difference-in-differences analysis to compare changes in the risk-adjusted complication rate of 7 elective operations performed in the consolidated hospitals and in the matched control group. Of the 7 procedures studied, 2 procedures saw a decrease in complication rate (lumbar and lumbosacral fusion of the posterior column posterior technique, difference-in-differences = -0.6%, P < .01; total hip replacement, difference-in-differences = -0.6%, P < .01); 3 procedures saw an increase in complication rate (transurethral prostatectomy, difference-in-differences = 4.1%, P < .01; cervical fusion of the anterior column anterior technique, difference-in-differences = 1.5%, P < .01; total knee replacement, difference-in-differences = 0.3%, P < .01); and 2 procedures saw no change in complication rate (laparoscopic cholecystectomy, lumbar and lumbosacral fusion of the anterior column posterior technique, both P > .05) after hospital consolidation. Arguments have been made that consolidated health care systems can share high-performing clinical services and infrastructure resources, such as electronic medical records, to improve quality. Our results indicate that hospital consolidation does not uniformly improve postoperative complication rates. Copyright © 2016 Elsevier Inc. All rights reserved.

Gas chromatographic/mass spectrometric analysis of the essential oil of Houttuynia cordata Thunb by using on-column methylation with tetramethylammonium acetate.

PubMed

Ch, Muhammad Ishtiaq; Wen, Yang F; Cheng, YiYu

2007-01-01

This paper describes a simple and novel on-column derivatization procedure used with gas chromatography/mass spectrometry (GC/MS) for the analysis of essential oil of Houttuynia cordata Thunb (HCT), a traditional Chinese medicine. In the procedure, the essential oil was obtained by hydrodistillation, and the fatty acid components were derivatized with tetramethylammonium acetate (TMAA) at 250 degrees C and identified by GC/MS. Methylation improved the determination of both the fatty acids and the other components in the essential oil of HCT. To obtain optimum methylation conditions, several important factors were investigated with pentadecane as the internal standard and a GC inlet temperature of 250 degres C. Tetramethylammonium hydroxide (TMAH) and TMAA were compared as the derivatization agent, and a 2:1 ratio of TMAA to capric acid was evaluated. Fatty acid methyl esters produced good chromatographic peak shapes and did not interfere with the determination of dodecanal and caryophyllene. TMAA is a neutral methylation reagent, and it yielded no side reactions during derivatization. It was found that the fatty acid content of the essential oil was about 81%; among the methylated fatty acids found were capric acid, methyl (43.66%), methyl laurate (16.15%), methyl hexadecanoate (9.27%), undecanoic acid, methyl (5.62%), methyl oleate (1.98%), and methyl linoleate (1.40%). Other major constituents were (-)-beta-pinene (1.02%), beta-myrcene (1.62%), 1-terpinen-4-ol (1.59%), decanal (1.49%), and 2-undecanone (1.47%). The results obtained demonstrated good efficiency for the procedure. Pure chromatograms allowed quantitation, which was obtained by total volume integration. The on-column derivatization procedure was simple to perform, and it improved the sensitivity, the peak resolution, and the selectivity of the GC/MS determination.

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

PubMed Central

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

2013-01-01

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

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

NASA Technical Reports Server (NTRS)

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

2000-01-01

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

Scaling a Conditional Proximity Matrix to Symmetry.

ERIC Educational Resources Information Center

Levin, Joseph; Brown, Morton

1979-01-01

Two least squares procedures for symmetrization of a conditional proximity matrix are derived. The solutions provide multiplicative constants for scaling the rows or columns of the matrix to maximize symmetry. (Author/JKS)

Collapse of a Liquid Column: Numerical Simulation and Experimental Validation

NASA Astrophysics Data System (ADS)

Cruchaga, Marcela A.; Celentano, Diego J.; Tezduyar, Tayfun E.

2007-03-01

This paper is focused on the numerical and experimental analyses of the collapse of a liquid column. The measurements of the interface position in a set of experiments carried out with shampoo and water for two different initial column aspect ratios are presented together with the corresponding numerical predictions. The experimental procedure was found to provide acceptable recurrence in the observation of the interface evolution. Basic models describing some of the relevant physical aspects, e.g. wall friction and turbulence, are included in the simulations. Numerical experiments are conducted to evaluate the influence of the parameters involved in the modeling by comparing the results with the data from the measurements. The numerical predictions reasonably describe the physical trends.

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

ERIC Educational Resources Information Center

Downes, Stephen

2007-01-01

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

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

NASA Astrophysics Data System (ADS)

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

2013-09-01

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

Feeding Currents generated by Cassiopea jellyfish

NASA Astrophysics Data System (ADS)

Gaddam, M. G.; Santhanakrishnan, A.

2016-02-01

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

A New Resonance Tube

ERIC Educational Resources Information Center

Bates, Alan

2017-01-01

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

Investigation of Gas Holdup in a Vibrating Bubble Column

NASA Astrophysics Data System (ADS)

Mohagheghian, Shahrouz; Elbing, Brian

2015-11-01

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

Congestion patterns of electric vehicles with limited battery capacity.

PubMed

Jing, Wentao; Ramezani, Mohsen; An, Kun; Kim, Inhi

2018-01-01

The path choice behavior of battery electric vehicle (BEV) drivers is influenced by the lack of public charging stations, limited battery capacity, range anxiety and long battery charging time. This paper investigates the congestion/flow pattern captured by stochastic user equilibrium (SUE) traffic assignment problem in transportation networks with BEVs, where the BEV paths are restricted by their battery capacities. The BEV energy consumption is assumed to be a linear function of path length and path travel time, which addresses both path distance limit problem and road congestion effect. A mathematical programming model is proposed for the path-based SUE traffic assignment where the path cost is the sum of the corresponding link costs and a path specific out-of-energy penalty. We then apply the convergent Lagrangian dual method to transform the original problem into a concave maximization problem and develop a customized gradient projection algorithm to solve it. A column generation procedure is incorporated to generate the path set. Finally, two numerical examples are presented to demonstrate the applicability of the proposed model and the solution algorithm.

Congestion patterns of electric vehicles with limited battery capacity

PubMed Central

2018-01-01

The path choice behavior of battery electric vehicle (BEV) drivers is influenced by the lack of public charging stations, limited battery capacity, range anxiety and long battery charging time. This paper investigates the congestion/flow pattern captured by stochastic user equilibrium (SUE) traffic assignment problem in transportation networks with BEVs, where the BEV paths are restricted by their battery capacities. The BEV energy consumption is assumed to be a linear function of path length and path travel time, which addresses both path distance limit problem and road congestion effect. A mathematical programming model is proposed for the path-based SUE traffic assignment where the path cost is the sum of the corresponding link costs and a path specific out-of-energy penalty. We then apply the convergent Lagrangian dual method to transform the original problem into a concave maximization problem and develop a customized gradient projection algorithm to solve it. A column generation procedure is incorporated to generate the path set. Finally, two numerical examples are presented to demonstrate the applicability of the proposed model and the solution algorithm. PMID:29543875

Dynamic interpretation of slug tests in highly permeable aquifers

USGS Publications Warehouse

Zurbuchen, Brian R.; Zlotnik, Vitaly A.; Butler, James J.

2002-01-01

Considerable progress has been made in developing a theoretical framework for modeling slug test responses in formations with high hydraulic conductivity K. However, several questions of practical significance remain unresolved. Given the rapid and often oscillatory nature of test responses, the traditional hydrostatic relationship between the water level and the transducer‐measured head in the water column may not be appropriate. A general dynamic interpretation is proposed that describes the relationship between water level response and transducer‐measured head. This theory is utilized to develop a procedure for transforming model‐generated water level responses to transducer readings. The magnitude of the difference between the actual water level position and the apparent position based on the transducer measurement is a function of the acceleration and velocity of the water column, test geometry, and depth of the transducer. The dynamic approach explains the entire slug test response, including the often‐noted discrepancy between the actual initial water level displacement and that measured by a transducer in the water column. Failure to use this approach can lead to a significant underestimation of K when the transducer is a considerable distance below the static water level. Previous investigators have noted a dependence of test responses on the magnitude of the initial water level displacement and have developed various approximate methods for analyzing such data. These methods are re‐examined and their limitations clarified. Practical field guidelines are proposed on the basis of findings of this work. The soundness of the dynamic approach is demonstrated through a comparison of K profiles from a series of multilevel slug tests with those from dipole‐flow tests performed in the same wells.

Atmospheric electron x-ray spectrometer

NASA Technical Reports Server (NTRS)

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

2002-01-01

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

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

PubMed

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

2010-06-25

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

Time-Temperature Studies of High Temperature Deterioration Phenomena in Lubricant Systems: Synthetic Ester Lubricants

DTIC Science & Technology

1979-01-01

fro:n the reduction procedures described below were analyzed by GLC on a 6 ft x 4 mm glass column using 3% Silar -IOC, 3,% OV-1 or 3% OV-17 on 100-120...Computer) follow:ng. gas chromatographic separation of reaction products obtained’from the -reduction and derivatization procedures wi h a 3% Silar -10C

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

Code of Federal Regulations, 2010 CFR

2010-07-01

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

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

PubMed

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

2018-04-01

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

30 CFR 735.18 - Grant application procedures.

Code of Federal Regulations, 2014 CFR

2014-07-01

... Column 5A of Forms OSM-51A and OSM-51B which reports the quantitative Program Management information of... of Form OSM-51C which reports the quantitative Program Management information of the Small Operator...

30 CFR 735.18 - Grant application procedures.

Code of Federal Regulations, 2011 CFR

2011-07-01

... Column 5A of Forms OSM-51A and OSM-51B which reports the quantitative Program Management information of... of Form OSM-51C which reports the quantitative Program Management information of the Small Operator...

30 CFR 735.18 - Grant application procedures.

Code of Federal Regulations, 2012 CFR

2012-07-01

... Column 5A of Forms OSM-51A and OSM-51B which reports the quantitative Program Management information of... of Form OSM-51C which reports the quantitative Program Management information of the Small Operator...

30 CFR 735.18 - Grant application procedures.

Code of Federal Regulations, 2013 CFR

2013-07-01

... Column 5A of Forms OSM-51A and OSM-51B which reports the quantitative Program Management information of... of Form OSM-51C which reports the quantitative Program Management information of the Small Operator...

Mixed Stationary Liquid Phases for Gas-Liquid Chromatography.

ERIC Educational Resources Information Center

Koury, Albert M.; Parcher, Jon F.

1979-01-01

Describes a laboratory technique for use in an undergraduate instrumental analysis course that, using the interpretation of window diagrams, prepares a mixed liquid phase column for gas-liquid chromatography. A detailed procedure is provided. (BT)

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 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.

Method for removing solid particulate material from within liquid fuel injector assemblies

DOEpatents

Simandl, R.F.; Brown, J.D.; Andriulli, J.B.; Strain, P.D.

1998-09-08

A method is described for removing residual solid particulate material from the interior of liquid fuel injectors and other fluid flow control mechanisms having or being operatively associated with a flow-regulating fixed or variable orifice. The method comprises the sequential and alternate introduction of columns of a non-compressible liquid phase and columns of a compressed gas phase into the body of a fuel injector whereby the expansion of each column of the gas phase across the orifice accelerates the liquid phase in each trailing column of the liquid phase and thereby generates turbulence in each liquid phase for lifting and entraining the solid particulates for the subsequent removal thereof from the body of the fuel injector. 1 fig.

Method for removing solid particulate material from within liquid fuel injector assemblies

DOEpatents

Simandl, Ronald F.; Brown, John D.; Andriulli, John B.; Strain, Paul D.

1998-01-01

A method for removing residual solid particulate material from the interior of liquid fuel injectors and other fluid flow control mechanisms having or being operatively associated with a flow-regulating fixed or variable orifice. The method comprises the sequential and alternate introduction of columns of a non-compressible liquid phase and columns of a compressed gas phase into the body of a fuel injector whereby the expansion of each column of the gas phase across the orifice accelerates the liquid phase in each trailing column of the liquid phase and thereby generates turbulence in each liquid phase for lifting and entraining the solid particulates for the subsequent removal thereof from the body of the fuel injector.

Removal of phosphorus from water by using volcanic ash soil (VAS): batch and column experiments.

PubMed

Nguyen, Huy Van; Maeda, Morihiro

2016-09-01

Using low-cost and naturally available materials is considered an optimal adsorbent for removing phosphorus (P) from water due to its simplicity and economic efficiency. This study examined the removal of P from water using volcanic ash soil (VAS) by batch and column experiments. The maximum adsorption capacity of P was 2.94 mg g -1 , estimated from the batch experiment according to a Langmuir isotherm. The column study showed a higher adsorption capacity of 5.57 mg g -1 . The breakthrough curve showed that influent water containing 2 mg L -1 P was completely purified by VAS within 1,230 pore volumes (PV). The breakthrough and saturation points of the curves were 3,100 PV and 14,875 PV, respectively. After an adsorption column was loaded with 20,508 PV, a regeneration procedure was developed to determine whether an ion exchange of P with chloride occurred or adsorbed P in the columns could be eluted. Approximately 20% of P was recovered from columns by desorption tests, regardless of NaCl solution or deionized water. Specific surface area and mineral concentrations are both important characteristics that improve the adsorption capacity of VAS. The present study suggests that VAS is a promising adsorbent to remove P in water.

Rapid, direct extraction of DNA from soils for PCR analysis using polyvinylpolypyrrolidone spin columns.

PubMed

Berthelet, M; Whyte, L G; Greer, C W

1996-04-15

Polyvinylpolypyrrolidone spin columns were used to rapidly purify crude soil DNA extracts from humic materials for polymerase chain reaction (PCR) analysis. The PCR detection limit for the tfdC gene, encoding chlorocatechol dioxygenase from the 2,4-dichlorophenoxyacetic acid degradation pathway, was 10(1)-10(2) cells/g soil in inoculated soils. The procedure could be applied to the amplification of biodegradative genes from indigenous microbial populations from a wide variety of soil types, and the entire analysis could be performed within 8 h.

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.

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

Cancer.gov

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

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.

Numerical modelling techniques of soft soil improvement via stone columns: A brief review

NASA Astrophysics Data System (ADS)

Zukri, Azhani; Nazir, Ramli

2018-04-01

There are a number of numerical studies on stone column systems in the literature. Most of the studies found were involved with two-dimensional analysis of the stone column behaviour, while only a few studies used three-dimensional analysis. The most popular software utilised in those studies was Plaxis 2D and 3D. Other types of software that used for numerical analysis are DIANA, EXAMINE, ZSoil, ABAQUS, ANSYS, NISA, GEOSTUDIO, CRISP, TOCHNOG, CESAR, GEOFEM (2D & 3D), FLAC, and FLAC 3. This paper will review the methodological approaches to model stone column numerically, both in two-dimensional and three-dimensional analyses. The numerical techniques and suitable constitutive model used in the studies will also be discussed. In addition, the validation methods conducted were to verify the numerical analysis conducted will be presented. This review paper also serves as a guide for junior engineers through the applicable procedures and considerations when constructing and running a two or three-dimensional numerical analysis while also citing numerous relevant references.

On-column trypsinization allows for re-use of matrix in modified multiplexed inhibitor beads assay.

PubMed

Petrovic, Voin; Olaisen, Camilla; Sharma, Animesh; Nepal, Anala; Bugge, Steffen; Sundby, Eirik; Hoff, Bård Helge; Slupphaug, Geir; Otterlei, Marit

2017-04-15

The Multiplexed Inhibitor Bead (MIB) assay is a previously published quantitative proteomic MS-based approach to study cellular kinomes. A rather extensive procedure, need for multiple custom-made kinase inhibitors and an inability to re-use the MIB-columns, has limited its applicability. Here we present a modified MIB assay in which elution of bound proteins is facilitated by on-column trypsinization. We tested the modified MIB assay by analyzing extract from three human cancer cell lines treated with the cytotoxic drugs cisplatin or docetaxel. Using only three immobilized kinase inhibitors, we were able to detect about 6000 proteins, including ∼40% of the kinome, as well as other signaling, metabolic and structural proteins. The method is reproducible and the MIB-columns are re-usable without loss of performance. This makes the MIB assay a simple, affordable, and rapid assay for monitoring changes in cellular signaling. Copyright © 2017 The Author(s). Published by Elsevier Inc. All rights reserved.

Investigation of radioactivity concentration in spent technetium generators

NASA Astrophysics Data System (ADS)

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

2014-04-01

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

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.

Optimization of Feasibility Stage for Hydrogen/Deuterium Exchange Mass Spectrometry

NASA Astrophysics Data System (ADS)

Hamuro, Yoshitomo; Coales, Stephen J.

2018-03-01

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

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

PubMed

Gritti, Fabrice; McDonald, Thomas; Gilar, Martin

2016-06-17

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

Isolation and characterization of a Ca/sup 2 +/ carrier candidate from calf heart inner mitochondrial membrane

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

Jeng, A.Y.

1979-01-01

A protein was isolated from calf heart inner mitochondrial membrane with the aid of an electron paramagnetic resonance assay based on the relative binding properties of Ca/sup 2 +/, Mn/sup 2 +/, and Mg/sup 2 +/ to the protein. Partial delipidation of the protein was performed by using either the organic solvent extraction procedure or the silicic acid column chromatography. Control experiments indicated that the Ca/sup 2 +/ transport properties of the isolated protein were not due to the contaminating phospholipids. A complete delipidation procedure was developd by using Sephadex LH-20 column chromatography. Further characterization of the physical and chemicalmore » properties of the delipidated protein showed that delipidated protein becomes more hydrophobic in the presence of Ca/sup 2 +/ and alkaline pH in the organic solvent extraction experiments. Two possible models of calciphorin-mediated Ca/sup 2 +/ transport in mitochondria are proposed. (PCS)« less

Biosorption of platinum and palladium for their separation/preconcentration prior to graphite furnace atomic absorption spectrometric determination

NASA Astrophysics Data System (ADS)

Godlewska-Żyłkiewicz, Beata

2003-08-01

Inexpensive baker's yeast Saccharomyces cerevisiae and green algae Chlorella vulgaris, either free or immobilized on silica gel have been shown to selectively accumulate platinum and palladium from water samples in acidic medium (pH 1.6-1.8). Optimization of conditions of metals biosorption (sample pH, algae and yeast masses, adsorption time, temperature) was performed in batch mode. The procedure of matrix separation based on biosorption of platinum and palladium on algae C. vulgaris covalently immobilized on silica gel in flow mode was developed. The use of algae in flow procedure offers several advantages compared with its use in the batch mode. The procedure shows better reproducibility (<2%), improved efficiency of platinum retention on the column (93.3±1.6%), is less laborious and less time consuming. The best recovery of biosorbed metals from column (87.7±3.3% for platinum and 96.8±1.1 for palladium) was obtained with solution of 0.3 mol l -1 thiourea in 1 mol l -1 hydrochloric acid. The influence of thiourea on analytical signals of examined metals during GFAAS determination is discussed. The procedure has been applied for separation of noble metals from tap and waste water samples spiked with platinum and palladium.

High-throughput biomonitoring of dioxins and polychlorinated biphenyls at the sub-picogram level in human serum.

PubMed

Focant, Jean-François; Eppe, Gauthier; Massart, Anne-Cécile; Scholl, Georges; Pirard, Catherine; De Pauw, Edwin

2006-10-13

We report on the use of a state-of-the-art method for the measurement of selected polychlorinated dibenzo-p-dioxins, polychlorinated dibenzofurans and polychlorinated biphenyls in human serum specimens. The sample preparation procedure is based on manual small size solid-phase extraction (SPE) followed by automated clean-up and fractionation using multi-sorbent liquid chromatography columns. SPE cartridges and all clean-up columns are disposable. Samples are processed in batches of 20 units, including one blank control (BC) sample and one quality control (QC) sample. The analytical measurement is performed using gas chromatography coupled to isotope dilution high-resolution mass spectrometry. The sample throughput corresponds to one series of 20 samples per day, from sample reception to data quality cross-check and reporting, once the procedure has been started and series of samples keep being produced. Four analysts are required to ensure proper performances of the procedure. The entire procedure has been validated under International Organization for Standardization (ISO) 17025 criteria and further tested over more than 1500 unknown samples during various epidemiological studies. The method is further discussed in terms of reproducibility, efficiency and long-term stability regarding the 35 target analytes. Data related to quality control and limit of quantification (LOQ) calculations are also presented and discussed.

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

Development of a screening method for the determination of 49 priority pollutants in soil

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

Kiang, P.H.; Grob, R.L.

1986-01-01

A screening procedure was develop for the determination of 49 priority pollutants in soil. An extraction procedure followed by the capillary gas chromatographic technique was used. Dual pH solutions with methylene chloride were used as extraction solvent system; no sample clean-up procedure was applied. Both base/neutral and acid fractions were analyzed on the same capillary column (SPB-1). The relative standard deviation for 5.1 ppm (51 ..mu..g/ 10 g) concentration in zero soil was less than 25%.

Analogy for the effect of material and geometrical variables on energy-absorption capability of composite tubes

NASA Technical Reports Server (NTRS)

Farley, Gary L.; Jones, Robert M.

1992-01-01

Simplified procedures for determining the qualitative effect a variable has on structural response of a composite tube are very useful in both preliminary design as well as in providing insight into the general response. An analysis procedure is presented that can be used to determine the qualitative change in the sustained crushing load due to a change in specimen material properties or geometry. The analysis procedure is similar in form to the equation for the buckling load of a column on an elastic foundation.

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

NASA Technical Reports Server (NTRS)

Sullivan, M. R.

1982-01-01

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

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

NASA Astrophysics Data System (ADS)

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

2016-09-01

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

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

PubMed

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

2015-08-28

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

Iridium 191-m generator

DOEpatents

Treves, S.; Cheng, C.C.

1988-03-08

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

Sequential extraction procedure for determination of uranium, thorium, radium, lead and polonium radionuclides by alpha spectrometry in environmental samples

NASA Astrophysics Data System (ADS)

Oliveira, J. M.; Carvalho, F. P.

2006-01-01

A sequential extraction technique was developed and tested for common naturally-occurring radionuclides. This technique allows the extraction and purification of uranium, thorium, radium, lead, and polonium radionuclides from the same sample. Environmental materials such as water, soil, and biological samples can be analyzed for those radionuclides without matrix interferences in the quality of radioelement purification and in the radiochemical yield. The use of isotopic tracers (232U, 229Th, 224Ra, 209Po, and stable lead carrier) added to the sample in the beginning of the chemical procedure, enables an accurate control of the radiochemical yield for each radioelement. The ion extraction procedure, applied after either complete dissolution of the solid sample with mineral acids or co-precipitation of dissolved radionuclide with MnO2 for aqueous samples, includes the use of commercially available pre-packed columns from Eichrom® and ion exchange columns packed with Bio-Rad resins, in altogether three chromatography columns. All radioactive elements but one are purified and electroplated on stainless steel discs. Polonium is spontaneously plated on a silver disc. The discs are measured using high resolution silicon surface barrier detectors. 210Pb, a beta emitter, can be measured either through the beta emission of 210Bi, or stored for a few months and determined by alpha spectrometry through the in-growth of 210Po. This sequential extraction chromatography technique was tested and validated with the analysis of certified reference materials from the IAEA. Reproducibility was tested through repeated analysis of the same homogeneous material (water sample).

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

Marron, A.C.

Middle ultraviolet spectra of the atmospheric airglow were obtained from a March 1992 rocket flight of the NPS MUSTANG instrument. These spectra are analyzed from 1900 A to 3100 A, over an altitude range of 100 km to 320 km. The data are modeled with computer generated synthetic spectra for the following emissions: N2 Vegard Kaplan (VK); N2 Lyman-Birge-Hopfield (LBH); and NO Gamma, Delta, and Epsilon bands. A best fit procedure was developed. The resulting synthetic spectra agree well with obtained airglow data. Confirmation was made of the theoretical self absorption versus non-self absorption processes of the NO (0,0), (1,0),more » (2,0) gamma resonance band emissions. NO self absorption is a necessary inclusion of any atmospheric nitric oxide analysis stratagem. Profiles of temperature versus altitude and NO column density versus altitude for the rocket flight are estimated. Airglow, Ionosphere, Ultraviolet spectroscopy.« less

Catalysis Meets Nonthermal Separation for the Production of (Alkyl)phenols and Hydrocarbons from Pyrolysis Oil.

PubMed

Cao, Zhengwen; Engelhardt, Jan; Dierks, Michael; Clough, Matthew T; Wang, Guang-Hui; Heracleous, Eleni; Lappas, Angelos; Rinaldi, Roberto; Schüth, Ferdi

2017-02-20

A simple and efficient hydrodeoxygenation strategy is described to selectively generate and separate high-value alkylphenols from pyrolysis bio-oil, produced directly from lignocellulosic biomass. The overall process is efficient and only requires low pressures of hydrogen gas (5 bar). Initially, an investigation using model compounds indicates that MoC x /C is a promising catalyst for targeted hydrodeoxygenation, enabling selective retention of the desired Ar-OH substituents. By applying this procedure to pyrolysis bio-oil, the primary products (phenol/4-alkylphenols and hydrocarbons) are easily separable from each other by short-path column chromatography, serving as potential valuable feedstocks for industry. The strategy requires no prior fractionation of the lignocellulosic biomass, no further synthetic steps, and no input of additional (e.g., petrochemical) platform molecules. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Electron-transfer-initiated benzoin- and Stetter-like reactions in packed-bed reactors for process intensification.

PubMed

Zaghi, Anna; Ragno, Daniele; Di Carmine, Graziano; De Risi, Carmela; Bortolini, Olga; Giovannini, Pier Paolo; Fantin, Giancarlo; Massi, Alessandro

2016-01-01

A convenient heterogeneous continuous-flow procedure for the polarity reversal of aromatic α-diketones is presented. Propaedeutic batch experiments have been initially performed to select the optimal supported base capable to initiate the two electron-transfer process from the carbamoyl anion of the N , N -dimethylformamide (DMF) solvent to the α-diketone and generate the corresponding enediolate active species. After having identified the 2- tert -butylimino-2-diethylamino-1,3-dimethylperhydro-1,3,2-diazaphosphorine on polystyrene (PS-BEMP) as the suitable base, packed-bed microreactors (pressure-resistant stainless-steel columns) have been fabricated and operated to accomplish the chemoselective synthesis of aroylated α-hydroxy ketones and 2-benzoyl-1,4-diones (benzoin- and Stetter-like products, respectively) with a good level of efficiency and with a long-term stability of the packing material (up to five days).

Electron-transfer-initiated benzoin- and Stetter-like reactions in packed-bed reactors for process intensification

PubMed Central

Zaghi, Anna; Ragno, Daniele; Di Carmine, Graziano; De Risi, Carmela; Bortolini, Olga; Giovannini, Pier Paolo; Fantin, Giancarlo

2016-01-01

A convenient heterogeneous continuous-flow procedure for the polarity reversal of aromatic α-diketones is presented. Propaedeutic batch experiments have been initially performed to select the optimal supported base capable to initiate the two electron-transfer process from the carbamoyl anion of the N,N-dimethylformamide (DMF) solvent to the α-diketone and generate the corresponding enediolate active species. After having identified the 2-tert-butylimino-2-diethylamino-1,3-dimethylperhydro-1,3,2-diazaphosphorine on polystyrene (PS-BEMP) as the suitable base, packed-bed microreactors (pressure-resistant stainless-steel columns) have been fabricated and operated to accomplish the chemoselective synthesis of aroylated α-hydroxy ketones and 2-benzoyl-1,4-diones (benzoin- and Stetter-like products, respectively) with a good level of efficiency and with a long-term stability of the packing material (up to five days). PMID:28144342

Chamber for Aerosol Deposition of Bioparticles

NASA Technical Reports Server (NTRS)

Kern, Roger; Kirschner, Larry

2008-01-01

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

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

Kaczmarski, Krzysztof; Guiochon, Georges A

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

Surface-imprinted microspheres prepared by a template-oriented method for the chiral separation of amlodipine.

PubMed

Lai, Shenzhi; Ouyang, Xiaoli; Cai, Changqun; Xu, Wensheng; Chen, Chunyan; Chen, Xiaoming

2017-05-01

The surface imprinting technique has been developed to overcome the mass-transfer difficulty, but the utilization ratio of template molecules in the imprinting procedure still remains a challengeable task to be improved. In this work, specifically designed surface-imprinted microspheres were prepared by a template-oriented method for enantioseparation of amlodipine besylate. Submicron mesoporous silica microspheres were surface-modified with double bonds, followed by polymerizing methacrylic acid to generate carboxyl modified mesoporous silica microspheres (PMAA@SiO 2 ). Afterwards, PMAA@SiO 2 was densely adsorbed with (S)-amlodipine molecules to immobilize template molecules through multiple hydrogen bonding interactions. Then surface molecular imprinting was carried out by cross-linking the carboxyl group of PMAA@SiO 2 with ethylene glycol diglycidyl ether. The surface-imprinted microspheres showed fast binding kinetics of only 20 min for equilibrium adsorption, and the saturation adsorption capacity reached 137 mg/g. The imprinted materials displayed appreciable chiral separation ability when used as column chromatography for enantioseparation of amlodipine from amlodipine besylate, and the enantiomeric excess of (S)-amlodipine reached 13.8% with only 2.3 cm column length by no extra chiral additives. Besides, the imprinted materials exhibited excellent reusability, and this allows the potential application for amplification production of amlodipine enantiomer. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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)

Ecology in a Jar.

ERIC Educational Resources Information Center

Corner, Thomas R.

1992-01-01

In a hands-on experiment to illustrate the concept of cycles in ecology, students use the Winogradsky column to explore the operation of the sulfur cycle and the interrelatedness of organisms in an environment. Lesson plans include materials needed and class procedures. (MDH)

Tested Demonstrations.

ERIC Educational Resources Information Center

Gilbert, George L., Ed.

1985-01-01

List of materials needed, procedures used, and results obtained are provided for two demonstrations. The first is an inexpensive and quick method for demonstrating column chromatography of plant pigments of spinach extract. The second is a demonstration of cathodic protection by impressed current. (JN)

Generating multiple independent retention index data in dual-secondary column comprehensive two-dimensional gas chromatography.

PubMed

Bieri, Stefan; Marriott, Philip J

2006-12-01

A method producing simultaneously three retention indexes for compounds has been developed for comprehensive two-dimensional gas chromatography by using a dual secondary column approach (GC x 2GC). For this purpose, the primary flow of the first dimension column was equally diverted into two secondary microbore columns of identical geometry by means of a three-way flow splitter positioned after the longitudinally modulated cryogenic system. This configuration produced a pair of comprehensive two-dimensional chromatograms and generated retention data on three different stationary phases in a single run. First dimension retention indexes were determined on a polar SolGel-Wax column under linear programmed-temperature conditions according to the van den Dool approach using primary alcohol homologues as the reference scale. Calculation of pseudoisothermal retention indexes in both second dimensions was performed on low-polarity 5% phenyl equivalent polysilphenylene/siloxane (BPX5) and 14% cyanopropylphenyl/86% dimethylpolysiloxane (BP10) columns. To construct a retention correlation map in the second dimension separation space upon which KovAts indexes can be derived, two methods exploiting "isovolatility" relationships of alkanes were developed. The first involved 15 sequential headspace samplings of selected n-alkanes by solid-phase microextraction (SPME), with each sampling followed by their injection into the GC at predetermined times during the chromatographic run. The second method extended the second dimension retention map and consisted of repetitive introduction of SPME-sampled alkane mixtures at various isothermal conditions incremented over the temperature program range. Calculated second dimension retention indexes were compared with experimental values obtained in conventional one-dimensional GC. A case study mixture including 24 suspected allergens (i.e., fragrance ingredients) was used to demonstrate the feasibility and potential of retention index information in comprehensive 2D-GC.

Automated synthesis of N-(2-[18 F]Fluoropropionyl)-l-glutamic acid as an amino acid tracer for tumor imaging on a modified [18 F]FDG synthesis module.

PubMed

Liu, Shaoyu; Sun, Aixia; Zhang, Zhanwen; Tang, Xiaolan; Nie, Dahong; Ma, Hui; Jiang, Shende; Tang, Ganghua

2017-06-15

N-(2-[ 18 F]Fluoropropionyl)-l-glutamic acid ([ 18 F]FPGLU) is a potential amino acid tracer for tumor imaging with positron emission tomography. However, due to the complicated multistep synthesis, the routine production of [ 18 F]FPGLU presents many challenging laboratory requirements. To simplify the synthesis process of this interesting radiopharmaceutical, an efficient automated synthesis of [ 18 F]FPGLU was performed on a modified commercial fluorodeoxyglucose synthesizer via a 2-step on-column hydrolysis procedure, including 18 F-fluorination and on-column hydrolysis reaction. [ 18 F]FPGLU was synthesized in 12 ± 2% (n = 10, uncorrected) radiochemical yield based on [ 18 F]fluoride using the tosylated precursor 2. The radiochemical purity was ≥98%, and the overall synthesis time was 35 minutes. To further optimize the radiosynthesis conditions of [ 18 F]FPGLU, a brominated precursor 3 was also used for the preparation of [ 18 F]FPGLU, and the improved radiochemical yield was up to 20 ± 3% (n = 10, uncorrected) in 35 minutes. Moreover, all these results were achieved using the similar on-column hydrolysis procedure on the modified fluorodeoxyglucose synthesis module. Copyright © 2017 John Wiley & Sons, Ltd.

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

DOEpatents

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

1988-01-01

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

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

NASA Astrophysics Data System (ADS)

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

2000-07-01

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

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.

A dynamic pressure calibration standard

NASA Technical Reports Server (NTRS)

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

1985-01-01

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

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

PubMed

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

2011-10-15

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

Phthalocyanines functionalized with 2-methyl-5-nitro-1H-imidazolylethoxy and 1,4,7-trioxanonyl moieties and the effect of metronidazole substitution on photocytotoxicity.

PubMed

Wierzchowski, Marcin; Sobotta, Lukasz; Skupin-Mrugalska, Paulina; Kruk, Justyna; Jusiak, Weronika; Yee, Michael; Konopka, Krystyna; Düzgüneş, Nejat; Tykarska, Ewa; Gdaniec, Maria; Mielcarek, Jadwiga; Goslinski, Tomasz

2013-10-01

Four novel magnesium(II) and zinc(II) phthalocyanines bearing 1,4,7-trioxanonyl, polyether and/or (2-methyl-5-nitro-1H-imidazol-1-yl)ethoxy, heterocyclic substituents at their non-peripheral positions were synthesized and assessed in terms of physicochemical and biological properties. Magnesium phthalocyanine derivatives bearing polyether substituents (Pc-1), a mixed system of polyether and heterocyclic substituents (Pc-3), and four heterocyclic substituents (Pc-4), respectively, were synthesized following the Linstead macrocyclization reaction procedure. Zinc phthalocyanine (Pc-2) bearing polyether substituents at non-peripheral positions was synthesized following the procedure in n-pentanol with the zinc acetate, and DBU. Novel phthalocyanines were purified by flash column chromatography and characterized using NMR, MS, UV-Vis and HPLC. Moreover, two precursors in macrocyclization reaction phthalonitriles were characterized using X-ray. Photophysical properties of the novel macrocycles were evaluated, including UV-Vis spectra analysis and aggregation study. All macrocycles subjected to singlet oxygen generation and the oxidation rate constant measurements exhibited lower quantum yields of singlet oxygen generation in DMSO than in DMF. In addition, the Pc-2 molecule was found to be the most efficient singlet oxygen generator from the group of macrocycles studied. The photocytotoxicity evaluated on the human oral squamous cell carcinoma cell line, HSC-3, for Pc-3 was significantly higher than that for Pc-1, Pc-2, and Pc-4. Interestingly, Pc-3 was found to be the most active macrocycle in vitro although its ability to generate singlet oxygen was significantly lower than those of Pc-1 and Pc-2. However, attempts to encapsulate phthalocyanines Pc-1-Pc-3 in liposomal membranes were unsuccessful. The phthalocyanine-nitroimidazole conjugate, Pc-4 was encapsulated in phosphatidylglycerol:phosphatidylcholine unilamellar liposomes and subjected to photocytotoxicity study. © 2013.

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

PubMed

Ravald, L; Fornstedt, T

2001-01-26

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

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

PubMed

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

2005-06-16

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

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

PubMed

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

2012-09-01

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

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

NASA Astrophysics Data System (ADS)

Vikhrev, Victor V.; Baronova, Elena O.

1997-05-01

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

Seismic Tremors and Three-Dimensional Magma Wagging

NASA Astrophysics Data System (ADS)

Liao, Y.; Bercovici, D.

2015-12-01

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

Enhanced reductive dechlorination in columns treated with edible oil emulsion

NASA Astrophysics Data System (ADS)

Long, Cameron M.; Borden, Robert C.

2006-09-01

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

DETERMINATION OF PESTICIDES AND PCB'S IN INDUSTRIAL AND MUNICIPAL WASTEWATERS

EPA Science Inventory

Steps in the procedure for the analysis of 25 chlorinated pesticides and polychlorinated biphenyls were studied. Two gas chromatographic columns and two detectors (electron capture and Hall electrolytic conductivity) were evaluated. Extractions were performed with two solvents (d...

A new procedure for the determination of distillation temperature distribution of high-boiling petroleum products and fractions.

PubMed

Boczkaj, Grzegorz; Przyjazny, Andrzej; Kamiński, Marian

2011-03-01

The distribution of distillation temperatures of liquid and semi-fluid products, including petroleum fractions and products, is an important process and practical parameter. It provides information on properties of crude oil and content of particular fractions, classified on the basis of their boiling points, as well as the optimum conditions of atmospheric or vacuum distillation. At present, the distribution of distillation temperatures is often investigated by simulated distillation (SIMDIS) using capillary gas chromatography (CGC) with a short capillary column with polydimethylsiloxane as the stationary phase. This paper presents the results of investigations on the possibility of replacing currently used CGC columns for SIMDIS with a deactivated fused silica capillary tube without any stationary phase. The SIMDIS technique making use of such an empty fused silica column allows a considerable lowering of elution temperature of the analytes, which results in a decrease of the final oven temperature while ensuring a complete separation of the mixture. This eliminates the possibility of decomposition of less thermally stable mixture components and bleeding of the stationary phase which would result in an increase of the detector signal. It also improves the stability of the baseline, which is especially important in the determination of the end point of elution, which is the basis for finding the final temperature of distillation. This is the key parameter for the safety process of hydrocracking, where an excessively high final temperature of distillation of a batch can result in serious damage to an expensive catalyst bed. This paper compares the distribution of distillation temperatures of the fraction from vacuum distillation of petroleum obtained using SIMDIS with that obtained by the proposed procedure. A good agreement between the two procedures was observed. In addition, typical values of elution temperatures of n-paraffin standards obtained by the two procedures were compared. Finally, the agreement between boiling points of polar compounds determined from their retention times and actual boiling points was investigated.

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.

Two-step purification method of vitellogenin from three teleost fish species: rainbow trout (Oncorhynchus mykiss), gudgeon (Gobio gobio) and chub (Leuciscus cephalus).

PubMed

Brion, F; Rogerieux, F; Noury, P; Migeon, B; Flammarion, P; Thybaud, E; Porcher, J M

2000-01-14

A two-step purification protocol was developed to purify rainbow trout (Oncorhynchus mykiss) vitellogenin (Vtg) and was successfully applied to Vtg of chub (Leuciscus cephalus) and gudgeon (Gobio gobio). Capture and intermediate purification were performed by anion-exchange chromatography on a Resource Q column and a polishing step was performed by gel permeation chromatography on Superdex 200 column. This method is a rapid two-step purification procedure that gave a pure solution of Vtg as assessed by silver staining electrophoresis and immunochemical characterisation.

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.

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

NASA Astrophysics Data System (ADS)

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

2018-01-01

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

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

PubMed

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

2015-10-01

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

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

PubMed

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

2006-08-15

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

Rotation Capacity of Bolted Flush End-Plate Stiffened Beam-to-Column Connection

NASA Astrophysics Data System (ADS)

Ostrowski, Krzysztof; Kozłowski, Aleksander

2017-06-01

One of the flexibility parameters of semi-rigid joints is rotation capacity. Plastic rotation capacity is especially important in plastic design of framed structures. Current design codes, including Eurocode 3, do not posses procedures enabling designers to obtain value of rotation capacity. In the paper the calculation procedure of the rotation capacity for stiffened bolted flush end-plate beam-to-column connections has been proposed. Theory of experiment design was applied with the use of Hartley's PS/DS-P:Ha3 plan. The analysis was performed with the use of finite element method (ANSYS), based on the numerical experiment plan. The determination of maximal rotation angle was carried out with the use of regression analysis. The main variables analyzed in parametric study were: pitch of the bolt "w" (120-180 mm), the distance between the bolt axis and the beam upper edge cg1 (50-90 mm) and the thickness of the end-plate tp (10-20 mm). Power function was proposed to describe available rotation capacity of the joint. Influence of the particular components on the rotation capacity was also investigated. In the paper a general procedure for determination of rotation capacity was proposed.

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

PubMed

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

2003-01-01

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

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

DTIC Science & Technology

2004-06-03

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

Filtrates and Residues: Chlorophyll Separation and Spectral Identification.

ERIC Educational Resources Information Center

Diehl-Jones, Susan M.

1984-01-01

Describes an experiment in which students become familiar with the organic chemistry extraction process, perform analyses by thin layer and column chromatography, and use the absorption spectrum (obtained from a spectrophotometer) for identification. List of materials needed and procedures used are provided. (JN)

Development and Application of Immunoaffinity Chromatography for Coplanar PCBs in Soil and Sediment

EPA Science Inventory

An immunoaffinity chromatography (IAC) column was developed as a simple cleanup procedure for preparing environmental samples for analysis of polychlorinated biphenyls (PCBs). Soil and sediment samples were prepared using pressurized liquid extraction (PLE), followed by the IAC c...

Evaluation of Soil Media for Stormwater Infiltration Best Management Practices (BMPs)

EPA Science Inventory

This project will improve the performance of structural management practices, and provide guidance that will allow designers to balance infiltration rates with sorption capacity. This project will also perform a standard column test procedure for evaluating candidate soil media.

Flexible and Accessible Automated Operation of Miniature Chromatography Columns on a Liquid Handling Station.

PubMed

Konstantinidis, Spyridon; Goh, Hai-Yuan; Martin Bufájer, José M; de Galbert, Paul; Parau, Maria; Velayudhan, Ajoy

2018-03-01

The High Throughput (HT) investigation of chromatographic separations is an important element of downstream bioprocess development due to the importance of chromatography as a technique for achieving stringent regulatory requirements on product purity. Various HT formats for chromatography exist, but the miniature column approach has characteristics resembling large scale packed bed column chromatography the most. The operation of such columns on robotic stations can be automated, but this is not always a straightforward procedure; the robotic manipulations are highly dependent on the settings of each experiment and the standard commands of the supporting software may not provide readily the required flexibility and accessibility for "plug and play" functionality. These can limit the potential of this technique in laboratories engaging on HT activities. In this work, we present an application which aims to overcome this challenge by providing end-users with a flexible operation of the miniature column technique on an automated liquid handler. The application includes a script which is written on Freedom EVOware, and is supplemented by custom compiled executables. Here, the manipulations carried out by the application are described in detail and its functionality is demonstrated through typical experiments based on bind and elute miniature column chromatography. The application is shown to allow for the unsupervised "on-the-fly" programming of the robotic station and to ultimately make the technique accessible to non-automation experts. This application is therefore well suited to simplifying development activities based on the robotic deployment of the miniature column chromatography technique. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

PubMed

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

2014-03-01

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

Optimal Artificial Boundary Condition Configurations for Sensitivity-Based Model Updating and Damage Detection

DTIC Science & Technology

2010-09-01

matrix is used in many methods, like Jacobi or Gauss Seidel , for solving linear systems. Also, no partial pivoting is necessary for a strictly column...problems that arise during the procedure, which in general, converges to the solving of a linear system. The most common issue with the solution is the... iterative procedure to find an appropriate subset of parameters that produce an optimal solution commonly known as forward selection. Then, the

Sorbent materials for rapid remediation of wash water during radiological event relief

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

Jolin, William C.; Kaminski, Michael

2016-11-01

Procedures for removing harmful radiation from interior and exterior surfaces of homes and businesses after a nuclear or radiological disaster may generate large volumes of radiologically contaminated waste water. Rather than releasing this waste water to potentially contaminate surrounding areas, it is preferable to treat it onsite. Retention barrels are a viable option because of their simplicity in preparation and availability of possible sorbent materials. This study investigated the use of aluminosilicate clay minerals as sorbent materials to retain 137Cs, 85Sr, and 152Eu. Vermiculite strongly retained 137Cs, though other radionuclides displayed diminished affinity for the surface. Montmorillonite exhibited increased affinitymore » to sorb 85Sr and 152Eu in the presence of higher concentrations of 137Cs. To simulate flow within retention barrels, vermiculite was mixed with sand and used in small-scale column experiments. The GoldSim contaminate fate module was used to model breakthrough and assess the feasibility of using clay minerals as sorbent materials in retention barrels. The modeled radionuclide breakthrough profiles suggest that vermiculite-sand and montmorillonite-sand filled barrels could be used for treatment of contaminated water generated from field operations.« less

Liquid chromatography-hydride generation-atomic absorption spectrometry for the speciation of tin in seafoods.

PubMed

Viñas, Pilar; López-García, Ignacio; Merino-Meroño, Beatriz; Campillo, Natalia; Hernández-Cordóba, Manuel

2004-04-01

Liquid chromatography with hydride generation atomic absorption spectrometry as the detection system was applied to the separation and determination of inorganic tin, tributyltin, dibutyltin, monobutyltin, diphenyltin and monophenyltin. A reversed phase C18 column and a methanol/water/acetic acid (70:27:3, v/v/v) mixture containing 0.05%(v/v) triethylamine and 0.1%(w/v) tropolone as the mobile phase (isocratic elution) were used. Extraction of organotins from the samples was carried out using methanol containing 0.05%(w/v) tropolone, a process that was repeated twice. The supernatants were shaken with water and dichloromethane in a separating funnel and the organic phase was collected and evaporated to dryness. When the method was applied to the speciation of tin in fresh and canned mussels, no organotins above the detection limits were identified in any of the samples, inorganic tin being the only species detected. The reliability of the procedure was checked by analyzing the total tin content of the samples by electrothermal atomic absorption spectrometry and by speciation of tin in a certified reference material, mussel tissue (CRM 477). The method can be used for environmental monitoring of organotins contaminated samples.

PLIF in thoracolumbar trauma: technique and radiological results

PubMed Central

Dietmar, Krappinger; Peter, Seykora; Michael, Blauth; Anton, Kathrein

2010-01-01

Patients with fractures from the 11th thoracic to the 5th lumbar vertebra had a reconstruction of the anterior column with monocortical iliac crest autograft by using a single dorsal approach. The loss of correction was observed using X-rays pre- and post-operatively, at 3 months and after implant removal (IR). Successful fusion was assessed using computed tomography after the implant removal. To assess the loss of correction and intervertebral fusion rate of this technique. There are still controversial discussions about the treatment modalities of spine lesions, especially in cases of burst fractures. Dorsal, combined and ventral procedures are reported with different assets and drawbacks. We want to present a method to restore the weight-bearing capability of the anterior column using a single dorsal approach. From 2001 to 2005, a total of 100 patients was treated with this technique at our department. Follow-up examination was possible in 82 patients. The X-rays and CT scans were proofed for loss of correction and fusion rate. The anterior column has been restored using a monocortical strut graft via a partial resection of the lamina and the apophyseal joint on one side to access the disc space. The dorsal reduction has been achieved using an angular stable pedicle screw system. The mean follow-up time was 15 months (range 8–39); 67 patients had a CT scan at follow-up and 83% showed a 360° fusion. The average post-operative loss of correction was 3.3° (range 0–21). The average duration of operation was 192 min (range 120–360) and the mean blood loss was 790 ml (range 300–3,400 ml). Regarding the complications we did not have any deep wound infections. We had two epidural haematomas postoperatively with a neurological deterioration that had to be revised. We were able to decompress the neurological structures and restore the weight-bearing capability of the anterior column in a one-stage procedure. So we think that this technique can be an alternative procedure to combined operations regarding the presented radiological results of successful fusion and loss of correction. PMID:20217152

Lordosis Re-Creation in TLIF and PLIF: A Cadaveric Study of the Influence of Surgical Bone Resection and Cage Angle.

PubMed

Robertson, Peter A; Armstrong, William A; Woods, Daniel L; Rawlinson, Jeremy J

2018-04-24

Controlled cadaveric study of surgical technique in Transforaminal and Posterior Lumbar Interbody Fusion (TLIF & PLIF) OBJECTIVE.: To evaluate the contribution of surgical techniques and cage variables in lordosis re-creation in posterior interbody fusion (TLIF/PLIF). The major contributors to lumbar lordosis are the lordotic lower lumbar discs. The pathologies requiring treatment with segmental fusion are frequently hypolordotic or kyphotic. Current posterior based interbody techniques have a poor track record for recreating lordosis, although re-creation of lordosis with optimum anatomical alignment is associated with better outcomes and reduced adjacent segment change needing revision. It is unclear whether surgical techniques or cage parameters contribute significantly to lordosis re-creation. Eight instrumented cadaveric motion segments were evaluated with pre and post experimental radiological assessment of lordosis. Each motion segment was instrumented with pedicle screw fixation to allow segmental stabilization. The surgical procedures were unilateral TLIF with an 18° lordotic and 27 mm length cage, unilateral TLIF (18°, 27 mm) with bilateral facetectomy, unilateral TLIF (18°, 27 mm) with posterior column osteotomy, PLIF with bilateral cages (18°, 22 mm), and PLIF with bilateral cages (24°, 22 mm). Cage insertion used and 'insert and rotate' technique. Pooled results demonstrated a mean increase in lordosis of 2.2° with each procedural step (Lordosis increase was serially 1.8°, 3.5°, 1.6°, 2.5° & 1.6° through the procedures). TLIF and PLIF with posterior column osteotomy increased lordosis significantly compared with Unilateral TLIF and TLIF with bilateral facetectomy. The major contributors to lordosis re-creation were posterior column osteotomy, and PLIF with paired shorter cages rather than TLIF. This study demonstrates that the surgical approach to posterior interbody surgery influences lordosis gain and posterior column osteotomy optimizes lordosis gain in TLIF. The bilateral cages used in PLIF are shorter and associated with further gain in lordosis. This information has the potential to aid surgical planning when attempting to recreate lordosis to optimize outcomes. N/A.

Rapid determination of glyphosate in cereal samples by means of pre-column derivatisation with 9-fluorenylmethyl chloroformate and coupled-column liquid chromatography with fluorescence detection.

PubMed

Hogendoorn, E A; Ossendrijver, F M; Dijkman, E; Baumann, R A

1999-02-12

A rapid procedure for the determination of glyphosate in cereals has been developed. Convenient sample pretreatment is carried out by (i) a overnight standing extraction of 1.0 g homogenized sample with 20 ml of water, (ii) centrifugation of the samples, (iii) a passing of 2.5 ml of the clear layer through a 100 mg C18 solid-phase extraction cartridge and (iv) collection of the last 1.5 ml of the eluent into a calibrated tube. For the instrumental analysis, the efficient approach developed earlier for environmental water samples [J.V. Sancho, F. Hernández, F.J. LUpez, E.A. Hogendoorn, E. Dijkman, P. van Zoonen, J. Chromatogr. A, 737 (1996) 75] was successfully adopted for the determination of glyphosate in the obtained cereal extracts. The procedure includes a 15 min derivatisation step of the analyte with 9-fluorenylmethyl chloroformate and a 16 times dilution step prior to instrumental analysis employing coupled-column LC with fluorescence detection. The developed procedure has a sample throughput of more than 25 samples per day and a limit of quantification of 0.5 mg/kg. The method was validated by analyzing freshly spiked cereal samples and samples with aged residues at levels between 1.0 and 10 mg/kg. The overall recovery of the freshly spiked samples was 86% (n = 10) with a repeatability of 6.5% and a reproducibility of 9.5%. For samples with aged residues recoveries performed at different time intervals (range 80-150 days) did not differ significantly; the overall recovery (n = 10) was 74% with a repeatability and reproducibility of 14 and 20%, respectively.

Comparison of batch and column tests for the elution of artificial turf system components.

PubMed

Krüger, O; Kalbe, U; Berger, W; Nordhauβ, K; Christoph, G; Walzel, H-P

2012-12-18

Synthetic athletic tracks and turf areas for outdoor sporting grounds may release contaminants due to the chemical composition of some components. A primary example is that of zinc from reused scrap tires (main constituent, styrene butadiene rubber, SBR), which might be harmful to the environment. Thus, methods for the risk assessment of those materials are required. Laboratory leaching methods like batch and column tests are widely used to examine the soil-groundwater pathway. We tested several components for artificial sporting grounds with batch tests at a liquid to solid (LS) ratio of 2 L/kg and column tests with an LS up to 26.5 L/kg. We found a higher zinc release in the batch test eluates for all granules, ranging from 15% higher to 687% higher versus data from column tests for SBR granules. Accompanying parameters, especially the very high turbidity of one ethylene propylene diene monomer rubber (EPDM) or thermoplastic elastomer (TPE) eluates, reflect the stronger mechanical stress of batch testing. This indicates that batch test procedures might not be suitable for the risk assessment of synthetic sporting ground components. Column tests, on the other hand, represent field conditions more closely and allow for determination of time-dependent contaminants release.

Developing procedures for the large-scale purification of human serum butyrylcholinesterase.

PubMed

Saxena, Ashima; Luo, Chunyuan; Doctor, Bhupendra P

2008-10-01

Human serum butyrylcholinesterase (Hu BChE) is the most viable candidate for the prophylactic treatment of organophosphate poisoning. A dose of 200 mg/70 kg is predicted to protect humans against 2x LD(50) of soman. Therefore, the aim of this study was to develop procedures for the purification of gram quantities of this enzyme from outdated human plasma or Cohn Fraction IV-4. The purification of Hu BChE was accomplished by batch adsorption on procainamide-Sepharose-CL-4B affinity gel followed by ion-exchange chromatography on a DEAE-Sepharose column. For the purification of enzyme from Cohn Fraction IV-4, it was resuspended in 25 mM sodium phosphate buffer, pH 8.0, and fat was removed by decantation, prior to batch adsorption on procainamide-Sepharose gel. In both cases, the procainamide gel was thoroughly washed with 25 mM sodium phosphate buffer, pH 8.0, containing 0.05 M NaCl, and the enzyme was eluted with the same buffer containing 0.1 M procainamide. The enzyme was dialyzed and the pH was adjusted to 4.0 before loading on the DEAE column equilibrated in sodium acetate buffer, pH 4.0. The column was thoroughly washed with 25 mM sodium phosphate buffer, pH 8.0 containing 0.05 M NaCl before elution with a gradient of 0.05-0.2M NaCl in the same buffer. The purity of the enzyme following these steps ranged from 20% to 40%. The purity of the enzyme increased to >90% by chromatography on an analytical procainamide affinity column. Results show that Cohn Fraction IV-4 is a much better source than plasma for the large-scale isolation of purified Hu BChE.

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

PubMed

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

2010-03-12

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

Isolated dorsal column dysfunction due to an intraspinal Osteolipoma - Case report and review of literature.

PubMed

Aiyer, Siddharth N; Shetty, Ajoy Prasad; Kanna, Rishi; Maheswaran, Anupama; Rajasekaran, S

2016-01-01

Osteolipoma is a rare variant of the ubiquitous lipoma. Published literature appears in the form of isolated case reports affecting soft tissue structures in the head, neck and rarely affecting the spine. We present a unique instance of an intraspinal osteolipoma in the cervical spine, without evidence of accompanying spinal dysraphism and an atypical clinical presentation of isolated dorsal column dysfunction. We describe the clinical presentation, operative procedure and post-operative outcomes with histopathological findings of this rare entity. A 61-year-old male presented with impaired dorsal column sensation due to an intraspinal extradural ossifying lesion in the cervical spinal canal. The patient underwent excision of the lesion with complete resolution of symptoms. Ossifying lesion in the spinal canal may be frequent finding on radiological imaging but presence of possible adipose tissue in the lesion should raise suspicion of rare clinical scenario of an osteolipoma.

Application of EDTA decontamination on soils affected by mining activities and impact of treatment on the geochemical partition of metal contaminants.

PubMed

Xia, Wenbin; Gao, Hui; Wang, Xianhai; Zhou, Chunhua; Liu, Yunguo; Fan, Ting; Wang, Xin

2009-05-30

Two soil samples were collected at mining areas located in southern Hunan Province, China. EDTA extraction of Pb, Zn, Cu and Cd from these two tailing soils was studied using column leaching experiments. The redistributions of heavy metals (HMs) were determined using the modified BCR (Community Bureau of Reference) sequential extraction procedure, before and after EDTA extraction. The results indicated that EDTA was an effective extractant because of its strong chelating ability for various HMs. The proportions of Pb, Zn, Cu and Cd in the four fractions varied largely after EDTA extraction. The extraction efficiency of EDTA of the acid-extractable fraction (AEX) was significant in shallow soil column, while in deeper soil column, decrease of the extraction efficiency of reduced (RED), oxidizable (OX) and residual fractions (RES) was obtained, which was mainly due to the decrease of EDTA concentration.

Nonlinear earthquake analysis of reinforced concrete frames with fiber and Bernoulli-Euler beam-column element.

PubMed

Karaton, Muhammet

2014-01-01

A beam-column element based on the Euler-Bernoulli beam theory is researched for nonlinear dynamic analysis of reinforced concrete (RC) structural element. Stiffness matrix of this element is obtained by using rigidity method. A solution technique that included nonlinear dynamic substructure procedure is developed for dynamic analyses of RC frames. A predicted-corrected form of the Bossak-α method is applied for dynamic integration scheme. A comparison of experimental data of a RC column element with numerical results, obtained from proposed solution technique, is studied for verification the numerical solutions. Furthermore, nonlinear cyclic analysis results of a portal reinforced concrete frame are achieved for comparing the proposed solution technique with Fibre element, based on flexibility method. However, seismic damage analyses of an 8-story RC frame structure with soft-story are investigated for cases of lumped/distributed mass and load. Damage region, propagation, and intensities according to both approaches are researched.

Improving Signal-to-Noise Ratio in Scanning Transmission Electron Microscopy Energy-Dispersive X-Ray (STEM-EDX) Spectrum Images Using Single-Atomic-Column Cross-Correlation Averaging.

PubMed

Jeong, Jong Seok; Mkhoyan, K Andre

2016-06-01

Acquiring an atomic-resolution compositional map of crystalline specimens has become routine practice, thus opening possibilities for extracting subatomic information from such maps. A key challenge for achieving subatomic precision is the improvement of signal-to-noise ratio (SNR) of compositional maps. Here, we report a simple and reliable solution for achieving high-SNR energy-dispersive X-ray (EDX) spectroscopy spectrum images for individual atomic columns. The method is based on standard cross-correlation aided by averaging of single-column EDX maps with modifications in the reference image. It produces EDX maps with minimal specimen drift, beam drift, and scan distortions. Step-by-step procedures to determine a self-consistent reference map with a discussion on the reliability, stability, and limitations of the method are presented here.

[Application of solid-phase extraction column for determination of matrine and oxymatrine in Sophora flavescens].

PubMed

Yang, Xia; Guo, Bao-Lin; Hu, Hong-Yu; Huang, Wen-Hua; Qiao, He-Ping; Fan, Sheng-Ci; Guan, Zha-Gen

2013-09-01

A Cleanert Alumina-N-SPE column (0.5 g/6 mL) chromatograpy with 5 mL of chloroform-methanol (7: 3) as eluent, instead of aluminum oxide column (100-200 mesh, 5 g, 1 cm) chromatograpy eluted successively with chloroform and the chloroform-methanol (7:3) (20 mL each), was applied to enrich matrine and oxymatrine in Sophora flavescens. Also, the optimization of the HPLC determination conditions with acetonitrile-ethanol absolute-3% phosphoric acid solution (84: 6: 10) as mobile phase, instead of acetonitrile-ethanol absolute -3% Phosphoric acid solution (80: 10: 10) recorded in Chinese Pharmacopoeia 2010 Edition, was more suitable for determination of matrine and oxymatrine in S. flavescens. This method has advantage of reducing sample handling time and solvent volume and increasing the accuracy and feasibility, which can simplify the procedure for determination of matrine and oxymatrine in S. flavescens.

Nitrogen removal from landfill leachate using single or combined processes.

PubMed

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

2005-04-01

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

76 FR 2109 - Next Generation Risk Assessment Public Dialogue Conference

Federal Register 2010, 2011, 2012, 2013, 2014

2011-01-12

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

Dry column-thermal energy analyzer method for determining N-nitrosopyrrolidine in fried bacon: collaborative study.

PubMed

Fiddler, W; Pensabene, J W; Gates, R A; Phillips, J G

1984-01-01

A dry column method for isolating N-nitrosopyrrolidine (NPYR) from fried, cure-pumped bacon and detection by gas chromatography-thermal energy analyzer (TEA) was studied collaboratively. Testing the results obtained from 11 collaborators for homogeneous variances among samples resulted in splitting the nonzero samples into 2 groups of sample levels, each with similar variances. Outlying results were identified by AOAC-recommended procedures, and laboratories having outliers within a group were excluded. Results from the 9 collaborators remaining in the low group yielded coefficients of variation (CV) of 6.00% and 7.47% for repeatability and reproducibility, respectively, and the 8 collaborators remaining in the high group yielded CV values of 5.64% and 13.72%, respectively. An 85.2% overall average recovery of the N-nitrosoazetidine internal standard was obtained with an average laboratory CV of 10.5%. The method has been adopted official first action as an alternative to the mineral oil distillation-TEA screening procedure.

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.

Reproducibility of up-flow column percolation tests for contaminated soils

PubMed Central

Naka, Angelica; Sakanakura, Hirofumi; Kurosawa, Akihiko; Inui, Toru; Takeo, Miyuki; Inoba, Seiji; Watanabe, Yasutaka; Fujikawa, Takuro; Miura, Toshihiko; Miyaguchi, Shinji; Nakajou, Kunihide; Sumikura, Mitsuhiro; Ito, Kenichi; Tamoto, Shuichi; Tatsuhara, Takeshi; Chida, Tomoyuki; Hirata, Kei; Ohori, Ken; Someya, Masayuki; Katoh, Masahiko; Umino, Madoka; Negishi, Masanori; Ito, Keijiro; Kojima, Junichi; Ogawa, Shohei

2017-01-01

Up-flow column percolation tests are used at laboratory scale to assess the leaching behavior of hazardous substance from contaminated soils in a specific condition as a function of time. Monitoring the quality of these test results inter or within laboratory is crucial, especially if used for Environment-related legal policy or for routine testing purposes. We tested three different sandy loam type soils (Soils I, II and III) to determine the reproducibility (variability inter laboratory) of test results and to evaluate the difference in the test results within laboratory. Up-flow column percolation tests were performed following the procedure described in the ISO/TS 21268–3. This procedure consists of percolating solution (calcium chloride 1 mM) from bottom to top at a flow rate of 12 mL/h through softly compacted soil contained in a column of 5 cm diameter and 30 ± 5 cm height. Eluate samples were collected at liquid-to-solid ratio of 0.1, 0.2, 0.5, 1, 2, 5 and 10 L/kg and analyzed for quantification of the target elements (Cu, As, Se, Cl, Ca, F, Mg, DOC and B in this research). For Soil I, 17 institutions in Japan joined this validation test. The up-flow column experiments were conducted in duplicate, after 48 h of equilibration time and at a flow rate of 12 mL/h. Column percolation test results from Soils II and III were used to evaluate the difference in test results from the experiments conducted in duplicate in a single laboratory, after 16 h of equilibration time and at a flow rate of 36 mL/h. Overall results showed good reproducibility (expressed in terms of the coefficient of variation, CV, calculated by dividing the standard deviation by the mean), as the CV was lower than 30% in more than 90% of the test results associated with Soil I. Moreover, low variability (expressed in terms of difference between the two test results divided by the mean) was observed in the test results related to Soils II and III, with a variability lower than 30% in more than 88% of the cases for Soil II and in more than 96% of the cases for Soil III. We also discussed the possible factors that affect the reproducibility and variability in the test results from the up-flow column percolation tests. The low variability inter and within laboratory obtained in this research indicates that the ISO/TS 21268–3 can be successfully upgraded to a fully validated ISO standard. PMID:28582458

Method of recovering adsorbed liquid compounds from molecular sieve columns

DOEpatents

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

1983-12-20

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

Method of recovering adsorbed liquid compounds from molecular sieve columns

DOEpatents

Burkholder, Harvey R.; Fanslow, Glenn E.

1983-01-01

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

Antibody-immobilized column for quick cell separation based on cell rolling.

PubMed

Mahara, Atsushi; Yamaoka, Tetsuji

2010-01-01

Cell separation using methodological standards that ensure high purity is a very important step in cell transplantation for regenerative medicine and for stem cell research. A separation protocol using magnetic beads has been widely used for cell separation to isolate negative and positive cells. However, not only the surface marker pattern, e.g., negative or positive, but also the density of a cell depends on its developmental stage and differentiation ability. Rapid and label-free separation procedures based on surface marker density are the focus of our interest. In this study, we have successfully developed an antiCD34 antibody-immobilized cell-rolling column, that can separate cells depending on the CD34 density of the cell surfaces. Various conditions for the cell-rolling column were optimized including graft copolymerization, and adjustment of the column tilt angle, and medium flow rate. Using CD34-positive and -negative cell lines, the cell separation potential of the column was established. We observed a difference in the rolling velocities between CD34-positive and CD34-negative cells on antibody-immobilized microfluidic device. Cell separation was achieved by tilting the surface 20 degrees and the increasing medium flow. Surface marker characteristics of the isolated cells in each fraction were analyzed using a cell-sorting system, and it was found that populations containing high density of CD34 were eluted in the delayed fractions. These results demonstrate that cells with a given surface marker density can be continuously separated using the cell rolling column.

Monolithic column based on a poly(glycidyl methacrylate-co-4-vinylphenylboronic acid-co-ethylene dimethacrylate) copolymer for capillary liquid chromatography of small molecules and proteins.

PubMed

Lin, Zian; Huang, Hui; Sun, Xiaobo; Lin, Yao; Zhang, Lan; Chen, Guonan

2012-07-13

A new polymer monolith with three modes of reverse-phase, hydrophilic and cation-exchange interaction was synthesized in 100 μm i.d. fused-silica capillary by in situ polymerization procedure. The pre-polymerization mixture consisted of glycidyl methacrylate (GMA) and 4-vinylphenylboronic acid (VPBA) as bifunctional monomers, ethylene dimethacrylate (EDMA) as crosslinker, 1,4-butanediol (BDO) and diethylene glycol (DEG) as binary porogenic solvents, and azobisisobutyronitrile (AIBN) as initiator. The resulting poly(GMA-co-VPBA-co-EDMA) monolith showed a relatively homogeneous monolithic structure, good permeability and mechanical stability. Different ratios of monomers and porogens were used for optimizing the properties of monolithic column. The column performance was assessed by the separation of a series of neutral solutes, charge solutes, phenols and anilines. Compared with poly(GMA-co-EDMA) monolith, the proposed monolith exhibited more flexible adjustment of selectivity in terms of hydrophobic, hydrophilic, as well as cation-exchange interaction in the same chromatographic conditions. High column efficiencies for benzene derivatives with 70,000-102,000 theoretical plates/m could be obtained at a linear velocity of 0.265 mm/s. The run-to-run, column-to-column, and batch-to-batch repeatabilities of the retention times were less than 8.23%. Additionally, the purposed monolith was also applied to efficient separation of alkaloids and proteins for demonstrating its potential in biomolecule separation. Crown Copyright © 2012. Published by Elsevier B.V. All rights reserved.

Optimized Enrichment of Phosphoproteomes by Fe-IMAC Column Chromatography.

PubMed

Ruprecht, Benjamin; Koch, Heiner; Domasinska, Petra; Frejno, Martin; Kuster, Bernhard; Lemeer, Simone

2017-01-01

Phosphorylation is among the most important post-translational modifications of proteins and has numerous regulatory functions across all domains of life. However, phosphorylation is often substoichiometric, requiring selective and sensitive methods to enrich phosphorylated peptides from complex cellular digests. Various methods have been devised for this purpose and we have recently described a Fe-IMAC HPLC column chromatography setup which is capable of comprehensive, reproducible, and selective enrichment of phosphopeptides out of complex peptide mixtures. In contrast to other formats such as StageTips or batch incubations using TiO 2 or Ti-IMAC beads, Fe-IMAC HPLC columns do not suffer from issues regarding incomplete phosphopeptide binding or elution and enrichment efficiency scales linearly with the amount of starting material. Here, we provide a step-by-step protocol for the entire phosphopeptide enrichment procedure including sample preparation (lysis, digestion, desalting), Fe-IMAC column chromatography (column setup, operation, charging), measurement by LC-MS/MS (nHPLC gradient, MS parameters) and data analysis (MaxQuant). To increase throughput, we have optimized several key steps such as the gradient time of the Fe-IMAC separation (15 min per enrichment), the number of consecutive enrichments possible between two chargings (>20) and the column recharging itself (<1 h). We show that the application of this protocol enables the selective (>90 %) identification of more than 10,000 unique phosphopeptides from 1 mg of HeLa digest within 2 h of measurement time (Q Exactive Plus).

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

PubMed

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

2010-06-15

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

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

NASA Technical Reports Server (NTRS)

Choi, S.; Joiner, J.; Choi, Y.; Duncan, B. N.; Bucsela, E.

2014-01-01

We derive free-tropospheric NO2 volume mixing ratios (VMRs) and stratospheric column amounts of NO2 by applying a cloud slicing technique to data from the Ozone Monitoring Instrument (OMI) on the Aura satellite. In the cloud-slicing approach, the slope of the above-cloud NO2 column versus the cloud scene pressure is proportional to the NO2 VMR. In this work, we use a sample of nearby OMI pixel data from a single orbit for the linear fit. The OMI data include cloud scene pressures from the rotational-Raman algorithm and above-cloud NO2 vertical column density (VCD) (defined as the NO2 column from the cloud scene pressure to the top-of-the-atmosphere) from a differential optical absorption spectroscopy (DOAS) algorithm. Estimates of stratospheric column NO2 are obtained by extrapolating the linear fits to the tropopause. We compare OMI-derived NO2 VMRs with in situ aircraft profiles measured during the NASA Intercontinental Chemical Transport Experiment Phase B (INTEX-B) campaign in 2006. The agreement is generally within the estimated uncertainties when appropriate data screening is applied. We then derive a global seasonal climatology of free-tropospheric NO2 VMR in cloudy conditions. Enhanced NO2 in the free troposphere commonly appears near polluted urban locations where NO2 produced in the boundary layer may be transported vertically out of the boundary layer and then horizontally away from the source. Signatures of lightning NO2 are also shown throughout low and middle latitude regions in summer months. A profile analysis of our cloud slicing data indicates signatures of uplifted and transported anthropogenic NO2 in the middle troposphere as well as lightning-generated NO2 in the upper troposphere. Comparison of the climatology with simulations from the Global Modeling Initiative (GMI) for cloudy conditions (cloud optical thicknesses > 10) shows similarities in the spatial patterns of continental pollution outflow. However, there are also some differences in the seasonal variation of free-tropospheric NO2 VMRs near highly populated regions and in areas affected by lightning-generated NOx. Stratospheric column NO2 obtained from cloud slicing agrees well with other independently-generated estimates, providing further confidence in the free-tropospheric results.

Biclustering of gene expression data using reactive greedy randomized adaptive search procedure.

PubMed

Dharan, Smitha; Nair, Achuthsankar S

2009-01-30

Biclustering algorithms belong to a distinct class of clustering algorithms that perform simultaneous clustering of both rows and columns of the gene expression matrix and can be a very useful analysis tool when some genes have multiple functions and experimental conditions are diverse. Cheng and Church have introduced a measure called mean squared residue score to evaluate the quality of a bicluster and has become one of the most popular measures to search for biclusters. In this paper, we review basic concepts of the metaheuristics Greedy Randomized Adaptive Search Procedure (GRASP)-construction and local search phases and propose a new method which is a variant of GRASP called Reactive Greedy Randomized Adaptive Search Procedure (Reactive GRASP) to detect significant biclusters from large microarray datasets. The method has two major steps. First, high quality bicluster seeds are generated by means of k-means clustering. In the second step, these seeds are grown using the Reactive GRASP, in which the basic parameter that defines the restrictiveness of the candidate list is self-adjusted, depending on the quality of the solutions found previously. We performed statistical and biological validations of the biclusters obtained and evaluated the method against the results of basic GRASP and as well as with the classic work of Cheng and Church. The experimental results indicate that the Reactive GRASP approach outperforms the basic GRASP algorithm and Cheng and Church approach. The Reactive GRASP approach for the detection of significant biclusters is robust and does not require calibration efforts.

Incidental intrathecal injection of meglumine diatrizoate.

PubMed

Masjedi, Mansour; Khosravi, Abbas; Sabetian, Golnar; Rahmanian, Mohammad Reza

2014-05-01

Myelograghy is a process of instilling contrast medium to the subarachnoid space for evaluating the spinal column by radiography. There are various contrast solutions for different radiographic studies but not all of them are suitable for spinal column evaluation. Our patient was a 60-year-old man who developed severe pain, tonic clonic convulsions and cardiopulmonary arrest after intrathecal injection of 14 mL of meglumine diatrizoate during an elective myelography procedure. Many of these cases would die or suffer from permanent sequelae if appropriate treatment is not received. Our subject recovered completely without any sequelae after receiving appropriate treatment in a multidisciplinary intensive care unit.

Osmium-191/iridium-191m radionuclide

DOEpatents

Knapp, Jr., Furn F.; Butler, Thomas A.; Brihaye, Claude

1987-01-01

A generator system to provide iridium-191m for clinical imaging applications comprises an activated carbon adsorbent loaded with a compound containing the parent nuclide, osmium-191. The generator, which has a shelf-life in excess of two weeks and does not require a scavenger column, can be eluted with physiologically compatible saline.

Liquid chromatography of polymers under limiting conditions of desorption II. Tandem injection and quantitative molar mass determination.

PubMed

Snauko, Marián; Berek, Dusan

2005-11-11

Liquid chromatography under limiting conditions of desorption (LC LCD) is a method which allows molar mass independent elution of various synthetic polymers. A narrow, slowly moving zone of small molecules, which promotes full adsorption of one kind of polymer species within column (an adsorli) acts as an impermeable barrier for the fast moving macromolecules. The latter accumulate on the barrier edge and elute nearly in total volume of liquid within column. At the same time, transport of less adsorptive macromolecules is not hampered so that these are eluted in the size exclusion (SEC) mode. As result, polymers differing in their polarity and adsorptivity can be easily separated without molar mass interference. Three methods of barrier creation are discussed and compared. It is shown that a fraction of sample may elute unretained if the adsorli sample solvent is used as a barrier in connection with a narrow-pore column packing. One part of excluded macromolecules likely breaks-out from the adsorli zone and this results in partial loss of sample and distortion of the LC LCD peaks. This problem can be avoided if the adsorli zone is injected immediately before sample solution. Applicability of the LC LCD method for polymer separation has been demonstrated with a model mixture of poly(methyl methacrylate) (adsorbing polymer) and polystyrene (non adsorbing polymer) using bare silica gel as a column packing with a combination of tetrahydrofuran (a desorption promoting liquid -a desorli) and toluene (adsorli). It has been shown that the LC LCD procedure with tandem injection allows simple and fast discrimination of polymer blend components with good repeatability and high sample recovery. For quantitative determination of molar masses of both LC LCD and SEC eluted polymers, an additional size exclusion chromatographic column can be applied either in a conventional way or in combination with a multi-angle light scattering detector. A single eluent is used in the latter column, which separates the mixed mobile phase, system peaks and the desorli zone from the polymer peaks so that measurements are free from disturbances caused by the changing eluent composition. The resulting LC LCD x SEC procedure has been successfully applied to poly(methyl methacrylate) samples.

HPLC, MS, and pharmacokinetics of melphalan, bisantrene and 13-cis retinoic acid.

PubMed

Davis, T P; Peng, Y M; Goodman, G E; Alberts, D S

1982-11-01

High performance liquid chromatographic procedures are described for melphalan, bisantrene, and 13-cis retinoic acid, three important anticancer drugs in various stages of clinical development. The procedures require a rapid and simple sample clean-up followed by a 10-to 20-min chromatographic separation on a reversed-phase C18 column. Precisions are all less than 8% with recoveries greater than 80%. Mass spectrometry confirmation of each drug from patient sample separations is presented to provide unambiguous identification for valid pharmacokinetic parameter determination.

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

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

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

1997-05-01

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

Density Gradients in Chemistry Teaching

ERIC Educational Resources Information Center

Miller, P. J.

1972-01-01

Outlines experiments in which a density gradient might be used to advantage. A density gradient consists of a column of liquid, the composition and density of which varies along its length. The procedure can be used in analysis of solutions and mixtures and in density measures of solids. (Author/TS)

Ion Exchange Chromatography and Spectrophotometry: An Introductory Undergraduate Laboratory Experiment.

ERIC Educational Resources Information Center

Foster, N.; And Others

1985-01-01

Describes an experiment in which students use ion exchange chromatography to separate a mixture of chloro complexes of transition metal ions and then use spectrophotometry to define qualitatively the efficiency of the ion exchange columns. Background information, materials needed, and procedures used are included. (JN)

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

PubMed

Rittfeldt, L

2001-06-01

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

Quantifying the condition of eruption column collapse during explosive volcanic eruptions

NASA Astrophysics Data System (ADS)

Koyaguchi, Takehiro; Suzuki, Yujiro

2016-04-01

During an explosive eruption, a mixture of pyroclasts and volcanic gas forms a buoyant eruption column or a pyroclastic flow. Generation of a pyroclastic flow caused by eruption column collapse is one of the most hazardous phenomena during explosive volcanic eruptions. The quantification of column collapse condition (CCC) is, therefore, highly desired for volcanic hazard assessment. Previously the CCC was roughly predicted by a simple relationship between magma discharge rate and water content (e.g., Carazzo et al., 2008). When a crater is present above the conduit, because of decompression/compression process inside/above the crater, the CCC based on this relationship can be strongly modified (Woods and Bower, 1995; Koyaguchi et al., 2010); however, the effects of the crater on CCC has not been fully understood in a quantitative fashion. Here, we have derived a semi-analytical expression of CCC, in which the effects of the crater is taken into account. The CCC depends on magma properties, crater shape (radius, depth and opening angle) as well as the flow rate at the base of crater. Our semi-analytical CCC expresses all these dependencies by a single surface in a parameter space of the dimensionless magma discharge rate, the dimensionless magma flow rate (per unit area) and the ratio of the cross-sectional areas at the top and the base of crater. We have performed a systematic parameter study of three-dimensional (3D) numerical simulations of eruption column dynamics to confirm the semi-analytical CCC. The results of the 3D simulations are consistent with the semi-analytical CCC, while they show some additional fluid dynamical features in the transitional state (e.g., partial column collapse). Because the CCC depends on such many parameters, the scenario towards the generation of pyroclastic flow during explosive eruptions is considered to be diverse. Nevertheless, our semi-analytical CCC together with the existing semi-analytical solution for the 1D conduit flow model (Koyaguchi, 2005) allows us to intuitively and quantitatively understand how the eruption column dynamics approaches to the CCC as the crater radius increases during the waxing stage of an eruption, or as the magma chamber pressure decreases during the waning stage.

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

PubMed

Andrzejewska, Anna; Kaczmarski, Krzysztof; Guiochon, Georges

2009-02-13

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

Selenium adsorption and speciation with Mg-FeCO₃ layered double hydroxides loaded cellulose fibre.

PubMed

Chen, Ming-Li; An, Myog-Il

2012-06-15

A novel adsorbent was developed by coating Mg-FeCO(3) layered double hydroxides (LDHs) on cellulose fibre. The LDHs take up significant amount of selenite and selenate in a wide pH range with similar sorption capacities (pH 3.8-8.0 for selenite and pH 5.8-7.0 for selenate). A mini-column packed with Mg-FeCO(3) LDHs layer coated cellulose fibre particles was incorporated into a sequential injection system for uptake of selenite at pH 6.0. The retained selenite was afterwards collected with 70 μ L of 0.8%(m/v) NaOH as eluent, followed by hydride generation and atomic fluorescence spectrometric detection. Total inorganic selenium was adsorbed at pH 6.0 by the LDHs-cellulose fibre mini-column after selenate was pre-reduced to selenite by 2.0 mol L(-1) HCl at 80°C, and selenium speciation was performed by difference. With a sample volume of 1.0 mL, an enrichment factor of 13.3 was derived with a detection limit of 11 ng L(-1) within a linear range of 0.04-4.0 μg L(-1). A relative standard deviation (RSD) of 3.3% (0.5 μg L(-1), n=11) was achieved. The procedure was validated by analyzing selenium in a certified reference material GBW 10010 (rice), and speciation of inorganic selenium in natural water samples. Copyright © 2012 Elsevier B.V. All rights reserved.

Feasibility of treating emulsified oily and salty wastewaters through coagulation and bio-regenerated GAC filtration.

PubMed

Mancini, Giuseppe; Panzica, Michele; Fino, Debora; Cappello, Simone; Yakimov, Michail M; Luciano, Antonella

2017-12-01

In the present study, chemical oxygen demand (COD) removal by coagulation and packed-columns of both fresh and bioregenerated granular activated carbon (GAC) is reported as a feasible treatment for saline and oily wastewaters (slops) generated from marine oil tankers cleaning. The use of Ferric chloride (FeCl 3 ), Aluminium sulphate (Al 2 (SO 4 ) 3 ) and Polyaluminum chloride (Al 2 (OH 3 )Cl 3 ) was evaluated in the pre-treatment by coagulation of a real slop, after a de-oiling phase in a tank skimmer Comparison of coagulation process indicated that Polyaluminum chloride and Aluminium sulphate operate equally well (20-30% of COD removal) when applied at their optimal dose (40 and 90 mg/l respectively) but the latter should be preferred in order to significantly control the sludge production. The results from the column filtration tests indicated the feasibility of using the selected GAC (Filtrasorb 400 -Calgon Carbon Corporation) to achieve the respect of the discharge limits in the slops treatment with a carbon usage rate in the range 0.1-0.3 kg/m 3 of treated effluent. Moreover, biological regeneration through Alcalinovorax borkumensis SK2 was proved to be a cost-effective procedure since the reuse of spent GAC through such regeneration process for further treatment could still achieve approximately 90% of the initial sorption capacity, reducing then costs for the use of new sorbents and also the need for waste disposal. Copyright © 2016 Elsevier Ltd. All rights reserved.

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

PubMed

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

2017-01-06

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

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.

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

PubMed

Can, Nafiz O

2011-08-01

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

Effects of local meteorology and aerosols on ozone and nitrogen dioxide retrievals from OMI and pandora spectrometers in Maryland, USA during DISCOVER-AQ 2011.

PubMed

Reed, Andra J; Thompson, Anne M; Kollonige, Debra E; Martins, Douglas K; Tzortziou, Maria A; Herman, Jay R; Berkoff, Timothy A; Abuhassan, Nader K; Cede, Alexander

An analysis is presented for both ground- and satellite-based retrievals of total column ozone and nitrogen dioxide levels from the Washington, D.C., and Baltimore, Maryland, metropolitan area during the NASA-sponsored July 2011 campaign of D eriving I nformation on S urface CO nditions from Column and VER tically Resolved Observations Relevant to A ir Q uality (DISCOVER-AQ). Satellite retrievals of total column ozone and nitrogen dioxide from the Ozone Monitoring Instrument (OMI) on the Aura satellite are used, while Pandora spectrometers provide total column ozone and nitrogen dioxide amounts from the ground. We found that OMI and Pandora agree well (residuals within ±25 % for nitrogen dioxide, and ±4.5 % for ozone) for a majority of coincident observations during July 2011. Comparisons with surface nitrogen dioxide from a Teledyne API 200 EU NO x Analyzer showed nitrogen dioxide diurnal variability that was consistent with measurements by Pandora. However, the wide OMI field of view, clouds, and aerosols affected retrievals on certain days, resulting in differences between Pandora and OMI of up to ±65 % for total column nitrogen dioxide, and ±23 % for total column ozone. As expected, significant cloud cover (cloud fraction >0.2) was the most important parameter affecting comparisons of ozone retrievals; however, small, passing cumulus clouds that do not coincide with a high (>0.2) cloud fraction, or low aerosol layers which cause significant backscatter near the ground affected the comparisons of total column nitrogen dioxide retrievals. Our results will impact post-processing satellite retrieval algorithms and quality control procedures.

Compression-bending of multi-component semi-rigid columns in response to axial loads and conjugate reciprocal extension-prediction of mechanical behaviours and implications for structural design.

PubMed

Lau, Ernest W

2013-01-01

The mathematical modelling of column buckling or beam bending under an axial or transverse load is well established. However, the existent models generally assume a high degree of symmetry in the structure of the column and minor longitudinal and transverse displacements. The situation when the column is made of several components with different mechanical properties asymmetrically distributed in the transverse section, semi-rigid, and subjected to multiple axial loads with significant longitudinal and transverse displacements through compression and bending has not been well characterised. A more comprehensive theoretical model allowing for these possibilities and assuming a circular arc contour for the bend is developed, and used to establish the bending axes, balance between compression and bending, and equivalent stiffness of the column. In certain situations, such as with pull cable catheters commonly used for minimally invasive surgical procedures, the compression loads are applied via cables running through channels inside a semi-rigid column. The model predicts the mathematical relationships between the radius of curvature of the bend and the tension in and normal force exerted by such cables. Conjugate extension with reciprocal compression-bending is a special structural arrangement for a semi-rigid column such that extension of one segment is linked to compression-bending of another by inextensible cables running between them. Leads are cords containing insulated electrical conductor coil and cables between the heart muscle and cardiac implantable electronic devices. Leads can behave like pull cable catheters through differential component pulling, providing a possible mechanism for inside-out abrasion and conductor cable externalisation. Certain design features may predispose to this mode of structural failure. Copyright © 2012 Elsevier Ltd. All rights reserved.

Single-column purification of the tag-free, recombinant form of the neuronal calcium sensor protein, hippocalcin expressed in Escherichia coli.

PubMed

Krishnan, Anuradha; Viviano, Jeffrey; Morozov, Yaroslav; Venkataraman, Venkat

2016-07-01

Hippocalcin is a 193 aa protein that is a member of the neuronal calcium sensor protein family, whose functions are regulated by calcium. Mice that lack the function of this protein are compromised in the long term potentiation aspect of memory generation. Recently, mutations in the gene have been linked with dystonia in human. The protein has no intrinsic enzyme activity but is known to bind to variety of target proteins. Very little information is available on how the protein executes its critical role in signaling pathways, except that it is regulated by binding of calcium. Further delineation of its function requires large amounts of pure protein. In this report, we present a single-step purification procedure that yields high quantities of the bacterially expressed, recombinant protein. The procedure may be adapted to purify the protein from inclusion bodies or cytosol in its myristoylated or non-myristoylated forms. MALDI-MS (in source decay) analyses demonstrates that the myristoylation occurs at the glycine residue. The protein is also biologically active as measured through tryptophan fluorescence, mobility shift and guanylate cyclase activity assays. Thus, further analyses of hippocalcin, both structural and functional, need no longer be limited by protein availability. Copyright © 2016 Elsevier Inc. All rights reserved.

Comparison of three methods for determination of N-nitrosopyrrolidine in fried dry-cured bacon.

PubMed

Gates, R A; Pensabene, J W; Fiddler, W

1984-01-01

The recently developed Eastern Regional Research Center ( ERRC ) dry column chromatographic procedure for determining N-nitrosopyrrolidine (NPYR) in fried cure-pumped bacon was evaluated for its applicability to fried dry-cured bacon. The method was then compared with 2 established procedures for volatile nitrosamine analysis in cured meat products: the multidetection thermal energy analyzer (MD) method and the mineral oil distillation (MOD) screening procedure. No significant difference (P less than 0.05) in NPYR values was found between the ERRC and MD procedures, but significant differences were found between the ERRC and MOD procedures and between the MOD and MD procedures. No artifactual nitrosamine formation was found in the ERRC procedure, but significant amounts were found in samples analyzed by the MOD procedure. The ERRC method was demonstrated to be rugged and very rapid. It is proposed that the ERRC method replace the MOD method as the official screening procedure for NPYR in fried bacon.

40 CFR 63.786 - Test methods and procedures.

Code of Federal Regulations, 2010 CFR

2010-07-01

... by Gas Chromatography (incorporation by reference—see § 63.14). In determining the sensitivity, the... Practice for Gas Chromatography [incorporation by reference—see § 63.14].) (c) A coating manufacturer or... mixture under analysis are not known. In such cases a single column gas chromatograph (GC) may not be...

40 CFR 63.786 - Test methods and procedures.

Code of Federal Regulations, 2011 CFR

2011-07-01

... by Gas Chromatography (incorporation by reference—see § 63.14). In determining the sensitivity, the... Practice for Gas Chromatography [incorporation by reference—see § 63.14].) (c) A coating manufacturer or... mixture under analysis are not known. In such cases a single column gas chromatograph (GC) may not be...

Program Review: A Critical Analysis of Departmental Effectiveness. Revised.

ERIC Educational Resources Information Center

Huffman, Zoula; And Others

Describing the evaluation and planning process at Mississippi Gulf Coast Community College, this document presents guidelines, procedures, and indicators used at the college for the systematic review of academic departmental effectiveness. First, the five-column program review model used at the college is outlined and the purposes of review are…

SW-846 Test Method 4025: Screening for Polychlorinated Dibenzodioxins and Polychlorinated Dibenzofurans (PCDD/PCDFs) by Immunoassay

EPA Pesticide Factsheets

a procedure for the analysis of (PCDDs/PCDFs) in soil at 500 ppt (pg/g) using a simple onestep liquid phase oxidative cleanup or, at mid to low ppt levels, using a two step coupled column cleanup (oxidation and activated carbon binding)

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

ERIC Educational Resources Information Center

Ondrus, Martin G.; And Others

1983-01-01

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

High Performance Liquid Chromatography of Some Analgesic Compounds: An Instrumental Analysis Experiment.

ERIC Educational Resources Information Center

Haddad, Paul; And Others

1983-01-01

Background information, procedures, and results are provided for an experiment demonstrating techniques of solvent selection, gradient elution, pH control, and ion-pairing in the analysis of an analgesic mixture using reversed-phase liquid chromatography on an octadecylsilane column. Although developed using sophisticated/expensive equipment, less…

Chairside Assisting Skill Evaluation (CASE). Clinical Setting. Health Manpower References.

ERIC Educational Resources Information Center

Innovative Programming Systems, Minneapolis, Minn.

These checklists are designed for use during the dental assistant student's extramural clinical experience assignment. Checklists test students on their knowledge of terminology, equipment, procedures, and patient relations. Objectives are listed outline style with columns to check progress during a first and a second evaluation. Areas included…

Iron-Sulfur-Carbonyl and -Nitrosyl Complexes: A Laboratory Experiment.

ERIC Educational Resources Information Center

Glidewell, Christopher; And Others

1985-01-01

Background information, materials needed, procedures used, and typical results obtained, are provided for an experiment on iron-sulfur-carbonyl and -nitrosyl complexes. The experiment involved (1) use of inert atmospheric techniques and thin-layer and flexible-column chromatography and (2) interpretation of infrared, hydrogen and carbon-13 nuclear…

DEVELOPING CRITICAL READING POWER THROUGH NEWSPAPER READING.

ERIC Educational Resources Information Center

SAILER, CARL

A METHOD OF DEVELOPING CRITICAL READING POWER BY ANALYZING ADVERTISEMENTS, CARTOONS, EDITORIALS, AND CONTROVERSIAL ISSUES FOUND IN NEWSPAPERS IS DESCRIBED. SPECIFIC EXAMPLES OF TEACHING PROCEDURES ARE GIVEN. IT IS SUGGESTED THAT A WIDE RANGE OF NEWSPAPERS BE USED SO THAT THE DIFFERENT VIEWPOINTS EXPRESSED IN COLUMNS, EDITORIALS, AND POLITICAL NEWS…

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

PubMed

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

2005-12-15

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

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

PubMed

Gritti, Fabrice; Guiochon, Georges

2011-08-05

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

Leaching of cadmium and tellurium from cadmium telluride (CdTe) thin-film solar panels under simulated landfill conditions

PubMed Central

Ramos-Ruiz, Adriana; Wilkening, Jean V.; Field, James A.; Sierra-Alvarez, Reyes

2017-01-01

A crushed non-encapsulated CdTe thin-film solar cell was subjected to two standardized batch leaching tests (i.e., Toxicity Characteristic Leaching Procedure (TCLP) and California Waste Extraction Test (WET)) and to a continuous-flow column test to assess cadmium (Cd) and tellurium (Te) dissolution under conditions simulating the acidic- and the methanogenic phases of municipal solid waste landfills. Low levels of Cd and Te were solubilized in both batch leaching tests (<8.2% and <3.6% of added Cd and Te, respectively). On the other hand, over the course of 30 days, 73% of the Cd and 21% of the Te were released to the synthetic leachate of a continuous-flow column simulating the acidic landfill phase. The dissolved Cd concentration was 3.24-fold higher than the TCLP limit (1 mg L-1), and 650-fold higher than the maximum contaminant level established by the US-EPA for this metal in drinking water (0.005 mg L-1). In contrast, the release of Cd and Te to the effluent of the continuous-flow column simulating the methanogenic phase of a landfill was negligible. The remarkable difference in the leaching behavior of CdTe in the columns is related to different aqueous pH and redox conditions promoted by the microbial communities in the columns, and is in agreement with thermodynamic predictions. PMID:28472709

A New Resonance Tube

NASA Astrophysics Data System (ADS)

Bates, Alan

2017-12-01

The measurement of the speed of sound in air with the resonance tube is a popular experiment that often yields accurate results. One approach is to hold a vibrating tuning fork over an air column that is partially immersed in water. The column is raised and lowered in the water until the generated standing wave produces resonance: this occurs at the point where sound is perceived to have maximum loudness, or at the point where the amplitude of the standing wave has maximum value, namely an antinode. An antinode coincides with the position of the tuning fork, beyond the end of the air column, which consequently introduces an end correction. One way to minimize this end correction is to measure the distance between consecutive antinodes.

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

PubMed

Chong, Andrea D; Mayer, K Ulrich

2017-09-01

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

Quantitative structure-retention relationship models for the prediction of the reversed-phase HPLC gradient retention based on the heuristic method and support vector machine.

PubMed

Du, Hongying; Wang, Jie; Yao, Xiaojun; Hu, Zhide

2009-01-01

The heuristic method (HM) and support vector machine (SVM) were used to construct quantitative structure-retention relationship models by a series of compounds to predict the gradient retention times of reversed-phase high-performance liquid chromatography (HPLC) in three different columns. The aims of this investigation were to predict the retention times of multifarious compounds, to find the main properties of the three columns, and to indicate the theory of separation procedures. In our method, we correlated the retention times of many diverse structural analytes in three columns (Symmetry C18, Chromolith, and SG-MIX) with their representative molecular descriptors, calculated from the molecular structures alone. HM was used to select the most important molecular descriptors and build linear regression models. Furthermore, non-linear regression models were built using the SVM method; the performance of the SVM models were better than that of the HM models, and the prediction results were in good agreement with the experimental values. This paper could give some insights into the factors that were likely to govern the gradient retention process of the three investigated HPLC columns, which could theoretically supervise the practical experiment.

A macro-enzyme cause of an isolated increase of alkaline phosphatase.

PubMed

Cervinski, Mark A; Lee, Hong Kee; Martin, Isabella W; Gavrilov, Dimitar K

2015-02-02

Macroenzyme complexes of serum enzymes and antibody can increase the circulating enzymatic activity and may lead to unnecessary additional testing and procedures. Laboratory physicians and scientists need to be aware of techniques to identify macroenzyme complexes when suspected. To investigate the possibility of a macro-alkaline phosphatase in the serum of a 74 year old male with persistently increased alkaline phosphatase we coupled a protein A/G agarose affinity chromatography technique with isoenzyme electrophoresis to look for the presence of macro-alkaline phosphatase. The majority of the alkaline phosphatase activity in the patient's serum sample was bound to the column and only a minor fraction (25%) of alkaline phosphatase activity was present in the column flow-through. The alkaline phosphatase activity was also found to co-elute with the immunoglobulins in the patient sample. The alkaline phosphatase activity in a control serum sample concurrently treated in the same manner did not bind to the column and was found in the column flow-through. The use of protein A/G agarose affinity chromatography is a rapid and simple method that can be applied to the investigation of other macro-enzyme complexes. Copyright © 2014 Elsevier B.V. All rights reserved.

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

Code of Federal Regulations, 2014 CFR

2014-07-01

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

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

Code of Federal Regulations, 2013 CFR

2013-07-01

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

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

Code of Federal Regulations, 2012 CFR

2012-07-01

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

Osmium-191/iridium-191m radionuclide

DOEpatents

Knapp, F.F. Jr.; Butler, T.A.; Brihaye, C.

1985-08-26

A generator system to provide iridium-191m for clinical imaging applications comprises an activated carbon adsorbent loaded with a compound containing the parent nuclide, osmium-191. The generator, which has a shelf-life in excess of two weeks and does not require a scavenger column, can be eluted with physiologically compatible saline. 4 figs. 3 tabs.

Vertically migrating swimmers generate aggregation-scale eddies in a stratified column.

PubMed

Houghton, Isabel A; Koseff, Jeffrey R; Monismith, Stephen G; Dabiri, John O

2018-04-01

Biologically generated turbulence has been proposed as an important contributor to nutrient transport and ocean mixing 1-3 . However, to produce non-negligible transport and mixing, such turbulence must produce eddies at scales comparable to the length scales of stratification in the ocean. It has previously been argued that biologically generated turbulence is limited to the scale of the individual animals involved 4 , which would make turbulence created by highly abundant centimetre-scale zooplankton such as krill irrelevant to ocean mixing. Their small size notwithstanding, zooplankton form dense aggregations tens of metres in vertical extent as they undergo diurnal vertical migration over hundreds of metres 3,5,6 . This behaviour potentially introduces additional length scales-such as the scale of the aggregation-that are of relevance to animal interactions with the surrounding water column. Here we show that the collective vertical migration of centimetre-scale swimmers-as represented by the brine shrimp Artemia salina-generates aggregation-scale eddies that mix a stable density stratification, resulting in an effective turbulent diffusivity up to three orders of magnitude larger than the molecular diffusivity of salt. These observed large-scale mixing eddies are the result of flow in the wakes of the individual organisms coalescing to form a large-scale downward jet during upward swimming, even in the presence of a strong density stratification relative to typical values observed in the ocean. The results illustrate the potential for marine zooplankton to considerably alter the physical and biogeochemical structure of the water column, with potentially widespread effects owing to their high abundance in climatically important regions of the ocean 7 .

Improved optimization of polycyclic aromatic hydrocarbons (PAHs) mixtures resolution in reversed-phase high-performance liquid chromatography by using factorial design and response surface methodology.

PubMed

Andrade-Eiroa, Auréa; Diévart, Pascal; Dagaut, Philippe

2010-04-15

A new procedure for optimizing PAHs separation in very complex mixtures by reverse phase high performance (RPLC) is proposed. It is based on changing gradually the experimental conditions all along the chromatographic procedure as a function of the physical properties of the compounds eluted. The temperature and speed flow gradients allowed obtaining the optimum resolution in large chromatographic determinations where PAHs with very different medium polarizability have to be separated. Whereas optimization procedures of RPLC methodologies had always been accomplished regardless of the physico-chemical properties of the target analytes, we found that resolution is highly dependent on the physico-chemical properties of the target analytes. Based on resolution criterion, optimization process for a 16 EPA PAHs mixture was performed on three sets of difficult-to-separate PAHs pairs: acenaphthene-fluorene (for the optimization procedure in the first part of the chromatogram where light PAHs elute), benzo[g,h,i]perylene-dibenzo[a,h]anthracene and benzo[g,h,i]perylene-indeno[1,2,3-cd]pyrene (for the optimization procedure of the second part of the chromatogram where the heavier PAHs elute). Two-level full factorial designs were applied to detect interactions among variables to be optimized: speed flow, temperature of column oven and mobile-phase gradient in the two parts of the studied chromatogram. Experimental data were fitted by multivariate nonlinear regression models and optimum values of speed flow and temperature were obtained through mathematical analysis of the constructed models. An HPLC system equipped with a reversed phase 5 microm C18, 250 mm x 4.6mm column (with acetonitrile/water mobile phase), a column oven, a binary pump, a photodiode array detector (PDA), and a fluorimetric detector were used in this work. Optimum resolution was achieved operating at 1.0 mL/min in the first part of the chromatogram (until 45 min) and 0.5 mL/min in the second one (from 45 min to the end) and by applying programmed temperature gradient (15 degrees C until 30 min and progressively increasing temperature until reaching 40 degrees C at 45 min). (c) 2009 Elsevier B.V. All rights reserved.

Technical advance: identification of plant actin-binding proteins by F-actin affinity chromatography

NASA Technical Reports Server (NTRS)

Hu, S.; Brady, S. R.; Kovar, D. R.; Staiger, C. J.; Clark, G. B.; Roux, S. J.; Muday, G. K.

2000-01-01

Proteins that interact with the actin cytoskeleton often modulate the dynamics or organization of the cytoskeleton or use the cytoskeleton to control their localization. In plants, very few actin-binding proteins have been identified and most are thought to modulate cytoskeleton function. To identify actin-binding proteins that are unique to plants, the development of new biochemical procedures will be critical. Affinity columns using actin monomers (globular actin, G-actin) or actin filaments (filamentous actin, F-actin) have been used to identify actin-binding proteins from a wide variety of organisms. Monomeric actin from zucchini (Cucurbita pepo L.) hypocotyl tissue was purified to electrophoretic homogeneity and shown to be native and competent for polymerization to actin filaments. G-actin, F-actin and bovine serum albumin affinity columns were prepared and used to separate samples enriched in either soluble or membrane-associated actin-binding proteins. Extracts of soluble actin-binding proteins yield distinct patterns when eluted from the G-actin and F-actin columns, respectively, leading to the identification of a putative F-actin-binding protein of approximately 40 kDa. When plasma membrane-associated proteins were applied to these columns, two abundant polypeptides eluted selectively from the F-actin column and cross-reacted with antiserum against pea annexins. Additionally, a protein that binds auxin transport inhibitors, the naphthylphthalamic acid binding protein, which has been previously suggested to associate with the actin cytoskeleton, was eluted in a single peak from the F-actin column. These experiments provide a new approach that may help to identify novel actin-binding proteins from plants.

Technical advance: identification of plant actin-binding proteins by F-actin affinity chromatography.

PubMed

Hu, S; Brady, S R; Kovar, D R; Staiger, C J; Clark, G B; Roux, S J; Muday, G K

2000-10-01

Proteins that interact with the actin cytoskeleton often modulate the dynamics or organization of the cytoskeleton or use the cytoskeleton to control their localization. In plants, very few actin-binding proteins have been identified and most are thought to modulate cytoskeleton function. To identify actin-binding proteins that are unique to plants, the development of new biochemical procedures will be critical. Affinity columns using actin monomers (globular actin, G-actin) or actin filaments (filamentous actin, F-actin) have been used to identify actin-binding proteins from a wide variety of organisms. Monomeric actin from zucchini (Cucurbita pepo L.) hypocotyl tissue was purified to electrophoretic homogeneity and shown to be native and competent for polymerization to actin filaments. G-actin, F-actin and bovine serum albumin affinity columns were prepared and used to separate samples enriched in either soluble or membrane-associated actin-binding proteins. Extracts of soluble actin-binding proteins yield distinct patterns when eluted from the G-actin and F-actin columns, respectively, leading to the identification of a putative F-actin-binding protein of approximately 40 kDa. When plasma membrane-associated proteins were applied to these columns, two abundant polypeptides eluted selectively from the F-actin column and cross-reacted with antiserum against pea annexins. Additionally, a protein that binds auxin transport inhibitors, the naphthylphthalamic acid binding protein, which has been previously suggested to associate with the actin cytoskeleton, was eluted in a single peak from the F-actin column. These experiments provide a new approach that may help to identify novel actin-binding proteins from plants.

Experimental framework to study tip vortex interactions in multirotor wakes

NASA Astrophysics Data System (ADS)

Yao, Rongnan; Araya, Daniel

2017-11-01

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

Chaotic bubbling and nonstagnant foams.

PubMed

Tufaile, Alberto; Sartorelli, José Carlos; Jeandet, Philippe; Liger-Belair, Gerard

2007-06-01

We present an experimental investigation of the agglomeration of bubbles obtained from a nozzle working in different bubbling regimes. This experiment consists of a continuous production of bubbles from a nozzle at the bottom of a liquid column, and these bubbles create a two-dimensional (2D) foam (or a bubble raft) at the top of this column. The bubbles can assemble in various dynamically stable arrangement, forming different kinds of foams in a liquid mixture of water and glycerol, with the effect that the bubble formation regimes influence the foam obtained from this agglomeration of bubbles. The average number of bubbles in the foam is related to the bubble formation frequency and the bubble mean lifetime. The periodic bubbling can generate regular or irregular foam, while a chaotic bubbling only generates irregular foam.

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

PubMed

Di Giulio, Andrea; Muzzi, Maurizio

2018-03-01

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

Activated Carbon-hydrogen based Continuous Sorption Cooling in Single Adsorbent Bed with LN2 Heat Sink

NASA Astrophysics Data System (ADS)

Koley, Susmita; Ghosh, Indranil

Quick and periodic inflow-outflow of adsorbate in an adsorbent column createsa differential temperature between the two ends of it, allowing for the generation of continuous sorption cooling in a single adsorbent tube. The concept has been proven experimentally and theoretically for near room temperature applications using activated carbon-nitrogen. The feasibility of generating continuous solid sorption cooling in a single adsorbent tube in the cryogenic domainhas been studied theoretically with a different adsorbent-adsorbate pair, namely, activated carbon-hydrogen. Precooling of gaseous hydrogen (before it enters the adsorbent column) and removal of the heat of adsorption has been achieved using liquid nitrogen. Theoretical estimation shows nearly 20 K temperature difference between the two ends under no load condition. Finally, parametric variations have been performed.

Gas chromatography with pulsed flame photometric detection multiresidue method for organophosphate pesticide and metabolite residues at the parts-per-billion level in representatives commodities of fruits and vegetable crop groups.

PubMed

Podhorniak, L V; Negron, J F; Griffith, F D

2001-01-01

A gas chromatographic method with a pulsed flame photometric detector (P-FPD) is presented for the analysis of 28 parent organophosphate (OP) pesticides and their OP metabolites. A total of 57 organophosphates were analyzed in 10 representative fruit and vegetable crop groups. The method is based on a judicious selection of known procedures from FDA sources such as the Pesticide Analytical Manual and Laboratory Information Bulletins, combined in a manner to recover the OPs and their metabolite(s) at the part-per-billion (ppb) level. The method uses an acetone extraction with either miniaturized Hydromatrix column partitioning or alternately a miniaturized methylene dichloride liquid-liquid partitioning, followed by solid-phase extraction (SPE) cleanup with graphitized carbon black (GCB) and PSA cartridges. Determination of residues is by programmed temperature capillary column gas chromatography fitted with a P-FPD set in the phosphorus mode. The method is designed so that a set of samples can be prepared in 1 working day for overnight instrumental analysis. The recovery data indicates that a daily column-cutting procedure used in combination with the SPE extract cleanup effectively reduces matrix enhancement at the ppb level for many organophosphates. The OPs most susceptible to elevated recoveries around or greater than 150%, based on peak area calculations, were trichlorfon, phosmet, and the metabolites of dimethoate, fenamiphos, fenthion, and phorate.

Quasi-static shape adjustment of a 15 meter diameter space antenna

NASA Technical Reports Server (NTRS)

Belvin, W. Keith; Herstrom, Catherine L.; Edighoffer, Harold H.

1987-01-01

A 15 meter diameter Hoop-Column antenna has been analyzed and tested to study shape adjustment of the reflector surface. The Hoop-Column antenna concept employs pretensioned cables and mesh to produce a paraboloidal reflector surface. Fabrication errors and thermal distortions may significantly reduce surface accuracy and consequently degrade electromagnetic performance. Thus, the ability to adjust the surface shape is desirable. The shape adjustment algorithm consisted of finite element and least squares error analyses to minimize the surface distortions. Experimental results verified the analysis. Application of the procedure resulted in a reduction of surface error by 38 percent. Quasi-static shape adjustment has the potential for on-orbit compensation for a variety of surface shape distortions.

Determination of the cyanobacterial toxin cylindrospermopsin in algal food supplements.

PubMed

Liu, H; Scott, P M

2011-06-01

For the analysis of blue-green algal food supplements for cylindrospermopsin (CYN), a C18 solid-phase extraction column and a polygraphitized carbon solid-phase extraction column in series was an effective procedure for the clean-up of extracts. Determination of CYN was by liquid chromatography with ultraviolet light detection. At extract spiking levels of CYN equivalent to 25-500 µg g(-1), blue-green algal supplement recoveries were in the range 70-90%. CYN was not detected in ten samples of food supplements and one chocolate product, all containing blue-green algae. The limit of detection for the method was 16 µg g(-1), and the limit of quantification was 52 µg g(-1).

Determination of alpha-hydroxy acids in cosmetic products by high-performance liquid chromatography with a narrow-bore column.

PubMed

Nicoletti, I; Corradini, C; Cogliandro, E; Cavazza, A

1999-08-01

This paper reports the results of a study carried out to develop a simple, rapid and sensitive method for the separation, identification and quantitative measurement of alpha-hydroxy acids in commercial cosmetics using high-performance liquid chromatography (HPLC). This method is successfully applied to the simultaneous identification and quantitative determination of glycolic, lactic, malic, tartaric and citric acids employing a reversed phase narrow-bore column under isocratic condition and UV detection. The method is validated by determining the precision of replicate analyses and accuracy by analyzing samples with and without adding know amount of the alpha-hydroxy acids. The procedure is suitable for routine analyses of commercial cosmetics.

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

PubMed

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

2016-04-01

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

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

PubMed

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

2018-02-17

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

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

PubMed

Gritti, Fabrice; Guiochon, Georges

2013-07-05

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

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

PubMed

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

2017-09-01

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

Low-frequency instabilities and plasma turbulence

NASA Technical Reports Server (NTRS)

Ilic, D. B.

1973-01-01

A theoretical and experimental study is reported of steady-state and time-dependent characteristics of the positive column and the hollow cathode discharge (HCD). The steady state of a non-isothermal, cylindrical positive column in an axial magnetic field is described by three moment equations in the plasma approximation. Volume generation of electron-ion pairs by single-stage ionization, the presence of axial current, and collisions with neutrals are considered. The theory covers the range from the low pressure, collisionless regime to the intermediate pressure, collisional regime. It yields radial profiles of the charged particle velocities, density, potential, electron and ion temperatures, and demonstrates similarity laws for the positive column. The results are compared with two moment theories and with experimental data on He, Ar and Hg found in the literature for a wide range of pressures. A simple generalization of the isothermal theory for an infinitely long cylinder in an axial magnetic field to the case of a finite column with axial current flow is also demonstrated.

[Spectral investigation of atmospheric pressure plasma column].

PubMed

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

2012-07-01

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

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

PubMed

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

2011-02-01

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

Microbial impacts on 99mTc migration through sandstone under highly alkaline conditions relevant to radioactive waste disposal.

PubMed

Smith, Sarah L; Boothman, Christopher; Williams, Heather A; Ellis, Beverly L; Wragg, Joanna; West, Julia M; Lloyd, Jonathan R

2017-01-01

Geological disposal of intermediate level radioactive waste in the UK is planned to involve the use of cementitious materials, facilitating the formation of an alkali-disturbed zone within the host rock. The biogeochemical processes that will occur in this environment, and the extent to which they will impact on radionuclide migration, are currently poorly understood. This study investigates the impact of biogeochemical processes on the mobility of the radionuclide technetium, in column experiments designed to be representative of aspects of the alkali-disturbed zone. Results indicate that microbial processes were capable of inhibiting 99m Tc migration through columns, and X-ray radiography demonstrated that extensive physical changes had occurred to the material within columns where microbiological activity had been stimulated. The utilisation of organic acids under highly alkaline conditions, generating H 2 and CO 2 , may represent a mechanism by which microbial processes may alter the hydraulic conductivity of a geological environment. Column sediments were dominated by obligately alkaliphilic H 2 -oxidising bacteria, suggesting that the enrichment of these bacteria may have occurred as a result of H 2 generation during organic acid metabolism. The results from these experiments show that microorganisms are able to carry out a number of processes under highly alkaline conditions that could potentially impact on the properties of the host rock surrounding a geological disposal facility for intermediate level radioactive waste. Copyright © 2016. Published by Elsevier B.V.

Nonlinear Earthquake Analysis of Reinforced Concrete Frames with Fiber and Bernoulli-Euler Beam-Column Element

PubMed Central

Karaton, Muhammet

2014-01-01

A beam-column element based on the Euler-Bernoulli beam theory is researched for nonlinear dynamic analysis of reinforced concrete (RC) structural element. Stiffness matrix of this element is obtained by using rigidity method. A solution technique that included nonlinear dynamic substructure procedure is developed for dynamic analyses of RC frames. A predicted-corrected form of the Bossak-α method is applied for dynamic integration scheme. A comparison of experimental data of a RC column element with numerical results, obtained from proposed solution technique, is studied for verification the numerical solutions. Furthermore, nonlinear cyclic analysis results of a portal reinforced concrete frame are achieved for comparing the proposed solution technique with Fibre element, based on flexibility method. However, seismic damage analyses of an 8-story RC frame structure with soft-story are investigated for cases of lumped/distributed mass and load. Damage region, propagation, and intensities according to both approaches are researched. PMID:24578667

Column studies on the evaluation of novel spacer granules for the removal of arsenite and arsenate from contaminated water.

PubMed

Gupta, Anjali; Sankararamakrishnan, Nalini

2010-04-01

Decontamination of arsenic ions from aqueous media has been investigated using iron chitosan spacer granules (ICS) as an adsorbent. Drying of beads saturated with a spacer sucrose was considered as simple treatment, to prevent the restriction of polymer network and enhance sorption capacity. The novel sorbent was studied in up flow column experiments conducted at different flow rates, pH and bed depth to quantify the treatment performance. It was found that silicate was more inhibitory than phosphate, and the silicate in groundwater controlled the arsenic removal efficiency. The column regeneration studies were carried out for two sorption-desorption cycles using 0.1N NaOH as the eluant. TCLP leaching tests were conducted on the arsenic loaded adsorbent which revealed the containment of arsenic-laden sludge can be managed without adverse environmental impact. The developed procedure was successfully applied for the removal of both As(III) and As(V) from arsenic contaminated drinking water samples. Copyright 2009 Elsevier Ltd. All rights reserved.

Post-column reaction for simultaneous analysis of chromatic and leuco forms of malachite green and crystal violet by high-performance liquid chromatography with photometric detection

USGS Publications Warehouse

Allen, J.L.; Meinertz, J.R.

1991-01-01

The chromatic and leuco forms of malachite green and crystal violet were readily separated and detected by a sensitive and selective high-performance liquid chromatographic procedure. The chromatic and leuco forms of the dyes were separated within 11 min on a C18 column with a mobile phase of 0.05 M sodium acetate and 0.05 M acetic acid in water (19%) and methanol (81%). A reaction chamber, containing 10% PbO2 in Celite 545, was placed between the column and the spectrophotometric detector to oxidize the leuco forms of the dyes to their chromatic forms. Chromatic and leuco malachite green were quantified by their absorbance at 618 nm; and chromatic and leuco Crystal Violet by their absorbance at 588 nm. Detection limits for chromatic and leuco forms of both dyes ranged from 0.12 to 0.28 ng. A linear range of 1 to 100 ng was established for both forms of the dyes.

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

PubMed

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

2017-01-01

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

Polygalacturonase from Rhizopus stolonifer, an Elicitor of Casbene Synthetase Activity in Castor Bean (Ricinus communis L.) Seedlings 1

PubMed Central

Lee, Sung-Chul; West, Charles A.

1981-01-01

Apparently homogeneous polygalacturonase-elicitor purified from the filtrates of Rhizopus stolonifer cultures stimulates germinating castor bean seedlings to produce greatly increased levels of casbene synthetase activity. The purification procedure involved gel-filtration chromatography on Sephadex G-25 and G-75 columns followed by cation-exchange chromatography on a Sephadex CM C-50 column. Homogeneity of the purified preparation was indicated by the results of cationic polyacrylamide disc gel electrophoresis and isoelectric focusing (pI = 8.0). The identity of the casbene elicitor activity and polygalacturonase were indicated by the coincidence of the two activities at all stages of purification, the coincidence of both activities with the single protein-staining band detected on a cationic polyacrylamide disc gel and an isoelectric focusing gel, and the identical behavior of both activities on an agarose gel affinity column. The purified polygalacturonase-elicitor is a glycoprotein with approximately 20% carbohydrate content and an estimated molecular weight of 32,000 by polyacrylamide disc gel electrophoresis. PMID:16661728

Tropospheric NO2 retrieved from OMI, GOME(-2), and SCIAMACHY within the Quality Assurance For Essential Climate Variables (QA4ECV) project: retrieval improvement, harmonization, and quality assurance

NASA Astrophysics Data System (ADS)

Folkert Boersma, K.

2017-04-01

One of the prime targets of the EU-project Quality Assurance for Essential Climate Variables (QA4ECV, www.qa4ecv.eu) is the generation and subsequent quality assurance of harmonized, long-term data records of ECVs or precursors thereof. Here we report on a new harmonized and improved retrieval algorithm for NO2 columns and its application to spectra measured by the GOME, SCIAMACHY, OMI, and GOME-2(A) sensors over the period 1996-2016. Our community 'best practices' algorithm is based on the classical 3-step DOAS method. It benefits from a thorough comparison and iteration of spectral fitting and air mass factor calculation approaches between IUP Bremen, BIRA, Max Planck Institute for Chemistry, KNMI, WUR, and a number of external partners. For step 1 of the retrieval, we show that improved spectral calibration and the inclusion of liquid water and intensity-offset correction terms in the fitting procedure, lead to 10-30% smaller NO2 slant columns, in better agreement with independent measurements. Moreover, the QA4ECV NO2 slant columns show 15-35% lower uncertainties relative to earlier versions of the spectral fitting algorithm. For step 2, the stratospheric correction, the algorithm relies on the assimilation of NO2 slant columns over remote regions in the Tracer Model 5 (TM5-MP) chemistry transport model. The representation of stratospheric NOy in the model is improved by nudging towards ODIN HNO3:O3 ratios, leading to more realistic NO2 concentrations in the free-running mode, which is relevant at high latitudes near the terminator. The coupling to TM5-Mass Parallel also allows the calculation of air mass factors (AMFs, step 3) from a priori NO2 vertical profiles simulated at a spatial resolution of 1°×1°, so that hotspot gradients are better resolved in the a priori profile shapes. Other AMF improvements include the use of improved cloud information, and a correction for photon scattering in a spherical atmosphere. Preliminary comparisons indicate that the new QA4ECV tropospheric NO2 columns are ±10% lower than operational products, and provide more spatial detail on the horizontal distribution of NO2 in the troposphere. Our comparisons provide more insight in the origin and nature of the retrieval uncertainties. The final QAECV NO2 product therefore contains overall uncertainty estimates for every measurement, but also information on the contribution of uncertainties of each retrieval sub-step to the overall uncertainty budget. We conclude with a presentation of the data format and a verification of the QA4ECV NO2 columns using the traceable quality assurance methodologies developed in the QA4ECV-project, and via validation against independent measurements (using the online QA4ECV Atmospheric Validation Server tool).

Simultaneous beam sampling and aperture shape optimization for SPORT.

PubMed

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

2015-02-01

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

Simultaneous beam sampling and aperture shape optimization for SPORT

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

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

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

32 CFR 623.4 - Accounting procedures.

Code of Federal Regulations, 2014 CFR

2014-07-01

... will follow. Informal records should be also maintained.) Card columns Code or data 1-3 “AOE”. 4-6 RIC... of materiel loaned to rifle clubs and schools will conform with § 623.5. (2) Accountable property... the prepositioned materiel receipt card, the item will be processed as a normal receipt. (B) If there...

Isolation of Cholesterol from an Egg Yolk

ERIC Educational Resources Information Center

Taber, Douglass F.; Li, Rui; Anson, Cory M.

2011-01-01

A simple procedure for the isolation of the cholesterol, by hydrolysis and extraction followed by column chromatography, is described. The cholesterol can be further purified by complexation with oxalic acid. It can also be oxidized and conjugated to cholestenone. The source of the cholesterol is one egg yolk, which contains about 200 mg of…

Purification and Electrophoretic Characterization of Lactate Dehydrogenase from Mammalian Blood: A Different Twist on a Classic Experiment

ERIC Educational Resources Information Center

Brunauer, Linda S.

2016-01-01

A multiweek protein purification suite, suitable for upper-division biochemistry or biotechnology undergraduate students, is described. Students work in small teams to isolate the enzyme lactate dehydrogenase (LDH) from a nontraditional tissue source, mammalian blood, using a sequence of three column chromatographic procedures: ion-exchange, size…

Laboratory, Field, and Analytical Procedures for Using Passive Sampling in the Evaluation of Contaminated Sediments: User's Manual

EPA Science Inventory

Regardless of the remedial technology invoked to address contaminated sediments in the environment, there is a critical need to have tools for assessing the effectiveness of the remedy. In the past, these tools have included chemical and biomonitoring of the water column and sedi...

In vivo genome-wide analysis of multiple tissues identifies gene regulatory networks, novel functions and downstream regulatory genes for Bapx1 and its co-regulation with Sox9 in the mammalian vertebral column.

PubMed

Chatterjee, Sumantra; Sivakamasundari, V; Yap, Sook Peng; Kraus, Petra; Kumar, Vibhor; Xing, Xing; Lim, Siew Lan; Sng, Joel; Prabhakar, Shyam; Lufkin, Thomas

2014-12-05

Vertebrate organogenesis is a highly complex process involving sequential cascades of transcription factor activation or repression. Interestingly a single developmental control gene can occasionally be essential for the morphogenesis and differentiation of tissues and organs arising from vastly disparate embryological lineages. Here we elucidated the role of the mammalian homeobox gene Bapx1 during the embryogenesis of five distinct organs at E12.5 - vertebral column, spleen, gut, forelimb and hindlimb - using expression profiling of sorted wildtype and mutant cells combined with genome wide binding site analysis. Furthermore we analyzed the development of the vertebral column at the molecular level by combining transcriptional profiling and genome wide binding data for Bapx1 with similarly generated data sets for Sox9 to assemble a detailed gene regulatory network revealing genes previously not reported to be controlled by either of these two transcription factors. The gene regulatory network appears to control cell fate decisions and morphogenesis in the vertebral column along with the prevention of premature chondrocyte differentiation thus providing a detailed molecular view of vertebral column development.

Hierarchy of facies of pyroclastic flow deposits generated by Laacher See type eruptions

NASA Astrophysics Data System (ADS)

Freundt, A.; Schmincke, H.-U.

1985-04-01

The upper Quaternary pyroclastic flow deposits of Laacher See volcano show compositional and structural facies variations on four different scales: (1) eruptive units of pyroclastic flows, composed of many flow units; (2) depositional cycles of as many as five flow units; flow units containing (3) regional intraflow-unit facies; and (4) local intraflow-unit subfacies. These facies can be explained by successively overlapping processes beginning in the magma column and ending with final deposition. The pyroclastic flow deposits thus reflect major aspects of the eruptive history of Laacher See volcano: (a) drastic changes in eruptive mechanism due to increasing access of water to the magma chamber and (b) change in chemical composition and crystal and gas content as evacuation of a compositionally zoned magma column progressed. The four scales of facies result from four successive sets of processes: (1) differentiation in the magma column and external factors governing the mechanism of eruption; (2) temporal variations of factors inducing eruption column collapse; (3) physical conditions in the eruption column and the way in which its collapse proceeds; and (4) interplay of flow-inherent and morphology-induced transport mechanics.

Vertebral anatomy in the Florida manatee, Trichechus manatus latirostris: a developmental and evolutionary analysis.

PubMed

Buchholtz, Emily A; Booth, Amy C; Webbink, Katherine E

2007-06-01

The vertebral column of the Florida manatee presents an unusual suite of morphological traits. Key among these are a small precaudal count, elongate thoracic vertebrae, extremely short neural spines, lack of a sacral series, high lumbar variability, and the presence of six instead of seven cervical vertebrae. This study documents vertebral morphology, size, and lumbar variation in 71 skeletons of Trichechus manatus latirostris (Florida manatee) and uses the skeletons of Trichechus senegalensis (west African manatee) and Dugong dugon (dugong) in comparative analysis. Vertebral traits are used to define morphological, and by inference developmental, column modules and to propose their hierarchical relationships. A sequence of evolutionary innovations in column morphology is proposed. Results suggest that the origin of the fluke and low rates of cervical growth originated before separation of trichechids (manatees) and dugongids (dugongs). Meristic reduction in count is a later, trichechid innovation and is expressed across the entire precaudal column. Elongation of thoracic vertebrae may be an innovative strategy to generate an elongate column in an animal with a small precaudal count. Elimination of the lumbus through both meristic and homeotic reduction is currently in progress. 2007 Wiley-Liss, Inc.

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

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

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

2009-09-15

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

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.

Tetrahedral Arrangements of Perylene Bisimide Columns via Supramolecular Orientational Memory.

PubMed

Sahoo, Dipankar; Peterca, Mihai; Aqad, Emad; Partridge, Benjamin E; Heiney, Paul A; Graf, Robert; Spiess, Hans W; Zeng, Xiangbing; Percec, Virgil

2017-01-24

Chiral, shape, and liquid crystalline memory effects are well-known to produce commercial macroscopic materials with important applications as springs, sensors, displays, and memory devices. A supramolecular orientational memory effect that provides complex nanoscale arrangements was only recently reported. This supramolecular orientational memory was demonstrated to preserve the molecular orientation and packing within supramolecular units of a self-assembling cyclotriveratrylene crown at the nanoscale upon transition between its columnar hexagonal and Pm3̅n cubic periodic arrays. Here we report the discovery of supramolecular orientational memory in a dendronized perylene bisimide (G2-PBI) that self-assembles into tetrameric crowns and subsequently self-organizes into supramolecular columns and spheres. This supramolecular orientation memory upon transition between columnar hexagonal and body-centered cubic (BCC) mesophases preserves the 3-fold cubic [111] orientations rather than the 4-fold [100] axes, generating an unusual tetrahedral arrangement of supramolecular columns. These results indicate that the supramolecular orientational memory concept may be general for periodic arrays of self-assembling dendrons and dendrimers as well as for other periodic and quasiperiodic nanoscale organizations comprising supramolecular spheres, generated from other organized complex soft matter including block copolymers and surfactants.

A computational model of the human visual cortex

NASA Astrophysics Data System (ADS)

Albus, James S.

2008-04-01

The brain is first and foremost a control system that is capable of building an internal representation of the external world, and using this representation to make decisions, set goals and priorities, formulate plans, and control behavior with intent to achieve its goals. The computational model proposed here assumes that this internal representation resides in arrays of cortical columns. More specifically, it models each cortical hypercolumn together with its underlying thalamic nuclei as a Fundamental Computational Unit (FCU) consisting of a frame-like data structure (containing attributes and pointers) plus the computational processes and mechanisms required to maintain it. In sensory-processing areas of the brain, FCUs enable segmentation, grouping, and classification. Pointers stored in FCU frames link pixels and signals to objects and events in situations and episodes that are overlaid with meaning and emotional values. In behavior-generating areas of the brain, FCUs make decisions, set goals and priorities, generate plans, and control behavior. Pointers are used to define rules, grammars, procedures, plans, and behaviors. It is suggested that it may be possible to reverse engineer the human brain at the FCU level of fidelity using nextgeneration massively parallel computer hardware and software. Key Words: computational modeling, human cortex, brain modeling, reverse engineering the brain, image processing, perception, segmentation, knowledge representation

Estimation of internal exposure to 99Mo in nuclear medicine patients.

PubMed

Silva, I C O A; Lucena, E A; Souza, W O; Dantas, A L A; Dantas, B M

2010-05-10

(99m)Tc is the most widely used radionuclide in nuclear medicine. It is obtained by elution of (99)Mo-(99m)Tc generators. Depending on the quality of the generator and its integrity, (99)Mo may be extracted from the column during the elution process, becoming a radionuclidic impurity in the (99m)Tc eluate. This fact would impart an unnecessary dose to the patients submitted to diagnostic procedures. The aim of this work is to evaluate (99)Mo incorporation and internal effective doses in nuclear medicine patients through bioassay techniques, providing information on the metabolism of molybdenum in humans. A methodology based on in vivo and in vitro measurements was developed. In vivo measurements were performed with a NaI detector installed in the IRD WBC. Urine samples were analysed with a HPGe at the IRD bioassay laboratory. Patients showed detectable activities of (99)Mo in whole body and urine. Results were interpreted with AIDE software. Estimated incorporation was compared to predicted values based on ICRP model. Effective doses were in the order of micro sieverts. Results suggest the need to implement a routine quality control program of radionuclidic impurity of (99)Mo in (99m)Tc eluates to be conducted by radiopharmacy laboratories of nuclear medicine centers.

Determination of linuron and related compounds in soil by microwave-assisted solvent extraction and reversed-phase liquid chromatography with UV detection.

PubMed

Molins, C; Hogendoorn, E A; Dijkman, E; Heusinkveld, H A; Baumann, R A

2000-02-11

The combination of microwave-assisted solvent extraction (MASE) and reversed-phase liquid chromatography (RPLC) with UV detection has been investigated for the efficient determination of phenylurea herbicides in soils involving the single-residue method (SRM) approach (linuron) and the multi-residue method (MRM) approach (monuron, monolinuron, isoproturon, metobromuron, diuron and linuron). Critical parameters of MASE, viz, extraction temperature, water content and extraction solvent were varied in order to optimise recoveries of the analytes while simultaneously minimising co-extraction of soil interferences. The optimised extraction procedure was applied to different types of soil with an organic carbon content of 0.4-16.7%. Besides freshly spiked soil samples, method validation included the analysis of samples with aged residues. A comparative study between the applicability of RPLC-UV without and with the use of column switching for the processing of uncleaned extracts, was carried out. For some of the tested analyte/matrix combinations the one-column approach (LC mode) is feasible. In comparison to LC, coupled-column LC (LC-LC mode) provides high selectivity in single-residue analysis (linuron) and, although less pronounced in multi-residue analysis (all six phenylurea herbicides), the clean-up performance of LC-LC improves both time of analysis and sample throughput. In the MRM approach the developed procedure involving MASE and LC-LC-UV provided acceptable recoveries (range, 80-120%) and RSDs (<12%) at levels of 10 microg/kg (n=9) and 50 microg/kg (n=7), respectively, for most analyte/matrix combinations. Recoveries from aged residue samples spiked at a level of 100 microg/kg (n=7) ranged, depending of the analyte/soil type combination, from 41-113% with RSDs ranging from 1-35%. In the SRM approach the developed LC-LC procedure was applied for the determination of linuron in 28 sandy soil samples collected in a field study. Linuron could be determined in soil with a limit of quantitation of 10 microg/kg.

Bi-dimensional null model analysis of presence-absence binary matrices.

PubMed

Strona, Giovanni; Ulrich, Werner; Gotelli, Nicholas J

2018-01-01

Comparing the structure of presence/absence (i.e., binary) matrices with those of randomized counterparts is a common practice in ecology. However, differences in the randomization procedures (null models) can affect the results of the comparisons, leading matrix structural patterns to appear either "random" or not. Subjectivity in the choice of one particular null model over another makes it often advisable to compare the results obtained using several different approaches. Yet, available algorithms to randomize binary matrices differ substantially in respect to the constraints they impose on the discrepancy between observed and randomized row and column marginal totals, which complicates the interpretation of contrasting patterns. This calls for new strategies both to explore intermediate scenarios of restrictiveness in-between extreme constraint assumptions, and to properly synthesize the resulting information. Here we introduce a new modeling framework based on a flexible matrix randomization algorithm (named the "Tuning Peg" algorithm) that addresses both issues. The algorithm consists of a modified swap procedure in which the discrepancy between the row and column marginal totals of the target matrix and those of its randomized counterpart can be "tuned" in a continuous way by two parameters (controlling, respectively, row and column discrepancy). We show how combining the Tuning Peg with a wise random walk procedure makes it possible to explore the complete null space embraced by existing algorithms. This exploration allows researchers to visualize matrix structural patterns in an innovative bi-dimensional landscape of significance/effect size. We demonstrate the rational and potential of our approach with a set of simulated and real matrices, showing how the simultaneous investigation of a comprehensive and continuous portion of the null space can be extremely informative, and possibly key to resolving longstanding debates in the analysis of ecological matrices. © 2017 The Authors. Ecology, published by Wiley Periodicals, Inc., on behalf of the Ecological Society of America.

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.

FLOWCHART; a computer program for plotting flowcharts

USGS Publications Warehouse

Bender, Bernice

1982-01-01

The computer program FLOWCHART can be used to very quickly and easily produce flowcharts of high quality for publication. FLOWCHART centers each element or block of text that it processes on one of a set of (imaginary) vertical lines. It can enclose a text block in a rectangle, circle or other selected figure. It can draw a 'line connecting the midpoint of any side of any figure with the midpoint of any side of any other figure and insert an arrow pointing in the direction of flow. It can write 'yes' or 'no' next to the line joining two figures. FLOWCHART creates flowcharts using some basic plotting subroutine* which permit plots to be generated interactively and inspected on a Tektronix compatible graphics screen or plotted in a deferred mode on a Houston Instruments 42' pen plotter. The size of the plot, character set and character height in inches are inputs to the program. Plots generated using the pen plotter can be up to 42' high--the larger size plots being directly usable as visual aids in a talk. FLOWCHART centers each block of text on an imaginary column line. (The number of columns and column width are specified as input.) The midpoint of the longest line of text within the block is defined to be the center of the block and is placed on the column line. The spacing of individual words within the block is not altered when the block is positioned. The program writes the first block of text in a designated column and continues placing each subsequent block below the previous block in the same column. A block of text may be placed in a different column by specifying the number of the column and an earlier block of text with which the new block is to be aligned. If block zero is given as the earlier block, the new text is placed in the new column continuing down the page below the previous block. Optionally a column and number of inches from the top of the page may be given for positioning the next block of text. The program will normally draw one of five types of figure to enclose a block of text: a rectangle, circle, diamond, eight sided figure or figure with parallel sides and rounded ends. It can connect the figure with a line to the preceding figure, and place an arrow pointing toward the second figure. Text blocks not in sequence can also be connected and 'yes' or 'no' written next to any line to indicate branching. Figure 1 illustrates the various types of figures that can be drawn, spacings, connecting lines and the like. * The plotting package employed is Buplot available on the VAX and PDP-1170 computers at the USGS Office of Earthquake Studies, Golden, Colo. Calls to the plotting subroutines must be adjusted if some other plotting package is used.

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.

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.

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

PubMed

Benhaim, Deborah; Grushka, Eli

2008-10-31

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

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.

Biclustering of gene expression data using reactive greedy randomized adaptive search procedure

PubMed Central

Dharan, Smitha; Nair, Achuthsankar S

2009-01-01

Background Biclustering algorithms belong to a distinct class of clustering algorithms that perform simultaneous clustering of both rows and columns of the gene expression matrix and can be a very useful analysis tool when some genes have multiple functions and experimental conditions are diverse. Cheng and Church have introduced a measure called mean squared residue score to evaluate the quality of a bicluster and has become one of the most popular measures to search for biclusters. In this paper, we review basic concepts of the metaheuristics Greedy Randomized Adaptive Search Procedure (GRASP)-construction and local search phases and propose a new method which is a variant of GRASP called Reactive Greedy Randomized Adaptive Search Procedure (Reactive GRASP) to detect significant biclusters from large microarray datasets. The method has two major steps. First, high quality bicluster seeds are generated by means of k-means clustering. In the second step, these seeds are grown using the Reactive GRASP, in which the basic parameter that defines the restrictiveness of the candidate list is self-adjusted, depending on the quality of the solutions found previously. Results We performed statistical and biological validations of the biclusters obtained and evaluated the method against the results of basic GRASP and as well as with the classic work of Cheng and Church. The experimental results indicate that the Reactive GRASP approach outperforms the basic GRASP algorithm and Cheng and Church approach. Conclusion The Reactive GRASP approach for the detection of significant biclusters is robust and does not require calibration efforts. PMID:19208127

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.

A review of oscillating water columns.

PubMed

Heath, T V

2012-01-28

This paper considers the history of oscillating water column (OWC) systems from whistling buoys to grid-connected power generation systems. The power conversion from the wave resource through to electricity via pneumatic and shaft power is discussed in general terms and with specific reference to Voith Hydro Wavegen's land installed marine energy transformer (LIMPET) plant on the Scottish island of Islay and OWC breakwater systems. A report on the progress of other OWC systems and power take-off units under commercial development is given, and the particular challenges faced by OWC developers reviewed.

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

PubMed

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

2014-08-13

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

Tunable thick porous silica coating fabricated by multilayer-by-multilayer bonding of silica nanoparticles for open-tubular capillary chromatographic separation.

PubMed

Qu, Qishu; Liu, Yuanyuan; Shi, Wenjun; Yan, Chao; Tang, Xiaoqing

2015-06-19

A simple coating procedure employing a multilayer-by-multilayer process to modify the inner surface of bare fused-silica capillaries with silica nanoparticles was established. The silica nanoparticles were adsorbed onto the capillary wall via a strong electrostatic interaction between amino functional groups and silica particles. The thickness of the coating could be tuned from 130 to 600 nm by increasing the coating cycles from one to three. Both the retention factor and the resolution were greatly increased with increasing coating cycles. The loading capacity determined by naphthalene in the column with three coating cycles is 152.1 pmol. The effects of buffer concentration and pH value on the stability of the coating were evaluated. The retention reproducibility of the separation of toluene was 0.8, 1.2, 2.3, and 4.5%, respectively, for run-to-run, day-to-day, column-to-column, and batch-to-batch, respectively. The chromatographic performance of these columns was evaluated by both capillary liquid chromatography and open-tubular capillary electrochromatography (OT-CEC). Separation of aromatic hydrocarbons in the column with three coating cycles provided high theoretical plate numbers (up to 269,280 plates m(-1) for toluene) and short separation time (<15 min) by using OT-CEC mode. The method was also used to separate egg white proteins. Both acidic and basic proteins as well as four glycoisoforms were separated in a single run. Copyright © 2015 Elsevier B.V. All rights reserved.

Leaching of cadmium and tellurium from cadmium telluride (CdTe) thin-film solar panels under simulated landfill conditions.

PubMed

Ramos-Ruiz, Adriana; Wilkening, Jean V; Field, James A; Sierra-Alvarez, Reyes

2017-08-15

A crushed non-encapsulated CdTe thin-film solar cell was subjected to two standardized batch leaching tests (i.e., Toxicity Characteristic Leaching Procedure (TCLP) and California Waste Extraction Test (WET)) and to a continuous-flow column test to assess cadmium (Cd) and tellurium (Te) dissolution under conditions simulating the acidic- and the methanogenic phases of municipal solid waste landfills. Low levels of Cd and Te were solubilized in both batch leaching tests (<8.2% and <3.6% of added Cd and Te, respectively). On the other hand, over the course of 30days, 73% of the Cd and 21% of the Te were released to the synthetic leachate of a continuous-flow column simulating the acidic landfill phase. The dissolved Cd concentration was 3.24-fold higher than the TCLP limit (1mgL -1 ), and 650-fold higher than the maximum contaminant level established by the US-EPA for this metal in drinking water (0.005mgL -1 ). In contrast, the release of Cd and Te to the effluent of the continuous-flow column simulating the methanogenic phase of a landfill was negligible. The remarkable difference in the leaching behavior of CdTe in the columns is related to different aqueous pH and redox conditions promoted by the microbial communities in the columns, and is in agreement with thermodynamic predictions. Copyright © 2017 Elsevier B.V. All rights reserved.

Experimental Verification of the Structural Glass Beam-Columns Strength

NASA Astrophysics Data System (ADS)

Pešek, Ondřej; Melcher, Jindřich; Balázs, Ivan

2017-10-01

This paper deals with experimental research of axially and laterally loaded members made of structural (laminated) glass. The purpose of the research is the evaluation of buckling strength and actual behaviour of the beam-columns due to absence of standards for design of glass load-bearing structures. The experimental research follows the previous one focusing on measuring of initial geometrical imperfections of glass members, testing of glass beams and columns. Within the frame of the research 9 specimens were tested. All of them were of the same geometry (length 2000 mm, width 200 mm and thickness 16 mm) but different composition - laminated double glass made of annealed glass or fully tempered glass panes bonded together by PVB or EVASAFE foil. Specimens were at first loaded by axial force and then by constantly increasing bending moment up to failure. During testing lateral deflections, vertical deflection and normal stresses at mid-span were measured. A maximum load achieved during testing has been adopted as flexural-lateral-torsional buckling strength. The results of experiments were statistically evaluated according to the European standard for design of structures EN 1990, appendix D. There are significant differences between specimens made of annealed glass or fully tempered glass. Differences between specimens loaded by axial forces 1 kN and 2 kN are negligible. The next step was to determine the design strength by calculation procedure based on buckling curves approach intended for design of steel columns and develop interaction criterion for glass beams-columns.

The generation of vertebral segmental patterning in the chick embryo

PubMed Central

Senthinathan, Biruntha; Sousa, Cátia; Tannahill, David; Keynes, Roger

2012-01-01

We have carried out a series of experimental manipulations in the chick embryo to assess whether the notochord, neural tube and spinal nerves influence segmental patterning of the vertebral column. Using Pax1 expression in the somite-derived sclerotomes as a marker for segmentation of the developing intervertebral disc, our results exclude such an influence. In contrast to certain teleost species, where the notochord has been shown to generate segmentation of the vertebral bodies (chordacentra), these experiments indicate that segmental patterning of the avian vertebral column arises autonomously in the somite mesoderm. We suggest that in amniotes, the subdivision of each sclerotome into non-miscible anterior and posterior halves plays a critical role in establishing vertebral segmentation, and in maintaining left/right alignment of the developing vertebral elements at the body midline. PMID:22458512

78 FR 29672 - Small Generator Interconnection Agreements and Procedures

Federal Register 2010, 2011, 2012, 2013, 2014

2013-05-21

...] Small Generator Interconnection Agreements and Procedures AGENCY: Federal Energy Regulatory Commission... 7524). The regulations revised the pro forma Small Generator Interconnection Procedures (SGIP) and pro forma Small Generator Interconnection Agreement (SGIA) originally set forth in Order No. 2006. DATES...

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

PubMed

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

2015-02-01

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

Characterization of granular collapse onto hard substrates by acoustic emissions

NASA Astrophysics Data System (ADS)

Farin, Maxime; Mangeney, Anne; Toussaint, Renaud; De Rosny, Julien

2013-04-01

Brittle deformation in granular porous media can generate gravitational instabilities such as debris flows and rock avalanches. These phenomena constitute a major natural hazard for the population in mountainous, volcanic and coastal areas but their direct observation on the field is very dangerous. Recent studies showed that gravitational instabilities can be detected and characterized (volume, duration,...) thanks to the seismic signal they generate. In an avalanche, individual block bouncing and rolling on the ground are expected to generated signals of higher frequencies than the main flow spreading. The identification of the time/frequency signature of individual blocks in the recorded signal remains however difficult. Laboratory experiments were conducted to investigate the acoustic signature of diverse simple sources corresponding to grains falling over thin plates of plexiglas and rock blocks. The elastic energy emitted by a single bouncing steel bead into the support was first quantitatively estimated and compared to the potential energy of fall and to the potential energy change during the shock. Next, we consider the collapse of granular columns made of steel spherical beads onto hard substrates. Initially, these columns were held by a magnetic field allowing to suppress suddenly the cohesion between the beads, and thus to minimize friction effects that would arise from side walls. We varied systematically the column volume, the column aspect ratio (height over length) and the grain size. This is shown to affect the signal envelope and frequency content. In the experiments, two types of acoustic sensors were used to record the signals in a wide frequency range: accelerometers (1 Hz to 56 kHz) and piezoelectric sensors (100 kHz to 1 MHz). The experiments were also monitored optically using fast cameras. We developed a technique to use quantitatively both types of sensors to evaluate the elastic energy emitted by the sources. Eventually, we looked at what types of features in the signal are affected by individual shocks or by the large scale geometry of the avalanche.

Experimental and numerical validation of the effective medium theory for the B-term band broadening in 1st and 2nd generation monolithic silica columns.

PubMed

Deridder, Sander; Vanmessen, Alison; Nakanishi, Kazuki; Desmet, Gert; Cabooter, Deirdre

2014-07-18

Effective medium theory (EMT) expressions for the B-term band broadening in monolithic silica columns are presented at the whole-column as well as at the mesoporous skeleton level. Given the bi-continuous nature of the monolithic medium, regular as well as inverse formulations of the EMT-expressions have been established. The established expressions were validated by applying them to a set of experimental effective diffusion (Deff)-data obtained via peak parking on a number of 1st and 2nd generation monolithic silica columns, as well as to a set of numerical diffusion simulations in a simplified monolithic column representation (tetrahedral skeleton model) with different external porosities and internal diffusion coefficients. The numerically simulated diffusion data can be very closely represented over a very broad range of zone retention factors (up to k″=80) using the established EMT-expressions, especially when using the inverse variant. The expressions also allow representing the experimentally measured effective diffusion data very closely. The measured Deff/Dmol-values were found to decrease significantly with increasing retention factor, in general going from about Deff/Dmol=0.55 to 0.65 at low k″ (k″≅1.5-3.8) to Deff/Dmol=0.25 at very high k″ (k″≅40-80). These values are significantly larger than observed in fully-porous and core-shell particles. The intra-skeleton diffusion coefficient (Dpz) was typically found to be of the order of Dpz/Dmol=0.4, compared to Dpz/Dmol=0.2-0.35 observed in most particle-based columns. These higher Dpz/Dmol values are the cause of the higher Deff/Dmol values observed. In addition, it also appears that the higher internal diffusion is linked to the higher porosity of the mesoporous skeleton that has a relatively open structure with relatively wide pores. The observed (weak) relation between Dpz/Dmol and the zone retention factor appears to be in good agreement with that predicted when applying the regular variant of the EMT-expression directly to the mesoporous skeleton level. Copyright © 2014 Elsevier B.V. All rights reserved.

Procedure for the determination of retinol and alpha-tocopherol in poultry tissues using capillary gas chromatography with solvent venting injection.

PubMed

Maraschiello, C; García Regueiro, J A

1998-08-28

A procedure designed for the determination of retinol (vitamin A) and alpha-tocopherol (vitamin E) in poultry tissues has been developed. The procedure involves lipid extraction, saponification, solid-phase clean-up and capillary gas chromatography (cGC). Retinol and alpha-tocopherol were determined separately by cGC-flame ionisation detection using a fused-silica open tubular capillary column, 30 m x 0.25 mm I.D. coated with 5% phenylmethylsilicone and with a film thickness of 0.25 micron. Solvent extraction followed by saponification were sufficient to provide a purified extract which was directly analyzed for retinol by cGC in the solvent venting mode. However, in order to accurately determine alpha-tocopherol by cGC, further purification of the extract by solid-phase extraction was necessary. A silica SPE column was used to remove interfering cholesterol from the extract. alpha-Tocopherol was analyzed in its derivatized form. Absolute and relative recoveries for both vitamins from spiked samples were evaluated. Absolute and relative recoveries ranging from 80 to 95% were obtained for both compounds. 5 alpha-Cholestane and alpha-tocopheryl acetate were used as internal standards. Poultry muscle meat and liver tissue were analyzed for their retinol and alpha-tocopherol content and the peaks detected by cGC were confirmed by cGC-mass spectrometry.

Effects of model error on control of large flexible space antenna with comparisons of decoupled and linear quadratic regulator control procedures

NASA Technical Reports Server (NTRS)

Hamer, H. A.; Johnson, K. G.

1986-01-01

An analysis was performed to determine the effects of model error on the control of a large flexible space antenna. Control was achieved by employing two three-axis control-moment gyros (CMG's) located on the antenna column. State variables were estimated by including an observer in the control loop that used attitude and attitude-rate sensors on the column. Errors were assumed to exist in the individual model parameters: modal frequency, modal damping, mode slope (control-influence coefficients), and moment of inertia. Their effects on control-system performance were analyzed either for (1) nulling initial disturbances in the rigid-body modes, or (2) nulling initial disturbances in the first three flexible modes. The study includes the effects on stability, time to null, and control requirements (defined as maximum torque and total momentum), as well as on the accuracy of obtaining initial estimates of the disturbances. The effects on the transients of the undisturbed modes are also included. The results, which are compared for decoupled and linear quadratic regulator (LQR) control procedures, are shown in tabular form, parametric plots, and as sample time histories of modal-amplitude and control responses. Results of the analysis showed that the effects of model errors on the control-system performance were generally comparable for both control procedures. The effect of mode-slope error was the most serious of all model errors.

In-column ATR-FTIR spectroscopy to monitor affinity chromatography purification of monoclonal antibodies

NASA Astrophysics Data System (ADS)

Boulet-Audet, Maxime; Kazarian, Sergei G.; Byrne, Bernadette

2016-07-01

In recent years many monoclonal antibodies (mAb) have entered the biotherapeutics market, offering new treatments for chronic and life-threatening diseases. Protein A resin captures monoclonal antibody (mAb) effectively, but the binding capacity decays over repeated purification cycles. On an industrial scale, replacing fouled Protein A affinity chromatography resin accounts for a large proportion of the raw material cost. Cleaning-in-place (CIP) procedures were developed to extend Protein A resin lifespan, but chromatograms cannot reliably quantify any remaining contaminants over repeated cycles. To study resin fouling in situ, we coupled affinity chromatography and Fourier transform infrared (FTIR) spectroscopy for the first time, by embedding an attenuated total reflection (ATR) sensor inside a micro-scale column while measuring the UV 280 nm and conductivity. Our approach quantified the in-column protein concentration in the resin bed and determined protein conformation. Our results show that Protein A ligand leached during CIP. We also found that host cell proteins bound to the Protein A resin even more strongly than mAbs and that typical CIP conditions do not remove all fouling contaminants. The insights derived from in-column ATR-FTIR spectroscopic monitoring could contribute to mAb purification quality assurance as well as guide the development of more effective CIP conditions to optimise resin lifespan.

In-column ATR-FTIR spectroscopy to monitor affinity chromatography purification of monoclonal antibodies

PubMed Central

Boulet-Audet, Maxime; Kazarian, Sergei G.; Byrne, Bernadette

2016-01-01

In recent years many monoclonal antibodies (mAb) have entered the biotherapeutics market, offering new treatments for chronic and life-threatening diseases. Protein A resin captures monoclonal antibody (mAb) effectively, but the binding capacity decays over repeated purification cycles. On an industrial scale, replacing fouled Protein A affinity chromatography resin accounts for a large proportion of the raw material cost. Cleaning-in-place (CIP) procedures were developed to extend Protein A resin lifespan, but chromatograms cannot reliably quantify any remaining contaminants over repeated cycles. To study resin fouling in situ, we coupled affinity chromatography and Fourier transform infrared (FTIR) spectroscopy for the first time, by embedding an attenuated total reflection (ATR) sensor inside a micro-scale column while measuring the UV 280 nm and conductivity. Our approach quantified the in-column protein concentration in the resin bed and determined protein conformation. Our results show that Protein A ligand leached during CIP. We also found that host cell proteins bound to the Protein A resin even more strongly than mAbs and that typical CIP conditions do not remove all fouling contaminants. The insights derived from in-column ATR-FTIR spectroscopic monitoring could contribute to mAb purification quality assurance as well as guide the development of more effective CIP conditions to optimise resin lifespan. PMID:27470880

A strategy for identification and structural characterization of compounds from Gardenia jasminoides by integrating macroporous resin column chromatography and liquid chromatography-tandem mass spectrometry combined with ion-mobility spectrometry.

PubMed

Wang, Lu; Liu, Shu; Zhang, Xueju; Xing, Junpeng; Liu, Zhiqiang; Song, Fengrui

2016-06-24

In this paper, an analysis strategy integrating macroporous resin (AB-8) column chromatography and high performance liquid chromatography-electrospray ionization-tandem mass spectrometry (HPLC-ESI-MS/MS) combined with ion mobility spectrometry (IMS) was proposed and applied for identification and structural characterization of compounds from the fruits of Gardenia jasminoides. The extracts of G. jasminoides were separated by AB-8 resin column chromatography combined with reversed phase liquid chromatography (C18 column) and detected by electrospray ionization tandem mass spectrometry. Additionally, ion mobility spectrometry (IMS) was employed as a supplementary separation technique to discover previously undetected isomers from the fruits of G. jasminoides. A total of 71 compounds, including iridoids, flavonoids, triterpenes, monoterpenoids, carotenoids and phenolic acids were identified by the characteristic high resolution mass spectrometry and the ESI-MS/MS fragmentations. In conclusion, the IMS-MS technique achieved the separation of isomers in crocin-3 and crocin-4 according to their acquired mobility drift times differing from classical analysis by mass spectrometry. The proposed strategy can be used as a highly sensitive and efficient procedure for identification and separation isomeric components in extracts of herbal medicines. Copyright © 2016 Elsevier B.V. All rights reserved.

[Relationship among glycated compounds, superoxide dismutase activities, and other related analytes in diabetic patients classified by ages].

PubMed

Maehata, E; Shimomura, H; Kiyose, H; Hayashi, A; Sakagishi, Y

1991-07-01

Among several glycated compounds (GC) which are based on Maillard reaction, glycated hemoglobin (HbA1c) and fructosamine (FRA) have been utilized widely as a markers of diabetes. Recently, glycated albumin (GA) has been pointed out as a new indicator. For the determination of GA, spectrophotometry combined with an affinity column method has been mainly used, however the procedure is complicated. Recently a two-column HPLC method (ion-exchange column and affinity column) has been developed by Shima. We have evaluated a GA analyzer GAA-2000 based on Shima's method. After a series of fundamental and performance evaluation studies, the GAA-2000 was found to be appropriate for our study. Reference values obtained from this equipment were 10.56-16.87%. Correlation coefficients based on GA using diabetic and diabetic nephropathy patient specimens (n = 87) were: FRA (r = 0.944) greater than HbA1c (r = 0.842) greater than Glucose (r = 0.510) Superoxide dismutase (SOD) and lipid peroxidase (LPO) with are produced in relation to active oxygen did not show a good correlation. Although we tried classify the patients according to juvenile (20-39), middle (40-64) and senile (greater than 65) the method of Asada et al., we could not find any distinct tendencies.

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of pesticides in water by C-18 solid-phase extraction and capillary-column gas chromatography/mass spectrometry with selected-ion monitoring

USGS Publications Warehouse

Zaugg, Steven D.; Sandstrom, Mark W.; Smith, Steven G.; Fehlberg, Kevin M.

1995-01-01

A method for the isolation of 41 pesticides and pesticide metabolites in natural-water samples using C-18 solid-phase extraction and determination by capillary-column gas chromatography/mass spectrometry with selected-ion monitoring is described. Water samples are filtered to remove suspended particulate matter and then are pumped through disposable solid-phase extraction columns containing octadecyl-bonded porous silica to extract the pesticides. The columns are dried using carbon dioxide or nitrogen gas, and adsorbed pesticides are removed from the columns by elution with 3.0 milliliters of hexane-isopropanol (3:1). Extracted pesticides are determined by capillary- column gas chromatography/mass spectrometry with selected-ion monitoring of three characteristic ions. The upper concentration limit is 4 micrograms per liter (g/L) for most pesticides, with the exception of widely used corn herbicides--atrazine, alachlor, cyanazine, and metolachlor--which have upper concentration limits of 20 g/L. Single- operator method detection limits in reagent-water samples range from 0.001 to 0.018 g/L. Average short-term single-operator precision in reagent- water samples is 7 percent at the 0.1- and 1.0-g/L levels and 8 percent at the 0.01-g/L level. Mean recoveries in reagent-water samples are 73 percent at the 0.1- and 1.0-g/L levels and 83 percent at the 0.01-g/L level. The estimated holding time for pesticides after extraction on the solid-phase extraction columns was 7 days. An optional on-site extraction procedure allows for samples to be collected and processed at remote sites where it is difficult to ship samples to the laboratory within the recommended pre-extraction holding time.

Transport of Intrinsic Plutonium Colloids in Saturated Porous Media

NASA Astrophysics Data System (ADS)

Zhou, D.; Abdel-Fattah, A.; Boukhalfa, H.; Ware, S. D.; Tarimala, S.; Keller, A. A.

2011-12-01

Actinide contaminants were introduced to the subsurface environment as a result of nuclear weapons development and testing, as well as for nuclear power generation and related research activities for defense and civilian applications. Even though most actinide species were believed to be fairly immobile once in the subsurface, recent studies have shown the transport of actinides kilometers away from their disposal sites. For example, the treated liquid wastes released into Mortandad Canyon at the Los Alamos National Laboratory were predicted to travel less than a few meters; however, plutonium and americium have been detected 3.4 km away from the waste outfall. A colloid-facilitated mechanism has been suggested to account for this unexpected transport of these radioactive wastes. Clays, oxides, organic matters, and actinide hydroxides have all been proposed as the possible mobile phase. Pu ions associated with natural colloids are often referred to as pseudo-Pu colloids, in contrast with the intrinsic Pu colloids that consist of Pu oxides. Significant efforts have been made to investigate the role of pseudo-Pu colloids, while few studies have evaluated the environmental behavior of the intrinsic Pu colloids. Given the fact that Pu (IV) has extremely low solubility product constant, it can be inferred that the transport of Pu in the intrinsic form is highly likely at suitable environmental conditions. This study investigates the transport of intrinsic Pu colloids in a saturated alluvium material packed in a cylindrical column (2.5-cm Dia. x 30-cm high) and compares the results to previous data on the transport of pseudo Pu colloids in the same material. A procedure to prepare a stable intrinsic Pu colloid suspension that produced consistent and reproducible electrokinetic and stability data was developed. Electrokinetic properties and aggregation stability were characterized. The Pu colloids, together with trillium as a conservative tracer, were injected into the column at a flow rate of ~ 6 mL/hr. Despite that the Pu intrinsic colloids are positively charged while the alluvium grain surfaces are negatively charged under the current experimental conditions, about 30% of the Pu colloids population transported through the column and broke through earlier than trillium. Our previous experiments in the same column have shown a highly unretarded transport of the negatively charged pseudo Pu colloids (Pu sorbed onto smectite colloids) and complete retardation of the dissolved Pu. The enhanced transport of Pu colloids was explained by the effective pore volume concept. Combining the results of these two experiments, it is concluded that the intrinsic Pu colloids transported in the column by adsorbing onto the background clay colloids due to electrostatic repulsion.

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

PubMed

Jia, Yu; Maurice, Christian; Öhlander, Björn

2016-01-01

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

Generation of High Frequency Response in a Dynamically Loaded, Nonlinear Soil Column

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

Spears, Robert Edward; Coleman, Justin Leigh

2015-08-01

Detailed guidance on linear seismic analysis of soil columns is provided in “Seismic Analysis of Safety-Related Nuclear Structures and Commentary (ASCE 4, 1998),” which is currently under revision. A new Appendix in ASCE 4-2014 (draft) is being added to provide guidance for nonlinear time domain analysis which includes evaluation of soil columns. When performing linear analysis, a given soil column is typically evaluated with a linear, viscous damped constitutive model. When submitted to a sine wave motion, this constitutive model produces a smooth hysteresis loop. For nonlinear analysis, the soil column can be modelled with an appropriate nonlinear hysteretic soilmore » model. For the model in this paper, the stiffness and energy absorption result from a defined post yielding shear stress versus shear strain curve. This curve is input with tabular data points. When submitted to a sine wave motion, this constitutive model produces a hysteresis loop that looks similar in shape to the input tabular data points on the sides with discontinuous, pointed ends. This paper compares linear and nonlinear soil column results. The results show that the nonlinear analysis produces additional high frequency response. The paper provides additional study to establish what portion of the high frequency response is due to numerical noise associated with the tabular input curve and what portion is accurately caused by the pointed ends of the hysteresis loop. Finally, the paper shows how the results are changed when a significant structural mass is added to the top of the soil column.« less

The Two-Column Aerosol Project: Phase I - Overview and Impact of Elevated Aerosol Layers on Aerosol Optical Depth

NASA Technical Reports Server (NTRS)

Berg, Larry K.; Fast, Jerome D.; Barnard, James C.; Burton, Sharon P.; Cairns, Brian; Chand, Duli; Comstock, Jennifer M.; Dunagan, Stephen; Ferrare, Richard A.; Flynn, Connor J.;

The Two-Column Aerosol Project: Phase I—Overview and impact of elevated aerosol layers on aerosol optical depth

NASA Astrophysics Data System (ADS)

Berg, Larry K.; Fast, Jerome D.; Barnard, James C.; Burton, Sharon P.; Cairns, Brian; Chand, Duli; Comstock, Jennifer M.; Dunagan, Stephen; Ferrare, Richard A.; Flynn, Connor J.; Hair, Johnathan W.; Hostetler, Chris A.; Hubbe, John; Jefferson, Anne; Johnson, Roy; Kassianov, Evgueni I.; Kluzek, Celine D.; Kollias, Pavlos; Lamer, Katia; Lantz, Kathleen; Mei, Fan; Miller, Mark A.; Michalsky, Joseph; Ortega, Ivan; Pekour, Mikhail; Rogers, Ray R.; Russell, Philip B.; Redemann, Jens; Sedlacek, Arthur J.; Segal-Rosenheimer, Michal; Schmid, Beat; Shilling, John E.; Shinozuka, Yohei; Springston, Stephen R.; Tomlinson, Jason M.; Tyrrell, Megan; Wilson, Jacqueline M.; Volkamer, Rainer; Zelenyuk, Alla; Berkowitz, Carl M.

2016-01-01

The Two-Column Aerosol Project (TCAP), conducted from June 2012 through June 2013, was a unique study designed to provide a comprehensive data set that can be used to investigate a number of important climate science questions, including those related to aerosol mixing state and aerosol radiative forcing. The study was designed to sample the atmosphere between and within two atmospheric columns; one fixed near the coast of North America (over Cape Cod, MA) and a second moveable column over the Atlantic Ocean several hundred kilometers from the coast. The U.S. Department of Energy's (DOE) Atmospheric Radiation Measurement (ARM) Mobile Facility (AMF) was deployed at the base of the Cape Cod column, and the ARM Aerial Facility was utilized for the summer and winter intensive observation periods. One important finding from TCAP is that four of six nearly cloud-free flight days had aerosol layers aloft in both the Cape Cod and maritime columns that were detected using the nadir pointing second-generation NASA high-spectral resolution lidar (HSRL-2). These layers contributed up to 60% of the total observed aerosol optical depth (AOD). Many of these layers were also intercepted by the aircraft configured for in situ sampling, and the aerosol in the layers was found to have increased amounts of biomass burning material and nitrate compared to aerosol found near the surface. In addition, while there was a great deal of spatial and day-to-day variability in the aerosol chemical composition and optical properties, no systematic differences between the two columns were observed.

Assiduous String-Savers: The Idea-Generating Strategies of Professional Expository Writers.

ERIC Educational Resources Information Center

Root, Robert L., Jr.

A study was conducted over a two-year period to investigate the idea-generating strategies of six professional writers and their implications for students. Because finding an idea that leads to a journal or newspaper column is so important to a writer, an attempt was made to learn ways professional writers establish working plans and develop a…

Special Research Column: Empathetic Genres, Empathetic Spaces, and Mentoring: Examining Contemporary Research on First-Generation College Students in First-Year Writing

ERIC Educational Resources Information Center

Borchert, Jessica Jorgenson

2017-01-01

This article focuses on contemporary research on first-generation college students bringing to light pedagogical interventions that can be used in the classroom to help engage and retain these students. The pedagogical interventions focus on reflective and personal writing in the classroom, creating safe spaces, and opening up opportunities for…

Low pressure arc discharge lamp apparatus with magnetic field generating means

DOEpatents

Grossman, Mark W.; George, William A.; Maya, Jakob

1987-01-01

A low-pressure arc discharge apparatus having a magnetic field generating means for increasing the output of a discharge lamp is disclosed. The magnetic field generating means, which in one embodiment includes a plurality of permanent magnets, is disposed along the lamp for applying a constant transverse magnetic field over at least a portion of the positive discharge column produced in the arc discharge lamp operating at an ambient temperature greater than about 25.degree. C.

Maskless micro-ion-beam reduction lithography system

DOEpatents

Leung, Ka-Ngo; Barletta, William A.; Patterson, David O.; Gough, Richard A.

2005-05-03

A maskless micro-ion-beam reduction lithography system is a system for projecting patterns onto a resist layer on a wafer with feature size down to below 100 nm. The MMRL system operates without a stencil mask. The patterns are generated by switching beamlets on and off from a two electrode blanking system or pattern generator. The pattern generator controllably extracts the beamlet pattern from an ion source and is followed by a beam reduction and acceleration column.

Fire resistance of exposed wood members

Treesearch

Robert H. White

2004-01-01

Fire resistance data on exposed wood beams and columns are plentiful, but few studies have been done on exposed wood members in tension and in decks. To provide data to verify the application of a new calculation procedure, a limited series of fire resistance tests were conducted on wood members loaded in tension and on exposed wood decks.

40 CFR Appendix C to Part 61 - Quality Assurance Procedures

Code of Federal Regulations, 2013 CFR

2013-07-01

.... EC01MY92.034 In judging the suitability of alternate GC columns or the effects of altering chromatographic... that has a leading edge that rises sharply but the curve then tails off, it may be possible to define an effective width for tc as “twice the distance from the leading edge to a perpendicular line...

40 CFR Appendix C to Part 61 - Quality Assurance Procedures

Code of Federal Regulations, 2011 CFR

2011-07-01

.... EC01MY92.034 In judging the suitability of alternate GC columns or the effects of altering chromatographic... that has a leading edge that rises sharply but the curve then tails off, it may be possible to define an effective width for tc as “twice the distance from the leading edge to a perpendicular line...

40 CFR Appendix C to Part 61 - Quality Assurance Procedures

Code of Federal Regulations, 2012 CFR

2012-07-01

.... EC01MY92.034 In judging the suitability of alternate GC columns or the effects of altering chromatographic... that has a leading edge that rises sharply but the curve then tails off, it may be possible to define an effective width for tc as “twice the distance from the leading edge to a perpendicular line...

Parsimonious extreme learning machine using recursive orthogonal least squares.

PubMed

Wang, Ning; Er, Meng Joo; Han, Min

2014-10-01

Novel constructive and destructive parsimonious extreme learning machines (CP- and DP-ELM) are proposed in this paper. By virtue of the proposed ELMs, parsimonious structure and excellent generalization of multiinput-multioutput single hidden-layer feedforward networks (SLFNs) are obtained. The proposed ELMs are developed by innovative decomposition of the recursive orthogonal least squares procedure into sequential partial orthogonalization (SPO). The salient features of the proposed approaches are as follows: 1) Initial hidden nodes are randomly generated by the ELM methodology and recursively orthogonalized into an upper triangular matrix with dramatic reduction in matrix size; 2) the constructive SPO in the CP-ELM focuses on the partial matrix with the subcolumn of the selected regressor including nonzeros as the first column while the destructive SPO in the DP-ELM operates on the partial matrix including elements determined by the removed regressor; 3) termination criteria for CP- and DP-ELM are simplified by the additional residual error reduction method; and 4) the output weights of the SLFN need not be solved in the model selection procedure and is derived from the final upper triangular equation by backward substitution. Both single- and multi-output real-world regression data sets are used to verify the effectiveness and superiority of the CP- and DP-ELM in terms of parsimonious architecture and generalization accuracy. Innovative applications to nonlinear time-series modeling demonstrate superior identification results.

Influence of sulfur-bearing polyatomic species on high precision measurements of Cu isotopic composition

USGS Publications Warehouse

Pribil, M.J.; Wanty, R.B.; Ridley, W.I.; Borrok, D.M.

2010-01-01

An increased interest in high precision Cu isotope ratio measurements using multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS) has developed recently for various natural geologic systems and environmental applications, these typically contain high concentrations of sulfur, particularly in the form of sulfate (SO42-) and sulfide (S). For example, Cu, Fe, and Zn concentrations in acid mine drainage (AMD) can range from 100??g/L to greater than 50mg/L with sulfur species concentrations reaching greater than 1000mg/L. Routine separation of Cu, Fe and Zn from AMD, Cu-sulfide minerals and other geological matrices usually incorporates single anion exchange resin column chromatography for metal separation. During chromatographic separation, variable breakthrough of SO42- during anion exchange resin column chromatography into the Cu fractions was observed as a function of the initial sulfur to Cu ratio, column properties, and the sample matrix. SO42- present in the Cu fraction can form a polyatomic 32S-14N-16O-1H species causing a direct mass interference with 63Cu and producing artificially light ??65Cu values. Here we report the extent of the mass interference caused by SO42- breakthrough when measuring ??65Cu on natural samples and NIST SRM 976 Cu isotope spiked with SO42- after both single anion column chromatography and double anion column chromatography. A set of five 100??g/L Cu SRM 976 samples spiked with 500mg/L SO42- resulted in an average ??65Cu of -3.50?????5.42??? following single anion column separation with variable SO42- breakthrough but an average concentration of 770??g/L. Following double anion column separation, the average SO42-concentration of 13??g/L resulted in better precision and accuracy for the measured ??65Cu value of 0.01?????0.02??? relative to the expected 0??? for SRM 976. We conclude that attention to SO42- breakthrough on sulfur-rich samples is necessary for accurate and precise measurements of ??65Cu and may require the use of a double ion exchange column procedure. ?? 2010.

Theory for the alignment of cortical feature maps during development.

PubMed

Bressloff, Paul C; Oster, Andrew M

2010-08-01

We present a developmental model of ocular dominance column formation that takes into account the existence of an array of intrinsically specified cytochrome oxidase blobs. We assume that there is some molecular substrate for the blobs early in development, which generates a spatially periodic modulation of experience-dependent plasticity. We determine the effects of such a modulation on a competitive Hebbian mechanism for the modification of the feedforward afferents from the left and right eyes. We show how alternating left and right eye dominated columns can develop, in which the blobs are aligned with the centers of the ocular dominance columns and receive a greater density of feedforward connections, thus becoming defined extrinsically. More generally, our results suggest that the presence of periodically distributed anatomical markers early in development could provide a mechanism for the alignment of cortical feature maps.

Sample pretreatment optimization for the analysis of short chain chlorinated paraffins in soil with gas chromatography-electron capture negative ion-mass spectrometry.

PubMed

Chen, Laiguo; Huang, Yumei; Han, Shuang; Feng, Yongbin; Jiang, Guo; Tang, Caiming; Ye, Zhixiang; Zhan, Wei; Liu, Ming; Zhang, Sukun

2013-01-25

Accurately quantifying short chain chlorinated paraffins (SCCPs) in soil samples with gas chromatograph coupled with electron capture negative ionization mass spectrometry (GC-ECNI-MS) is difficult because many other polychlorinated pollutants are present in the sample matrices. These pollutants (e.g., polychlorinated biphenyls (PCBs), organochlorine pesticides (OCPs) and toxaphene) can cause serious interferences during SCCPs analysis with GC-MS. Four main columns packed with different adsorbents, including silica gel, Florisil and alumina, were investigated in this study to determine their performance for separating interfering pollutants from SCCPs. These experimental results suggest that the optimum cleanup procedure uses a silica gel column and a multilayer silica gel-Florisil composite column. This procedure completely separated 22 PCB congeners, 23 OCPs and three toxaphene congeners from SCCPs. However, p,p'-DDD, cis-nonachlor and o,p'-DDD were not completely removed and only 53% of the total toxaphene was removed. This optimized method was successfully and effectively applied for removing interfering pollutants from real soil samples. SCCPs in 17 soil samples from different land use areas within a suburban region were analyzed with the established method. The concentrations of SCCPs in these samples were between 7 and 541 ng g(-1) (mean: 84 ng g(-1)). Similar homologue SCCPs patterns were observed between the soil samples collected from different land use areas. In addition, lower chlorinated (Cl(6/7)) C(10)- and C(11)- SCCPs were the dominant congeners. Copyright © 2012 Elsevier B.V. All rights reserved.

{sup 99m}Tc generators for clinical use based on zirconium molybdate gel and (n, gamma) produced {sup 99}Mo: Indian experience in the development and deployment of indigenous technology and processing facilities

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

Saraswathy, P.; Dey, A.C.; Sarkar, S.K.

The Indian pursuit of gel generator technology for {sup 99m}Tc was driven mainly by three considerations, namely, (i) well-established and ease of reliable production of (n, gamma)-based {sup 99}Mo in several tens of GBq quantities in the research reactors in Trombay/Mumbai, India, (ii) need for relatively low-cost alternate technology to replace the solvent (MEK) extraction generator system in use in India since 1970s and (iii) minimize dependency on weekly import of fission-produced {sup 99}Mo raw material required for alumina column generator. Extensive investigations on process standardisation for zirconium molybdate gel (ZMG) led to a steady progress, achieved both in termsmore » of process technology and final performance of {sup 99m}Tc gel generators. The {sup 99m}Tc final product purity from the Indian gel system was comparable to that obtained from the gold-standard alumina column generators. Based on the feasibility established for reliable small-scale production, as well as satisfactory clinical experience with a number of gel generators used in collaborating hospital radiopharmacies, full-fledged mechanised processing facilities for handling up to 150 g of ZMG were set up. The indigenous design and development included setting up of shielded plant facilities with pneumatic-driven as well as manual controls and special gadgets such as, microwave heating of the zirconium molybdate cake, dispenser for gel granules, loading of gel columns into pre-assembled generator housing etc. Formal review of the safety features was carried out by the regulatory body and stage-wise clearance for processing low and medium level {sup 99}Mo activity was granted. Starting from around 70 GBq {sup 99}Mo handling, the processing facilities have since been successfully operated at a level of 740 GBq {sup 99}Mo, twice a month. In all 18 batches of gel have been processed and 156 generators produced. The individual generator capacity was 15 to 30 GBq with an elution yield of nearly 75%. 129 generators were supplied to 11 user hospitals and the estimated number of clinical studies done is well over 5000. The salient aspects of the Indian experience have been reported in many a forum and shared with the IAEA through the on-going CRP. The detailed process know-how is available for technology transfer from BRIT, India. (author)« less

Mars Ozone Absorption Line Shapes from Infrared Heterodyne Spectra Applied to GCM-Predicted Ozone Profiles and to MEX/SPICAM Column Retrievals

NASA Technical Reports Server (NTRS)

Fast, Kelly E.; Kostiuk, T.; Annen, J.; Hewagama, T.; Delgado, J.; Livengood, T. A.; Lefevre, F.

2008-01-01

We present the application of infrared heterodyne line shapes of ozone on Mars to those produced by radiative transfer modeling of ozone profiles predicted by general circulation models (GCM), and to contemporaneous column abundances measured by Mars Express SPICAM. Ozone is an important tracer of photochemistry Mars' atmosphere, serving as an observable with which to test predictions of photochemistry-coupled GCMs. Infrared heterodyne spectroscopy at 9.5 microns with spectral resolving power >1,000,000 is the only technique that can directly measure fully-resolved line shapes of Martian ozone features from the surface of the Earth. Measurements were made with Goddard Space Flight Center's Heterodyne instrument for Planetary Wind And Composition (HIPWAC) at the NASA Infrared Telescope Facility (IRTF) on Mauna Kea, Hawaii on February 21-24 2008 UT at Ls=35deg on or near the MEX orbital path. The HIPWAC observations were used to test GCM predictions. For example, a GCM-generated ozone profile for 60degN 112degW was scaled so that a radiative transfer calculation of its absorption line shape matched an observed HIPWAC absorption feature at the same areographic position, local time, and season. The RMS deviation of the model from the data was slightly smaller for the GCM-generated profile than for a line shape produced by a constant-with-height profile, even though the total column abundances were the same, showing potential for testing and constraining GCM ozone-profiles. The resulting ozone column abundance from matching the model to the HIPWAC line shape was 60% higher than that observed by SPICAM at the same areographic position one day earlier and 2.5 hours earlier in local time. This could be due to day-to-day, diurnal, or north polar region variability, or to measurement sensitivity to the ozone column and its distribution, and these possibilities will be explored. This work was supported by NASA's Planetary Astronomy Program.

Magma Vesiculation and Infrasonic Activity in Open Conduit Volcanoes

NASA Astrophysics Data System (ADS)

Colo', L.; Baker, D. R.; Polacci, M.; Ripepe, M.

2007-12-01

At persistently active basaltic volcanoes such as Stromboli, Italy degassing of the magma column can occur in "passive" and "active" conditions. Passive degassing is generally understood as a continuous, non explosive release of gas mainly from the open summit vents and subordinately from the conduit's wall or from fumaroles. In passive degassing generally gas is in equilibrium with atmospheric pressure, while in active degassing the gas approaches the surface at overpressurized conditions. During active degassing (or puffing), the magma column is interested by the bursting of small gas bubbles at the magma free surface and, as a consequence, the active degassing process generates infrasonic signals. We postulated, in this study, that the rate and the amplitude of infrasonic activity is somehow linked to the rate and the volume of the overpressured gas bubbles, which are generated in the magma column. Our hypothesis is that infrasound is controlled by the quantities of gas exsolved in the magma column and then, that a relationship between infrasound and the vesiculation process should exist. In order to achieve this goal, infrasonic records and bubble size distributions of scoria samples from normal explosive activity at Stromboli processed via X ray tomography have been compared. We observed that the cumulative distribution for both data sets follow similar power laws, indicating that both processes are controlled by a scale invariant phenomenon. However the power law is not stable but changes in different scoria clasts, reflecting when gas bubble nucleation is predominant over bubbles coalescence and viceversa. The power law also changes for the infrasonic activity from time to time, suggesting that infrasound may be controlled also by a different gas exsolution within the magma column. Changes in power law distributions are the same for infrasound and scoria indicating that they are linked to the same process acting in the magmatic system. We suggest that monitoring infrasound on an active volcano could represent an alternative way to monitor the vesiculation process of an open conduit system.

The minimal residual QR-factorization algorithm for reliably solving subset regression problems

NASA Technical Reports Server (NTRS)

Verhaegen, M. H.

1987-01-01

A new algorithm to solve test subset regression problems is described, called the minimal residual QR factorization algorithm (MRQR). This scheme performs a QR factorization with a new column pivoting strategy. Basically, this strategy is based on the change in the residual of the least squares problem. Furthermore, it is demonstrated that this basic scheme might be extended in a numerically efficient way to combine the advantages of existing numerical procedures, such as the singular value decomposition, with those of more classical statistical procedures, such as stepwise regression. This extension is presented as an advisory expert system that guides the user in solving the subset regression problem. The advantages of the new procedure are highlighted by a numerical example.

EVA manipulation and assembly of space structure columns

NASA Technical Reports Server (NTRS)

Loughead, T. E.; Pruett, E. C.

1980-01-01

Assembly techniques and hardware configurations used in assembly of the basic tetrahedral cell by A7LB pressure-suited subjects in a neutral bouyancy simulator were studied. Eleven subjects participated in assembly procedures which investigated two types of structural members and two configurations of attachment hardware. The assembly was accomplished through extra-vehicular activity (EVA) only, EVA with simulated manned maneuvering unit (MMU), and EVA with simulated MMU and simulated remote manipulator system (RMS). Assembly times as low as 10.20 minutes per tetrahedron were achieved. Task element data, as well as assembly procedures, are included.

Test procedures and instructions for single shell tank saltcake cesium removal with crystalline silicotitanate

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

Duncan, J.B.

1997-01-07

This document provides specific test procedures and instructions to implement the test plan for the preparation and conduct of a cesium removal test, using Hanford Single Shell Tank Saltcake from tanks 24 t -BY- I 10, 24 1 -U- 108, 24 1 -U- 109, 24 1 -A- I 0 1, and 24 t - S-102, in a bench-scale column. The cesium sorbent to be tested is crystalline siticotitanate. The test plan for which this provides instructions is WHC-SD-RE-TP-024, Hanford Single Shell Tank Saltcake Cesium Removal Test Plan.

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

Molecular structure and gas chromatographic retention behavior of the components of Ylang-Ylang oil.

PubMed

Olivero, J; Gracia, T; Payares, P; Vivas, R; Díaz, D; Daza, E; Geerlings, P

1997-05-01

Using quantitative structure-retention relationships (QSRR) methodologies the Kovats gas chromatographic retention indices for both apolar (DB-1) and polar (DB-Wax) columns for 48 compounds from Ylang-Ylang essential oil were empirically predicted from calculated and experimental data on molecular structure. Topological, geometric, and electronic descriptors were obtained for model generation. Relationships between descriptors and the retention data reported were established by linear multiple regression, giving equations that can be used to predict the Kovats indices for compounds present in essential oils, both in DB-1 and DB-Wax columns. Factor analysis was performed to interpret the meaning of the descriptors included in the models. The prediction model for the DB-1 column includes descriptors such as Randic's first-order connectivity index (1X), the molecular surface (MSA), the sum of the atomic charge on all the hydrogens (QH), Randic's third-order connectivity index (3X) and the molecular electronegativity (chi). The prediction model for the DB-Wax column includes the first three descriptors mentioned for the DB-1 column (1X, MSA and QH) and the most negative charge (MNC), the global softness (S), and the difference between Randic's and Kier and Hall's third-order connectivity indexes (3X-3XV).

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

NASA Astrophysics Data System (ADS)

Zielińska, M.; Grębowski, K.

2015-02-01

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

The generation of vertebral segmental patterning in the chick embryo.

PubMed

Senthinathan, Biruntha; Sousa, Cátia; Tannahill, David; Keynes, Roger

2012-06-01

We have carried out a series of experimental manipulations in the chick embryo to assess whether the notochord, neural tube and spinal nerves influence segmental patterning of the vertebral column. Using Pax1 expression in the somite-derived sclerotomes as a marker for segmentation of the developing intervertebral disc, our results exclude such an influence. In contrast to certain teleost species, where the notochord has been shown to generate segmentation of the vertebral bodies (chordacentra), these experiments indicate that segmental patterning of the avian vertebral column arises autonomously in the somite mesoderm. We suggest that in amniotes, the subdivision of each sclerotome into non-miscible anterior and posterior halves plays a critical role in establishing vertebral segmentation, and in maintaining left/right alignment of the developing vertebral elements at the body midline. © 2012 The Authors. Journal of Anatomy © 2012 Anatomical Society.

Benthic exchange and biogeochemical cycling in permeable sediments.

PubMed

Huettel, Markus; Berg, Peter; Kostka, Joel E

2014-01-01

The sandy sediments that blanket the inner shelf are situated in a zone where nutrient input from land and strong mixing produce maximum primary production and tight coupling between water column and sedimentary processes. The high permeability of the shelf sands renders them susceptible to pressure gradients generated by hydrodynamic and biological forces that modulate spatial and temporal patterns of water circulation through these sediments. The resulting dynamic three-dimensional patterns of particle and solute distribution generate a broad spectrum of biogeochemical reaction zones that facilitate effective decomposition of the pelagic and benthic primary production products. The intricate coupling between the water column and sediment makes it challenging to quantify the production and decomposition processes and the resultant fluxes in permeable shelf sands. Recent technical developments have led to insights into the high biogeochemical and biological activity of these permeable sediments and their role in the global cycles of matter.

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

NASA Technical Reports Server (NTRS)

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

1981-01-01

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

Sustained diffusive alternating current gliding arc discharge in atmospheric pressure air

NASA Astrophysics Data System (ADS)

Zhu, Jiajian; Gao, Jinlong; Li, Zhongshan; Ehn, Andreas; Aldén, Marcus; Larsson, Anders; Kusano, Yukihiro

2014-12-01

Rapid transition from glow discharge to thermal arc has been a common problem in generating stable high-power non-thermal plasmas especially at ambient conditions. A sustained diffusive gliding arc discharge was generated in a large volume in atmospheric pressure air, driven by an alternating current (AC) power source. The plasma column extended beyond the water-cooled stainless steel electrodes and was stabilized by matching the flow speed of the turbulent air jet with the rated output power. Comprehensive investigations were performed using high-speed movies measured over the plasma column, synchronized with simultaneously recorded current and voltage waveforms. Dynamic details of the novel non-equilibrium discharge are revealed, which is characterized by a sinusoidal current waveform with amplitude stabilized at around 200 mA intermediate between thermal arc and glow discharge, shedding light to the governing mechanism of the sustained spark-suppressed AC gliding arc discharge.

Room temperature ionic liquids: new GC stationary phases with a novel selectivity for flavor and fragrance analyses.

PubMed

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

2012-12-14

Ionic liquids (ILs) are of great interest as moderately polar to polar stationary phases for GC, because their selectivity differs markedly from that of conventionally used phases. In the flavor, fragrance and essential oil fields, analysts often deal with complex mixtures of compounds having similar structural and physical characteristics (e.g., mono- and sesquiterpenoids), therefore requiring an interactive combination between chromatographic and mass spectral data for correct identification. New GC stationary phases with different selectivity must therefore be continually tested. Performance and evolution over time of commercially available IL columns versus those commonly used in these fields are here evaluated, mainly in view of their routine use. Chromatographic and separative properties (efficiency, separation capability, inertness and/or activity) of commercially available IL columns were compared to those of columns coated with 5% phenyl-95% methylpolysiloxane, 14% cyanopropyl-86% polysiloxane, and polyethylene glycol, on different complexity samples, including standard mixtures of volatile suspected allergens and pesticides, and cornmint and vetiver essential oils. The results show that IL columns can successfully be used for a wide range of applications characteristic of these fields, mainly because of their unusual selectivity, in particular when separations based on functional groups are required. Moreover, the latest generation of IL columns (IL61 and IL60) presents chromatographic performance comparable to or only slightly lower than that of the conventional columns routinely used in these fields. Copyright © 2012 Elsevier B.V. All rights reserved.

Ionization of Xenon to the Nickel-Like Stage and Beyond in Micro-Capillary Plasma Columns Heated by Ultrafast Current Pulses

NASA Astrophysics Data System (ADS)

Avaria, G.; Grisham, M.; Li, J.; Tomasel, F. G.; Shlyapstsev, V. N.; Busquet, M.; Woolston, M.; Rocca, J. J.

Homogeneous plasma columns with ionization levels typical of MA discharges were created by rapidly heating gas-filled 520 µm diameter channels with ns rise-time current pulses of unusually low amplitude, 40 kA. These conditions allow the generation of high aspect ratio (eg. > 300:1) plasma columns with very high degrees of ionization (e.g. Ni-like Xenon) of interest for soft x-ray lasers below λ = 10 nm. Spectra and simulations of plasmas generated in 520 µm diameter alumina capillaries driven by 35-40 kA current pulses with 4 ns rise time were obtained for discharges in Xenon and Neon discharges. The first shows the presence of lines corresponding to ionization stages up to Fe-like Xe. The latter show that Al impurities from the walls are ionized to the H-like and He-like stages. He-like Al spectra containing the resonance line significantly broaden by opacity, the intercombination line, and Li-like satellites are analyzed. For Xenon discharges, the spectral lines from the Ni-like transitions the 3d94d (3/2, 3/2)J = 0 to the 3d94p(5/2, 3/2)J = 1 and to 3d94p(3/2, 1/2)J = 1 are observed.

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

PubMed

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

2018-01-16

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

Low pressure arc discharge lamp apparatus with magnetic field generating means

DOEpatents

Grossman, M.W.; George, W.A.; Maya, J.

1987-10-06

A low-pressure arc discharge apparatus having a magnetic field generating means for increasing the output of a discharge lamp is disclosed. The magnetic field generating means, which in one embodiment includes a plurality of permanent magnets, is disposed along the lamp for applying a constant transverse magnetic field over at least a portion of the positive discharge column produced in the arc discharge lamp operating at an ambient temperature greater than about 25 C. 3 figs.

Considerations on comprehensive and off-line supercritical fluid chromatography x reversed-phase liquid chromatography for the analysis of triacylglycerols in fish oil.

PubMed

François, Isabelle; Pereira, Alberto dos Santos; Sandra, Pat

2010-06-01

The separation of the triacylglycerols in fish oil was performed by comprehensive and off-line supercritical fluid chromatography combined with RP-LC. The first dimension consisted of two serially coupled silver-ion (SI)-loaded columns operated with a supercritical mobile phase (supercritical fluid chromatography, SFC) in both the cases, whereas the second dimension was performed in non-aqueous RP mode (NARP-LC) on a 10-cm monolithic octadecyl silica (ODS) or a 45-cm long ODS column packed with 1.8 microm particles for the comprehensive and off-line separations, respectively. Despite the outstanding performance of the SI-SFC x NARP-LC interface, the high complexity of the sample rendered the online separation far from complete. The off-line approach gave much better separation mainly because of the higher peak capacity of the second-dimension column, but even in this case, the use of MS was mandatory to elucidate the different triacylglycerols in fish oil. The disadvantage of the off-line procedure was the long analysis time.

Optimising mobile phase composition, its flow-rate and column temperature in HPLC using taboo search.

PubMed

Guillaume, Y C; Peyrin, E

2000-03-06

A chemometric methodology is proposed to study the separation of seven p-hydroxybenzoic esters in reversed phase liquid chromatography (RPLC). Fifteen experiments were found to be necessary to find a mathematical model which linked a novel chromatographic response function (CRF) with the column temperature, the water fraction in the mobile phase and its flow rate. The CRF optimum was determined using a new algorithm based on Glover's taboo search (TS). A flow-rate of 0.9 ml min(-1) with a water fraction of 0.64 in the ACN-water mixture and a column temperature of 10 degrees C gave the most efficient separation conditions. The usefulness of TS was compared with the pure random search (PRS) and simplex search (SS). As demonstrated by calculations, the algorithm avoids entrapment in local minima and continues the search to give a near-optimal final solution. Unlike other methods of global optimisation, this procedure is generally applicable, easy to implement, derivative free, conceptually simple and could be used in the future for much more complex optimisation problems.

Explosive decomposition of hydrazine by rapid compression of a gas volume

NASA Technical Reports Server (NTRS)

Bunker, R. L.; Baker, D. L.; Lee, J. H. S.

1991-01-01

In the present investigation of the initiation mechanism and the explosion mode of hydrazine decomposition, a 20 cm-long column of liquid hydrazine was accelerated into a column of gaseous nitrogen, from which it was separated by a thin Teflon diaphragm, in a close-ended cylindrical chamber. Video data obtained reveal the formation of a froth generated by the acceleration of hydrazine into nitrogen at the liquid hydrazine-gaseous nitrogen interface. The explosive hydrazine decomposition had as its initiation mechanism the formation of a froth at a critical temperature; the explosion mode of hydrazine is a confined thermal runaway reaction.

Study of the Anatomy of the X-Ray and Neutron Production Scaling Laws in the Plasma Focus (Particle Energy Spectrum and Optimization Criteria).

DTIC Science & Technology

1979-11-01

plasma focus operations have been experimentally analyzed in terms of (A) The fine structure of the axial-current channel during maximum of compression. (B) Correlation coefficient, for neutron yield n (by D2 discharges) and the multiplicity of the electron beam pulses; (C) Different values of the electrode voltage. The current distribution near the axial plasma column during the explosive decay of the column has been monitored and correlated with the electron beam production. Plasma focus discharges by our mode of operation generate high-intensity

Transport and Transformation of Selenium and Other Constituents of Flue-Gas Desulfurization Wastewater in Water-Saturated Soil Materials.

PubMed

Galkaduwa, Madhubhashini B; Hettiarachchi, Ganga M; Kluitenberg, Gerard J; Hutchinson, Stacy L; Davis, Lawrence; Erickson, Larry E

2017-03-01

Constructed wetland treatment systems are used to remove selenium (Se) from flue-gas desulfurization (FGD) wastewater (WW). However, direct confirmation of the mechanism responsible for FGD WW Se retention in soil is lacking. A laboratory-based soil column study was performed to develop an evidence-based mechanism of Se retention and to study the behavior and the retention capacity of FGD WW constituents in water-saturated soil. A deoxygenated 1:1 mixture of FGD WW and raw water was delivered to the columns bottom-up at a flux of 1.68 cm d for 100 d. Some of the columns were flushed with the raw water at the same rate for an additional 100 d. Column effluent was analyzed for constituents of concern. Results showed a complete retention of FGD WW Se in the soil materials. Boron and fluorine were partially retained; however, sulfur, sodium, and chlorine retention was poor, agreeing with field observations. The FGD WW Se was retained in soil near the inlet end of the columns, indicating its limited mobility under reduced conditions. Sequential extraction procedure revealed that retained Se was mainly sequestered as stable/residual forms. Bulk- and micro-X-ray absorption near-edge structure spectroscopy confirmed that Se was mainly retained as reduced/stable species [Se(IV), organic Se, and Se(0)]. This study provides direct evidence for FGD WW Se retention in water-saturated soil via the transformation of oxidized Se into reduced/stable forms. Copyright © by the American Society of Agronomy, Crop Science Society of America, and Soil Science Society of America, Inc.

Virus elimination during the purification of monoclonal antibodies by column chromatography and additional steps.

PubMed

Roberts, Peter L

2014-01-01

The theoretical potential for virus transmission by monoclonal antibody based therapeutic products has led to the inclusion of appropriate virus reduction steps. In this study, virus elimination by the chromatographic steps used during the purification process for two (IgG-1 & -3) monoclonal antibodies (MAbs) have been investigated. Both the Protein G (>7log) and ion-exchange (5 log) chromatography steps were very effective for eliminating both enveloped and non-enveloped viruses over the life-time of the chromatographic gel. However, the contribution made by the final gel filtration step was more limited, i.e., 3 log. Because these chromatographic columns were recycled between uses, the effectiveness of the column sanitization procedures (guanidinium chloride for protein G or NaOH for ion-exchange) were tested. By evaluating standard column runs immediately after each virus spiked run, it was possible to directly confirm that there was no cross contamination with virus between column runs (guanidinium chloride or NaOH). To further ensure the virus safety of the product, two specific virus elimination steps have also been included in the process. A solvent/detergent step based on 1% triton X-100 rapidly inactivating a range of enveloped viruses by >6 log inactivation within 1 min of a 60 min treatment time. Virus removal by virus filtration step was also confirmed to be effective for those viruses of about 50 nm or greater. In conclusion, the combination of these multiple steps ensures a high margin of virus safety for this purification process. © 2014 American Institute of Chemical Engineers.

Simultaneous determination of D-aspartic acid and D-glutamic acid in rat tissues and physiological fluids using a multi-loop two-dimensional HPLC procedure.

PubMed

Han, Hai; Miyoshi, Yurika; Ueno, Kyoko; Okamura, Chieko; Tojo, Yosuke; Mita, Masashi; Lindner, Wolfgang; Zaitsu, Kiyoshi; Hamase, Kenji

2011-11-01

For a metabolomics study focusing on the analysis of aspartic and glutamic acid enantiomers, a fully automated two-dimensional HPLC system employing a microbore-ODS column and a narrowbore-enantioselective column was developed. By using this system, a detailed distribution of D-Asp and D-Glu besides L-Asp and L-Glu in mammals was elucidated. For the total analysis concept, the amino acids were first pre-column derivatized with 4-fluoro-7-nitro-2,1,3-benzoxadiazole (NBD-F) to be sensitively and fluorometrically detected. For the non-stereoselective separation of the analytes in the first dimension a monolithic ODS column (750 mm × 0.53 mm i.d.) was adopted, and a self-packed narrowbore-Pirkle type enantioselective column (Sumichiral OA-2500S, 250 mm × 1.5 mm i.d.) was selected for the second dimension. In the rat plasma, RSD values for intra-day and inter-day precision were less than 6.8%, and the accuracy ranged between 96.1% and 105.8%. The values of LOQ of D-Asp and D-Glu were 5 fmol/injection (0.625 nmol/g tissue). The present method was successfully applied to the simultaneous determination of free aspartic acid and glutamic acid enantiomers in 7 brain areas, 11 peripheral tissues, plasma and urine of Wistar rats. Biologically significant D-Asp values were found in various tissue samples whereas for D-Glu the values were very low possibly indicating less significance. Copyright © 2011 Elsevier B.V. All rights reserved.

Shear wave velocity-based evaluation and design of stone column improved ground for liquefaction mitigation

NASA Astrophysics Data System (ADS)

Zhou, Yanguo; Sun, Zhengbo; Chen, Jie; Chen, Yunmin; Chen, Renpeng

2017-04-01

The evaluation and design of stone column improvement ground for liquefaction mitigation is a challenging issue for the state of practice. In this paper, a shear wave velocity-based approach is proposed based on the well-defined correlations of liquefaction resistance (CRR)-shear wave velocity ( V s)-void ratio ( e) of sandy soils, and the values of parameters in this approach are recommended for preliminary design purpose when site specific values are not available. The detailed procedures of pre- and post-improvement liquefaction evaluations and stone column design are given. According to this approach, the required level of ground improvement will be met once the target V s of soil is raised high enough (i.e., no less than the critical velocity) to resist the given earthquake loading according to the CRR- V s relationship, and then this requirement is transferred to the control of target void ratio (i.e., the critical e) according to the V s- e relationship. As this approach relies on the densification of the surrounding soil instead of the whole improved ground and is conservative by nature, specific considerations of the densification mechanism and effect are given, and the effects of drainage and reinforcement of stone columns are also discussed. A case study of a thermal power plant in Indonesia is introduced, where the effectiveness of stone column improved ground was evaluated by the proposed V s-based method and compared with the SPT-based evaluation. This improved ground performed well and experienced no liquefaction during subsequent strong earthquakes.

Generalized field-splitting algorithms for optimal IMRT delivery efficiency.

PubMed

Kamath, Srijit; Sahni, Sartaj; Li, Jonathan; Ranka, Sanjay; Palta, Jatinder

2007-09-21

Intensity-modulated radiation therapy (IMRT) uses radiation beams of varying intensities to deliver varying doses of radiation to different areas of the tissue. The use of IMRT has allowed the delivery of higher doses of radiation to the tumor and lower doses to the surrounding healthy tissue. It is not uncommon for head and neck tumors, for example, to have large treatment widths that are not deliverable using a single field. In such cases, the intensity matrix generated by the optimizer needs to be split into two or three matrices, each of which may be delivered using a single field. Existing field-splitting algorithms used the pre-specified arbitrary split line or region where the intensity matrix is split along a column, i.e., all rows of the matrix are split along the same column (with or without the overlapping of split fields, i.e., feathering). If three fields result, then the two splits are along the same two columns for all rows. In this paper we study the problem of splitting a large field into two or three subfields with the field width as the only constraint, allowing for an arbitrary overlap of the split fields, so that the total MU efficiency of delivering the split fields is maximized. Proof of optimality is provided for the proposed algorithm. An average decrease of 18.8% is found in the total MUs when compared to the split generated by a commercial treatment planning system and that of 10% is found in the total MUs when compared to the split generated by our previously published algorithm.

Beneficiation of limestone plant rejects for value addition.

PubMed

Jena, M S; Sahu, P; Dash, P; Mohanty, J K

2013-11-15

Investigations were carried out on lime stone rejects (-1mm) generated at a lime stone washing plant in southern India. These rejects contain 12.09% CaO, 2.95% MgO, 10.73% Al2O3, 4.99% Fe2O3, 43.05% SiO2 and 24.92% LOI. Mineralogical studies including SEM-EDAX, XRD, FTIR and TGA were conducted to confirm relative distribution of minerals in the flotation feed and products. These studies revealed that feed sample consists of quartz and calcite as the major minerals with minor amounts of montmorillonite and dolomite whereas flotation concentrate dominantly consists of calcite, and tailings mostly of quartz and montmorillonite. A commercial grade sodium silicate, oleic acid and MIBC were used as depressant, collector and frother respectively in flotation studies. The effects of different operating parameters were evaluated for both conventional and column flotation. Two stage conventional cell flotation results indicate that a cleaner concentrate of 42.50% lime (CaO) content could be obtained at a yield of 15.65%. The lime (CaO) content of the concentrate was further enhanced up to 44.23% at 20.73% yield using single stage column flotation. The column flotation is more efficient in comparison to the conventional cell for treating this sample. A process flowsheet was developed to treat these rejects based on the studies carried out. This process can minimize the waste generation and the concentrate generated during this process can be directly utilized in the Indian cement industries. Copyright © 2013 Elsevier B.V. All rights reserved.

The Two-Column Aerosol Project: Phase I-Overview and impact of elevated aerosol layers on aerosol optical depth

DOE PAGES

Berg, Larry K.; Fast, Jerome D.; Barnard, James C.; ...

2016-01-08

The Two-Column Aerosol Project (TCAP), conducted from June 2012 through June 2013, was a unique study designed to provide a comprehensive data set that can be used to investigate a number of important climate science questions, including those related to aerosol mixing state and aerosol radiative forcing. The study was designed to sample the atmosphere between and within two atmospheric columns; one fixed near the coast of North America (over Cape Cod, MA) and a second moveable column over the Atlantic Ocean several hundred kilometers from the coast. The U.S. Department of Energy's (DOE) Atmospheric Radiation Measurement (ARM) Mobile Facilitymore » (AMF) was deployed at the base of the Cape Cod column, and the ARM Aerial Facility was utilized for the summer and winter intensive observation periods. One important finding from TCAP is that four of six nearly cloud-free flight days had aerosol layers aloft in both the Cape Cod and maritime columns that were detected using the nadir pointing second-generation NASA high-spectral resolution lidar (HSRL-2). In addition, these layers contributed up to 60% of the total observed aerosol optical depth (AOD). Many of these layers were also intercepted by the aircraft configured for in situ sampling, and the aerosol in the layers was found to have increased amounts of biomass burning material and nitrate compared to aerosol found near the surface. Lastly, while there was a great deal of spatial and day-to-day variability in the aerosol chemical composition and optical properties, no systematic differences between the two columns were observed.« less

First Reprocessing of Southern Hemisphere Additional Ozonesondes (SHADOZ) Ozone Profiles (1998-2016): 2. Comparisons With Satellites and Ground-Based Instruments

NASA Astrophysics Data System (ADS)

Thompson, Anne M.; Witte, Jacquelyn C.; Sterling, Chance; Jordan, Allen; Johnson, Bryan J.; Oltmans, Samuel J.; Fujiwara, Masatomo; Vömel, Holger; Allaart, Marc; Piters, Ankie; Coetzee, Gert J. R.; Posny, Françoise; Corrales, Ernesto; Diaz, Jorge Andres; Félix, Christian; Komala, Ninong; Lai, Nga; Ahn Nguyen, H. T.; Maata, Matakite; Mani, Francis; Zainal, Zamuna; Ogino, Shin-ya; Paredes, Francisco; Penha, Tercio Luiz Bezerra; da Silva, Francisco Raimundo; Sallons-Mitro, Sukarni; Selkirk, Henry B.; Schmidlin, F. J.; Stübi, Rene; Thiongo, Kennedy

2017-12-01

The Southern Hemisphere ADditional OZonesonde (SHADOZ) network was assembled to validate a new generation of ozone-monitoring satellites and to better characterize the vertical structure of tropical ozone in the troposphere and stratosphere. Beginning with nine stations in 1998, more than 7,000 ozone and P-T-U profiles are available from 14 SHADOZ sites that have operated continuously for at least a decade. We analyze ozone profiles from the recently reprocessed SHADOZ data set that is based on adjustments for inconsistencies caused by varying ozonesonde instruments and operating techniques. First, sonde-derived total ozone column amounts are compared to the overpasses from the Earth Probe/Total Ozone Mapping Spectrometer, Ozone Monitoring Instrument, and Ozone Mapping and Profiler Suite satellites that cover 1998-2016. Second, characteristics of the stratospheric and tropospheric columns are examined along with ozone structure in the tropical tropopause layer (TTL). We find that (1) relative to our earlier evaluations of SHADOZ data, in 2003, 2007, and 2012, sonde-satellite total ozone column offsets at 12 stations are 2% or less, a significant improvement; (2) as in prior studies, the 10 tropical SHADOZ stations, defined as within ±19° latitude, display statistically uniform stratospheric column ozone, 229 ± 3.9 DU (Dobson units), and a tropospheric zonal wave-one pattern with a 14 DU mean amplitude; (3) the TTL ozone column, which is also zonally uniform, masks complex vertical structure, and this argues against using satellites for lower stratospheric ozone trends; and (4) reprocessing has led to more uniform stratospheric column amounts across sites and reduced bias in stratospheric profiles. As a consequence, the uncertainty in total column ozone now averages 5%.

Normal-Phase Open Column versus Reversed-Phase High Performance Liquid Chromatography: Separation of Chlorophyll a and Chlorophyll b from their Diastereomers.

ERIC Educational Resources Information Center

Schaber, Peter M.

1985-01-01

Background information, procedures used, and typical results obtained are provided for an experiment involving the separation of chlorophyll a and chlorophyll b from their diastereomers. Reasons why the experiment can be easily integrated into most laboratory curricula where high-performance liquid chromatography capabilities exist are given. (JN)

Water Harvesting II: Working toward Being Green

ERIC Educational Resources Information Center

Farenga, Stephen J.; Ness, Daniel; Craven, John A.

2008-01-01

As you have read in the previous "After the Bell" column, water harvesting is a process of diverting and collecting rainwater. One of the main reasons to harvest rainwater is to reduce the demand on local sources of water. The objective of the harvesting procedure is to gather water from a weather event that is usually lost as runoff and either…

Nanocatalysis for Primary and Secondary High Energy Lithium Oxygen Cells

DTIC Science & Technology

2011-04-01

Synthesis of sulfoxyphenyldiazonium Chloride 2.2.3 Assessment of -COOH and –SO3H surface groups on carbon .- Attempts to prepare sulfoxyphenyl...alumina column before used for electrolyte preparation. Synthesis of the electrolyte solvent, methyl n- propyl carbonate (MPC).- The ele- ctrolyte co...2 2.0 EXPERIMENTAL APPROACH AND PROCEDURES ............................ 3 2.1 Synthesis of the Hollow Carbon Sphere

75 FR 18403 - Rules of Procedure; Regulations Implementing the Government in the Sunshine Act; Implementation...

Federal Register 2010, 2011, 2012, 2013, 2014

2010-04-12

... directed that a hyphen be placed between the number ``20'' and the word ``day,'' so that the relevant... 63985, in the center column, in the second paragraph of SUPPLEMENTARY INFORMATION, remove the word ``Second'' and add in its place the word ``First'' in the third sentence. 0 2. On page 63985, in the center...

OPTIMIZED DETERMINATION OF TRACE JET FUEL VOLATILE ORGANIC COMPOUNDS IN HUMAN BLOOD USING IN-FIELD LIQUID-LIQUID EXTRACTION WITH SUBSEQUENT LABORATORY GAS CHROMATOGRAPHIC-MASS SPECTROMETRIC ANALYSIS AND ON-COLUMN LARGE VOLUME INJECTION

EPA Science Inventory

A practical and sensitive method to assess volatile organic compounds (VOCs) from JP-8 jet fuel in human whole blood was developed by modifying previously established liquid-liquid extraction procedures, optimizing extraction times, solvent volume, specific sample processing te...

46 CFR Appendix D to Subpart C of... - Sampling and Analytical Methods for Benzene Monitoring-Measurement Procedures

Code of Federal Regulations, 2013 CFR

2013-10-01

... samples are analyzed directly by high performance liquid chromatography (HPLC). Detection limits: 0.01% by... proper selection of HPLC parameters. 2.4. Samples must be free of any particulates that may clog the... clarification kit. 3. Apparatus 3.1. Liquid chromatograph equipped with a UV detector. 3.2. HPLC Column that...

46 CFR Appendix D to Subpart C of... - Sampling and Analytical Methods for Benzene Monitoring-Measurement Procedures

Code of Federal Regulations, 2012 CFR

2012-10-01

... samples are analyzed directly by high performance liquid chromatography (HPLC). Detection limits: 0.01% by... proper selection of HPLC parameters. 2.4. Samples must be free of any particulates that may clog the... clarification kit. 3. Apparatus 3.1. Liquid chromatograph equipped with a UV detector. 3.2. HPLC Column that...

46 CFR Appendix D to Subpart C of... - Sampling and Analytical Methods for Benzene Monitoring-Measurement Procedures

Code of Federal Regulations, 2014 CFR

2014-10-01

... samples are analyzed directly by high performance liquid chromatography (HPLC). Detection limits: 0.01% by... proper selection of HPLC parameters. 2.4. Samples must be free of any particulates that may clog the... clarification kit. 3. Apparatus 3.1. Liquid chromatograph equipped with a UV detector. 3.2. HPLC Column that...

49 CFR 571.203 - Standard No. 203; Impact protection for the driver from the steering control system.

Code of Federal Regulations, 2011 CFR

2011-10-01

... Practice J944, “Steering Wheel Assembly Laboratory Test Procedure,” December 1965, or an approved.... 208 (49 CFR 571.208) by means of other than seat belt assemblies. It also does not apply to walk-in... trim hardware, including any portion of a steering column assembly that provides energy absorption upon...

49 CFR 571.203 - Standard No. 203; Impact protection for the driver from the steering control system.

Code of Federal Regulations, 2010 CFR

2010-10-01

... Practice J944, “Steering Wheel Assembly Laboratory Test Procedure,” December 1965, or an approved.... 208 (49 CFR 571.208) by means of other than seat belt assemblies. It also does not apply to walk-in... trim hardware, including any portion of a steering column assembly that provides energy absorption upon...

[Hurt eczematiforme column (chronicle) of the breast after implementation of a surgical clip].

PubMed

Motton, S; Gardinal, I; Soulé-Tholy, M; Viraben, R; Hoff, J; Leguevaque, P

2011-04-01

We report a case of atopic dermatitis in relation with a surgical titanium clip. Such a complication has only been reported once in the literature. We advocate to ask the patients about query atopic manifestations especially contact dermatitis to metal before any procedure involving metallic implants. Copyright © 2010 Elsevier Masson SAS. All rights reserved.

A simple and rapid microplate assay for glycoprotein-processing glycosidases

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

Kang, M.S.; Zwolshen, J.H.; Harry, B.S.

1989-08-15

A simple and convenient microplate assay for glycosidases involved in the glycoprotein-processing reactions is described. The assay is based on specific binding of high-mannose-type oligosaccharide substrates to concanavalin A-Sepharose, while monosaccharides liberated by enzymatic hydrolysis do not bind to concanavalin A-Sepharose. By the use of radiolabeled substrates (( 3H)glucose for glucosidases and (3H)mannose for mannosidases), the radioactivity in the liberated monosaccharides can be determined as a measure of the enzymatic activity. This principle was employed earlier for developing assays for glycosidases previously reported. These authors have reported the separation of substrate from the product by concanavalin A-Sepharose column chromatography. Thismore » procedure is handicapped by the fact that it cannot be used for a large number of samples and is time consuming. We have simplified this procedure and adapted it to the use of a microplate (96-well plate). This would help in processing a large number of samples in a short time. In this report we show that the assay is comparable to the column assay previously reported. It is linear with time and enzyme concentration and shows expected kinetics with castanospermine, a known inhibitor of alpha-glucosidase I.« less

Scaled-up production of poacic acid, a plant-derived antifungal agent

DOE PAGES

Yue, Fengxia; Gao, Ruili; Piotrowski, Jeff S.; ...

2017-09-01

Poacic acid, a decarboxylated product from 8–5-diferulic acid that is commonly found in monocot lignocellulosic hydrolysates, has been identified as a natural antifungal agent against economically significant fungi and oomycete plant pathogens. Starting from commercially available or monocot-derivable ferulic acid, a three-step synthetic procedure has been developed for the production of poacic acid needed for field testing in a controlled agricultural setting. First, ferulic acid was esterified to produce ethyl ferulate in 92% yield. Second, peroxidase-catalyzed free radical dehydrodimerization of ethyl ferulate produced crude diferulates, mainly 8–5-diferulate, in 91% yield. Finally, crystalline poacic acid was obtained in 25% yield viamore » alkaline hydrolysis of the crude diferulates after purification by flash-column chromatography. Thus, this new procedure offers two key improvements relevant to large-scale production: 1) bubbling air through the reaction mixture in the second step to remove acetone greatly improves the recovery efficiency of the crude diferulates; and 2) telescoping minor impurities directly into the alkaline hydrolysis step eliminates the need for additional column purifications, thus reducing the overall cost of production and removing a major impediment to process scale-up.« less